# Electronic Supplementary Material (ESI) for Chemical Science. # This journal is © The Royal Society of Chemistry 2020 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_rt235_260k_des _database_code_depnum_ccdc_archive 'CCDC 2018378' loop_ _audit_author_name _audit_author_address 'Carlos Bartual-Murgui' ;Universitat de Valencia Spain ; _audit_update_record ; 2020-07-22 deposited with the CCDC. 2020-09-22 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT342_rt235_260k_des ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.035 Ang. RESPONSE: The crystal may be some twined or/and can be damaged during the dehydration process. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT934_rt235_260k_des ; PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers .. 2 Check RESPONSE: This alerts arises from 3 slighly disagreeable reflections in our refinements which were not omited as we believe that the difference between I(obs) and I(calc) was not two large. ; _vrf_PLAT971_rt235_260k_des ; PROBLEM: Check Calcd Resid. Dens. 1.18A From Pd1 3.20 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO/dehyration processes. ; # Added during the CSD deposition process: Wednesday 22 July 2020 04:49 PM # end Validation Reply Form _audit_creation_date 2019-11-20 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '0.5(C24 H20 Fe2 N20 Pd2)' _chemical_formula_sum 'C12 H10 Fe N10 Pd' _chemical_formula_weight 456.55 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_H-M_alt 'P n m a' _space_group_name_Hall '-P 2ac 2n' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.2723(10) _cell_length_b 7.3843(5) _cell_length_c 15.9189(12) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1677.7(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2332 _cell_measurement_temperature 260.00(10) _cell_measurement_theta_max 22.6110 _cell_measurement_theta_min 3.8140 _shelx_estimated_absorpt_T_max 0.909 _shelx_estimated_absorpt_T_min 0.696 _exptl_absorpt_coefficient_mu 1.953 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.57762 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 896 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0761 _diffrn_reflns_av_unetI/netI 0.0718 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.930 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 11692 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.930 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.989 _diffrn_reflns_theta_min 3.360 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 260.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0267 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.930 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -59.00 43.00 1.00 15.00 -- -15.20 19.00 -30.00 102 2 \w -43.00 -18.00 1.00 15.00 -- -15.20 77.00 150.00 25 3 \w 9.00 51.00 1.00 15.00 -- -15.20 77.00 150.00 42 4 \w -85.00 15.00 1.00 15.00 -- -15.20 -77.00 30.00 100 5 \w -12.00 22.00 1.00 15.00 -- -15.20 -99.00 -90.00 34 6 \w -4.00 31.00 1.00 15.00 -- 15.98 57.00 -60.00 35 7 \w 36.00 90.00 1.00 15.00 -- 15.98-178.00 -90.00 54 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0059061000 _diffrn_orient_matrix_UB_12 -0.0284015000 _diffrn_orient_matrix_UB_13 -0.0731922000 _diffrn_orient_matrix_UB_21 -0.0492615000 _diffrn_orient_matrix_UB_22 0.0014312000 _diffrn_orient_matrix_UB_23 0.0121297000 _diffrn_orient_matrix_UB_31 -0.0027943000 _diffrn_orient_matrix_UB_32 0.0343138000 _diffrn_orient_matrix_UB_33 -0.0609954000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1419 _reflns_number_total 2021 _reflns_odcompleteness_completeness 99.42 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 24.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 3.004 _refine_diff_density_min -1.545 _refine_diff_density_rms 0.288 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.176 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 87 _refine_ls_number_reflns 2021 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1300 _refine_ls_R_factor_gt 0.0902 _refine_ls_restrained_S_all 1.176 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+73.0831P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2291 _refine_ls_wR_factor_ref 0.2483 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C7) = Uanis(C6) = Uanis(C5) = Uanis(N2) = Uanis(C8) = Uanis(N7) = Uanis(N8) Uanis(N1) = Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(N5) = Uanis(C4) = Uanis(N6) 3. Others Fixed Sof: H6A(0.5) H6B(0.5) H8A(0.5) H8B(0.5) 4.a Rotating group: N6(H6A,H6B), N8(H8A,H8B) 4.b Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.54979(9) 1.250000 0.22945(9) 0.0215(4) Uani 1 2 d S T P . . Fe1 Fe 0.79573(17) 0.750000 0.30759(18) 0.0221(6) Uani 1 2 d S T P . . N1 N 0.7670(13) 0.750000 0.4417(11) 0.0423(19) Uani 1 2 d S T P . . N2 N 0.8056(16) 0.750000 0.1679(14) 0.057(2) Uani 1 2 d S T P . . N3 N 0.6907(8) 0.9552(15) 0.2925(7) 0.028(2) Uani 1 1 d . . . . . N4 N 0.4019(8) 1.5481(16) 0.1855(8) 0.035(3) Uani 1 1 d . . . . . N5 N 0.8157(13) 0.750000 0.5839(11) 0.0423(19) Uani 1 2 d S T P . . N6 N 0.5602(12) 0.750000 0.5769(11) 0.0423(19) Uani 1 2 d S T P . . H6A H 0.540438 0.640090 0.581032 0.051 Uiso 0.5 1 d GR . . . . H6B H 0.553466 0.803750 0.624594 0.051 Uiso 0.5 1 d GR . . . . N7 N 0.9021(16) 0.750000 0.0447(14) 0.057(2) Uani 1 2 d S T P . . N8 N 0.6532(16) 0.750000 -0.0160(15) 0.057(2) Uani 1 2 d S T P . . H8A H 0.662646 0.683376 -0.060522 0.068 Uiso 0.5 1 d GR . . . . H8B H 0.604936 0.706605 0.010918 0.068 Uiso 0.5 1 d GR . . . . C1 C 0.6808(16) 0.750000 0.4686(13) 0.0423(19) Uani 1 2 d S T P . . H1 H 0.632909 0.750000 0.429020 0.051 Uiso 1 2 calc RS T P . . C2 C 0.6560(16) 0.750000 0.5538(13) 0.0423(19) Uani 1 2 d S T P . . C3 C 0.7299(15) 0.750000 0.6070(14) 0.0423(19) Uani 1 2 d S T P . . H3 H 0.717489 0.750000 0.664335 0.051 Uiso 1 2 calc RS T P . . C4 C 0.8322(16) 0.750000 0.5045(13) 0.0423(19) Uani 1 2 d S T P . . H4 H 0.894792 0.750000 0.488254 0.051 Uiso 1 2 calc RS T P . . C5 C 0.732(2) 0.750000 0.1137(18) 0.057(2) Uani 1 2 d S T P . . H5 H 0.672696 0.750000 0.138214 0.068 Uiso 1 2 calc RS T P . . C6 C 0.734(2) 0.750000 0.0366(18) 0.057(2) Uani 1 2 d S T P . . C7 C 0.8228(19) 0.750000 -0.0028(18) 0.057(2) Uani 1 2 d S T P . . H7 H 0.827085 0.750000 -0.061047 0.068 Uiso 1 2 calc RS T P . . C8 C 0.888(2) 0.750000 0.1262(17) 0.057(2) Uani 1 2 d S T P . . H8 H 0.941552 0.750000 0.159434 0.068 Uiso 1 2 calc RS T P . . C9 C 0.6383(8) 1.0610(16) 0.2704(8) 0.023(2) Uani 1 1 d . . . . . C10 C 0.4577(9) 1.4410(17) 0.1976(8) 0.025(3) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0213(6) 0.0133(6) 0.0299(8) 0.000 -0.0022(6) 0.000 Fe1 0.0205(12) 0.0154(12) 0.0303(15) 0.000 0.0002(11) 0.000 N1 0.045(4) 0.057(5) 0.025(4) 0.000 -0.001(3) 0.000 N2 0.066(6) 0.051(5) 0.054(6) 0.000 -0.007(5) 0.000 N3 0.036(6) 0.020(5) 0.028(6) -0.002(5) 0.000(5) -0.001(5) N4 0.029(6) 0.024(6) 0.051(8) -0.002(6) -0.006(5) 0.005(5) N5 0.045(4) 0.057(5) 0.025(4) 0.000 -0.001(3) 0.000 N6 0.045(4) 0.057(5) 0.025(4) 0.000 -0.001(3) 0.000 N7 0.066(6) 0.051(5) 0.054(6) 0.000 -0.007(5) 0.000 N8 0.066(6) 0.051(5) 0.054(6) 0.000 -0.007(5) 0.000 C1 0.045(4) 0.057(5) 0.025(4) 0.000 -0.001(3) 0.000 C2 0.045(4) 0.057(5) 0.025(4) 0.000 -0.001(3) 0.000 C3 0.045(4) 0.057(5) 0.025(4) 0.000 -0.001(3) 0.000 C4 0.045(4) 0.057(5) 0.025(4) 0.000 -0.001(3) 0.000 C5 0.066(6) 0.051(5) 0.054(6) 0.000 -0.007(5) 0.000 C6 0.066(6) 0.051(5) 0.054(6) 0.000 -0.007(5) 0.000 C7 0.066(6) 0.051(5) 0.054(6) 0.000 -0.007(5) 0.000 C8 0.066(6) 0.051(5) 0.054(6) 0.000 -0.007(5) 0.000 C9 0.024(6) 0.015(5) 0.030(7) 0.000(6) -0.002(5) 0.002(5) C10 0.030(6) 0.022(6) 0.025(6) -0.003(5) -0.003(6) -0.001(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C9 1.993(12) . ? Pd1 C9 1.993(12) 7_585 ? Pd1 C10 1.993(13) 7_585 ? Pd1 C10 1.993(13) . ? Fe1 N1 2.174(18) . ? Fe1 N2 2.23(2) . ? Fe1 N3 2.145(11) . ? Fe1 N3 2.145(11) 7_575 ? Fe1 N4 2.129(11) 4_575 ? Fe1 N4 2.129(11) 6_646 ? N1 C1 1.30(3) . ? N1 C4 1.37(3) . ? N2 C5 1.36(3) . ? N2 C8 1.35(3) . ? N3 C9 1.136(15) . ? N4 C10 1.139(16) . ? N5 C3 1.28(3) . ? N5 C4 1.29(3) . ? N6 C2 1.42(3) . ? N7 C7 1.36(3) . ? N7 C8 1.31(3) . ? N8 C6 1.42(3) . ? C1 C2 1.40(3) . ? C2 C3 1.35(3) . ? C5 C6 1.23(4) . ? C6 C7 1.42(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 Pd1 C9 88.9(7) . 7_585 ? C9 Pd1 C10 175.5(5) 7_585 7_585 ? C9 Pd1 C10 175.5(5) . . ? C9 Pd1 C10 90.3(5) . 7_585 ? C9 Pd1 C10 90.3(5) 7_585 . ? C10 Pd1 C10 90.1(7) . 7_585 ? N1 Fe1 N2 172.8(8) . . ? N3 Fe1 N1 88.7(5) . . ? N3 Fe1 N1 88.7(5) 7_575 . ? N3 Fe1 N2 86.1(5) . . ? N3 Fe1 N2 86.1(5) 7_575 . ? N3 Fe1 N3 89.9(6) 7_575 . ? N4 Fe1 N1 94.8(5) 6_646 . ? N4 Fe1 N1 94.8(5) 4_575 . ? N4 Fe1 N2 90.4(5) 6_646 . ? N4 Fe1 N2 90.4(5) 4_575 . ? N4 Fe1 N3 90.5(4) 6_646 7_575 ? N4 Fe1 N3 176.5(5) 6_646 . ? N4 Fe1 N3 176.5(5) 4_575 7_575 ? N4 Fe1 N3 90.5(4) 4_575 . ? N4 Fe1 N4 88.9(6) 4_575 6_646 ? C1 N1 Fe1 120.1(15) . . ? C1 N1 C4 113.7(19) . . ? C4 N1 Fe1 126.2(15) . . ? C5 N2 Fe1 125.7(19) . . ? C8 N2 Fe1 123.1(18) . . ? C8 N2 C5 111(2) . . ? C9 N3 Fe1 168.4(11) . . ? C10 N4 Fe1 167.2(12) . 6_566 ? C3 N5 C4 117(2) . . ? C8 N7 C7 115(2) . . ? N1 C1 C2 124(2) . . ? C1 C2 N6 120(2) . . ? C3 C2 N6 126(2) . . ? C3 C2 C1 114(2) . . ? N5 C3 C2 125(2) . . ? N5 C4 N1 126(2) . . ? C6 C5 N2 128(3) . . ? C5 C6 N8 125(3) . . ? C5 C6 C7 117(3) . . ? C7 C6 N8 118(2) . . ? N7 C7 C6 120(3) . . ? N7 C8 N2 128(3) . . ? N3 C9 Pd1 178.2(12) . . ? N4 C10 Pd1 174.6(12) . . ? _shelx_res_file ; TITL rt235_260k_des_a.res in Pnma rt235_260k_des.res created by SHELXL-2018/3 at 14:14:39 on 20-Nov-2019 REM Old TITL RT235_260K_des in Pna2(1) REM SHELXT solution in Pnma: R1 0.202, Rweak 0.033, Alpha 0.053 REM 0.419 for 145 systematic absences, Orientation a'=-a, b'=c, c'=b REM Formula found by SHELXT: C6 C6 O9 I2 CELL 0.71073 14.2723 7.3843 15.9189 90 90 90 ZERR 4 0.001 0.0005 0.0012 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,-Z SYMM 0.5+X,0.5-Y,0.5-Z SFAC C H Fe N Pd UNIT 48 40 4 40 4 EADP C7 C6 C5 N2 C8 N7 N8 EADP N1 C1 C2 C3 N5 C4 N6 L.S. 20 PLAN 20 SIZE 0.05 0.2 0.15 list 4 fmap 2 53 acta REM REM REM WGHT 0.040300 73.083099 FVAR 0.23918 PD1 5 0.549788 1.250000 0.229453 10.50000 0.02129 0.01332 = 0.02989 0.00000 -0.00219 0.00000 FE1 3 0.795734 0.750000 0.307587 10.50000 0.02053 0.01543 = 0.03031 0.00000 0.00017 0.00000 N1 4 0.766965 0.750000 0.441688 10.50000 0.04481 0.05713 = 0.02508 0.00000 -0.00128 0.00000 N2 4 0.805640 0.750000 0.167916 10.50000 0.06626 0.05101 = 0.05393 0.00000 -0.00669 0.00000 N3 4 0.690658 0.955177 0.292501 11.00000 0.03637 0.01984 = 0.02839 -0.00196 0.00042 -0.00131 N4 4 0.401896 1.548059 0.185457 11.00000 0.02898 0.02391 = 0.05070 -0.00168 -0.00560 0.00546 N5 4 0.815708 0.750000 0.583920 10.50000 0.04481 0.05713 = 0.02508 0.00000 -0.00128 0.00000 N6 4 0.560187 0.750000 0.576937 10.50000 0.04481 0.05713 = 0.02508 0.00000 -0.00128 0.00000 AFIX 7 H6A 2 0.540438 0.640090 0.581032 10.50000 -1.20000 H6B 2 0.553466 0.803750 0.624594 10.50000 -1.20000 AFIX 0 N7 4 0.902140 0.750000 0.044703 10.50000 0.06626 0.05101 = 0.05393 0.00000 -0.00669 0.00000 N8 4 0.653227 0.750000 -0.015993 10.50000 0.06626 0.05101 = 0.05393 0.00000 -0.00669 0.00000 AFIX 7 H8A 2 0.662646 0.683376 -0.060522 10.50000 -1.20000 H8B 2 0.604936 0.706605 0.010918 10.50000 -1.20000 AFIX 0 C1 1 0.680797 0.750000 0.468638 10.50000 0.04481 0.05713 = 0.02508 0.00000 -0.00128 0.00000 AFIX 43 H1 2 0.632909 0.750000 0.429020 10.50000 -1.20000 AFIX 0 C2 1 0.656002 0.750000 0.553793 10.50000 0.04481 0.05713 = 0.02508 0.00000 -0.00128 0.00000 C3 1 0.729946 0.750000 0.606991 10.50000 0.04481 0.05713 = 0.02508 0.00000 -0.00128 0.00000 AFIX 43 H3 2 0.717489 0.750000 0.664335 10.50000 -1.20000 AFIX 0 C4 1 0.832216 0.750000 0.504544 10.50000 0.04481 0.05713 = 0.02508 0.00000 -0.00128 0.00000 AFIX 43 H4 2 0.894792 0.750000 0.488254 10.50000 -1.20000 AFIX 0 C5 1 0.731864 0.750000 0.113740 10.50000 0.06626 0.05101 = 0.05393 0.00000 -0.00669 0.00000 AFIX 43 H5 2 0.672696 0.750000 0.138214 10.50000 -1.20000 AFIX 0 C6 1 0.733587 0.750000 0.036632 10.50000 0.06626 0.05101 = 0.05393 0.00000 -0.00669 0.00000 C7 1 0.822820 0.750000 -0.002751 10.50000 0.06626 0.05101 = 0.05393 0.00000 -0.00669 0.00000 AFIX 43 H7 2 0.827085 0.750000 -0.061047 10.50000 -1.20000 AFIX 0 C8 1 0.887973 0.750000 0.126185 10.50000 0.06626 0.05101 = 0.05393 0.00000 -0.00669 0.00000 AFIX 43 H8 2 0.941552 0.750000 0.159434 10.50000 -1.20000 AFIX 0 C9 1 0.638329 1.060970 0.270431 11.00000 0.02365 0.01521 = 0.03003 -0.00001 -0.00205 0.00186 C10 1 0.457694 1.440964 0.197643 11.00000 0.02983 0.02168 = 0.02488 -0.00324 -0.00254 -0.00131 HKLF 4 REM rt235_260k_des_a.res in Pnma REM wR2 = 0.2483, GooF = S = 1.176, Restrained GooF = 1.176 for all data REM R1 = 0.0902 for 1419 Fo > 4sig(Fo) and 0.1300 for all 2021 data REM 87 parameters refined using 0 restraints END WGHT 0.0404 73.0642 REM Highest difference peak 3.004, deepest hole -1.545, 1-sigma level 0.288 Q1 1 0.4631 1.2500 0.2293 10.50000 0.05 3.00 Q2 1 0.7980 0.7500 0.2402 10.50000 0.05 2.60 Q3 1 0.5394 1.2500 0.2967 10.50000 0.05 1.95 Q4 1 0.7371 0.7500 0.2110 10.50000 0.05 1.79 Q5 1 0.7210 0.7500 0.2578 10.50000 0.05 1.74 Q6 1 0.7487 0.7500 0.7474 10.50000 0.05 1.45 Q7 1 0.5390 0.7500 0.7061 10.50000 0.05 1.44 Q8 1 0.9891 0.7500 0.2411 10.50000 0.05 1.38 Q9 1 0.5012 0.7500 0.5646 10.50000 0.05 1.30 Q10 1 0.5048 0.7500 0.0865 10.50000 0.05 1.11 Q11 1 0.5457 0.7500 -0.0824 10.50000 0.05 0.97 Q12 1 0.6748 0.7500 0.0722 10.50000 0.05 0.96 Q13 1 0.3812 1.5584 0.2375 11.00000 0.05 0.96 Q14 1 0.7629 0.7500 0.0200 10.50000 0.05 0.90 Q15 1 0.6232 0.9543 0.2585 11.00000 0.05 0.89 Q16 1 0.8332 0.7500 0.0845 10.50000 0.05 0.88 Q17 1 0.6527 0.7500 0.5108 10.50000 0.05 0.88 Q18 1 0.7431 0.7500 -0.0953 10.50000 0.05 0.87 Q19 1 0.5682 0.6578 0.5768 11.00000 0.05 0.85 Q20 1 0.6289 0.7500 0.5164 10.50000 0.05 0.82 ; _shelx_res_checksum 12266 _olex2_date_sample_data_collection 2019-04-12 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.113 _oxdiff_exptl_absorpt_empirical_full_min 0.648 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_rt235_120k_des _database_code_depnum_ccdc_archive 'CCDC 2018379' loop_ _audit_author_name _audit_author_address 'Carlos Bartual-Murgui' ;Universitat de Valencia Spain ; _audit_update_record ; 2020-07-22 deposited with the CCDC. 2020-09-22 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT430_rt235_120k_des ; PROBLEM: Short Inter D...A Contact N4 ..N4 . 2.75 Ang. RESPONSE: From chemical point of view no H-bond is formed arround these atoms and no H atoms are missed. ; _vrf_PLAT971_rt235_120k_des ; PROBLEM: Check Calcd Resid. Dens. 1.05A From Pd1 3.34 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO/dehydration process. ; _vrf_PLAT971_rt235_120k_des_2 ; PROBLEM: Check Calcd Resid. Dens. 1.12A From Fe1 2.55 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO/dehyration processes. ; # Added during the CSD deposition process: Wednesday 22 July 2020 04:49 PM # end Validation Reply Form _audit_creation_date 2019-11-20 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '0.5(C24 H20 Fe2 N20 Pd2)' _chemical_formula_sum 'C12 H10 Fe N10 Pd' _chemical_formula_weight 456.55 _chemical_melting_point ? _chemical_oxdiff_formula 'C11 H10 N O' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_H-M_alt 'P n m a' _space_group_name_Hall '-P 2ac 2n' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.1549(7) _cell_length_b 7.1808(4) _cell_length_c 15.6363(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1589.33(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2760 _cell_measurement_temperature 119.90(14) _cell_measurement_theta_max 26.6650 _cell_measurement_theta_min 3.4180 _shelx_estimated_absorpt_T_max 0.904 _shelx_estimated_absorpt_T_min 0.683 _exptl_absorpt_coefficient_mu 2.061 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.34893 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 896 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0955 _diffrn_reflns_av_unetI/netI 0.0707 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.939 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 16225 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.939 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.076 _diffrn_reflns_theta_min 3.438 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 119.90(14) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0267 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.939 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -49.00 47.00 1.00 20.00 -- -20.26 77.00 150.00 96 2 \w 18.00 49.00 1.00 20.00 -- -20.26 77.00-180.00 31 3 \w -25.00 4.00 1.00 20.00 -- -20.26 77.00-180.00 29 4 \w -7.00 88.00 1.00 20.00 -- 21.04 77.00 60.00 95 5 \w 34.00 62.00 1.00 20.00 -- 21.04 77.00 0.00 28 6 \w 2.00 30.00 1.00 20.00 -- 21.04 77.00 120.00 28 7 \w -9.00 91.00 1.00 20.00 -- 21.04 77.00 -90.00 100 8 \w -8.00 67.00 1.00 20.00 -- 21.04 77.00 -30.00 75 9 \w 49.00 86.00 1.00 20.00 -- 21.04 77.00 120.00 37 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0046492000 _diffrn_orient_matrix_UB_12 0.0742257000 _diffrn_orient_matrix_UB_13 -0.0296619000 _diffrn_orient_matrix_UB_21 -0.0498406000 _diffrn_orient_matrix_UB_22 -0.0097905000 _diffrn_orient_matrix_UB_23 0.0012071000 _diffrn_orient_matrix_UB_31 -0.0022200000 _diffrn_orient_matrix_UB_32 0.0645186000 _diffrn_orient_matrix_UB_33 0.0342703000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1759 _reflns_number_total 2347 _reflns_odcompleteness_completeness 99.53 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 27.42 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 3.487 _refine_diff_density_min -2.501 _refine_diff_density_rms 0.254 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 135 _refine_ls_number_reflns 2347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0959 _refine_ls_R_factor_gt 0.0644 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+18.8066P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1465 _refine_ls_wR_factor_ref 0.1613 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H,H) groups 2. Others Fixed Sof: H8A(0.5) H8B(0.5) H6A(0.5) H6B(0.5) 3.a Rotating group: N8(H8A,H8B), N6(H6A,H6B) 3.b Aromatic/amide H refined with riding coordinates: C5(H5), C7(H7), C8(H8), C1(H1), C3(H3), C4(H4) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.53512(5) 0.250000 0.76409(4) 0.0138(2) Uani 1 2 d S T P . . Fe1 Fe 0.78370(9) 0.750000 0.72449(8) 0.0137(3) Uani 1 2 d S T P . . N2 N 0.7948(6) 0.750000 0.8520(5) 0.0186(16) Uani 1 2 d S T P . . N1 N 0.7704(5) 0.750000 0.5966(5) 0.0158(16) Uani 1 2 d S T P . . N3 N 0.6880(4) 0.5584(7) 0.7339(3) 0.0153(11) Uani 1 1 d . . . . . N4 N 0.3797(4) -0.0584(8) 0.7812(3) 0.0159(11) Uani 1 1 d . . . . . N7 N 0.8939(8) 0.750000 0.9755(6) 0.036(2) Uani 1 2 d S T P . . N8 N 0.6469(10) 0.750000 1.0425(8) 0.052(3) Uani 1 2 d S T P . . H8A H 0.602666 0.682876 1.019979 0.063 Uiso 0.5 1 d GR . . . . H8B H 0.661226 0.704474 1.092088 0.063 Uiso 0.5 1 d GR . . . . N5 N 0.8397(6) 0.750000 0.4585(6) 0.030(2) Uani 1 2 d S T P . . N6 N 0.5832(7) 0.750000 0.4348(6) 0.034(2) Uani 1 2 d S T P . . H6A H 0.582843 0.679179 0.389770 0.041 Uiso 0.5 1 d GR . . . . H6B H 0.541133 0.708691 0.470560 0.041 Uiso 0.5 1 d GR . . . . C5 C 0.7176(8) 0.750000 0.9033(7) 0.024(2) Uani 1 2 d S T P . . H5 H 0.658046 0.750000 0.878217 0.029 Uiso 1 2 calc RS T P . . C6 C 0.7242(9) 0.750000 0.9905(7) 0.031(3) Uani 1 2 d S T P . . C7 C 0.8158(10) 0.750000 1.0231(7) 0.036(3) Uani 1 2 d S T P . . H7 H 0.822970 0.750000 1.082258 0.043 Uiso 1 2 calc RS T P . . C8 C 0.8803(8) 0.750000 0.8906(6) 0.025(2) Uani 1 2 d S T P . . H8 H 0.933505 0.750000 0.855740 0.030 Uiso 1 2 calc RS T P . . C1 C 0.6848(7) 0.750000 0.5604(6) 0.0185(19) Uani 1 2 d S T P . . H1 H 0.631529 0.750000 0.595231 0.022 Uiso 1 2 calc RS T P . . C2 C 0.6731(7) 0.750000 0.4725(6) 0.023(2) Uani 1 2 d S T P . . C3 C 0.7547(8) 0.750000 0.4238(7) 0.026(2) Uani 1 2 d S T P . . H3 H 0.749419 0.750000 0.364540 0.032 Uiso 1 2 calc RS T P . . C4 C 0.8429(7) 0.750000 0.5441(6) 0.023(2) Uani 1 2 d S T P . . H4 H 0.902649 0.750000 0.568875 0.028 Uiso 1 2 calc RS T P . . C9 C 0.6317(4) 0.4449(9) 0.7436(4) 0.0156(13) Uani 1 1 d . . . . . C10 C 0.4377(4) 0.0539(9) 0.7774(4) 0.0148(12) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0119(3) 0.0106(3) 0.0190(3) 0.000 0.0011(3) 0.000 Fe1 0.0100(6) 0.0089(6) 0.0221(7) 0.000 -0.0007(5) 0.000 N2 0.022(4) 0.012(4) 0.022(4) 0.000 0.001(3) 0.000 N1 0.016(4) 0.012(4) 0.020(4) 0.000 0.001(3) 0.000 N3 0.013(2) 0.011(3) 0.021(3) 0.000(2) 0.000(2) 0.003(2) N4 0.013(2) 0.015(3) 0.020(3) -0.002(2) 0.0012(19) 0.004(2) N7 0.062(7) 0.027(5) 0.021(5) 0.000 -0.016(5) 0.000 N8 0.074(9) 0.045(7) 0.038(6) 0.000 0.024(6) 0.000 N5 0.025(5) 0.032(5) 0.031(5) 0.000 0.006(4) 0.000 N6 0.030(5) 0.053(7) 0.019(4) 0.000 0.003(4) 0.000 C5 0.028(5) 0.018(5) 0.027(5) 0.000 -0.003(4) 0.000 C6 0.053(7) 0.016(5) 0.023(5) 0.000 0.008(5) 0.000 C7 0.073(9) 0.025(6) 0.011(5) 0.000 -0.015(5) 0.000 C8 0.035(6) 0.019(5) 0.021(5) 0.000 -0.010(4) 0.000 C1 0.020(5) 0.012(4) 0.023(5) 0.000 0.001(4) 0.000 C2 0.026(5) 0.024(5) 0.020(5) 0.000 -0.003(4) 0.000 C3 0.035(6) 0.022(5) 0.022(5) 0.000 0.009(4) 0.000 C4 0.023(5) 0.022(5) 0.025(5) 0.000 0.003(4) 0.000 C9 0.014(3) 0.012(3) 0.021(3) -0.001(2) 0.002(2) 0.003(2) C10 0.011(3) 0.009(3) 0.025(3) -0.001(2) 0.001(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C9 1.982(6) . ? Pd1 C9 1.982(6) 7_565 ? Pd1 C10 1.982(6) . ? Pd1 C10 1.982(6) 7_565 ? Fe1 N2 2.000(8) . ? Fe1 N1 2.008(8) . ? Fe1 N3 1.936(5) 7_575 ? Fe1 N3 1.936(5) . ? Fe1 N4 1.936(6) 6_667 ? Fe1 N4 1.936(5) 4_556 ? N2 C5 1.355(13) . ? N2 C8 1.352(13) . ? N1 C1 1.339(12) . ? N1 C4 1.315(12) . ? N3 C9 1.151(8) . ? N4 C10 1.152(8) . ? N7 C7 1.333(17) . ? N7 C8 1.341(13) . ? N8 C6 1.362(15) . ? N5 C3 1.320(14) . ? N5 C4 1.338(13) . ? N6 C2 1.402(14) . ? C5 C6 1.368(15) . ? C6 C7 1.393(18) . ? C1 C2 1.384(13) . ? C2 C3 1.382(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 Pd1 C9 89.8(4) . 7_565 ? C9 Pd1 C10 176.7(3) . . ? C9 Pd1 C10 89.7(2) . 7_565 ? C9 Pd1 C10 89.7(2) 7_565 . ? C9 Pd1 C10 176.7(3) 7_565 7_565 ? C10 Pd1 C10 90.6(3) 7_565 . ? N2 Fe1 N1 179.1(3) . . ? N3 Fe1 N2 88.8(2) . . ? N3 Fe1 N2 88.8(2) 7_575 . ? N3 Fe1 N1 90.6(2) 7_575 . ? N3 Fe1 N1 90.6(2) . . ? N3 Fe1 N3 90.6(3) . 7_575 ? N3 Fe1 N4 178.2(2) . 6_667 ? N3 Fe1 N4 178.2(2) 7_575 4_556 ? N3 Fe1 N4 89.4(2) 7_575 6_667 ? N3 Fe1 N4 89.4(2) . 4_556 ? N4 Fe1 N2 89.4(2) 6_667 . ? N4 Fe1 N2 89.4(2) 4_556 . ? N4 Fe1 N1 91.2(2) 4_556 . ? N4 Fe1 N1 91.2(2) 6_667 . ? N4 Fe1 N4 90.6(3) 6_667 4_556 ? C5 N2 Fe1 121.8(7) . . ? C8 N2 Fe1 121.0(7) . . ? C8 N2 C5 117.2(9) . . ? C1 N1 Fe1 120.4(6) . . ? C4 N1 Fe1 123.3(7) . . ? C4 N1 C1 116.3(8) . . ? C9 N3 Fe1 176.8(5) . . ? C10 N4 Fe1 174.4(5) . 6_547 ? C7 N7 C8 115.7(10) . . ? C3 N5 C4 116.3(9) . . ? N2 C5 C6 122.4(10) . . ? N8 C6 C5 122.7(12) . . ? N8 C6 C7 122.0(11) . . ? C5 C6 C7 115.4(11) . . ? N7 C7 C6 124.6(9) . . ? N7 C8 N2 124.8(11) . . ? N1 C1 C2 121.9(9) . . ? C1 C2 N6 121.7(9) . . ? C3 C2 N6 121.7(9) . . ? C3 C2 C1 116.6(10) . . ? N5 C3 C2 122.3(10) . . ? N1 C4 N5 126.7(10) . . ? N3 C9 Pd1 178.3(6) . . ? N4 C10 Pd1 176.7(6) . . ? _shelx_res_file ; TITL rt235_120k_des_a.res in Pnma rt235_120k_des.res created by SHELXL-2018/3 at 14:13:10 on 20-Nov-2019 REM Old TITL RT235_120K_des in Pnma #62 REM SHELXT solution in Pnma: R1 0.162, Rweak 0.030, Alpha 0.046 REM 0.444 for 139 systematic absences, Orientation as input REM Formula found by SHELXT: C11 N5 O5 Fe2 CELL 0.71073 14.1549 7.1808 15.6363 90 90 90 ZERR 4 0.0007 0.0004 0.0008 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,-Z SYMM 0.5+X,0.5-Y,0.5-Z SFAC C H Fe N Pd UNIT 48 40 4 40 4 L.S. 15 PLAN 20 0 0 SIZE 0.05 0.2 0.15 BOND list 4 fmap 2 acta REM REM REM WGHT 0.045700 18.806601 FVAR 0.22691 PD1 5 0.535119 0.250000 0.764093 10.50000 0.01189 0.01057 = 0.01901 0.00000 0.00114 0.00000 FE1 3 0.783700 0.750000 0.724489 10.50000 0.01004 0.00889 = 0.02210 0.00000 -0.00066 0.00000 N2 4 0.794806 0.750000 0.851973 10.50000 0.02166 0.01186 = 0.02229 0.00000 0.00112 0.00000 N1 4 0.770431 0.750000 0.596617 10.50000 0.01553 0.01240 = 0.01958 0.00000 0.00145 0.00000 N3 4 0.688045 0.558441 0.733921 11.00000 0.01343 0.01126 = 0.02122 0.00025 -0.00026 0.00304 N4 4 0.379690 -0.058394 0.781152 11.00000 0.01261 0.01547 = 0.01951 -0.00182 0.00116 0.00366 N7 4 0.893907 0.750000 0.975487 10.50000 0.06152 0.02651 = 0.02144 0.00000 -0.01586 0.00000 N8 4 0.646935 0.750000 1.042488 10.50000 0.07400 0.04514 = 0.03815 0.00000 0.02363 0.00000 AFIX 7 H8A 2 0.602666 0.682876 1.019979 10.50000 -1.20000 H8B 2 0.661226 0.704474 1.092088 10.50000 -1.20000 AFIX 0 N5 4 0.839667 0.750000 0.458528 10.50000 0.02506 0.03200 = 0.03147 0.00000 0.00564 0.00000 N6 4 0.583233 0.750000 0.434830 10.50000 0.02999 0.05282 = 0.01918 0.00000 0.00323 0.00000 AFIX 7 H6A 2 0.582843 0.679179 0.389770 10.50000 -1.20000 H6B 2 0.541133 0.708691 0.470560 10.50000 -1.20000 AFIX 0 C5 1 0.717638 0.750000 0.903263 10.50000 0.02813 0.01795 = 0.02721 0.00000 -0.00274 0.00000 AFIX 43 H5 2 0.658046 0.750000 0.878217 10.50000 -1.20000 AFIX 0 C6 1 0.724220 0.750000 0.990549 10.50000 0.05287 0.01638 = 0.02332 0.00000 0.00772 0.00000 C7 1 0.815806 0.750000 1.023136 10.50000 0.07257 0.02480 = 0.01053 0.00000 -0.01542 0.00000 AFIX 43 H7 2 0.822970 0.750000 1.082258 10.50000 -1.20000 AFIX 0 C8 1 0.880266 0.750000 0.890594 10.50000 0.03515 0.01863 = 0.02108 0.00000 -0.01035 0.00000 AFIX 43 H8 2 0.933505 0.750000 0.855740 10.50000 -1.20000 AFIX 0 C1 1 0.684757 0.750000 0.560364 10.50000 0.02045 0.01243 = 0.02253 0.00000 0.00081 0.00000 AFIX 43 H1 2 0.631529 0.750000 0.595231 10.50000 -1.20000 AFIX 0 C2 1 0.673129 0.750000 0.472506 10.50000 0.02565 0.02430 = 0.01957 0.00000 -0.00254 0.00000 C3 1 0.754653 0.750000 0.423828 10.50000 0.03523 0.02160 = 0.02228 0.00000 0.00861 0.00000 AFIX 43 H3 2 0.749419 0.750000 0.364540 10.50000 -1.20000 AFIX 0 C4 1 0.842942 0.750000 0.544055 10.50000 0.02286 0.02213 = 0.02470 0.00000 0.00299 0.00000 AFIX 43 H4 2 0.902649 0.750000 0.568875 10.50000 -1.20000 AFIX 0 C9 1 0.631656 0.444874 0.743626 11.00000 0.01437 0.01173 = 0.02074 -0.00052 0.00219 0.00329 C10 1 0.437713 0.053861 0.777393 11.00000 0.01123 0.00860 = 0.02472 -0.00130 0.00120 0.00270 HKLF 4 REM rt235_120k_des_a.res in Pnma REM wR2 = 0.1613, GooF = S = 1.117, Restrained GooF = 1.117 for all data REM R1 = 0.0644 for 1759 Fo > 4sig(Fo) and 0.0959 for all 2347 data REM 135 parameters refined using 0 restraints END WGHT 0.0457 18.8062 REM Highest difference peak 3.487, deepest hole -2.501, 1-sigma level 0.254 Q1 1 0.4620 0.2500 0.7612 10.50000 0.05 3.49 Q2 1 0.7202 0.7500 0.7620 10.50000 0.05 2.76 Q3 1 0.5375 0.2500 0.7021 10.50000 0.05 2.29 Q4 1 0.7812 0.7500 0.7817 10.50000 0.05 1.50 Q5 1 0.5676 0.7500 0.7485 10.50000 0.05 1.40 Q6 1 0.6798 0.2500 0.7302 10.50000 0.05 1.35 Q7 1 0.9211 0.7500 0.7696 10.50000 0.05 1.26 Q8 1 0.6936 0.7500 0.2717 10.50000 0.05 0.93 Q9 1 0.4199 -0.2500 0.7884 10.50000 0.05 0.88 Q10 1 0.7403 0.7500 0.6486 10.50000 0.05 0.87 Q11 1 0.5325 0.7500 0.5384 10.50000 0.05 0.86 Q12 1 0.4980 0.7500 0.3706 10.50000 0.05 0.85 Q13 1 0.6675 0.7500 0.2789 10.50000 0.05 0.82 Q14 1 0.3328 0.2500 0.7659 10.50000 0.05 0.75 Q15 1 0.7474 0.7500 0.8794 10.50000 0.05 0.75 Q16 1 0.3228 -0.0351 0.7511 11.00000 0.05 0.74 Q17 1 0.8427 0.7500 0.6794 10.50000 0.05 0.73 Q18 1 0.5488 0.4281 0.7637 11.00000 0.05 0.71 Q19 1 0.5953 0.7500 0.6308 10.50000 0.05 0.71 Q20 1 0.9797 0.7500 0.9441 10.50000 0.05 0.70 ; _shelx_res_checksum 56308 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.388 _oxdiff_exptl_absorpt_empirical_full_min 0.449 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mo_rt327_5apmdpth2o_120k_0ma _database_code_depnum_ccdc_archive 'CCDC 2018385' loop_ _audit_author_name _audit_author_address 'Carlos Bartual-Murgui' ;Universitat de Valencia Spain ; _audit_update_record ; 2020-09-17 deposited with the CCDC. 2020-09-22 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT971_mo_rt327_5apmdpth2o_120k_0ma ; PROBLEM: Check Calcd Resid. Dens. 1.02A From Pt1 9.82 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_mo_rt327_5apmdpth2o_120k_0ma_2 ; PROBLEM: Check Calcd Resid. Dens. 0.88A From Pt1 8.40 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_mo_rt327_5apmdpth2o_120k_0ma_3 ; PROBLEM: Check Calcd Resid. Dens. 0.86A From Pt1 7.03 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_mo_rt327_5apmdpth2o_120k_0ma ; PROBLEM: Check Calcd Resid. Dens. 0.71A From Pt1 -6.19 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_mo_rt327_5apmdpth2o_120k_0ma_2 ; PROBLEM: Check Calcd Resid. Dens. 0.70A From Pt1 -6.00 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_mo_rt327_5apmdpth2o_120k_0ma_3 ; PROBLEM: Check Calcd Resid. Dens. 0.70A From Pt1 -5.05 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_mo_rt327_5apmdpth2o_120k_0ma_4 ; PROBLEM: Check Calcd Resid. Dens. 0.72A From Pt1 -3.62 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT973_mo_rt327_5apmdpth2o_120k_0ma ; PROBLEM: Check Calcd Positive Resid. Density on Pt1 6.37 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT097_mo_rt327_5apmdpth2o_120k_0ma ; PROBLEM: Large Reported Max. (Positive) Residual Density 9.90 eA-3 RESPONSE: The crystal may be damaged during the SCO processes. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT342_mo_rt327_5apmdpth2o_120k_0ma ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0425 Ang. RESPONSE: The crystal may be damaged during the dehydration process. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT971_mo_rt327_5apmdpth2o_120k_0ma_4 ; PROBLEM: Check Calcd Resid. Dens. 1.25A From Pt1 2.93 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_mo_rt327_5apmdpth2o_120k_0ma_5 ; PROBLEM: Check Calcd Resid. Dens. 1.24A From Pt1 2.57 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; # Added during the CSD deposition process: Thursday 17 September 2020 12:29 PM # end Validation Reply Form _audit_creation_date 2020-09-09 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C12 H10 Fe N10 Pt, 0.8(H2 O)' _chemical_formula_sum 'C12 H11.60 Fe N10 O0.80 Pt' _chemical_formula_weight 559.65 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_H-M_alt 'C 1 2/m 1' _space_group_name_Hall '-C 2y' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 21.078(3) _cell_length_b 7.0587(9) _cell_length_c 14.488(3) _cell_angle_alpha 90 _cell_angle_beta 131.352(3) _cell_angle_gamma 90 _cell_volume 1618.1(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5588 _cell_measurement_temperature 119.83 _cell_measurement_theta_max 30.36 _cell_measurement_theta_min 2.57 _shelx_estimated_absorpt_T_max 0.448 _shelx_estimated_absorpt_T_min 0.278 _exptl_absorpt_coefficient_mu 9.556 _exptl_absorpt_correction_T_max 0.7468 _exptl_absorpt_correction_T_min 0.4117 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1465 before and 0.0947 after correction. The Ratio of minimum to maximum transmission is 0.5513. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 2.297 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1056 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.1 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1094 _diffrn_reflns_av_unetI/netI 0.0886 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.840 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 17861 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.840 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 34.343 _diffrn_reflns_theta_min 2.575 _diffrn_ambient_temperature 119.83 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.840 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2106 _reflns_number_total 3046 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 9.896 _refine_diff_density_min -7.238 _refine_diff_density_rms 0.529 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 160 _refine_ls_number_reflns 3046 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1431 _refine_ls_R_factor_gt 0.0814 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1197P)^2^+97.5723P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1954 _refine_ls_wR_factor_ref 0.2482 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All N(H,H) groups, All O(H,H) groups 2. Restrained distances N8-H8b 0.9 with sigma of 0.0001 H3b-N3 0.9 with sigma of 0.0001 H3a-N3 0.9 with sigma of 0.0001 H8a-N8 0.9 with sigma of 0.0001 H8b-O1 2.2 with sigma of 0.0001 H3a-H3b 1.7 with sigma of 0.0001 H8a-H8b 1.5 with sigma of 0.0001 H3b_$1-N7_$2 2.2 with sigma of 0.0001 O1-H1b 0.9 with sigma of 0.0001 N2_$3-H1a 2.2 with sigma of 0.0001 H1a-H1b 1.45 with sigma of 0.0001 O1-H1a 0.9 with sigma of 0.0001 3. Others Fixed Sof: O1(0.4) H1a(0.4) H1b(0.4) H8a(0.5) H3a(0.5) 4.a Aromatic/amide H refined with riding coordinates: C7(H7), C9(H9), C10(H10), C1(H1), C3(H3), C4(H4) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.48413(4) 0.500000 0.23587(6) 0.0242(2) Uani 1 2 d S T P . . Fe2 Fe 0.500000 1.000000 0.500000 0.0219(7) Uani 1 4 d S T P . . Fe1 Fe 0.500000 0.000000 0.000000 0.0222(7) Uani 1 4 d S T P . . O1 O 0.23857(13) 1.1632(3) 0.01456(16) 0.057(9) Uani 0.4 1 d D . P A -1 H1A H 0.23814(15) 1.1912(5) -0.04646(14) 0.085 Uiso 0.4 1 d D U P B -1 H1B H 0.2547(3) 1.2685(4) 0.0604(2) 0.085 Uiso 0.4 1 d D U P C -1 N6 N 0.3787(11) 1.000000 0.4188(13) 0.030(3) Uani 1 2 d S T P . . N7 N 0.27329(17) 1.000000 0.4390(2) 0.046(5) Uani 1 2 d S T P . . N8 N 0.16888(15) 1.000000 0.12021(17) 0.054(5) Uani 1 2 d DS T P . . H8A H 0.14231(15) 1.1053(3) 0.1143(2) 0.081 Uiso 0.5 1 d D U P . . H8B H 0.17834(11) 1.000000 0.06804(15) 0.081 Uiso 1 2 d DS U P . . N5 N 0.4826(7) 0.8063(14) 0.3902(9) 0.0238(19) Uani 1 1 d . . . . . N4 N 0.4958(7) 0.1934(14) 0.0912(9) 0.0222(18) Uani 1 1 d . . . . . N1 N 0.6237(12) 0.000000 0.1209(17) 0.033(4) Uani 1 2 d S T P . . N2 N 0.7550(3) 0.000000 0.1596(3) 0.052(6) Uani 1 2 d S T P . . N3 N 0.80480(11) 0.000000 0.4501(3) 0.052(6) Uani 1 2 d DS T P . . H3A H 0.85920(12) 0.0366(11) 0.4988(4) 0.078 Uiso 0.5 1 d D U P . . H3B H 0.76027(10) 0.000000 0.44589(19) 0.078 Uiso 1 2 d DS U P . . C7 C 0.3170(14) 1.000000 0.298(2) 0.036(4) Uani 1 2 d S T P . . H7 H 0.330275 1.000000 0.246935 0.043 Uiso 1 2 calc R U P . . C8 C 0.2316(12) 1.000000 0.2441(19) 0.032(4) Uani 1 2 d S T P . . C9 C 0.2148(13) 1.000000 0.322(2) 0.036(4) Uani 1 2 d S T P . . H9 H 0.157574 1.000000 0.286444 0.043 Uiso 1 2 calc R U P . . C10 C 0.3520(14) 1.000000 0.482(2) 0.037(4) Uani 1 2 d S T P . . H10 H 0.395452 1.000000 0.568932 0.045 Uiso 1 2 calc R U P . . C6 C 0.4800(8) 0.6970(15) 0.3297(11) 0.022(2) Uani 1 1 d . . . . . C5 C 0.4916(7) 0.3022(16) 0.1459(10) 0.021(2) Uani 1 1 d . . . . . C1 C 0.6707(14) 0.000000 0.2437(17) 0.033(4) Uani 1 2 d S T P . . H1 H 0.642376 0.000000 0.274312 0.040 Uiso 1 2 calc R U P . . C2 C 0.7611(12) 0.000000 0.3303(19) 0.032(4) Uani 1 2 d S T P . . C3 C 0.7994(15) 0.000000 0.279(2) 0.037(4) Uani 1 2 d S T P . . H3 H 0.859352 0.000000 0.333204 0.044 Uiso 1 2 calc R U P . . C4 C 0.6705(15) 0.000000 0.086(2) 0.043(5) Uani 1 2 d S T P . . H4 H 0.639591 0.000000 -0.000272 0.051 Uiso 1 2 calc R U P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0313(4) 0.0165(3) 0.0267(4) 0.000 0.0200(3) 0.000 Fe2 0.0404(19) 0.0099(13) 0.0246(15) 0.000 0.0255(15) 0.000 Fe1 0.0400(19) 0.0101(13) 0.0256(16) 0.000 0.0256(15) 0.000 O1 0.055(18) 0.08(2) 0.056(17) -0.029(17) 0.045(16) -0.024(18) N6 0.045(9) 0.009(5) 0.017(6) 0.000 0.012(6) 0.000 N7 0.040(10) 0.062(13) 0.049(11) 0.000 0.034(10) 0.000 N8 0.049(12) 0.065(15) 0.044(11) 0.000 0.028(10) 0.000 N5 0.040(6) 0.015(4) 0.022(4) 0.000(3) 0.023(4) -0.001(4) N4 0.033(5) 0.015(4) 0.028(5) -0.001(4) 0.024(4) 0.001(4) N1 0.053(10) 0.017(7) 0.049(10) 0.000 0.043(9) 0.000 N2 0.026(9) 0.085(17) 0.044(11) 0.000 0.023(8) 0.000 N3 0.029(9) 0.089(18) 0.036(9) 0.000 0.021(8) 0.000 C7 0.034(10) 0.032(10) 0.038(10) 0.000 0.022(9) 0.000 C8 0.024(8) 0.027(9) 0.037(10) 0.000 0.016(8) 0.000 C9 0.027(9) 0.027(9) 0.044(11) 0.000 0.019(9) 0.000 C10 0.037(10) 0.046(12) 0.035(10) 0.000 0.026(9) 0.000 C6 0.032(6) 0.010(4) 0.026(5) -0.001(4) 0.021(5) -0.004(4) C5 0.027(5) 0.015(4) 0.025(5) 0.005(4) 0.018(5) 0.000(4) C1 0.041(11) 0.031(9) 0.023(8) 0.000 0.020(8) 0.000 C2 0.026(9) 0.033(9) 0.033(9) 0.000 0.017(8) 0.000 C3 0.049(12) 0.028(9) 0.035(10) 0.000 0.028(10) 0.000 C4 0.037(11) 0.049(13) 0.053(13) 0.000 0.035(11) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C6 1.986(11) 6_565 ? Pt1 C6 1.986(11) . ? Pt1 C5 1.986(12) 6_565 ? Pt1 C5 1.986(12) . ? Fe2 N6 1.986(19) . ? Fe2 N6 1.986(19) 5_676 ? Fe2 N5 1.939(10) 6_575 ? Fe2 N5 1.939(10) 2_656 ? Fe2 N5 1.939(10) 5_676 ? Fe2 N5 1.939(10) . ? Fe1 N4 1.942(9) 5_655 ? Fe1 N4 1.942(9) 2_655 ? Fe1 N4 1.942(9) 6 ? Fe1 N4 1.942(9) . ? Fe1 N1 1.96(2) . ? Fe1 N1 1.96(2) 5_655 ? O1 H1A 0.9000(2) . ? O1 H1B 0.90000(14) . ? N6 C7 1.32(3) . ? N6 C10 1.35(3) . ? N7 C9 1.28(2) . ? N7 C10 1.33(2) . ? N8 H8A 0.90000(14) . ? N8 H8A 0.90001(13) 6_575 ? N8 H8B 0.9000(2) . ? N8 C8 1.35(2) . ? N5 C6 1.143(15) . ? N4 C5 1.148(16) . ? N1 C1 1.35(3) . ? N1 C4 1.38(3) . ? N2 C3 1.32(2) . ? N2 C4 1.34(2) . ? N3 H3A 0.90000(17) . ? N3 H3A 0.90000(18) 6 ? N3 H3B 0.90000(16) . ? N3 C2 1.32(2) . ? C7 H7 0.9500 . ? C7 C8 1.41(3) . ? C8 C9 1.38(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C1 H1 0.9500 . ? C1 C2 1.43(3) . ? C2 C3 1.41(3) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Pt1 C6 88.9(6) 6_565 . ? C6 Pt1 C5 90.9(5) 6_565 . ? C6 Pt1 C5 178.4(5) . . ? C6 Pt1 C5 178.4(5) 6_565 6_565 ? C6 Pt1 C5 90.9(5) . 6_565 ? C5 Pt1 C5 89.3(6) . 6_565 ? N6 Fe2 N6 180.0(9) . 5_676 ? N5 Fe2 N6 87.6(5) 2_656 . ? N5 Fe2 N6 92.4(5) 5_676 5_676 ? N5 Fe2 N6 87.6(5) 5_676 . ? N5 Fe2 N6 92.4(5) 2_656 5_676 ? N5 Fe2 N6 92.4(5) 6_575 . ? N5 Fe2 N6 92.4(5) . . ? N5 Fe2 N6 87.6(5) . 5_676 ? N5 Fe2 N6 87.6(5) 6_575 5_676 ? N5 Fe2 N5 180.0 6_575 2_656 ? N5 Fe2 N5 89.7(6) 6_575 . ? N5 Fe2 N5 180.0 5_676 . ? N5 Fe2 N5 89.7(6) 5_676 2_656 ? N5 Fe2 N5 90.3(6) 2_656 . ? N5 Fe2 N5 90.3(6) 5_676 6_575 ? N4 Fe1 N4 90.7(6) 5_655 6 ? N4 Fe1 N4 180.0 5_655 . ? N4 Fe1 N4 180.0(6) 6 2_655 ? N4 Fe1 N4 90.7(6) 2_655 . ? N4 Fe1 N4 89.3(6) 6 . ? N4 Fe1 N4 89.3(6) 5_655 2_655 ? N4 Fe1 N1 91.4(5) 5_655 5_655 ? N4 Fe1 N1 88.6(5) 2_655 . ? N4 Fe1 N1 91.4(5) 6 . ? N4 Fe1 N1 88.6(5) 6 5_655 ? N4 Fe1 N1 91.4(5) . . ? N4 Fe1 N1 88.6(5) . 5_655 ? N4 Fe1 N1 88.6(5) 5_655 . ? N4 Fe1 N1 91.4(5) 2_655 5_655 ? N1 Fe1 N1 180.0 . 5_655 ? H1A O1 H1B 107.33(2) . . ? C7 N6 Fe2 122.7(15) . . ? C7 N6 C10 114.1(19) . . ? C10 N6 Fe2 123.2(13) . . ? C9 N7 C10 115.4(13) . . ? H8A N8 H8A 111.4(4) . 6_575 ? H8A N8 H8B 112.885(19) . . ? H8B N8 H8A 112.887(19) . 6_575 ? C8 N8 H8A 97.3(5) . . ? C8 N8 H8A 97.3(5) . 6_575 ? C8 N8 H8B 123.3(9) . . ? C6 N5 Fe2 173.2(11) . . ? C5 N4 Fe1 177.1(10) . . ? C1 N1 Fe1 124.3(14) . . ? C1 N1 C4 114(2) . . ? C4 N1 Fe1 121.7(16) . . ? C3 N2 C4 117.6(15) . . ? H3A N3 H3A 33.3(10) . 6 ? H3A N3 H3B 141.62(4) . . ? H3B N3 H3A 141.63(4) . 6 ? C2 N3 H3A 116.8(8) . . ? C2 N3 H3A 116.8(8) . 6 ? C2 N3 H3B 97.0(9) . . ? N6 C7 H7 119.5 . . ? N6 C7 C8 121(2) . . ? C8 C7 H7 119.5 . . ? N8 C8 C7 120.4(18) . . ? N8 C8 C9 121.8(17) . . ? C9 C8 C7 117.8(19) . . ? N7 C9 C8 122.7(18) . . ? N7 C9 H9 118.7 . . ? C8 C9 H9 118.7 . . ? N6 C10 H10 115.5 . . ? N7 C10 N6 129.1(18) . . ? N7 C10 H10 115.5 . . ? N5 C6 Pt1 175.7(12) . . ? N4 C5 Pt1 177.4(10) . . ? N1 C1 H1 118.4 . . ? N1 C1 C2 123.3(19) . . ? C2 C1 H1 118.4 . . ? N3 C2 C1 121.3(17) . . ? N3 C2 C3 123.0(17) . . ? C3 C2 C1 115.7(18) . . ? N2 C3 C2 122(2) . . ? N2 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? N1 C4 H4 116.5 . . ? N2 C4 N1 127(2) . . ? N2 C4 H4 116.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe2 N6 C7 C8 180.000(4) . . . . ? Fe2 N6 C10 N7 180.000(4) . . . . ? Fe1 N1 C1 C2 180.000(4) . . . . ? Fe1 N1 C4 N2 180.000(1) . . . . ? N6 C7 C8 N8 180.000(6) . . . . ? N6 C7 C8 C9 0.000(7) . . . . ? N8 C8 C9 N7 180.000(2) . . . . ? N1 C1 C2 N3 180.000(2) . . . . ? N1 C1 C2 C3 0.000(6) . . . . ? N3 C2 C3 N2 180.000(6) . . . . ? C7 N6 C10 N7 0.000(8) . . . . ? C7 C8 C9 N7 0.000(4) . . . . ? C9 N7 C10 N6 0.000(9) . . . . ? C10 N6 C7 C8 0.000(6) . . . . ? C10 N7 C9 C8 0.000(5) . . . . ? C1 N1 C4 N2 0.000(3) . . . . ? C1 C2 C3 N2 0.000(6) . . . . ? C3 N2 C4 N1 0.000(2) . . . . ? C4 N1 C1 C2 0.000(4) . . . . ? C4 N2 C3 C2 0.000(5) . . . . ? _shelx_res_file ; TITL mo_rt327_5apmdpth2o_120k_0ma_a.res in C2/m mo_rt327_5apmdpth2o_120k_0ma.res created by SHELXL-2018/3 at 02:01:43 on 09-Sep-2020 REM Old TITL mo_RT327_5apmdPtH2O_120K_0ma in C2/m REM SHELXT solution in C2/m: R1 0.109, Rweak 0.002, Alpha 0.018 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C13 N2 Fe Pt CELL 0.71073 21.0776 7.0587 14.4881 90 131.352 90 ZERR 4 0.0026 0.0009 0.0033 0 0.003 0 LATT 7 SYMM -X,+Y,-Z SFAC C H Fe N O Pt UNIT 48 46.4 4 40 3.2 4 EQIV $1 +X,1-Y,+Z EQIV $2 1-X,2-Y,1-Z EQIV $3 1-X,1+Y,-Z DFIX 0.9 0.0001 N8 H8b DANG 2.2 0.0001 H8b O1 DANG 1.7 0.0001 H3a H3b DFIX 0.9 0.0001 H3b N3 DFIX 0.9 0.0001 H3a N3 DANG 1.5 0.0001 H8a H8b DFIX 0.9 0.0001 H8a N8 DANG 2.2 0.0001 H3b_$1 N7_$2 DANG 0.9 0.0001 O1 H1b DANG 2.2 0.0001 N2_$3 H1a DANG 1.45 0.0001 H1a H1b DANG 0.9 0.0001 O1 H1a L.S. 50 0 0 PLAN 5 SIZE 0.18 0.18 0.1 TEMP -153.32 CONF list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.119700 97.572296 FVAR 0.18560 PT1 6 0.484133 0.500000 0.235868 10.50000 0.03127 0.01652 = 0.02674 0.00000 0.02000 0.00000 FE2 3 0.500000 1.000000 0.500000 10.25000 0.04043 0.00991 = 0.02463 0.00000 0.02548 0.00000 FE1 3 0.500000 0.000000 0.000000 10.25000 0.04001 0.01012 = 0.02564 0.00000 0.02556 0.00000 PART -1 O1 5 0.238571 1.163244 0.014558 10.40000 0.05536 0.07775 = 0.05596 -0.02912 0.04482 -0.02434 H1A 2 0.238143 1.191192 -0.046461 10.40000 -1.50000 H1B 2 0.254690 1.268467 0.060396 10.40000 -1.50000 PART 0 N6 4 0.378714 1.000000 0.418839 10.50000 0.04492 0.00872 = 0.01663 0.00000 0.01156 0.00000 N7 4 0.273294 1.000000 0.439009 10.50000 0.03974 0.06194 = 0.04918 0.00000 0.03427 0.00000 N8 4 0.168880 1.000000 0.120206 10.50000 0.04905 0.06489 = 0.04357 0.00000 0.02848 0.00000 H8A 2 0.142314 1.105315 0.114280 10.50000 -1.50000 H8B 2 0.178336 1.000000 0.068040 10.50000 -1.50000 N5 4 0.482555 0.806344 0.390244 11.00000 0.04000 0.01464 = 0.02213 0.00007 0.02277 -0.00069 N4 4 0.495768 0.193358 0.091195 11.00000 0.03284 0.01541 = 0.02827 -0.00144 0.02436 0.00110 N1 4 0.623696 0.000000 0.120884 10.50000 0.05292 0.01749 = 0.04937 0.00000 0.04279 0.00000 N2 4 0.754994 0.000000 0.159551 10.50000 0.02602 0.08467 = 0.04425 0.00000 0.02323 0.00000 N3 4 0.804802 0.000000 0.450051 10.50000 0.02888 0.08944 = 0.03600 0.00000 0.02058 0.00000 H3A 2 0.859200 0.036559 0.498822 10.50000 -1.50000 H3B 2 0.760267 0.000000 0.445890 10.50000 -1.50000 C7 1 0.316978 1.000000 0.298098 10.50000 0.03441 0.03170 = 0.03772 0.00000 0.02199 0.00000 AFIX 43 H7 2 0.330275 1.000000 0.246935 10.50000 -1.20000 AFIX 0 C8 1 0.231574 1.000000 0.244055 10.50000 0.02386 0.02680 = 0.03691 0.00000 0.01640 0.00000 C9 1 0.214808 1.000000 0.321637 10.50000 0.02742 0.02685 = 0.04358 0.00000 0.01930 0.00000 AFIX 43 H9 2 0.157574 1.000000 0.286444 10.50000 -1.20000 AFIX 0 C10 1 0.352017 1.000000 0.481912 10.50000 0.03658 0.04612 = 0.03516 0.00000 0.02637 0.00000 AFIX 43 H10 2 0.395452 1.000000 0.568932 10.50000 -1.20000 AFIX 0 C6 1 0.480036 0.696996 0.329726 11.00000 0.03247 0.01001 = 0.02604 -0.00121 0.02093 -0.00405 C5 1 0.491627 0.302224 0.145896 11.00000 0.02678 0.01463 = 0.02466 0.00459 0.01790 0.00029 C1 1 0.670714 0.000000 0.243742 10.50000 0.04144 0.03108 = 0.02310 0.00000 0.01986 0.00000 AFIX 43 H1 2 0.642376 0.000000 0.274312 10.50000 -1.20000 AFIX 0 C2 1 0.761139 0.000000 0.330303 10.50000 0.02649 0.03256 = 0.03265 0.00000 0.01743 0.00000 C3 1 0.799411 0.000000 0.279405 10.50000 0.04859 0.02816 = 0.03487 0.00000 0.02809 0.00000 AFIX 43 H3 2 0.859352 0.000000 0.333204 10.50000 -1.20000 AFIX 0 C4 1 0.670521 0.000000 0.085659 10.50000 0.03716 0.04914 = 0.05302 0.00000 0.03476 0.00000 AFIX 43 H4 2 0.639591 0.000000 -0.000272 10.50000 -1.20000 AFIX 0 HKLF 4 REM mo_rt327_5apmdpth2o_120k_0ma_a.res in C2/m REM wR2 = 0.2482, GooF = S = 1.110, Restrained GooF = 1.108 for all data REM R1 = 0.0814 for 2106 Fo > 4sig(Fo) and 0.1431 for all 3046 data REM 160 parameters refined using 12 restraints END WGHT 0.1192 98.3285 REM Highest difference peak 9.896, deepest hole -7.238, 1-sigma level 0.529 Q1 1 0.5396 0.5000 0.2868 10.50000 0.05 9.90 Q2 1 0.4836 0.5000 0.1746 10.50000 0.05 7.87 Q3 1 0.4854 0.5000 0.2925 10.50000 0.05 5.09 Q4 1 0.5237 0.3766 0.2366 11.00000 0.05 4.10 Q5 1 0.5361 0.3822 0.3199 11.00000 0.05 2.86 ; _shelx_res_checksum 78687 _olex2_submission_special_instructions 'No special instructions were received' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_rt235_fe5apympd_120k_0m _database_code_depnum_ccdc_archive 'CCDC 2018380' loop_ _audit_author_name _audit_author_address 'Carlos Bartual-Murgui' ;Universitat de Valencia Spain ; _audit_update_record ; 2020-09-17 deposited with the CCDC. 2020-09-22 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT342_rt235_fe5apympd_120k_0m ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.025 Ang. RESPONSE: The crystal can be damaged during the dehydration process. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT971_rt235_fe5apympd_120k_0m ; PROBLEM: Check Calcd Resid. Dens. 0.79A From Pd1 3.05 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal, the deterioration of the crystal during the SCO process. ; # Added during the CSD deposition process: Thursday 17 September 2020 12:29 PM # end Validation Reply Form _audit_creation_date 2020-09-09 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C12 H9 Fe N10 Pd, H3 O' _chemical_formula_sum 'C12 H12 Fe N10 O Pd' _chemical_formula_weight 474.57 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_H-M_alt 'C 1 2/m 1' _space_group_name_Hall '-C 2y' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 21.092(3) _cell_length_b 7.0553(10) _cell_length_c 14.535(2) _cell_angle_alpha 90 _cell_angle_beta 131.372(4) _cell_angle_gamma 90 _cell_volume 1623.1(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3191 _cell_measurement_temperature 120.02 _cell_measurement_theta_max 29.08 _cell_measurement_theta_min 2.57 _shelx_estimated_absorpt_T_max 0.905 _shelx_estimated_absorpt_T_min 0.687 _exptl_absorpt_coefficient_mu 2.027 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_correction_T_min 0.5197 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1101 before and 0.0706 after correction. The Ratio of minimum to maximum transmission is 0.6968. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.942 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 936 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_unetI/netI 0.0624 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.949 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 9420 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.949 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.259 _diffrn_reflns_theta_min 2.574 _diffrn_ambient_temperature 120.02 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.949 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1699 _reflns_number_total 2266 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _refine_diff_density_max 3.606 _refine_diff_density_min -2.305 _refine_diff_density_rms 0.275 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 154 _refine_ls_number_reflns 2266 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1047 _refine_ls_R_factor_gt 0.0654 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+78.1367P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1332 _refine_ls_wR_factor_ref 0.1647 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All O(H,H) groups At 1.5 times of: All N(H,H) groups 2. Restrained distances H8A-N8 0.9 with sigma of 0.0001 O1-H1B 0.9 with sigma of 0.0001 H1A-O1 0.9 with sigma of 0.0001 N8-H8B 0.9 with sigma of 0.0001 H3A-N3 0.9 with sigma of 0.0001 N3-H3B 0.9 with sigma of 0.0001 H1A-H1B 1.45 with sigma of 0.0001 N2_$3-H1B 2 with sigma of 0.0001 H8A-H8B 1.5 with sigma of 0.0001 H3A-H3B 1.5 with sigma of 0.0001 N7_$1-H3B_$2 2.2 with sigma of 0.0001 3. Others Fixed Sof: H3B(0.5) O1(0.5) H1B(0.5) 4.a Aromatic/amide H refined with riding coordinates: C1(H1), C4(H4), C7(H7), C9(H9), C10(H10) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.48360(5) 0.500000 0.73519(7) 0.0178(2) Uani 1 2 d S T P . . Fe1 Fe 0.500000 0.000000 0.500000 0.0160(4) Uani 1 4 d S T P . . Fe2 Fe 0.500000 1.000000 1.000000 0.0151(4) Uani 1 4 d S T P . . N1 N 0.3739(6) 0.000000 0.3762(8) 0.0229(19) Uani 1 2 d S T P . . N2 N 0.24513(19) 0.000000 0.3392(2) 0.053(4) Uani 1 2 d S T P . . N3 N 0.19562(11) 0.000000 0.0507(2) 0.045(3) Uani 1 2 d DS T P . . H3A H 0.13882(10) 0.000000 -0.0067(3) 0.067 Uiso 1 2 d DS U P . . H3B H 0.21985(10) 0.0572(8) 0.02530(18) 0.067 Uiso 0.5 1 d D U P . . N4 N 0.4975(4) 0.1934(9) 0.5927(5) 0.0173(12) Uani 1 1 d . . . . . N5 N 0.4813(4) 0.8065(8) 0.8899(5) 0.0190(12) Uani 1 1 d . . . . . N6 N 0.3766(6) 1.000000 0.9167(9) 0.025(2) Uani 1 2 d S T P . . N7 N 0.27357(16) 1.000000 0.9400(2) 0.039(3) Uani 1 2 d S T P . . N8 N 0.16790(9) 1.000000 0.61972(14) 0.058(4) Uani 1 2 d DS T P . . H8A H 0.11408(10) 1.000000 0.5881(2) 0.087 Uiso 1 2 d DS U P . . H8B H 0.17192(12) 1.000000 0.56181(17) 0.087 Uiso 1 2 d DS U P . . C1 C 0.3295(8) 0.000000 0.2565(11) 0.027(2) Uani 1 2 d S T P . . H1 H 0.358312 0.000000 0.226788 0.033 Uiso 1 2 calc R U P . . C2 C 0.2393(7) 0.000000 0.1708(11) 0.026(2) Uani 1 2 d S T P . . C3 C 0.1991(8) 0.000000 0.2173(12) 0.033(3) Uani 1 2 d S T P . . C4 C 0.3294(8) 0.000000 0.4118(12) 0.036(3) Uani 1 2 d S T P . . H4 H 0.360891 0.000000 0.497665 0.043 Uiso 1 2 calc R U P . . C5 C 0.4928(4) 0.3021(10) 0.6465(6) 0.0146(13) Uani 1 1 d . . . . . C6 C 0.4789(4) 0.6977(10) 0.8294(6) 0.0166(13) Uani 1 1 d . . . . . C7 C 0.3161(8) 1.000000 0.7982(11) 0.032(3) Uani 1 2 d S T P . . H7 H 0.330141 1.000000 0.748089 0.038 Uiso 1 2 calc R U P . . C8 C 0.2296(7) 1.000000 0.7414(11) 0.029(2) Uani 1 2 d S T P . . C9 C 0.2132(8) 1.000000 0.8209(11) 0.032(3) Uani 1 2 d S T P . . H9 H 0.156189 1.000000 0.786638 0.038 Uiso 1 2 calc R U P . . C10 C 0.3542(8) 1.000000 0.9850(12) 0.031(3) Uani 1 2 d S T P . . H10 H 0.398517 1.000000 1.071628 0.038 Uiso 1 2 calc R U P . . O1 O 0.2677(2) 0.3646(6) 0.49390(19) 0.072(5) Uiso 0.5 1 d D . P A -1 H1A H 0.2283(2) 0.2742(5) 0.4645(4) 0.087 Uiso 1 1 d D U . . . H1B H 0.28739(17) 0.3969(6) 0.56875(17) 0.087 Uiso 0.5 1 d D U P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0252(4) 0.0136(4) 0.0202(4) 0.000 0.0173(3) 0.000 Fe1 0.0309(12) 0.0077(9) 0.0202(10) 0.000 0.0215(10) 0.000 Fe2 0.0292(11) 0.0062(9) 0.0193(9) 0.000 0.0200(9) 0.000 N1 0.026(5) 0.019(5) 0.019(4) 0.000 0.013(4) 0.000 N2 0.035(7) 0.096(12) 0.036(6) 0.000 0.027(6) 0.000 N3 0.039(7) 0.066(9) 0.035(6) 0.000 0.026(6) 0.000 N4 0.021(3) 0.015(3) 0.021(3) 0.001(2) 0.016(3) 0.001(2) N5 0.029(3) 0.010(3) 0.021(3) -0.001(2) 0.018(3) -0.001(2) N6 0.026(5) 0.013(4) 0.029(5) 0.000 0.015(4) 0.000 N7 0.033(6) 0.052(7) 0.038(6) 0.000 0.026(5) 0.000 N8 0.031(7) 0.102(13) 0.031(6) 0.000 0.017(6) 0.000 C1 0.041(7) 0.021(6) 0.034(6) 0.000 0.031(6) 0.000 C2 0.025(6) 0.024(6) 0.030(6) 0.000 0.019(5) 0.000 C3 0.030(7) 0.034(7) 0.034(6) 0.000 0.021(6) 0.000 C4 0.023(6) 0.060(9) 0.034(7) 0.000 0.023(6) 0.000 C5 0.021(3) 0.012(3) 0.019(3) -0.003(2) 0.017(3) -0.002(2) C6 0.018(3) 0.012(3) 0.023(3) 0.002(3) 0.015(3) 0.000(2) C7 0.034(7) 0.024(6) 0.027(6) 0.000 0.016(6) 0.000 C8 0.022(6) 0.031(6) 0.036(6) 0.000 0.019(5) 0.000 C9 0.029(6) 0.022(6) 0.028(6) 0.000 0.012(5) 0.000 C10 0.028(6) 0.040(7) 0.040(7) 0.000 0.028(6) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C5 1.994(6) 6_565 ? Pd1 C5 1.994(6) . ? Pd1 C6 2.003(7) 6_565 ? Pd1 C6 2.003(7) . ? Fe1 N1 1.996(9) . ? Fe1 N1 1.996(9) 5_656 ? Fe1 N4 1.943(6) 5_656 ? Fe1 N4 1.943(6) . ? Fe1 N4 1.943(6) 2_656 ? Fe1 N4 1.943(6) 6 ? Fe2 N5 1.935(6) . ? Fe2 N5 1.935(6) 2_657 ? Fe2 N5 1.935(6) 5_677 ? Fe2 N5 1.935(6) 6_575 ? Fe2 N6 2.019(10) . ? Fe2 N6 2.019(10) 5_677 ? N1 C1 1.324(14) . ? N1 C4 1.339(14) . ? N2 C3 1.345(13) . ? N2 C4 1.339(12) . ? N3 H3A 0.90000(18) . ? N3 H3B 0.89999(13) 6 ? N3 H3B 0.90000(13) . ? N3 C2 1.331(12) . ? N4 C5 1.146(8) . ? N5 C6 1.143(9) . ? N6 C7 1.300(15) . ? N6 C10 1.351(14) . ? N7 C9 1.306(12) . ? N7 C10 1.361(12) . ? N8 H8A 0.90000(19) . ? N8 H8B 0.90000(16) . ? N8 C8 1.334(13) . ? C1 H1 0.9500 . ? C1 C2 1.427(16) . ? C2 C3 1.390(17) . ? C4 H4 0.9500 . ? C7 H7 0.9500 . ? C7 C8 1.422(17) . ? C8 C9 1.408(17) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? O1 H1A 0.90000(15) . ? O1 H1B 0.90000(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Pd1 C5 88.9(4) 6_565 . ? C5 Pd1 C6 177.9(3) 6_565 6_565 ? C5 Pd1 C6 91.4(3) . 6_565 ? C5 Pd1 C6 91.4(3) 6_565 . ? C5 Pd1 C6 177.9(3) . . ? C6 Pd1 C6 88.3(4) 6_565 . ? N1 Fe1 N1 180.0 5_656 . ? N4 Fe1 N1 89.7(3) 5_656 5_656 ? N4 Fe1 N1 89.7(3) 2_656 5_656 ? N4 Fe1 N1 90.3(3) 2_656 . ? N4 Fe1 N1 90.3(3) 5_656 . ? N4 Fe1 N1 90.3(3) . 5_656 ? N4 Fe1 N1 90.3(3) 6 5_656 ? N4 Fe1 N1 89.7(3) 6 . ? N4 Fe1 N1 89.7(3) . . ? N4 Fe1 N4 90.8(3) . 2_656 ? N4 Fe1 N4 89.2(3) . 6 ? N4 Fe1 N4 89.2(3) 5_656 2_656 ? N4 Fe1 N4 90.8(3) 5_656 6 ? N4 Fe1 N4 180.0 . 5_656 ? N4 Fe1 N4 180.0 6 2_656 ? N5 Fe2 N5 89.7(3) 5_677 2_657 ? N5 Fe2 N5 90.3(4) 5_677 6_575 ? N5 Fe2 N5 180.0 6_575 2_657 ? N5 Fe2 N5 180.0 5_677 . ? N5 Fe2 N5 89.7(3) 6_575 . ? N5 Fe2 N5 90.3(4) 2_657 . ? N5 Fe2 N6 88.5(3) 6_575 5_677 ? N5 Fe2 N6 88.5(3) 2_657 . ? N5 Fe2 N6 91.5(3) 2_657 5_677 ? N5 Fe2 N6 91.5(3) 5_677 5_677 ? N5 Fe2 N6 91.5(3) . . ? N5 Fe2 N6 91.5(3) 6_575 . ? N5 Fe2 N6 88.5(3) 5_677 . ? N5 Fe2 N6 88.5(3) . 5_677 ? N6 Fe2 N6 180.0 . 5_677 ? C1 N1 Fe1 123.3(8) . . ? C1 N1 C4 116.1(10) . . ? C4 N1 Fe1 120.6(8) . . ? C4 N2 C3 117.6(8) . . ? H3A N3 H3B 112.89(2) . . ? H3A N3 H3B 112.88(2) . 6 ? H3B N3 H3B 53.3(8) . 6 ? C2 N3 H3A 124.0(5) . . ? C2 N3 H3B 116.7(5) . . ? C2 N3 H3B 116.7(5) . 6 ? C5 N4 Fe1 176.4(5) . . ? C6 N5 Fe2 172.3(6) . . ? C7 N6 Fe2 122.8(9) . . ? C7 N6 C10 117.4(11) . . ? C10 N6 Fe2 119.8(8) . . ? C9 N7 C10 116.8(8) . . ? H8A N8 H8B 112.89(2) . . ? C8 N8 H8A 118.2(5) . . ? C8 N8 H8B 128.9(5) . . ? N1 C1 H1 119.2 . . ? N1 C1 C2 121.6(10) . . ? C2 C1 H1 119.2 . . ? N3 C2 C1 120.8(9) . . ? N3 C2 C3 121.5(10) . . ? C3 C2 C1 117.7(11) . . ? N2 C3 C2 120.0(11) . . ? N1 C4 N2 126.9(11) . . ? N1 C4 H4 116.5 . . ? N2 C4 H4 116.5 . . ? N4 C5 Pd1 177.5(6) . . ? N5 C6 Pd1 175.5(7) . . ? N6 C7 H7 119.1 . . ? N6 C7 C8 121.8(12) . . ? C8 C7 H7 119.1 . . ? N8 C8 C7 121.5(10) . . ? N8 C8 C9 122.3(10) . . ? C9 C8 C7 116.2(11) . . ? N7 C9 C8 122.3(11) . . ? N7 C9 H9 118.8 . . ? C8 C9 H9 118.8 . . ? N6 C10 N7 125.4(11) . . ? N6 C10 H10 117.3 . . ? N7 C10 H10 117.3 . . ? H1A O1 H1B 107.328(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 N1 C1 C2 180.000(2) . . . . ? Fe1 N1 C4 N2 180.000(2) . . . . ? Fe2 N6 C7 C8 180.000(6) . . . . ? Fe2 N6 C10 N7 180.000(4) . . . . ? N1 C1 C2 N3 180.000(3) . . . . ? N1 C1 C2 C3 0.000(3) . . . . ? N3 C2 C3 N2 180.000(1) . . . . ? N6 C7 C8 N8 180.000(7) . . . . ? N6 C7 C8 C9 0.000(9) . . . . ? N8 C8 C9 N7 180.000(5) . . . . ? C1 N1 C4 N2 0.000(2) . . . . ? C1 C2 C3 N2 0.000(2) . . . . ? C3 N2 C4 N1 0.000(4) . . . . ? C4 N1 C1 C2 0.000(3) . . . . ? C4 N2 C3 C2 0.000(2) . . . . ? C7 N6 C10 N7 0.000(9) . . . . ? C7 C8 C9 N7 0.000(7) . . . . ? C9 N7 C10 N6 0.000(6) . . . . ? C10 N6 C7 C8 0.000(9) . . . . ? C10 N7 C9 C8 0.000(8) . . . . ? _shelx_res_file ; TITL rt235_fe5apympd_120k_0m_a.res in C2/m rt235_fe5apympd_120k_0m.res created by SHELXL-2018/3 at 02:12:12 on 09-Sep-2020 REM Old TITL RT235_Fe5apymPd_120K_0m in C2/m REM SHELXT solution in C2/m REM R1 0.103, Rweak 0.005, Alpha 0.051, Orientation as input REM Formula found by SHELXT: C12 N12 Fe Pd CELL 0.71073 21.0919 7.0553 14.5346 90 131.372 90 ZERR 4 0.0032 0.001 0.002 0 0.004 0 LATT 7 SYMM -X,+Y,-Z SFAC C H Fe N O Pd UNIT 48 48 4 40 4 4 EQIV $1 +X,1-Y,+Z EQIV $2 +X,-Y,1+Z EQIV $3 0.5-X,0.5-Y,1-Z DFIX 0.9 0.0001 H8a N8 DFIX 0.9 0.0001 O1 H1b DANG 1.45 0.0001 H1a H1b DFIX 0.9 0.0001 H1a O1 DANG 2 0.0001 N2_$3 H1b DANG 1.5 0.0001 H8a H8b DFIX 0.9 0.0001 N8 H8b DANG 1.5 0.0001 H3a H3b DFIX 0.9 0.0001 H3a N3 DFIX 0.9 0.0001 N3 H3b DANG 2.2 0.0001 N7_$1 H3b_$2 L.S. 50 PLAN 60 SIZE 0.05 0.15 0.2 TEMP -153.13 CONF list 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.017600 78.136696 FVAR 0.23035 PD1 6 0.483597 0.500000 0.735191 10.50000 0.02522 0.01359 = 0.02017 0.00000 0.01733 0.00000 FE1 3 0.500000 0.000000 0.500000 10.25000 0.03094 0.00774 = 0.02019 0.00000 0.02148 0.00000 FE2 3 0.500000 1.000000 1.000000 10.25000 0.02916 0.00625 = 0.01934 0.00000 0.02001 0.00000 N1 4 0.373896 0.000000 0.376218 10.50000 0.02623 0.01933 = 0.01864 0.00000 0.01294 0.00000 N2 4 0.245126 0.000000 0.339249 10.50000 0.03487 0.09565 = 0.03629 0.00000 0.02737 0.00000 N3 4 0.195615 0.000000 0.050696 10.50000 0.03893 0.06605 = 0.03473 0.00000 0.02646 0.00000 H3A 2 0.138817 0.000000 -0.006688 10.50000 -1.50000 H3B 2 0.219852 0.057222 0.025299 10.50000 -1.50000 N4 4 0.497493 0.193436 0.592740 11.00000 0.02130 0.01544 = 0.02096 0.00076 0.01638 0.00060 N5 4 0.481265 0.806550 0.889893 11.00000 0.02888 0.01016 = 0.02121 -0.00095 0.01798 -0.00072 N6 4 0.376585 1.000000 0.916725 10.50000 0.02616 0.01264 = 0.02856 0.00000 0.01490 0.00000 N7 4 0.273575 1.000000 0.940018 10.50000 0.03316 0.05171 = 0.03785 0.00000 0.02608 0.00000 N8 4 0.167901 1.000000 0.619723 10.50000 0.03149 0.10219 = 0.03071 0.00000 0.01672 0.00000 H8A 2 0.114085 1.000000 0.588097 10.50000 -1.50000 H8B 2 0.171917 1.000000 0.561808 10.50000 -1.50000 C1 1 0.329479 0.000000 0.256459 10.50000 0.04070 0.02130 = 0.03375 0.00000 0.03062 0.00000 AFIX 43 H1 2 0.358312 0.000000 0.226788 10.50000 -1.20000 AFIX 0 C2 1 0.239308 0.000000 0.170823 10.50000 0.02472 0.02431 = 0.03027 0.00000 0.01882 0.00000 C3 1 0.199143 0.000000 0.217312 10.50000 0.03046 0.03383 = 0.03420 0.00000 0.02063 0.00000 C4 1 0.329369 0.000000 0.411809 10.50000 0.02335 0.05958 = 0.03444 0.00000 0.02287 0.00000 AFIX 43 H4 2 0.360891 0.000000 0.497665 10.50000 -1.20000 AFIX 0 C5 1 0.492770 0.302145 0.646525 11.00000 0.02143 0.01180 = 0.01935 -0.00295 0.01715 -0.00173 C6 1 0.478889 0.697686 0.829441 11.00000 0.01801 0.01216 = 0.02341 0.00172 0.01536 0.00026 C7 1 0.316112 1.000000 0.798183 10.50000 0.03403 0.02379 = 0.02707 0.00000 0.01557 0.00000 AFIX 43 H7 2 0.330141 1.000000 0.748089 10.50000 -1.20000 AFIX 0 C8 1 0.229590 1.000000 0.741429 10.50000 0.02198 0.03067 = 0.03571 0.00000 0.01910 0.00000 C9 1 0.213203 1.000000 0.820894 10.50000 0.02906 0.02163 = 0.02849 0.00000 0.01202 0.00000 AFIX 43 H9 2 0.156189 1.000000 0.786638 10.50000 -1.20000 AFIX 0 C10 1 0.354247 1.000000 0.985032 10.50000 0.02803 0.03982 = 0.04022 0.00000 0.02834 0.00000 AFIX 43 H10 2 0.398517 1.000000 1.071628 10.50000 -1.20000 AFIX 0 PART -1 O1 5 0.267654 0.364624 0.493898 10.50000 0.07211 PART 0 H1A 2 0.228293 0.274182 0.464485 11.00000 -1.20000 H1B 2 0.287386 0.396878 0.568746 10.50000 -1.20000 HKLF 4 REM rt235_fe5apympd_120k_0m_a.res in C2/m REM wR2 = 0.1647, GooF = S = 1.045, Restrained GooF = 1.042 for all data REM R1 = 0.0654 for 1699 Fo > 4sig(Fo) and 0.1047 for all 2266 data REM 154 parameters refined using 11 restraints END WGHT 0.0175 78.1532 REM Highest difference peak 3.606, deepest hole -2.305, 1-sigma level 0.275 Q1 1 0.5322 0.5000 0.7786 10.50000 0.05 3.61 Q2 1 0.4715 0.5000 0.6699 10.50000 0.05 1.96 Q3 1 0.4929 0.5000 0.8010 10.50000 0.05 1.85 Q4 1 0.1426 0.0000 0.1786 10.50000 0.05 1.83 Q5 1 0.4983 0.0000 0.4415 10.50000 0.05 1.51 Q6 1 0.5414 0.6178 0.8183 11.00000 0.05 1.50 Q7 1 0.5358 0.3933 0.7412 11.00000 0.05 1.43 Q8 1 0.3211 1.0000 0.9099 10.50000 0.05 1.27 Q9 1 0.2845 0.0000 0.1290 10.50000 0.05 1.14 Q10 1 0.4562 1.0000 0.8191 10.50000 0.05 1.10 Q11 1 0.4503 0.3815 0.6411 11.00000 0.05 1.09 Q12 1 0.5126 1.0000 1.0686 10.50000 0.05 1.07 Q13 1 0.4203 0.4356 0.7193 11.00000 0.05 1.02 Q14 1 0.4991 0.7661 0.9624 11.00000 0.05 1.02 Q15 1 0.4871 0.6396 0.8003 11.00000 0.05 1.01 Q16 1 0.5636 0.9080 1.0871 11.00000 0.05 0.96 Q17 1 0.4203 0.4174 0.6505 11.00000 0.05 0.95 Q18 1 0.1808 1.0000 0.7078 10.50000 0.05 0.94 Q19 1 0.4599 0.0000 0.4629 10.50000 0.05 0.92 Q20 1 0.3719 1.0000 0.8072 10.50000 0.05 0.91 Q21 1 0.3836 1.1695 1.0281 11.00000 0.05 0.90 Q22 1 0.3450 1.0000 0.7087 10.50000 0.05 0.88 Q23 1 0.5110 1.0000 1.2015 10.50000 0.05 0.87 Q24 1 0.0925 1.0619 0.6915 11.00000 0.05 0.82 Q25 1 0.4827 0.8891 0.9176 11.00000 0.05 0.81 Q26 1 0.4490 0.5000 0.8429 10.50000 0.05 0.80 Q27 1 0.4404 0.1017 0.3970 11.00000 0.05 0.80 Q28 1 0.2635 0.0000 0.2718 10.50000 0.05 0.78 Q29 1 0.2153 1.0000 0.5910 10.50000 0.05 0.78 Q30 1 0.4143 1.1492 1.0092 11.00000 0.05 0.78 Q31 1 0.1289 0.0000 0.0571 10.50000 0.05 0.77 Q32 1 0.5000 0.2305 0.5000 10.50000 0.05 0.76 Q33 1 0.0503 1.0000 0.5579 10.50000 0.05 0.76 Q34 1 0.4346 0.0000 0.3161 10.50000 0.05 0.75 Q35 1 0.5000 0.9076 1.0000 10.50000 0.05 0.75 Q36 1 0.4687 0.1556 0.5123 11.00000 0.05 0.75 Q37 1 0.4634 0.0652 0.7118 11.00000 0.05 0.75 Q38 1 0.3704 0.4161 0.6888 11.00000 0.05 0.74 Q39 1 0.5562 0.2482 0.7995 11.00000 0.05 0.74 Q40 1 0.5230 0.2747 0.6426 11.00000 0.05 0.74 Q41 1 0.3097 1.0537 0.6391 11.00000 0.05 0.74 Q42 1 0.5439 0.3765 0.6794 11.00000 0.05 0.74 Q43 1 0.3221 0.0626 0.1275 11.00000 0.05 0.74 Q44 1 0.3440 0.5000 0.6521 10.50000 0.05 0.73 Q45 1 0.4337 0.5000 0.7560 10.50000 0.05 0.73 Q46 1 0.4033 0.0000 0.3270 10.50000 0.05 0.72 Q47 1 0.4155 0.1871 0.4768 11.00000 0.05 0.72 Q48 1 0.1835 0.0000 0.3317 10.50000 0.05 0.72 Q49 1 0.3540 1.0000 1.1157 10.50000 0.05 0.71 Q50 1 0.4274 0.0899 0.4369 11.00000 0.05 0.71 Q51 1 0.0743 0.0000 0.0580 10.50000 0.05 0.70 Q52 1 0.4685 0.2988 0.7101 11.00000 0.05 0.70 Q53 1 0.3626 1.0530 0.8611 11.00000 0.05 0.70 Q54 1 0.5000 -0.0843 0.5000 10.50000 0.05 0.70 Q55 1 0.2065 1.0467 0.7660 11.00000 0.05 0.69 Q56 1 0.3199 0.0000 0.3140 10.50000 0.05 0.69 Q57 1 0.4135 1.0000 0.8094 10.50000 0.05 0.68 Q58 1 0.5292 0.0000 0.4461 10.50000 0.05 0.68 Q59 1 0.3867 0.5000 0.7438 10.50000 0.05 0.68 Q60 1 0.2699 1.0000 0.8247 10.50000 0.05 0.68 ; _shelx_res_checksum 82819 _olex2_submission_special_instructions 'No special instructions were received' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_rt235_fe5apympd_260k_0ma_a _database_code_depnum_ccdc_archive 'CCDC 2018384' loop_ _audit_author_name _audit_author_address 'Carlos Bartual-Murgui' ;Universitat de Valencia Spain ; _audit_update_record ; 2020-09-17 deposited with the CCDC. 2020-09-22 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT934_rt235_fe5apympd_260k_0ma_a ; PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers .. 3 Check RESPONSE: his alerts arises from 4 slighly disagreeable reflections in our refinements which were not omitted as we believe that the difference between I(obs) and I(calc) was not two large. ; # Added during the CSD deposition process: Thursday 17 September 2020 12:29 PM # end Validation Reply Form _audit_creation_date 2020-09-09 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C12 H10 Fe N10 Pd, 0.5(H4 O2)' _chemical_formula_sum 'C12 H12 Fe N10 O Pd' _chemical_formula_weight 474.57 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_H-M_alt 'C 1 2/m 1' _space_group_name_Hall '-C 2y' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 21.770(3) _cell_length_b 7.3679(8) _cell_length_c 14.951(3) _cell_angle_alpha 90 _cell_angle_beta 131.902(3) _cell_angle_gamma 90 _cell_volume 1784.9(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4213 _cell_measurement_temperature 260.0 _cell_measurement_theta_max 29.90 _cell_measurement_theta_min 2.51 _shelx_estimated_absorpt_T_max 0.913 _shelx_estimated_absorpt_T_min 0.709 _exptl_absorpt_coefficient_mu 1.843 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_correction_T_min 0.5592 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1219 before and 0.0714 after correction. The Ratio of minimum to maximum transmission is 0.7496. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 936 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_unetI/netI 0.0472 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.962 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 11544 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.962 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.929 _diffrn_reflns_theta_min 2.514 _diffrn_ambient_temperature 260.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.962 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2122 _reflns_number_total 2671 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _refine_diff_density_max 2.340 _refine_diff_density_min -1.681 _refine_diff_density_rms 0.223 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 153 _refine_ls_number_reflns 2671 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0526 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+24.3621P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1292 _refine_ls_wR_factor_ref 0.1724 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All N(H,H) groups, All O(H,H) groups 2. Restrained distances N3-H3A 0.9 with sigma of 0.0001 H8A-N8 0.9 with sigma of 0.0001 N8-H8B 0.9 with sigma of 0.0001 H1B-O1 0.9 with sigma of 0.0001 O1-H1A 0.9 with sigma of 0.0001 H3B-N3 0.9 with sigma of 0.0001 O1-H8B 2.2 with sigma of 0.0001 H8A-H8B 1.5 with sigma of 0.0001 H1B-H1A 1.45 with sigma of 0.0001 H3B-H3A 1.5 with sigma of 0.0001 3. Others Fixed Sof: H8A(0.5) H8B(0.5) O1(0.5) H1B(0.5) Fixed Uiso: O1(0.08) 4.a Aromatic/amide H refined with riding coordinates: C10(H10), C1(H1), C9(H9), C7(H7), C4(H4), C3(H3) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd01 Pd 0.51650(4) 0.500000 0.26458(5) 0.0251(2) Uani 1 2 d S T P . . Fe2 Fe 0.500000 0.000000 0.000000 0.0247(3) Uani 1 4 d S T P . . Fe1 Fe 0.500000 1.000000 0.500000 0.0265(3) Uani 1 4 d S T P . . N4 N 0.5008(3) 0.7955(8) 0.3985(5) 0.0392(12) Uani 1 1 d . . . . . N5 N 0.5232(3) 0.2044(7) 0.1213(5) 0.0381(11) Uani 1 1 d . . . . . N6 N 0.3680(5) 0.000000 -0.0862(7) 0.0381(16) Uani 1 2 d S T P . . C6 C 0.5230(4) 0.3116(8) 0.1775(5) 0.0309(11) Uani 1 1 d . . . . . N1 N 0.3636(5) 1.000000 0.3652(7) 0.0390(17) Uani 1 2 d S T P . . C5 C 0.5066(4) 0.6888(8) 0.3484(5) 0.0306(11) Uani 1 1 d . . . . . N7 N 0.2693(6) 0.000000 -0.0646(10) 0.064(3) Uani 1 2 d S T P . . N3 N 0.19080(10) 1.000000 0.04633(19) 0.078(4) Uani 1 2 d DS T P . . H3A H 0.21665(11) 1.000000 0.0182(2) 0.118 Uiso 1 2 d DS U P . . H3B H 0.13545(9) 1.000000 -0.0126(3) 0.118 Uiso 1 2 d DS U P . . C2 C 0.2335(6) 1.000000 0.1633(10) 0.046(2) Uani 1 2 d S T P . . N2 N 0.2384(6) 1.000000 0.3279(10) 0.072(3) Uani 1 2 d S T P . . C10 C 0.3478(7) 0.000000 -0.0190(10) 0.049(2) Uani 1 2 d S T P . . H10 H 0.390301 0.000000 0.064167 0.059 Uiso 1 2 calc R U P . . C1 C 0.3198(6) 1.000000 0.2491(9) 0.042(2) Uani 1 2 d S T P . . H1 H 0.347797 1.000000 0.221986 0.051 Uiso 1 2 calc R U P . . C8 C 0.2249(6) 0.000000 -0.2582(10) 0.051(3) Uani 1 2 d S T P . . C9 C 0.2103(7) 0.000000 -0.1808(11) 0.055(3) Uani 1 2 d S T P . . H9 H 0.155983 0.000000 -0.213594 0.066 Uiso 1 2 calc R U P . . C7 C 0.3083(6) 0.000000 -0.2018(9) 0.043(2) Uani 1 2 d S T P . . H7 H 0.321438 0.000000 -0.249586 0.052 Uiso 1 2 calc R U P . . C4 C 0.3210(7) 1.000000 0.4016(10) 0.057(3) Uani 1 2 d S T P . . H4 H 0.351265 1.000000 0.483884 0.068 Uiso 1 2 calc R U P . . C3 C 0.1952(7) 1.000000 0.2104(11) 0.057(3) Uani 1 2 d S T P . . H3 H 0.137907 1.000000 0.157752 0.068 Uiso 1 2 calc R U P . . N8 N 0.16361(12) 0.000000 -0.3776(3) 0.081(4) Uani 1 2 d DS T P . . H8A H 0.11832(11) 0.0635(5) -0.4062(3) 0.121 Uiso 0.5 1 d D U P . . H8B H 0.19239(10) 0.0523(8) -0.39412(16) 0.121 Uiso 0.5 1 d D U P . . O1 O 0.22146(12) 0.1078(4) -0.50697(17) 0.080 Uiso 0.5 1 d D U P . . H1A H 0.2299(3) 0.000000 -0.5255(4) 0.120 Uiso 1 2 d DS U P . . H1B H 0.27070(17) 0.1637(4) -0.4551(6) 0.120 Uiso 0.5 1 d D U P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd01 0.0397(4) 0.0160(3) 0.0285(3) 0.000 0.0264(3) 0.000 Fe2 0.0393(8) 0.0159(7) 0.0287(7) 0.000 0.0267(7) 0.000 Fe1 0.0444(9) 0.0160(7) 0.0307(8) 0.000 0.0299(7) 0.000 N4 0.052(3) 0.032(3) 0.044(3) -0.002(2) 0.036(3) 0.001(2) N5 0.054(3) 0.029(3) 0.042(3) -0.004(2) 0.036(3) -0.001(2) N6 0.040(4) 0.035(4) 0.041(4) 0.000 0.028(3) 0.000 C6 0.042(3) 0.024(3) 0.032(3) 0.000(2) 0.027(2) 0.003(2) N1 0.048(4) 0.033(4) 0.045(4) 0.000 0.034(4) 0.000 C5 0.044(3) 0.023(3) 0.034(3) -0.002(2) 0.029(3) 0.001(2) N7 0.047(5) 0.097(9) 0.065(6) 0.000 0.045(5) 0.000 N3 0.043(5) 0.147(12) 0.040(5) 0.000 0.025(4) 0.000 C2 0.036(5) 0.049(6) 0.056(6) 0.000 0.032(5) 0.000 N2 0.052(5) 0.119(11) 0.064(6) 0.000 0.047(5) 0.000 C10 0.048(5) 0.064(7) 0.047(5) 0.000 0.036(5) 0.000 C1 0.050(5) 0.042(5) 0.045(5) 0.000 0.036(5) 0.000 C8 0.035(5) 0.054(6) 0.050(6) 0.000 0.023(5) 0.000 C9 0.034(5) 0.061(7) 0.060(7) 0.000 0.027(5) 0.000 C7 0.054(6) 0.048(6) 0.039(5) 0.000 0.036(5) 0.000 C4 0.057(6) 0.083(9) 0.048(6) 0.000 0.042(5) 0.000 C3 0.054(6) 0.063(8) 0.059(7) 0.000 0.040(6) 0.000 N8 0.051(6) 0.124(11) 0.051(6) 0.000 0.028(5) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd01 C6 1.973(6) . ? Pd01 C6 1.973(6) 6_565 ? Pd01 C5 1.978(6) 6_565 ? Pd01 C5 1.978(6) . ? Fe2 N5 2.142(5) 5_655 ? Fe2 N5 2.142(5) 2_655 ? Fe2 N5 2.142(5) . ? Fe2 N5 2.142(5) 6 ? Fe2 N6 2.230(8) 5_655 ? Fe2 N6 2.230(8) . ? Fe1 N4 2.146(5) 5_676 ? Fe1 N4 2.146(5) 6_575 ? Fe1 N4 2.146(5) . ? Fe1 N4 2.146(5) 2_656 ? Fe1 N1 2.211(8) 5_676 ? Fe1 N1 2.211(8) . ? N4 C5 1.150(8) . ? N5 C6 1.154(8) . ? N6 C10 1.339(12) . ? N6 C7 1.295(12) . ? N1 C1 1.309(12) . ? N1 C4 1.351(12) . ? N7 C10 1.351(13) . ? N7 C9 1.299(16) . ? N3 H3A 0.90000(15) . ? N3 H3B 0.90000(15) . ? N3 C2 1.323(11) . ? C2 C1 1.399(14) . ? C2 C3 1.406(15) . ? N2 C4 1.343(15) . ? N2 C3 1.327(16) . ? C10 H10 0.9300 . ? C1 H1 0.9300 . ? C8 C9 1.390(16) . ? C8 C7 1.401(14) . ? C8 N8 1.335(11) . ? C9 H9 0.9300 . ? C7 H7 0.9300 . ? C4 H4 0.9300 . ? C3 H3 0.9300 . ? N8 H8A 0.90004(14) 6 ? N8 H8A 0.90000(14) . ? N8 H8B 0.90005(13) 6 ? N8 H8B 0.90000(14) . ? O1 O1 1.589(6) 6 ? O1 H1A 0.90000(14) . ? O1 H1B 0.90000(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Pd01 C6 89.4(3) . 6_565 ? C6 Pd01 C5 178.4(2) 6_565 6_565 ? C6 Pd01 C5 90.6(2) . 6_565 ? C6 Pd01 C5 90.6(2) 6_565 . ? C6 Pd01 C5 178.4(2) . . ? C5 Pd01 C5 89.4(3) 6_565 . ? N5 Fe2 N5 90.7(3) 5_655 6 ? N5 Fe2 N5 180.0 5_655 . ? N5 Fe2 N5 180.0(3) 6 2_655 ? N5 Fe2 N5 90.7(3) 2_655 . ? N5 Fe2 N5 89.3(3) 6 . ? N5 Fe2 N5 89.3(3) 5_655 2_655 ? N5 Fe2 N6 91.5(2) 5_655 . ? N5 Fe2 N6 88.5(2) 2_655 5_655 ? N5 Fe2 N6 91.5(2) . 5_655 ? N5 Fe2 N6 91.5(2) 2_655 . ? N5 Fe2 N6 88.5(2) . . ? N5 Fe2 N6 91.5(2) 6 5_655 ? N5 Fe2 N6 88.5(2) 6 . ? N5 Fe2 N6 88.5(2) 5_655 5_655 ? N6 Fe2 N6 180.0 5_655 . ? N4 Fe1 N4 180.0 6_575 2_656 ? N4 Fe1 N4 89.2(3) 5_676 2_656 ? N4 Fe1 N4 89.2(3) 6_575 . ? N4 Fe1 N4 90.8(3) 2_656 . ? N4 Fe1 N4 180.0 5_676 . ? N4 Fe1 N4 90.8(3) 5_676 6_575 ? N4 Fe1 N1 89.8(2) . . ? N4 Fe1 N1 90.2(2) 2_656 . ? N4 Fe1 N1 89.8(2) 5_676 5_676 ? N4 Fe1 N1 89.8(2) 6_575 . ? N4 Fe1 N1 89.8(2) 2_656 5_676 ? N4 Fe1 N1 90.2(2) . 5_676 ? N4 Fe1 N1 90.2(2) 6_575 5_676 ? N4 Fe1 N1 90.2(2) 5_676 . ? N1 Fe1 N1 180.0 5_676 . ? C5 N4 Fe1 175.4(5) . . ? C6 N5 Fe2 169.5(5) . . ? C10 N6 Fe2 120.6(7) . . ? C7 N6 Fe2 121.9(6) . . ? C7 N6 C10 117.5(9) . . ? N5 C6 Pd01 176.6(6) . . ? C1 N1 Fe1 123.6(6) . . ? C1 N1 C4 116.5(9) . . ? C4 N1 Fe1 119.9(7) . . ? N4 C5 Pd01 178.4(6) . . ? C9 N7 C10 117.6(10) . . ? H3A N3 H3B 112.89(2) . . ? C2 N3 H3A 120.7(4) . . ? C2 N3 H3B 126.4(4) . . ? N3 C2 C1 122.7(8) . . ? N3 C2 C3 122.3(9) . . ? C1 C2 C3 115.0(10) . . ? C3 N2 C4 117.6(10) . . ? N6 C10 N7 124.0(10) . . ? N6 C10 H10 118.0 . . ? N7 C10 H10 118.0 . . ? N1 C1 C2 123.9(9) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C9 C8 C7 115.1(10) . . ? N8 C8 C9 122.2(9) . . ? N8 C8 C7 122.8(10) . . ? N7 C9 C8 122.8(10) . . ? N7 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? N6 C7 C8 123.0(9) . . ? N6 C7 H7 118.5 . . ? C8 C7 H7 118.5 . . ? N1 C4 H4 117.6 . . ? N2 C4 N1 124.9(10) . . ? N2 C4 H4 117.6 . . ? C2 C3 H3 119.0 . . ? N2 C3 C2 122.0(11) . . ? N2 C3 H3 119.0 . . ? C8 N8 H8A 115.8(5) . . ? C8 N8 H8A 115.8(5) . 6 ? C8 N8 H8B 96.3(5) . 6 ? C8 N8 H8B 96.3(5) . . ? H8A N8 H8A 62.6(6) . 6 ? H8A N8 H8B 146.5(5) . 6 ? H8A N8 H8B 112.89(2) 6 6 ? H8A N8 H8B 112.89(2) . . ? H8B N8 H8A 146.5(5) . 6 ? H8B N8 H8B 50.7(8) . 6 ? O1 O1 H1A 28.1(4) 6 . ? O1 O1 H1B 117.2(3) 6 . ? H1A O1 H1B 107.328(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe2 N6 C10 N7 180.000(1) . . . . ? Fe2 N6 C7 C8 180.000(1) . . . . ? Fe1 N1 C1 C2 180.000(2) . . . . ? Fe1 N1 C4 N2 180.000(2) . . . . ? N3 C2 C1 N1 180.000(2) . . . . ? N3 C2 C3 N2 180.000(2) . . . . ? C10 N6 C7 C8 0.000(2) . . . . ? C10 N7 C9 C8 0.000(2) . . . . ? C1 N1 C4 N2 0.000(4) . . . . ? C1 C2 C3 N2 0.000(3) . . . . ? C9 N7 C10 N6 0.000(1) . . . . ? C9 C8 C7 N6 0.000(2) . . . . ? C7 N6 C10 N7 0.000(1) . . . . ? C7 C8 C9 N7 0.000(2) . . . . ? C4 N1 C1 C2 0.000(3) . . . . ? C4 N2 C3 C2 0.000(3) . . . . ? C3 C2 C1 N1 0.000(2) . . . . ? C3 N2 C4 N1 0.000(4) . . . . ? N8 C8 C9 N7 180.000(2) . . . . ? N8 C8 C7 N6 180.000(2) . . . . ? _shelx_res_file ; TITL RT235_Fe5apymPd_260K_0ma_a.res in C2/m rt235_fe5apympd_260k_0ma_a.res created by SHELXL-2018/3 at 17:44:10 on 09-Sep-2020 CELL 0.71073 21.77 7.3679 14.9511 90 131.902 90 ZERR 4 0.0025 0.0008 0.0032 0 0.003 0 LATT 7 SYMM -X,+Y,-Z SFAC C H Fe N O Pd UNIT 48 48 4 40 4 4 DFIX 0.9 0.0001 N3 H3a DANG 2.2 0.0001 O1 H8b DFIX 0.9 0.0001 H8a N8 DANG 1.5 0.0001 H8a H8b DANG 1.45 0.0001 H1b H1a DFIX 0.9 0.0001 N8 H8b DFIX 0.9 0.0001 H1b O1 DFIX 0.9 0.0001 O1 H1a DANG 1.5 0.0001 H3b H3a DFIX 0.9 0.0001 H3b N3 L.S. 50 PLAN 1 0 0 SIZE 0.05 0.15 0.2 TEMP -13.15 CONF MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.067400 24.362099 FVAR 0.24385 PD01 6 0.516495 0.500000 0.264578 10.50000 0.03965 0.01599 = 0.02853 0.00000 0.02639 0.00000 FE2 3 0.500000 0.000000 0.000000 10.25000 0.03934 0.01586 = 0.02865 0.00000 0.02673 0.00000 FE1 3 0.500000 1.000000 0.500000 10.25000 0.04442 0.01595 = 0.03069 0.00000 0.02990 0.00000 N4 4 0.500759 0.795506 0.398509 11.00000 0.05181 0.03164 = 0.04406 -0.00235 0.03612 0.00109 N5 4 0.523175 0.204405 0.121311 11.00000 0.05358 0.02852 = 0.04188 -0.00412 0.03583 -0.00102 N6 4 0.367974 0.000000 -0.086179 10.50000 0.03978 0.03452 = 0.04124 0.00000 0.02757 0.00000 C6 1 0.523042 0.311564 0.177455 11.00000 0.04237 0.02355 = 0.03240 -0.00001 0.02725 0.00316 N1 4 0.363574 1.000000 0.365246 10.50000 0.04752 0.03290 = 0.04471 0.00000 0.03415 0.00000 C5 1 0.506616 0.688802 0.348430 11.00000 0.04359 0.02285 = 0.03398 -0.00202 0.02946 0.00068 N7 4 0.269314 0.000000 -0.064642 10.50000 0.04696 0.09672 = 0.06533 0.00000 0.04478 0.00000 N3 4 0.190796 1.000000 0.046332 10.50000 0.04275 0.14698 = 0.03987 0.00000 0.02531 0.00000 H3A 2 0.216654 1.000000 0.018201 10.50000 -1.50000 H3B 2 0.135451 1.000000 -0.012587 10.50000 -1.50000 C2 1 0.233513 1.000000 0.163307 10.50000 0.03649 0.04901 = 0.05620 0.00000 0.03206 0.00000 N2 4 0.238403 1.000000 0.327859 10.50000 0.05195 0.11913 = 0.06426 0.00000 0.04694 0.00000 C10 1 0.347765 0.000000 -0.018961 10.50000 0.04815 0.06362 = 0.04727 0.00000 0.03640 0.00000 AFIX 43 H10 2 0.390301 0.000000 0.064167 10.50000 -1.20000 AFIX 0 C1 1 0.319820 1.000000 0.249091 10.50000 0.05050 0.04170 = 0.04510 0.00000 0.03635 0.00000 AFIX 43 H1 2 0.347797 1.000000 0.221986 10.50000 -1.20000 AFIX 0 C8 1 0.224891 0.000000 -0.258231 10.50000 0.03525 0.05435 = 0.05009 0.00000 0.02284 0.00000 C9 1 0.210315 0.000000 -0.180812 10.50000 0.03428 0.06091 = 0.06020 0.00000 0.02705 0.00000 AFIX 43 H9 2 0.155983 0.000000 -0.213594 10.50000 -1.20000 AFIX 0 C7 1 0.308319 0.000000 -0.201787 10.50000 0.05392 0.04783 = 0.03887 0.00000 0.03566 0.00000 AFIX 43 H7 2 0.321438 0.000000 -0.249586 10.50000 -1.20000 AFIX 0 C4 1 0.321040 1.000000 0.401612 10.50000 0.05704 0.08335 = 0.04755 0.00000 0.04193 0.00000 AFIX 43 H4 2 0.351265 1.000000 0.483884 10.50000 -1.20000 AFIX 0 C3 1 0.195234 1.000000 0.210449 10.50000 0.05432 0.06331 = 0.05867 0.00000 0.03994 0.00000 AFIX 43 H3 2 0.137907 1.000000 0.157752 10.50000 -1.20000 AFIX 0 N8 4 0.163608 0.000000 -0.377551 10.50000 0.05145 0.12384 = 0.05104 0.00000 0.02785 0.00000 H8A 2 0.118324 0.063475 -0.406202 10.50000 -1.50000 H8B 2 0.192385 0.052346 -0.394125 10.50000 -1.50000 O1 5 0.221456 0.107800 -0.506967 10.50000 10.08000 H1A 2 0.229934 0.000000 -0.525499 10.50000 -1.50000 H1B 2 0.270704 0.163720 -0.455128 10.50000 -1.50000 HKLF 4 REM RT235_Fe5apymPd_260K_0ma_a.res in C2/m REM wR2 = 0.1724, GooF = S = 1.107, Restrained GooF = 1.104 for all data REM R1 = 0.0526 for 2122 Fo > 4sig(Fo) and 0.0787 for all 2671 data REM 153 parameters refined using 10 restraints END WGHT 0.0674 24.3682 REM Highest difference peak 2.340, deepest hole -1.681, 1-sigma level 0.223 Q1 1 0.4621 0.5000 0.2177 10.50000 0.05 2.34 ; _shelx_res_checksum 39748 _olex2_submission_special_instructions 'No special instructions were received' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mo_rt327_5apdmpth2o_260k_0m _database_code_depnum_ccdc_archive 'CCDC 2018383' loop_ _audit_author_name _audit_author_address 'Carlos Bartual-Murgui' ;Universitat de Valencia Spain ; _audit_update_record ; 2020-09-17 deposited with the CCDC. 2020-09-22 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT971_mo_rt327_5apdmpth2o_260k_0m ; PROBLEM: Check Calcd Resid. Dens. 0.93A From Pt1 4.57 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_mo_rt327_5apdmpth2o_260k_0m_2 ; PROBLEM: Check Calcd Resid. Dens. 0.72A From Pt1 4.11 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT342_mo_rt327_5apdmpth2o_260k_0m ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0375 Ang. RESPONSE: The crystal can be damaged during the SCO process. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT971_mo_rt327_5apdmpth2o_260k_0m_3 ; PROBLEM: Check Calcd Resid. Dens. 0.92A From Pt1 3.13 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_mo_rt327_5apdmpth2o_260k_0m ; PROBLEM: Check Calcd Resid. Dens. 0.73A From Pt1 -3.47 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_mo_rt327_5apdmpth2o_260k_0m_2 ; PROBLEM: Check Calcd Resid. Dens. 0.70A From Pt1 -3.36 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_mo_rt327_5apdmpth2o_260k_0m_3 ; PROBLEM: Check Calcd Resid. Dens. 0.65A From Pt1 -2.99 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; # Added during the CSD deposition process: Thursday 17 September 2020 12:29 PM # end Validation Reply Form _audit_creation_date 2020-09-09 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C12 H10 Fe N10 Pt, 0.8(H2 O)' _chemical_formula_sum 'C12 H11.60 Fe N10 O0.80 Pt' _chemical_formula_weight 559.65 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_H-M_alt 'C 1 2/m 1' _space_group_name_Hall '-C 2y' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 21.836(2) _cell_length_b 7.3747(6) _cell_length_c 14.8914(12) _cell_angle_alpha 90 _cell_angle_beta 131.952(3) _cell_angle_gamma 90 _cell_volume 1783.4(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6099 _cell_measurement_temperature 260.02 _cell_measurement_theta_max 32.19 _cell_measurement_theta_min 2.51 _shelx_estimated_absorpt_T_max 0.478 _shelx_estimated_absorpt_T_min 0.304 _exptl_absorpt_coefficient_mu 8.670 _exptl_absorpt_correction_T_max 0.7464 _exptl_absorpt_correction_T_min 0.5106 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1040 before and 0.0667 after correction. The Ratio of minimum to maximum transmission is 0.6841. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 2.084 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1056 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.1 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0681 _diffrn_reflns_av_unetI/netI 0.0623 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.982 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 16655 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.982 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.379 _diffrn_reflns_theta_min 2.508 _diffrn_ambient_temperature 260.02 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2601 _reflns_number_total 3361 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _refine_diff_density_max 4.596 _refine_diff_density_min -3.949 _refine_diff_density_rms 0.317 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 154 _refine_ls_number_reflns 3361 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0544 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+41.0043P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1267 _refine_ls_wR_factor_ref 0.1471 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All N(H,H) groups, All O(H,H) groups 2. Restrained distances N8-H8B 0.9 with sigma of 0.0001 H8A-N8 0.9 with sigma of 0.0001 O1-H1A 0.9 with sigma of 0.0001 O1-H1B 0.9 with sigma of 0.0001 H3B-N3 0.9 with sigma of 0.0001 H3A-N3 0.9 with sigma of 0.0001 H8B-O1 2.21 with sigma of 0.0001 H8A-H8B 1.5 with sigma of 0.0001 H1A-H1B 1.45 with sigma of 0.0001 H3B-H3A 1.5 with sigma of 0.0001 H1A-N2_$1 2.1 with sigma of 0.0001 3. Others Fixed Sof: H8A(0.5) O1(0.4) H1A(0.4) H1B(0.4) 4.a Aromatic/amide H refined with riding coordinates: C7(H7), C9(H9), C10(H10), C1(H1), C3(H3), C4(H4) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.48425(3) 0.500000 0.73593(4) 0.02265(13) Uani 1 2 d S T P . . Fe2 Fe 0.500000 1.000000 1.000000 0.0231(4) Uani 1 4 d S T P . . Fe1 Fe 0.500000 0.000000 0.500000 0.0237(4) Uani 1 4 d S T P . . N6 N 0.3676(8) 1.000000 0.9124(11) 0.043(3) Uani 1 2 d S T P . . N7 N 0.2682(11) 1.000000 0.9339(17) 0.072(5) Uani 1 2 d S T P . . N8 N 0.16760(12) 1.000000 0.62910(18) 0.095(7) Uani 1 2 d DS T P . . H8A H 0.12710(13) 0.9174(4) 0.5947(3) 0.143 Uiso 0.5 1 d D U P . . H8B H 0.19101(10) 1.000000 0.59726(15) 0.143 Uiso 1 2 d DS U P . . N5 N 0.4797(5) 0.7969(10) 0.8812(7) 0.0378(17) Uani 1 1 d . . . . . N4 N 0.4960(5) 0.2040(10) 0.5979(7) 0.0386(17) Uani 1 1 d . . . . . N1 N 0.3642(10) 0.000000 0.3650(14) 0.054(3) Uani 1 2 d S T P . . N2 N 0.2390(2) 0.000000 0.3285(2) 0.094(7) Uani 1 2 d S T P . . N3 N 0.19295(10) 0.000000 0.0519(2) 0.086(6) Uani 1 2 d DS T P . . H3A H 0.13800(9) 0.000000 -0.0098(3) 0.129 Uiso 1 2 d DS U P . . H3B H 0.22097(11) 0.000000 0.0272(2) 0.129 Uiso 1 2 d DS U P . . C7 C 0.3117(12) 1.000000 0.8007(17) 0.059(4) Uani 1 2 d S T P . . H7 H 0.325027 1.000000 0.753101 0.071 Uiso 1 2 calc R U P . . C8 C 0.2250(10) 1.000000 0.743(2) 0.064(5) Uani 1 2 d S T P . . C9 C 0.2090(12) 1.000000 0.8221(16) 0.065(5) Uani 1 2 d S T P . . H9 H 0.155147 1.000000 0.790539 0.078 Uiso 1 2 calc R U P . . C10 C 0.3469(11) 1.000000 0.9807(16) 0.054(4) Uani 1 2 d S T P . . H10 H 0.389163 1.000000 1.064279 0.065 Uiso 1 2 calc R U P . . C6 C 0.4796(5) 0.6895(9) 0.8250(7) 0.0283(16) Uani 1 1 d . . . . . C5 C 0.4911(5) 0.3104(9) 0.6486(7) 0.0269(15) Uani 1 1 d . . . . . C1 C 0.3236(11) 0.000000 0.2531(14) 0.049(4) Uani 1 2 d S T P . . H1 H 0.352047 0.000000 0.226792 0.058 Uiso 1 2 calc R U P . . C2 C 0.2319(10) 0.000000 0.1611(16) 0.052(4) Uani 1 2 d S T P . . C3 C 0.1951(14) 0.000000 0.2102(16) 0.070(6) Uani 1 2 d S T P . . H3 H 0.137947 0.000000 0.158169 0.084 Uiso 1 2 calc R U P . . C4 C 0.3216(13) 0.000000 0.4047(19) 0.069(5) Uani 1 2 d S T P . . H4 H 0.351731 0.000000 0.487335 0.083 Uiso 1 2 calc R U P . . O1 O 0.22653(13) 0.8841(3) 0.50080(17) 0.105(10) Uiso 0.4 1 d D . P A -1 H1A H 0.23673(15) 0.9632(4) 0.46612(17) 0.158 Uiso 0.4 1 d D U P B -1 H1B H 0.2182(4) 0.7748(3) 0.4674(4) 0.158 Uiso 0.4 1 d D U P C -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0346(2) 0.01497(17) 0.0262(2) 0.000 0.02357(19) 0.000 Fe2 0.0407(13) 0.0132(8) 0.0273(10) 0.000 0.0276(10) 0.000 Fe1 0.0431(13) 0.0139(8) 0.0268(10) 0.000 0.0287(10) 0.000 N6 0.064(8) 0.029(5) 0.037(6) 0.000 0.033(6) 0.000 N7 0.066(11) 0.087(12) 0.088(13) 0.000 0.062(10) 0.000 N8 0.072(13) 0.14(2) 0.080(13) 0.000 0.053(12) 0.000 N5 0.068(5) 0.023(3) 0.041(4) -0.001(3) 0.045(4) 0.001(3) N4 0.066(5) 0.025(3) 0.051(4) -0.004(3) 0.049(4) -0.001(3) N1 0.086(11) 0.038(6) 0.074(9) 0.000 0.068(9) 0.000 N2 0.076(12) 0.15(2) 0.105(15) 0.000 0.079(13) 0.000 N3 0.043(9) 0.148(19) 0.057(10) 0.000 0.030(8) 0.000 C7 0.075(12) 0.042(8) 0.066(11) 0.000 0.050(11) 0.000 C8 0.035(8) 0.053(9) 0.087(14) 0.000 0.034(10) 0.000 C9 0.045(9) 0.058(10) 0.043(9) 0.000 0.009(8) 0.000 C10 0.056(10) 0.069(10) 0.057(10) 0.000 0.046(9) 0.000 C6 0.047(5) 0.017(3) 0.029(4) -0.003(3) 0.029(4) -0.001(3) C5 0.042(5) 0.018(3) 0.032(4) 0.001(3) 0.030(4) 0.002(3) C1 0.071(11) 0.043(7) 0.052(9) 0.000 0.049(9) 0.000 C2 0.042(8) 0.055(9) 0.060(10) 0.000 0.035(8) 0.000 C3 0.083(14) 0.055(10) 0.039(9) 0.000 0.028(9) 0.000 C4 0.071(13) 0.094(15) 0.066(12) 0.000 0.056(11) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C6 1.975(7) . ? Pt1 C6 1.975(7) 6_565 ? Pt1 C5 1.983(7) 6_565 ? Pt1 C5 1.983(7) . ? Fe2 N6 2.239(14) 5_677 ? Fe2 N6 2.239(14) . ? Fe2 N5 2.127(7) 6_575 ? Fe2 N5 2.127(7) 2_657 ? Fe2 N5 2.127(7) 5_677 ? Fe2 N5 2.127(7) . ? Fe1 N4 2.136(7) . ? Fe1 N4 2.136(7) 5_656 ? Fe1 N4 2.136(7) 2_656 ? Fe1 N4 2.136(7) 6 ? Fe1 N1 2.205(16) . ? Fe1 N1 2.205(16) 5_656 ? N6 C7 1.24(2) . ? N6 C10 1.362(19) . ? N7 C9 1.25(2) . ? N7 C10 1.36(2) . ? N8 H8A 0.90000(12) . ? N8 H8A 0.90003(12) 6_575 ? N8 H8B 0.90000(12) . ? N8 C8 1.27(2) . ? N5 C6 1.151(10) . ? N4 C5 1.142(10) . ? N1 C1 1.26(2) . ? N1 C4 1.40(2) . ? N2 C3 1.328(18) . ? N2 C4 1.34(2) . ? N3 H3A 0.90000(13) . ? N3 H3B 0.90000(12) . ? N3 C2 1.233(18) . ? C7 H7 0.9300 . ? C7 C8 1.46(3) . ? C8 C9 1.44(3) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C1 H1 0.9300 . ? C1 C2 1.49(2) . ? C2 C3 1.40(3) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? O1 H1A 0.90000(11) . ? O1 H1B 0.90000(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Pt1 C6 90.1(4) . 6_565 ? C6 Pt1 C5 178.9(4) . . ? C6 Pt1 C5 90.1(3) 6_565 . ? C6 Pt1 C5 90.1(3) . 6_565 ? C6 Pt1 C5 178.9(4) 6_565 6_565 ? C5 Pt1 C5 89.7(4) . 6_565 ? N6 Fe2 N6 180.0 5_677 . ? N5 Fe2 N6 92.6(3) 2_657 5_677 ? N5 Fe2 N6 87.4(3) 5_677 . ? N5 Fe2 N6 92.6(3) 5_677 5_677 ? N5 Fe2 N6 87.4(3) 2_657 . ? N5 Fe2 N6 87.4(3) 6_575 5_677 ? N5 Fe2 N6 87.4(3) . 5_677 ? N5 Fe2 N6 92.6(3) . . ? N5 Fe2 N6 92.6(3) 6_575 . ? N5 Fe2 N5 180.0 6_575 2_657 ? N5 Fe2 N5 90.5(4) 5_677 6_575 ? N5 Fe2 N5 180.0 5_677 . ? N5 Fe2 N5 89.5(4) 5_677 2_657 ? N5 Fe2 N5 90.5(4) 2_657 . ? N5 Fe2 N5 89.5(4) 6_575 . ? N4 Fe1 N4 89.5(4) 5_656 2_656 ? N4 Fe1 N4 180.0 5_656 . ? N4 Fe1 N4 180.0 6 2_656 ? N4 Fe1 N4 90.5(4) 2_656 . ? N4 Fe1 N4 89.5(4) 6 . ? N4 Fe1 N4 90.5(4) 5_656 6 ? N4 Fe1 N1 88.8(3) . . ? N4 Fe1 N1 91.2(3) 2_656 . ? N4 Fe1 N1 91.2(3) 6 5_656 ? N4 Fe1 N1 88.8(3) 5_656 5_656 ? N4 Fe1 N1 91.2(3) . 5_656 ? N4 Fe1 N1 88.8(3) 2_656 5_656 ? N4 Fe1 N1 91.2(3) 5_656 . ? N4 Fe1 N1 88.8(3) 6 . ? N1 Fe1 N1 180.0 . 5_656 ? C7 N6 Fe2 120.8(12) . . ? C7 N6 C10 118.6(16) . . ? C10 N6 Fe2 120.6(11) . . ? C9 N7 C10 120.8(19) . . ? H8A N8 H8A 85.2(5) . 6_575 ? H8A N8 H8B 112.885(19) . . ? H8B N8 H8A 112.885(19) . 6_575 ? C8 N8 H8A 118.6(6) . 6_575 ? C8 N8 H8A 118.6(6) . . ? C8 N8 H8B 107.6(9) . . ? C6 N5 Fe2 171.0(8) . . ? C5 N4 Fe1 177.4(8) . . ? C1 N1 Fe1 122.3(12) . . ? C1 N1 C4 118.7(17) . . ? C4 N1 Fe1 118.9(13) . . ? C3 N2 C4 119.4(14) . . ? H3A N3 H3B 112.89(2) . . ? C2 N3 H3A 128.4(8) . . ? C2 N3 H3B 118.7(8) . . ? N6 C7 H7 119.5 . . ? N6 C7 C8 121.0(19) . . ? C8 C7 H7 119.5 . . ? N8 C8 C7 121.4(19) . . ? N8 C8 C9 122.2(15) . . ? C9 C8 C7 116.4(18) . . ? N7 C9 C8 119(2) . . ? N7 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? N6 C10 H10 118.1 . . ? N7 C10 N6 123.8(17) . . ? N7 C10 H10 118.1 . . ? N5 C6 Pt1 177.2(8) . . ? N4 C5 Pt1 178.4(7) . . ? N1 C1 H1 118.6 . . ? N1 C1 C2 122.8(15) . . ? C2 C1 H1 118.6 . . ? N3 C2 C1 122.1(14) . . ? N3 C2 C3 123.9(15) . . ? C3 C2 C1 114.0(16) . . ? N2 C3 C2 122.3(19) . . ? N2 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? N1 C4 H4 118.6 . . ? N2 C4 N1 122.8(17) . . ? N2 C4 H4 118.6 . . ? H1A O1 H1B 107.328(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe2 N6 C7 C8 180.000(10) . . . . ? Fe2 N6 C10 N7 180.000(12) . . . . ? Fe1 N1 C1 C2 180.000(3) . . . . ? Fe1 N1 C4 N2 180.000(3) . . . . ? N6 C7 C8 N8 180.000(12) . . . . ? N6 C7 C8 C9 0.000(15) . . . . ? N8 C8 C9 N7 180.000(9) . . . . ? N1 C1 C2 N3 180.000(4) . . . . ? N1 C1 C2 C3 0.000(5) . . . . ? N3 C2 C3 N2 180.000(2) . . . . ? C7 N6 C10 N7 0.000(17) . . . . ? C7 C8 C9 N7 0.000(14) . . . . ? C9 N7 C10 N6 0.000(17) . . . . ? C10 N6 C7 C8 0.000(14) . . . . ? C10 N7 C9 C8 0.000(13) . . . . ? C1 N1 C4 N2 0.000(7) . . . . ? C1 C2 C3 N2 0.000(3) . . . . ? C3 N2 C4 N1 0.000(7) . . . . ? C4 N1 C1 C2 0.000(5) . . . . ? C4 N2 C3 C2 0.000(4) . . . . ? _shelx_res_file ; TITL mo_rt327_5apdmpth2o_260k_0m_a.res in C2/m mo_rt327_5apdmpth2o_260k_0m.res created by SHELXL-2018/3 at 02:08:47 on 09-Sep-2020 REM Old TITL mo_RT327_5apdmPtH2O_260K_0m in C2/m REM SHELXT solution in C2/m REM R1 0.197, Rweak 0.032, Alpha 0.055, Orientation as input REM Formula found by SHELXT: C11 N5 O9 Pd I CELL 0.71073 21.836 7.3747 14.8914 90 131.952 90 ZERR 4 0.002 0.0006 0.0012 0 0.003 0 LATT 7 SYMM -X,+Y,-Z SFAC C H Fe N O Pt UNIT 48 46.4 4 40 3.2 4 EQIV $1 +X,1+Y,+Z DFIX 0.9 0.0001 N8 H8b DANG 2.21 0.0001 H8b O1 DFIX 0.9 0.0001 H8a N8 DFIX 0.9 0.0001 O1 H1a DFIX 0.9 0.0001 O1 H1b DANG 1.5 0.0001 H8a H8b DANG 1.45 0.0001 H1a H1b DANG 1.5 0.0001 H3b H3a DANG 2.1 0.0001 H1a N2_$1 DFIX 0.9 0.0001 H3b N3 DFIX 0.9 0.0001 H3a N3 L.S. 50 0 0 PLAN 80 SIZE 0.1 0.18 0.18 TEMP -13.13 CONF list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.068500 41.004303 FVAR 0.18814 PT1 6 0.484249 0.500000 0.735932 10.50000 0.03464 0.01497 = 0.02617 0.00000 0.02357 0.00000 FE2 3 0.500000 1.000000 1.000000 10.25000 0.04067 0.01317 = 0.02731 0.00000 0.02762 0.00000 FE1 3 0.500000 0.000000 0.500000 10.25000 0.04312 0.01391 = 0.02681 0.00000 0.02869 0.00000 N6 4 0.367632 1.000000 0.912412 10.50000 0.06365 0.02879 = 0.03687 0.00000 0.03348 0.00000 N7 4 0.268205 1.000000 0.933868 10.50000 0.06626 0.08679 = 0.08770 0.00000 0.06200 0.00000 N8 4 0.167602 1.000000 0.629098 10.50000 0.07214 0.13825 = 0.07987 0.00000 0.05261 0.00000 H8A 2 0.127096 0.917411 0.594740 10.50000 -1.50000 H8B 2 0.191007 1.000000 0.597258 10.50000 -1.50000 N5 4 0.479732 0.796872 0.881169 11.00000 0.06835 0.02337 = 0.04108 -0.00124 0.04462 0.00070 N4 4 0.496035 0.203962 0.597883 11.00000 0.06561 0.02480 = 0.05089 -0.00350 0.04948 -0.00053 N1 4 0.364231 0.000000 0.364984 10.50000 0.08625 0.03774 = 0.07370 0.00000 0.06778 0.00000 N2 4 0.239023 0.000000 0.328547 10.50000 0.07620 0.14707 = 0.10523 0.00000 0.07941 0.00000 N3 4 0.192953 0.000000 0.051904 10.50000 0.04348 0.14777 = 0.05682 0.00000 0.02962 0.00000 H3A 2 0.138004 0.000000 -0.009830 10.50000 -1.50000 H3B 2 0.220971 0.000000 0.027224 10.50000 -1.50000 C7 1 0.311677 1.000000 0.800747 10.50000 0.07496 0.04243 = 0.06627 0.00000 0.04956 0.00000 AFIX 43 H7 2 0.325027 1.000000 0.753101 10.50000 -1.20000 AFIX 0 C8 1 0.224993 1.000000 0.742870 10.50000 0.03539 0.05290 = 0.08697 0.00000 0.03399 0.00000 C9 1 0.208994 1.000000 0.822066 10.50000 0.04464 0.05829 = 0.04331 0.00000 0.00872 0.00000 AFIX 43 H9 2 0.155147 1.000000 0.790539 10.50000 -1.20000 AFIX 0 C10 1 0.346896 1.000000 0.980707 10.50000 0.05610 0.06893 = 0.05676 0.00000 0.04575 0.00000 AFIX 43 H10 2 0.389163 1.000000 1.064279 10.50000 -1.20000 AFIX 0 C6 1 0.479621 0.689494 0.824977 11.00000 0.04702 0.01669 = 0.02896 -0.00327 0.02857 -0.00108 C5 1 0.491141 0.310436 0.648551 11.00000 0.04218 0.01824 = 0.03246 0.00100 0.03002 0.00189 C1 1 0.323585 0.000000 0.253084 10.50000 0.07050 0.04312 = 0.05227 0.00000 0.04946 0.00000 AFIX 43 H1 2 0.352047 0.000000 0.226792 10.50000 -1.20000 AFIX 0 C2 1 0.231926 0.000000 0.161137 10.50000 0.04233 0.05497 = 0.06013 0.00000 0.03496 0.00000 C3 1 0.195100 0.000000 0.210249 10.50000 0.08342 0.05492 = 0.03864 0.00000 0.02751 0.00000 AFIX 43 H3 2 0.137947 0.000000 0.158169 10.50000 -1.20000 AFIX 0 C4 1 0.321645 0.000000 0.404704 10.50000 0.07087 0.09433 = 0.06559 0.00000 0.05558 0.00000 AFIX 43 H4 2 0.351731 0.000000 0.487335 10.50000 -1.20000 AFIX 0 PART -1 O1 5 0.226526 0.884142 0.500803 10.40000 0.10527 H1A 2 0.236732 0.963162 0.466116 10.40000 -1.50000 H1B 2 0.218237 0.774832 0.467369 10.40000 -1.50000 HKLF 4 REM mo_rt327_5apdmpth2o_260k_0m_a.res in C2/m REM wR2 = 0.1471, GooF = S = 1.038, Restrained GooF = 1.036 for all data REM R1 = 0.0544 for 2601 Fo > 4sig(Fo) and 0.0840 for all 3361 data REM 154 parameters refined using 11 restraints END WGHT 0.0685 40.9856 REM Highest difference peak 4.596, deepest hole -3.949, 1-sigma level 0.317 Q1 1 0.5465 0.5000 0.7918 10.50000 0.05 4.60 Q2 1 0.4805 0.5000 0.6834 10.50000 0.05 4.30 Q3 1 0.4400 0.5000 0.6827 10.50000 0.05 2.39 Q4 1 0.2399 1.0000 0.6427 10.50000 0.05 1.81 Q5 1 0.2796 0.0000 0.1144 10.50000 0.05 1.79 Q6 1 0.3005 1.0000 0.8638 10.50000 0.05 1.73 Q7 1 0.3790 0.0000 0.3201 10.50000 0.05 1.71 Q8 1 0.4184 0.5000 0.7202 10.50000 0.05 1.70 Q9 1 0.5403 0.5000 0.7295 10.50000 0.05 1.64 Q10 1 0.5392 0.6179 0.7778 11.00000 0.05 1.59 Q11 1 0.3897 0.5000 0.6314 10.50000 0.05 1.58 Q12 1 0.3851 1.0000 0.8728 10.50000 0.05 1.51 Q13 1 0.2991 0.0000 0.3065 10.50000 0.05 1.42 Q14 1 0.5249 0.4121 0.7129 11.00000 0.05 1.38 Q15 1 0.5329 0.5988 0.8164 11.00000 0.05 1.27 Q16 1 0.5428 0.5000 0.8515 10.50000 0.05 1.21 Q17 1 0.4835 0.5968 0.7999 11.00000 0.05 1.11 Q18 1 0.4359 0.5639 0.7450 11.00000 0.05 1.07 Q19 1 0.1560 0.0000 0.2254 10.50000 0.05 1.02 Q20 1 0.5047 0.0000 0.5514 10.50000 0.05 0.98 Q21 1 0.2546 1.0000 0.5412 10.50000 0.05 0.96 Q22 1 0.4407 0.4028 0.6438 11.00000 0.05 0.92 Q23 1 0.5611 0.7018 0.8396 11.00000 0.05 0.89 Q24 1 0.1019 0.8184 0.3564 11.00000 0.05 0.88 Q25 1 0.4653 0.0000 0.4574 10.50000 0.05 0.87 Q26 1 0.4974 0.5000 0.8211 10.50000 0.05 0.87 Q27 1 0.0788 1.0000 0.7433 10.50000 0.05 0.84 Q28 1 0.2404 0.0000 0.2197 10.50000 0.05 0.83 Q29 1 0.3359 1.0000 0.7020 10.50000 0.05 0.83 Q30 1 0.4375 0.0000 0.5006 10.50000 0.05 0.82 Q31 1 0.2658 0.0000 0.1731 10.50000 0.05 0.81 Q32 1 0.2015 0.6690 0.4581 11.00000 0.05 0.81 Q33 1 0.4204 0.0000 0.4007 10.50000 0.05 0.77 Q34 1 0.3991 1.0000 1.1663 10.50000 0.05 0.77 Q35 1 0.1009 0.9436 0.8085 11.00000 0.05 0.77 Q36 1 0.3046 1.0000 0.6243 10.50000 0.05 0.75 Q37 1 0.4585 1.0000 1.0214 10.50000 0.05 0.74 Q38 1 0.4204 1.1481 1.0020 11.00000 0.05 0.74 Q39 1 0.1231 0.0000 -0.1108 10.50000 0.05 0.74 Q40 1 0.5407 -0.0933 0.4988 11.00000 0.05 0.73 Q41 1 0.4380 1.0661 0.9813 11.00000 0.05 0.73 Q42 1 0.1548 1.0000 0.3999 10.50000 0.05 0.72 Q43 1 0.2217 0.2209 0.1003 11.00000 0.05 0.72 Q44 1 0.4403 1.0000 0.7832 10.50000 0.05 0.71 Q45 1 0.0787 -0.0391 0.1782 11.00000 0.05 0.71 Q46 1 0.1805 0.0000 0.1200 10.50000 0.05 0.71 Q47 1 0.3578 0.1675 0.3190 11.00000 0.05 0.70 Q48 1 0.0419 0.0000 -0.1068 10.50000 0.05 0.69 Q49 1 0.4575 0.1940 0.6026 11.00000 0.05 0.68 Q50 1 0.4224 0.5000 0.5992 10.50000 0.05 0.68 Q51 1 0.4407 0.3226 0.5940 11.00000 0.05 0.68 Q52 1 0.4383 1.0000 0.8415 10.50000 0.05 0.67 Q53 1 0.4404 1.0852 1.1813 11.00000 0.05 0.67 Q54 1 0.5206 0.6815 0.8589 11.00000 0.05 0.67 Q55 1 0.5021 0.7680 0.8632 11.00000 0.05 0.66 Q56 1 0.4401 1.0747 0.8980 11.00000 0.05 0.66 Q57 1 0.4806 0.3226 0.5785 11.00000 0.05 0.66 Q58 1 0.1798 1.0000 0.5170 10.50000 0.05 0.66 Q59 1 0.1213 0.9421 0.6565 11.00000 0.05 0.66 Q60 1 0.4423 0.1864 0.5183 11.00000 0.05 0.66 Q61 1 0.2212 0.7206 0.4341 11.00000 0.05 0.65 Q62 1 0.1236 1.0000 0.4385 10.50000 0.05 0.65 Q63 1 0.3594 1.2068 0.7629 11.00000 0.05 0.65 Q64 1 0.4413 0.3875 0.7146 11.00000 0.05 0.64 Q65 1 0.5765 0.6780 0.9408 11.00000 0.05 0.64 Q66 1 0.5420 0.3194 0.7192 11.00000 0.05 0.64 Q67 1 0.3734 -0.0533 0.2010 11.00000 0.05 0.64 Q68 1 0.0406 0.9419 0.5416 11.00000 0.05 0.63 Q69 1 0.2202 1.0000 0.4763 10.50000 0.05 0.62 Q70 1 0.2136 0.8465 0.4210 11.00000 0.05 0.62 Q71 1 0.4923 1.0000 0.9407 10.50000 0.05 0.62 Q72 1 0.4608 0.0000 0.3938 10.50000 0.05 0.62 Q73 1 0.5174 0.5000 0.6622 10.50000 0.05 0.62 Q74 1 0.1186 0.7256 0.5843 11.00000 0.05 0.62 Q75 1 0.0634 1.0000 0.5628 10.50000 0.05 0.61 Q76 1 0.2458 1.0000 0.8192 10.50000 0.05 0.61 Q77 1 0.2422 0.7202 0.5644 11.00000 0.05 0.60 Q78 1 0.1430 -0.0617 0.2655 11.00000 0.05 0.60 Q79 1 0.4400 0.2530 0.5546 11.00000 0.05 0.60 Q80 1 0.1783 1.0000 0.3394 10.50000 0.05 0.59 ; _shelx_res_checksum 9331 _olex2_submission_special_instructions 'No special instructions were received' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_rt174_nh2pymptmeoh_100k_3 _database_code_depnum_ccdc_archive 'CCDC 2018390' loop_ _audit_author_name _audit_author_address 'Carlos Bartual-Murgui' ;Universitat de Valencia Spain ; _audit_update_record ; 2020-09-17 deposited with the CCDC. 2020-09-22 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT971_rt174_nh2pymptmeoh_100k_3 ; PROBLEM: Check Calcd Resid. Dens. 1.01A From Pt1 9.40 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_rt174_nh2pymptmeoh_100k_3_2 ; PROBLEM: Check Calcd Resid. Dens. 0.68A From Pt1 8.57 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_rt174_nh2pymptmeoh_100k_3_3 ; PROBLEM: Check Calcd Resid. Dens. 1.40A From Pt1 8.39 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_rt174_nh2pymptmeoh_100k_3_4 ; PROBLEM: Check Calcd Resid. Dens. 0.98A From Pt2 6.81 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_rt174_nh2pymptmeoh_100k_3_5 ; PROBLEM: Check Calcd Resid. Dens. 1.10A From Pt2 6.29 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_rt174_nh2pymptmeoh_100k_3_6 ; PROBLEM: Check Calcd Resid. Dens. 1.01A From Pt2 5.55 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_rt174_nh2pymptmeoh_100k_3_7 ; PROBLEM: Check Calcd Resid. Dens. 1.56A From Pt2 5.49 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt174_nh2pymptmeoh_100k_3 ; PROBLEM: Check Calcd Resid. Dens. 1.34A From Pt2 -10.60 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT973_rt174_nh2pymptmeoh_100k_3 ; PROBLEM: Check Calcd Positive Resid. Density on Pt2 4.64 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_DIFMN02_rt174_nh2pymptmeoh_100k_3 ; PROBLEM: The minimum difference density is < -0.1*ZMAX*1.00 RESPONSE: The crystal may be damaged during the dehydration/readsorption/SCO processes. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT097_rt174_nh2pymptmeoh_100k_3 ; PROBLEM: Large Reported Max. (Positive) Residual Density 9.27 eA-3 RESPONSE: The crystal may be damaged during the dehydration/readsorption/SCO processes. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT098_rt174_nh2pymptmeoh_100k_3 ; PROBLEM: Large Reported Min. (Negative) Residual Density -8.37 eA-3 RESPONSE: The crystal may be damaged during the dehydration/readsorption/SCO processes. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT342_rt174_nh2pymptmeoh_100k_3 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.04375 Ang. RESPONSE: The crystal may be damaged during the dehydration/readsorption/SCO processes. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT910_rt174_nh2pymptmeoh_100k_3 ; PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 12 Note RESPONSE: The unit cell is relatively large and Mo radiation was used. Therefore several reflections were probably stopped by the beam stop. Nevertheless, this has not represented a problem to obtain good quality structural data ; _vrf_PLAT924_rt174_nh2pymptmeoh_100k_3 ; PROBLEM: The Reported and Calculated Rho(min) Differ by . 2.23 eA-3 RESPONSE: The crystal may be some twined or/and can be damaged during the dehydration/readsorption/SCO processes. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT971_rt174_nh2pymptmeoh_100k_3_8 ; PROBLEM: Check Calcd Resid. Dens. 1.34A From Pt1 3.40 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt174_nh2pymptmeoh_100k_3_2 ; PROBLEM: Check Calcd Resid. Dens. 1.08A From Pt2 -3.34 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt174_nh2pymptmeoh_100k_3_3 ; PROBLEM: Check Calcd Resid. Dens. 0.53A From Pt2 -3.26 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt174_nh2pymptmeoh_100k_3_4 ; PROBLEM: Check Calcd Resid. Dens. 0.14A From N3 -3.22 eA-3 RESPONSE: The residual electronic density may be due to the the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt174_nh2pymptmeoh_100k_3_5 ; PROBLEM: Check Calcd Resid. Dens. 0.27A From Pt1 -3.13 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt174_nh2pymptmeoh_100k_3_6 ; PROBLEM: Check Calcd Resid. Dens. 0.78A From Fe2 -2.95 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt174_nh2pymptmeoh_100k_3_7 ; PROBLEM: Check Calcd Resid. Dens. 0.95A From Pt1 -2.77 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt174_nh2pymptmeoh_100k_3_8 ; PROBLEM: Check Calcd Resid. Dens. 1.20A From C5 -2.60 eA-3 RESPONSE: The residual electronic density may be due to the the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT973_rt174_nh2pymptmeoh_100k_3_2 ; PROBLEM: Check Calcd Positive Resid. Density on Fe1 1.83 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; # Added during the CSD deposition process: Thursday 17 September 2020 12:29 PM # end Validation Reply Form _audit_creation_date 2020-09-09 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C12 H10 Fe N10 Pt, 0.5(C H4 O)' _chemical_formula_sum 'C12.50 H12 Fe N10 O0.50 Pt' _chemical_formula_weight 561.26 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system orthorhombic _space_group_IT_number 57 _space_group_name_H-M_alt 'P b c m' _space_group_name_Hall '-P 2c 2b' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y-1/2, z' _cell_length_a 14.8631(7) _cell_length_b 32.144(2) _cell_length_c 7.1639(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3422.6(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used 2210 _cell_measurement_temperature 100.0(8) _cell_measurement_theta_max 27.7750 _cell_measurement_theta_min 3.9890 _shelx_estimated_absorpt_T_max 0.840 _shelx_estimated_absorpt_T_min 0.465 _exptl_absorpt_coefficient_mu 9.035 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.60889 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 2.178 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 2120 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_unetI/netI 0.0632 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.850 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_number 9515 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.850 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.009 _diffrn_reflns_theta_min 3.336 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.0(8) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0267 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.850 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -76.00 -22.00 0.75 5.00 -- -14.97 -57.00 120.00 72 2 \w -14.00 14.50 0.75 5.00 -- 15.83 77.00 -30.00 38 3 \w 9.00 75.00 0.75 5.00 -- 15.83 38.00-120.00 88 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0191660000 _diffrn_orient_matrix_UB_12 0.0471746000 _diffrn_orient_matrix_UB_13 -0.0066454000 _diffrn_orient_matrix_UB_21 -0.0085674000 _diffrn_orient_matrix_UB_22 -0.0817718000 _diffrn_orient_matrix_UB_23 -0.0194360000 _diffrn_orient_matrix_UB_31 -0.0068379000 _diffrn_orient_matrix_UB_32 -0.0296244000 _diffrn_orient_matrix_UB_33 0.0430834000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3032 _reflns_number_total 3804 _reflns_odcompleteness_completeness 99.49 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 24.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 9.270 _refine_diff_density_min -8.372 _refine_diff_density_rms 0.464 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 131 _refine_ls_number_reflns 3804 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1159 _refine_ls_R_factor_gt 0.0979 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+553.5499P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1933 _refine_ls_wR_factor_ref 0.2026 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All N(H,H) groups, All O(H) groups 2. Restrained distances N3-H3B 0.9 with sigma of 0.0001 N3-H3A 0.9 with sigma of 0.0001 H14B_$1-N14_$1 0.9 with sigma of 0.0001 H14A_$1-N14_$1 0.9 with sigma of 0.0001 N11_$1-H11B_$1 0.9 with sigma of 0.0001 N11_$1-H11A_$1 0.9 with sigma of 0.0001 N8_$1-H8A_$1 0.9 with sigma of 0.0001 N8_$1-H8B_$1 0.9 with sigma of 0.0001 H3B_$1-H3A_$1 1.5 with sigma of 0.0001 H14B_$1-H14A_$1 1.5 with sigma of 0.0001 H11A_$1-H11B_$1 1.5 with sigma of 0.0001 H8B_$1-H8A_$1 1.5 with sigma of 0.0001 3. Uiso/Uaniso restraints and constraints Uanis(N6) = Uanis(C10) = Uanis(N7) = Uanis(C9) = Uanis(C8) = Uanis(N8) = Uanis(C7) = Uanis(N12) = Uanis(C18) = Uanis(N13) = Uanis(C17) = Uanis(C15) = Uanis(N14) = Uanis(N11) = Uanis(C12) = Uanis(C13) = Uanis(N10) = Uanis(C14) = Uanis(N9) = Uanis(C11) = Uanis(N1) = Uanis(C4) = Uanis(N2) = Uanis(C3) = Uanis(C2) = Uanis(C1) = Uanis(N3) Uanis(Fe1) = Uanis(N16) = Uanis(C20) = Uanis(Pt2) = Uanis(C19) = Uanis(N15) = Uanis(C6) = Uanis(Pt1) = Uanis(N4) = Uanis(C5) = Uanis(Fe2) = Uanis(N5) 4. Others Fixed Sof: H3A(0.5) H3B(0.5) H8A(0.5) H8B(0.5) H14A(0.5) H14B(0.5) O1(0.25) H1A(0.25) C21(0.25) H21A(0.25) H21B(0.25) H21C(0.25) O2(0.25) H2(0.25) C22(0.25) H22A(0.25) H22B(0.25) H22C(0.25) Fixed X: O1(0.001821) C21(-0.0001) O2(0.50464) C22(0.50367) Fixed Y: O1(0.237519) C21(0.239249) O2(0.51146) C22(0.50797) Fixed Z: O1(1.25) C21(1.06403) O2(1.25) C22(1.05438) 5.a Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C4(H4), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18) 5.b Idealised Me refined as rotating group: C21(H21A,H21B,H21C), C22(H22A,H22B,H22C) 5.c Idealised tetrahedral OH refined as rotating group: O1(H1A), O2(H2) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.99841(6) 0.36722(3) 0.750000 0.0075(2) Uani 1 2 d S T P . . Pt2 Pt 0.51569(5) 0.38440(3) 0.750000 0.0075(2) Uani 1 2 d S T P . . Fe1 Fe 0.2578(2) 0.37411(13) 1.250000 0.0075(2) Uani 1 2 d S T P . . Fe2 Fe 0.7575(2) 0.37747(13) 0.250000 0.0075(2) Uani 1 2 d S T P . . N1 N 0.2653(15) 0.3050(9) 1.250000 0.0227(12) Uani 1 2 d S T P . . N2 N 0.1883(15) 0.2429(8) 1.250000 0.0227(12) Uani 1 2 d S T P . . N3 N 0.4253(2) 0.22291(8) 1.250000 0.0227(12) Uani 1 2 d DS T P . . H3A H 0.4277(5) 0.19511(7) 1.2359(19) 0.034 Uiso 0.5 1 d D U P . . H3B H 0.4730(2) 0.23603(10) 1.1998(10) 0.034 Uiso 0.5 1 d D U P . . N4 N 1.1538(9) 0.3717(5) 0.457(2) 0.0075(2) Uani 1 1 d . . . . . N5 N 0.8489(9) 0.3689(4) 0.443(2) 0.0075(2) Uani 1 1 d . . . . . N6 N 0.7226(16) 0.3162(8) 0.250000 0.0227(12) Uani 1 2 d S T P . . N7 N 0.6030(15) 0.2676(8) 0.250000 0.0227(12) Uani 1 2 d S T P . . N8 N 0.8169(2) 0.21371(10) 0.250000 0.0227(12) Uani 1 2 d S T P . . H8A H 0.7977(3) 0.19023(9) 0.3057(9) 0.034 Uiso 0.5 1 d . U P . . H8B H 0.87090(19) 0.22219(13) 0.2920(11) 0.034 Uiso 0.5 1 d . U P . . N9 N 0.2444(15) 0.4426(9) 1.250000 0.0227(12) Uani 1 2 d S T P . . N10 N 0.3207(15) 0.5078(8) 1.250000 0.0227(12) Uani 1 2 d S T P . . N11 N 0.08468(19) 0.52772(7) 1.250000 0.0227(12) Uani 1 2 d S T P . . H11A H 0.0772(4) 0.55550(6) 1.250000 0.034 Uiso 1 2 d S U P . . H11B H 0.0322(2) 0.51374(9) 1.250000 0.034 Uiso 1 2 d S U P . . N12 N 0.7857(16) 0.4393(8) 0.250000 0.0227(12) Uani 1 2 d S T P . . N13 N 0.9053(15) 0.4902(8) 0.250000 0.0227(12) Uani 1 2 d S T P . . N14 N 0.6846(2) 0.54024(10) 0.250000 0.0227(12) Uani 1 2 d S T P . . H14A H 0.7066(3) 0.56444(9) 0.2936(10) 0.034 Uiso 0.5 1 d . U P . . H14B H 0.6374(2) 0.53086(12) 0.3166(7) 0.034 Uiso 0.5 1 d . U P . . N15 N 0.6667(8) 0.3867(5) 0.444(2) 0.0075(2) Uani 1 1 d . . . . . N16 N 0.3617(8) 0.3770(5) 1.045(2) 0.0075(2) Uani 1 1 d . . . . . C1 C 0.3430(19) 0.2865(10) 1.250000 0.0227(12) Uani 1 2 d S T P . . H1 H 0.396803 0.302433 1.250000 0.027 Uiso 1 2 calc R U P . . C2 C 0.3478(18) 0.2413(10) 1.250000 0.0227(12) Uani 1 2 d S T P . . C3 C 0.2654(18) 0.2239(11) 1.250000 0.0227(12) Uani 1 2 d S T P . . H3 H 0.263413 0.194338 1.250000 0.027 Uiso 1 2 calc R U P . . C4 C 0.1893(19) 0.2843(10) 1.250000 0.0227(12) Uani 1 2 d S T P . . H4 H 0.134038 0.299151 1.250000 0.027 Uiso 1 2 calc R U P . . C5 C 1.0962(10) 0.3695(5) 0.563(3) 0.0075(2) Uani 1 1 d . . . . . C6 C 0.9031(10) 0.3669(5) 0.550(3) 0.0075(2) Uani 1 1 d . . . . . C7 C 0.7867(19) 0.2875(10) 0.250000 0.0227(12) Uani 1 2 d S T P . . H7 H 0.848836 0.294330 0.250000 0.027 Uiso 1 2 calc R U P . . C8 C 0.7548(18) 0.2445(11) 0.250000 0.0227(12) Uani 1 2 d S T P . . C9 C 0.6632(18) 0.2374(10) 0.250000 0.0227(12) Uani 1 2 d S T P . . H9 H 0.642581 0.209444 0.250000 0.027 Uiso 1 2 calc R U P . . C10 C 0.6359(19) 0.3061(10) 0.250000 0.0227(12) Uani 1 2 d S T P . . H10 H 0.593707 0.328338 0.250000 0.027 Uiso 1 2 calc R U P . . C11 C 0.1652(19) 0.4637(10) 1.250000 0.0227(12) Uani 1 2 d S T P . . H11 H 0.110726 0.448188 1.250000 0.027 Uiso 1 2 calc R U P . . C12 C 0.1600(18) 0.5076(10) 1.250000 0.0227(12) Uani 1 2 d S T P . . C13 C 0.2426(18) 0.5279(11) 1.250000 0.0227(12) Uani 1 2 d S T P . . H13 H 0.243202 0.557491 1.250000 0.027 Uiso 1 2 calc R U P . . C14 C 0.3172(19) 0.4664(10) 1.250000 0.0227(12) Uani 1 2 d S T P . . H14 H 0.373383 0.452314 1.250000 0.027 Uiso 1 2 calc R U P . . C15 C 0.7279(19) 0.4676(10) 0.250000 0.0227(12) Uani 1 2 d S T P . . H15 H 0.665991 0.460261 0.250000 0.027 Uiso 1 2 calc R U P . . C16 C 0.753(2) 0.5108(9) 0.250000 0.018(6) Uani 1 2 d S T P . . C17 C 0.8420(18) 0.5194(10) 0.250000 0.0227(12) Uani 1 2 d S T P . . H17 H 0.860236 0.547712 0.250000 0.027 Uiso 1 2 calc R U P . . C18 C 0.8751(18) 0.4514(10) 0.250000 0.0227(12) Uani 1 2 d S T P . . H18 H 0.918880 0.429879 0.250000 0.027 Uiso 1 2 calc R U P . . C19 C 0.6112(10) 0.3876(5) 0.555(2) 0.0075(2) Uani 1 1 d . . . . . C20 C 0.4209(10) 0.3795(6) 0.943(2) 0.0075(2) Uani 1 1 d . . . . . O1 O 0.001821 0.237519 1.250000 0.066(19) Uiso 0.25 1 d S . P A -1 H1A H -0.004660 0.261563 1.293919 0.099 Uiso 0.25 1 calc R U P A -1 C21 C -0.000100 0.239249 1.064030 0.009(13) Uiso 0.25 1 d . . P A -1 H21A H -0.059175 0.230087 1.019291 0.013 Uiso 0.25 1 calc R U P A -1 H21B H 0.046652 0.221021 1.012888 0.013 Uiso 0.25 1 calc R U P A -1 H21C H 0.010811 0.267911 1.023263 0.013 Uiso 0.25 1 calc R U P A -1 O2 O 0.504640 0.511460 1.250000 0.055(16) Uiso 0.25 1 d S . P B -1 H2 H 0.504736 0.487596 1.297782 0.083 Uiso 0.25 1 calc R U P B -1 C22 C 0.503670 0.507970 1.054380 0.018(16) Uiso 0.25 1 d . . P B -1 H22A H 0.557010 0.521676 1.002571 0.026 Uiso 0.25 1 calc R U P B -1 H22B H 0.449348 0.521293 1.005006 0.026 Uiso 0.25 1 calc R U P B -1 H22C H 0.503975 0.478507 1.019210 0.026 Uiso 0.25 1 calc R U P B -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0046(3) 0.0144(4) 0.0035(3) 0.000 0.000 -0.0004(3) Pt2 0.0046(3) 0.0144(4) 0.0035(3) 0.000 0.000 -0.0004(3) Fe1 0.0046(3) 0.0144(4) 0.0035(3) 0.000 0.000 -0.0004(3) Fe2 0.0046(3) 0.0144(4) 0.0035(3) 0.000 0.000 -0.0004(3) N1 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) N2 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) N3 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) N4 0.0046(3) 0.0144(4) 0.0035(3) 0.000 0.000 -0.0004(3) N5 0.0046(3) 0.0144(4) 0.0035(3) 0.000 0.000 -0.0004(3) N6 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) N7 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) N8 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) N9 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) N10 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) N11 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) N12 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) N13 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) N14 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) N15 0.0046(3) 0.0144(4) 0.0035(3) 0.000 0.000 -0.0004(3) N16 0.0046(3) 0.0144(4) 0.0035(3) 0.000 0.000 -0.0004(3) C1 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) C2 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) C3 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) C4 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) C5 0.0046(3) 0.0144(4) 0.0035(3) 0.000 0.000 -0.0004(3) C6 0.0046(3) 0.0144(4) 0.0035(3) 0.000 0.000 -0.0004(3) C7 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) C8 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) C9 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) C10 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) C11 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) C12 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) C13 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) C14 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) C15 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) C16 0.026(15) 0.012(15) 0.017(15) 0.000 0.000 0.005(11) C17 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) C18 0.010(2) 0.027(3) 0.031(3) 0.000 0.000 -0.003(2) C19 0.0046(3) 0.0144(4) 0.0035(3) 0.000 0.000 -0.0004(3) C20 0.0046(3) 0.0144(4) 0.0035(3) 0.000 0.000 -0.0004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C5 1.980(17) . ? Pt1 C5 1.980(17) 6_557 ? Pt1 C6 2.013(17) 6_557 ? Pt1 C6 2.013(17) . ? Pt2 C19 1.995(16) 6_557 ? Pt2 C19 1.995(16) . ? Pt2 C20 1.980(16) 6_557 ? Pt2 C20 1.980(16) . ? Fe1 N1 2.22(3) . ? Fe1 N4 2.142(14) 1_456 ? Fe1 N4 2.142(14) 6_457 ? Fe1 N9 2.21(3) . ? Fe1 N16 2.134(14) 6_558 ? Fe1 N16 2.134(14) . ? Fe2 N5 1.959(14) . ? Fe2 N5 1.959(14) 6_556 ? Fe2 N6 2.04(3) . ? Fe2 N12 2.03(3) . ? Fe2 N15 1.959(14) . ? Fe2 N15 1.959(14) 6_556 ? N1 C1 1.30(4) . ? N1 C4 1.31(4) . ? N2 C3 1.30(4) . ? N2 C4 1.33(4) . ? N3 H3A 0.90000(12) . ? N3 H3A 0.90011(12) 6_558 ? N3 H3B 0.90000(12) . ? N3 H3B 0.90000(12) 6_558 ? N3 C2 1.29(3) . ? N4 C5 1.15(2) . ? N5 C6 1.11(2) . ? N6 C7 1.33(4) . ? N6 C10 1.33(3) . ? N7 C9 1.32(4) . ? N7 C10 1.33(4) . ? N8 H8A 0.90000(11) . ? N8 H8A 0.89995(11) 6_556 ? N8 H8B 0.90000(12) . ? N8 H8B 0.90001(12) 6_556 ? N8 C8 1.35(3) . ? N9 C11 1.36(4) . ? N9 C14 1.33(4) . ? N10 C13 1.33(4) . ? N10 C14 1.33(4) . ? N11 H11A 0.90000(12) . ? N11 H11B 0.90000(11) . ? N11 C12 1.29(3) . ? N12 C15 1.25(4) . ? N12 C18 1.38(3) . ? N13 C17 1.33(4) . ? N13 C18 1.33(4) . ? N14 H14A 0.90005(11) 6_556 ? N14 H14A 0.90000(11) . ? N14 H14B 0.90000(11) . ? N14 H14B 0.89999(11) 6_556 ? N14 C16 1.39(3) . ? N15 C19 1.15(2) . ? N16 C20 1.15(2) . ? C1 H1 0.9500 . ? C1 C2 1.45(4) . ? C2 C3 1.35(4) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C7 H7 0.9500 . ? C7 C8 1.46(4) . ? C8 C9 1.38(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C11 C12 1.41(4) . ? C12 C13 1.39(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C15 C16 1.44(4) . ? C16 C17 1.36(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? O1 H1A 0.8400 . ? O1 C21 1.33374(8) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? O2 H2 0.8400 . ? O2 C22 1.40596(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Pt1 C5 85.4(10) . 6_557 ? C5 Pt1 C6 92.0(6) 6_557 6_557 ? C5 Pt1 C6 92.0(6) . . ? C5 Pt1 C6 176.9(7) . 6_557 ? C5 Pt1 C6 176.9(7) 6_557 . ? C6 Pt1 C6 90.5(10) . 6_557 ? C19 Pt2 C19 88.9(9) 6_557 . ? C20 Pt2 C19 178.4(7) . . ? C20 Pt2 C19 91.3(7) 6_557 . ? C20 Pt2 C19 91.3(7) . 6_557 ? C20 Pt2 C19 178.4(7) 6_557 6_557 ? C20 Pt2 C20 88.5(9) . 6_557 ? N4 Fe1 N1 90.0(6) 1_456 . ? N4 Fe1 N1 90.0(6) 6_457 . ? N4 Fe1 N4 87.5(7) 6_457 1_456 ? N4 Fe1 N9 88.3(6) 1_456 . ? N4 Fe1 N9 88.3(6) 6_457 . ? N9 Fe1 N1 177.7(8) . . ? N16 Fe1 N1 90.4(6) 6_558 . ? N16 Fe1 N1 90.4(6) . . ? N16 Fe1 N4 92.7(5) 6_558 1_456 ? N16 Fe1 N4 92.7(5) . 6_457 ? N16 Fe1 N4 179.6(6) 6_558 6_457 ? N16 Fe1 N4 179.6(6) . 1_456 ? N16 Fe1 N9 91.3(6) . . ? N16 Fe1 N9 91.3(6) 6_558 . ? N16 Fe1 N16 87.1(7) . 6_558 ? N5 Fe2 N5 90.0(8) . 6_556 ? N5 Fe2 N6 92.3(6) . . ? N5 Fe2 N6 92.3(6) 6_556 . ? N5 Fe2 N12 89.7(6) 6_556 . ? N5 Fe2 N12 89.7(6) . . ? N5 Fe2 N15 89.9(6) 6_556 6_556 ? N5 Fe2 N15 89.9(6) . . ? N5 Fe2 N15 179.4(7) 6_556 . ? N5 Fe2 N15 179.4(7) . 6_556 ? N12 Fe2 N6 177.2(10) . . ? N15 Fe2 N6 88.3(6) . . ? N15 Fe2 N6 88.3(6) 6_556 . ? N15 Fe2 N12 89.7(7) . . ? N15 Fe2 N12 89.7(7) 6_556 . ? N15 Fe2 N15 90.3(8) . 6_556 ? C1 N1 Fe1 120(2) . . ? C1 N1 C4 122(3) . . ? C4 N1 Fe1 118(2) . . ? C3 N2 C4 117(3) . . ? H3A N3 H3A 12.9(18) . 6_558 ? H3A N3 H3B 112.885(19) . . ? H3A N3 H3B 112.881(19) 6_558 6_558 ? H3A N3 H3B 118.6(8) . 6_558 ? H3B N3 H3A 118.6(8) . 6_558 ? H3B N3 H3B 47.1(10) . 6_558 ? C2 N3 H3A 119.2(14) . 6_558 ? C2 N3 H3A 119.2(14) . . ? C2 N3 H3B 119.2(12) . 6_558 ? C2 N3 H3B 119.2(12) . . ? C5 N4 Fe1 177.3(14) . 1_654 ? C6 N5 Fe2 174.7(15) . . ? C7 N6 Fe2 119.4(19) . . ? C7 N6 C10 122(3) . . ? C10 N6 Fe2 119(2) . . ? C9 N7 C10 116(2) . . ? H8A N8 H8A 52.6(9) . 6_556 ? H8A N8 H8B 112.887(18) 6_556 6_556 ? H8A N8 H8B 112.885(18) . . ? H8A N8 H8B 133.2(6) . 6_556 ? H8B N8 H8A 133.2(6) . 6_556 ? H8B N8 H8B 39.0(10) . 6_556 ? C8 N8 H8A 113.4(12) . . ? C8 N8 H8A 113.4(12) . 6_556 ? C8 N8 H8B 112.8(12) . 6_556 ? C8 N8 H8B 112.8(12) . . ? C11 N9 Fe1 125(2) . . ? C14 N9 Fe1 120(2) . . ? C14 N9 C11 115(3) . . ? C13 N10 C14 117(3) . . ? H11A N11 H11B 112.885(19) . . ? C12 N11 H11A 127.1(14) . . ? C12 N11 H11B 120.1(14) . . ? C15 N12 Fe2 125(2) . . ? C15 N12 C18 117(3) . . ? C18 N12 Fe2 118(2) . . ? C18 N13 C17 115(2) . . ? H14A N14 H14A 40.6(9) . 6_556 ? H14A N14 H14B 112.888(18) 6_556 6_556 ? H14A N14 H14B 139.2(6) . 6_556 ? H14A N14 H14B 112.885(19) . . ? H14B N14 H14A 139.2(7) . 6_556 ? H14B N14 H14B 64.0(8) . 6_556 ? C16 N14 H14A 109.0(13) . . ? C16 N14 H14A 109.0(13) . 6_556 ? C16 N14 H14B 109.9(11) . 6_556 ? C16 N14 H14B 109.9(11) . . ? C19 N15 Fe2 172.5(15) . . ? C20 N16 Fe1 175.8(14) . . ? N1 C1 H1 119.9 . . ? N1 C1 C2 120(3) . . ? C2 C1 H1 119.9 . . ? N3 C2 C1 120(2) . . ? N3 C2 C3 128(3) . . ? C3 C2 C1 112(3) . . ? N2 C3 C2 127(3) . . ? N2 C3 H3 116.3 . . ? C2 C3 H3 116.3 . . ? N1 C4 N2 121(3) . . ? N1 C4 H4 119.4 . . ? N2 C4 H4 119.4 . . ? N4 C5 Pt1 178.1(16) . . ? N5 C6 Pt1 176.1(16) . . ? N6 C7 H7 122.4 . . ? N6 C7 C8 115(3) . . ? C8 C7 H7 122.4 . . ? N8 C8 C7 118(2) . . ? N8 C8 C9 123(3) . . ? C9 C8 C7 119(3) . . ? N7 C9 C8 123(3) . . ? N7 C9 H9 118.4 . . ? C8 C9 H9 118.4 . . ? N6 C10 N7 126(3) . . ? N6 C10 H10 117.2 . . ? N7 C10 H10 117.2 . . ? N9 C11 H11 118.5 . . ? N9 C11 C12 123(3) . . ? C12 C11 H11 118.5 . . ? N11 C12 C11 123(2) . . ? N11 C12 C13 122(3) . . ? C13 C12 C11 115(3) . . ? N10 C13 C12 123(3) . . ? N10 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? N9 C14 N10 127(3) . . ? N9 C14 H14 116.3 . . ? N10 C14 H14 116.3 . . ? N12 C15 H15 119.1 . . ? N12 C15 C16 122(3) . . ? C16 C15 H15 119.1 . . ? N14 C16 C15 118(2) . . ? C17 C16 N14 125(3) . . ? C17 C16 C15 117(3) . . ? N13 C17 C16 123(3) . . ? N13 C17 H17 118.3 . . ? C16 C17 H17 118.3 . . ? N12 C18 H18 116.9 . . ? N13 C18 N12 126(3) . . ? N13 C18 H18 116.9 . . ? N15 C19 Pt2 175.5(16) . . ? N16 C20 Pt2 175.3(14) . . ? C21 O1 H1A 109.5 . . ? O1 C21 H21A 109.5 . . ? O1 C21 H21B 109.5 . . ? O1 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22 O2 H2 109.5 . . ? O2 C22 H22A 109.5 . . ? O2 C22 H22B 109.5 . . ? O2 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 N1 C1 C2 180.0 . . . . ? Fe1 N1 C4 N2 180.0 . . . . ? Fe1 N9 C11 C12 180.0 . . . . ? Fe1 N9 C14 N10 180.0 . . . . ? Fe2 N6 C7 C8 180.0 . . . . ? Fe2 N6 C10 N7 180.0 . . . . ? Fe2 N12 C15 C16 180.0 . . . . ? Fe2 N12 C18 N13 180.0 . . . . ? N1 C1 C2 N3 180.0 . . . . ? N1 C1 C2 C3 0.0 . . . . ? N3 C2 C3 N2 180.0 . . . . ? N6 C7 C8 N8 180.0 . . . . ? N6 C7 C8 C9 0.0 . . . . ? N8 C8 C9 N7 180.0 . . . . ? N9 C11 C12 N11 180.0 . . . . ? N9 C11 C12 C13 0.0 . . . . ? N11 C12 C13 N10 180.0 . . . . ? N12 C15 C16 N14 180.0 . . . . ? N12 C15 C16 C17 0.0 . . . . ? N14 C16 C17 N13 180.0 . . . . ? C1 N1 C4 N2 0.0 . . . . ? C1 C2 C3 N2 0.0 . . . . ? C3 N2 C4 N1 0.0 . . . . ? C4 N1 C1 C2 0.0 . . . . ? C4 N2 C3 C2 0.0 . . . . ? C7 N6 C10 N7 0.0 . . . . ? C7 C8 C9 N7 0.0 . . . . ? C9 N7 C10 N6 0.0 . . . . ? C10 N6 C7 C8 0.0 . . . . ? C10 N7 C9 C8 0.0 . . . . ? C11 N9 C14 N10 0.0 . . . . ? C11 C12 C13 N10 0.0 . . . . ? C13 N10 C14 N9 0.0 . . . . ? C14 N9 C11 C12 0.0 . . . . ? C14 N10 C13 C12 0.0 . . . . ? C15 N12 C18 N13 0.0 . . . . ? C15 C16 C17 N13 0.0 . . . . ? C17 N13 C18 N12 0.0 . . . . ? C18 N12 C15 C16 0.0 . . . . ? C18 N13 C17 C16 0.0 . . . . ? _shelx_res_file ; TITL rt174_nh2pymptmeoh_100k_3_a.res in Pbcm rt174_nh2pymptmeoh_100k_3.res created by SHELXL-2018/3 at 11:35:24 on 09-Sep-2020 REM Old TITL RT174_NH2pymPtMeOH_100K_3 in Pmcm #51 REM SHELXT solution in Pbcm: R1 0.152, Rweak 0.008, Alpha 0.121 REM 2.203 for 206 systematic absences, Orientation a'=b, b'=c, c'=a REM Formula found by SHELXT: C35 N24 Fe2 Pt2 CELL 0.71073 14.8631 32.1439 7.1639 90 90 90 ZERR 8 0.0007 0.002 0.0004 0 0 0 LATT 1 SYMM -X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM +X,0.5-Y,-Z SFAC C H Fe N O Pt UNIT 100 96 8 80 4 8 EQIV $1 +X,+Y,1.5-Z EADP N6 C10 N7 C9 C8 N8 C7 N12 C18 N13 C17 C15 N14 N11 C12 C13 N10 C14 N9 = C11 N1 C4 N2 C3 C2 C1 N3 EADP Fe1 N16 C20 Pt2 C19 N15 C6 Pt1 N4 C5 Fe2 N5 DFIX 0.9 0.0001 N3 H3b DFIX 0.9 0.0001 N3 H3a DANG 1.5 0.0001 H3b_$1 H3a_$1 DANG 1.5 0.0001 H14b_$1 H14a_$1 DFIX 0.9 0.0001 H14b_$1 N14_$1 DFIX 0.9 0.0001 H14a_$1 N14_$1 DFIX 0.9 0.0001 N11_$1 H11b_$1 DFIX 0.9 0.0001 N11_$1 H11a_$1 DANG 1.5 0.0001 H11a_$1 H11b_$1 DANG 1.5 0.0001 H8b_$1 H8a_$1 DFIX 0.9 0.0001 N8_$1 H8a_$1 DFIX 0.9 0.0001 N8_$1 H8b_$1 L.S. 50 PLAN 5 SIZE 0.02 0.1 0.1 TEMP -173.1(8) CONF list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.000000 553.549866 FVAR 0.09092 PT1 6 0.998410 0.367224 0.750000 10.50000 0.00458 0.01435 = 0.00348 0.00000 0.00000 -0.00037 PT2 6 0.515687 0.384398 0.750000 10.50000 0.00458 0.01435 = 0.00348 0.00000 0.00000 -0.00037 FE1 3 0.257808 0.374109 1.250000 10.50000 0.00458 0.01435 = 0.00348 0.00000 0.00000 -0.00037 FE2 3 0.757516 0.377465 0.250000 10.50000 0.00458 0.01435 = 0.00348 0.00000 0.00000 -0.00037 N1 4 0.265295 0.305034 1.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 N2 4 0.188319 0.242850 1.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 N3 4 0.425251 0.222909 1.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 H3A 2 0.427671 0.195109 1.235932 10.50000 -1.50000 H3B 2 0.472964 0.236026 1.199799 10.50000 -1.50000 N4 4 1.153790 0.371692 0.456722 11.00000 0.00458 0.01435 = 0.00348 0.00000 0.00000 -0.00037 N5 4 0.848857 0.368866 0.443295 11.00000 0.00458 0.01435 = 0.00348 0.00000 0.00000 -0.00037 N6 4 0.722602 0.316241 0.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 N7 4 0.603002 0.267560 0.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 N8 4 0.816854 0.213707 0.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 H8A 2 0.797651 0.190231 0.305676 10.50000 -1.50000 H8B 2 0.870902 0.222185 0.291971 10.50000 -1.50000 N9 4 0.244378 0.442592 1.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 N10 4 0.320653 0.507821 1.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 N11 4 0.084676 0.527716 1.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 H11A 2 0.077239 0.555503 1.250000 10.50000 -1.50000 H11B 2 0.032204 0.513741 1.250000 10.50000 -1.50000 N12 4 0.785729 0.439251 0.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 N13 4 0.905278 0.490222 0.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 N14 4 0.684555 0.540235 0.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 H14A 2 0.706571 0.564444 0.293559 10.50000 -1.50000 H14B 2 0.637386 0.530860 0.316607 10.50000 -1.50000 N15 4 0.666693 0.386689 0.443877 11.00000 0.00458 0.01435 = 0.00348 0.00000 0.00000 -0.00037 N16 4 0.361672 0.376958 1.044808 11.00000 0.00458 0.01435 = 0.00348 0.00000 0.00000 -0.00037 C1 1 0.343030 0.286457 1.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 AFIX 43 H1 2 0.396803 0.302433 1.250000 10.50000 -1.20000 AFIX 0 C2 1 0.347766 0.241263 1.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 C3 1 0.265369 0.223879 1.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 AFIX 43 H3 2 0.263413 0.194338 1.250000 10.50000 -1.20000 AFIX 0 C4 1 0.189349 0.284341 1.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 AFIX 43 H4 2 0.134038 0.299151 1.250000 10.50000 -1.20000 AFIX 0 C5 1 1.096193 0.369508 0.562511 11.00000 0.00458 0.01435 = 0.00348 0.00000 0.00000 -0.00037 C6 1 0.903093 0.366933 0.550381 11.00000 0.00458 0.01435 = 0.00348 0.00000 0.00000 -0.00037 C7 1 0.786668 0.287464 0.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 AFIX 43 H7 2 0.848836 0.294330 0.250000 10.50000 -1.20000 AFIX 0 C8 1 0.754765 0.244534 0.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 C9 1 0.663239 0.237413 0.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 AFIX 43 H9 2 0.642581 0.209444 0.250000 10.50000 -1.20000 AFIX 0 C10 1 0.635902 0.306139 0.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 AFIX 43 H10 2 0.593707 0.328338 0.250000 10.50000 -1.20000 AFIX 0 C11 1 0.165166 0.463674 1.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 AFIX 43 H11 2 0.110726 0.448188 1.250000 10.50000 -1.20000 AFIX 0 C12 1 0.159978 0.507614 1.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 C13 1 0.242582 0.527937 1.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 AFIX 43 H13 2 0.243202 0.557491 1.250000 10.50000 -1.20000 AFIX 0 C14 1 0.317197 0.466403 1.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 AFIX 43 H14 2 0.373383 0.452314 1.250000 10.50000 -1.20000 AFIX 0 C15 1 0.727933 0.467550 0.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 AFIX 43 H15 2 0.665991 0.460261 0.250000 10.50000 -1.20000 AFIX 0 C16 1 0.752649 0.510799 0.250000 10.50000 0.02557 0.01227 = 0.01738 0.00000 0.00000 0.00539 C17 1 0.841996 0.519387 0.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 AFIX 43 H17 2 0.860236 0.547712 0.250000 10.50000 -1.20000 AFIX 0 C18 1 0.875052 0.451391 0.250000 10.50000 0.00971 0.02697 = 0.03132 0.00000 0.00000 -0.00263 AFIX 43 H18 2 0.918880 0.429879 0.250000 10.50000 -1.20000 AFIX 0 C19 1 0.611212 0.387599 0.554968 11.00000 0.00458 0.01435 = 0.00348 0.00000 0.00000 -0.00037 C20 1 0.420866 0.379536 0.942855 11.00000 0.00458 0.01435 = 0.00348 0.00000 0.00000 -0.00037 PART -1 O1 5 10.001821 10.237519 11.250000 10.25000 0.06615 AFIX 147 H1A 2 -0.004660 0.261563 1.293919 10.25000 -1.50000 AFIX 0 C21 1 9.999900 10.239249 11.064030 10.25000 0.00866 AFIX 137 H21A 2 -0.059175 0.230087 1.019291 10.25000 -1.50000 H21B 2 0.046652 0.221021 1.012888 10.25000 -1.50000 H21C 2 0.010811 0.267911 1.023263 10.25000 -1.50000 AFIX 0 O2 5 10.504640 10.511460 11.250000 10.25000 0.05543 AFIX 147 H2 2 0.504736 0.487596 1.297782 10.25000 -1.50000 AFIX 0 C22 1 10.503670 10.507970 11.054380 10.25000 0.01752 AFIX 137 H22A 2 0.557010 0.521676 1.002571 10.25000 -1.50000 H22B 2 0.449348 0.521293 1.005006 10.25000 -1.50000 H22C 2 0.503975 0.478507 1.019210 10.25000 -1.50000 AFIX 0 HKLF 4 REM rt174_nh2pymptmeoh_100k_3_a.res in Pbcm REM wR2 = 0.2026, GooF = S = 1.086, Restrained GooF = 1.084 for all data REM R1 = 0.0979 for 3032 Fo > 4sig(Fo) and 0.1159 for all 3804 data REM 131 parameters refined using 12 restraints END WGHT 0.0000 553.5228 REM Highest difference peak 9.270, deepest hole -8.372, 1-sigma level 0.464 Q1 1 1.0418 0.3606 0.7500 10.50000 0.05 9.27 Q2 1 1.0435 0.4029 0.7500 10.50000 0.05 7.32 Q3 1 1.0007 0.3365 0.7500 10.50000 0.05 7.09 Q4 1 0.4433 0.3815 0.7500 10.50000 0.05 4.72 Q5 1 0.4557 0.1600 1.2500 10.50000 0.05 4.17 ; _shelx_res_checksum 49664 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.637 _oxdiff_exptl_absorpt_empirical_full_min 0.579 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mo_rt327_5apmdpt_260kdes_0ma _database_code_depnum_ccdc_archive 'CCDC 2018381' loop_ _audit_author_name _audit_author_address 'Carlos Bartual-Murgui' ;Universitat de Valencia Spain ; _audit_update_record ; 2020-07-22 deposited with the CCDC. 2020-09-22 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT971_mo_rt327_5apmdpt_260kdes_0ma ; PROBLEM: Check Calcd Resid. Dens. 1.04A From Pt1 5.63 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration processes. ; _vrf_PLAT342_mo_rt327_5apmdpt_260kdes_0ma ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.035 Ang. RESPONSE: The crystal may be some twined or/and can be damaged during the dehydration process. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT972_mo_rt327_5apmdpt_260kdes_0ma ; PROBLEM: Check Calcd Resid. Dens. 1.92A From C10 -3.08 eA-3 RESPONSE: The residual electronic density may be due to a strong absorption of the C and the deterioration of the crystal during the dehydration/SCO processes. ; _vrf_PLAT972_mo_rt327_5apmdpt_260kdes_0ma_2 ; PROBLEM: Check Calcd Resid. Dens. 1.72A From C10 -2.65 eA-3 RESPONSE: The residual electronic density may be due to a strong absorption of the C and the deterioration of the crystal during the dehydration/SCO processes. ; # Added during the CSD deposition process: Wednesday 22 July 2020 04:49 PM # end Validation Reply Form _audit_creation_date 2019-11-20 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '0.5(C24 H20 Fe2 N20 Pt2)' _chemical_formula_sum 'C12 H10 Fe N10 Pt' _chemical_formula_weight 545.24 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_H-M_alt 'P n m a' _space_group_name_Hall '-P 2ac 2n' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.5857(6) _cell_length_b 7.3650(4) _cell_length_c 15.9543(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1713.87(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4331 _cell_measurement_temperature 260(2) _cell_measurement_theta_max 27.64 _cell_measurement_theta_min 2.55 _shelx_estimated_absorpt_T_max 0.466 _shelx_estimated_absorpt_T_min 0.294 _exptl_absorpt_coefficient_mu 9.016 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5382 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0983 before and 0.0636 after correction. The Ratio of minimum to maximum transmission is 0.7218. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 2.113 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1024 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.1 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_unetI/netI 0.0435 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 14384 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.724 _diffrn_reflns_theta_min 2.553 _diffrn_ambient_temperature 259.97 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1596 _reflns_number_total 2164 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 7.441 _refine_diff_density_min -3.285 _refine_diff_density_rms 0.292 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 135 _refine_ls_number_reflns 2164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0520 _refine_ls_restrained_S_all 1.190 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+43.7598P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1297 _refine_ls_wR_factor_ref 0.1557 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H,H) groups 2. Others Fixed Sof: H8A(0.5) H8B(0.5) H6A(0.5) H6B(0.5) 3.a Rotating group: N8(H8A,H8B), N6(H6A,H6B) 3.b Aromatic/amide H refined with riding coordinates: C5(H5), C7(H7), C8(H8), C1(H1), C3(H3), C4(H4) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.45856(4) 0.750000 0.76794(4) 0.0235(2) Uani 1 2 d S T P . . Fe1 Fe 0.21095(15) 0.250000 0.70499(15) 0.0242(5) Uani 1 2 d S T P . . N2 N 0.1970(10) 0.250000 0.8418(10) 0.036(4) Uani 1 2 d S T P . . N1 N 0.2375(10) 0.250000 0.5699(10) 0.036(3) Uani 1 2 d S T P . . N3 N 0.3136(7) 0.4556(15) 0.7212(7) 0.034(2) Uani 1 1 d . . . . . N4 N 0.6061(7) 1.0463(14) 0.8032(7) 0.034(2) Uani 1 1 d . . . . . N7 N 0.0984(17) 0.250000 0.9629(14) 0.074(7) Uani 1 2 d S T P . . N8 N 0.335(2) 0.250000 1.0342(17) 0.107(11) Uani 1 2 d S T P . . H8A H 0.358250 0.142840 1.035737 0.129 Uiso 0.5 1 d GR . . . . H8B H 0.374520 0.325131 1.014577 0.129 Uiso 0.5 1 d GR . . . . N5 N 0.1813(13) 0.250000 0.4299(12) 0.063(6) Uani 1 2 d S T P . . N6 N 0.4298(13) 0.250000 0.4269(13) 0.084(9) Uani 1 2 d S T P . . H6A H 0.465833 0.191369 0.461203 0.101 Uiso 0.5 1 d GR . . . . H6B H 0.433403 0.197921 0.377793 0.101 Uiso 0.5 1 d GR . . . . C5 C 0.2664(17) 0.250000 0.8943(14) 0.051(5) Uani 1 2 d S T P . . H5 H 0.325205 0.250000 0.871749 0.061 Uiso 1 2 calc RS T P . . C6 C 0.259(2) 0.250000 0.9806(16) 0.066(8) Uani 1 2 d S T P . . C7 C 0.172(3) 0.250000 1.0129(15) 0.074(9) Uani 1 2 d S T P . . H7 H 0.163953 0.250000 1.070780 0.089 Uiso 1 2 calc RS T P . . C8 C 0.1117(18) 0.250000 0.8810(15) 0.058(6) Uani 1 2 d S T P . . H8 H 0.060003 0.250000 0.846909 0.070 Uiso 1 2 calc RS T P . . C1 C 0.3219(13) 0.250000 0.5394(12) 0.038(4) Uani 1 2 d S T P . . H1 H 0.370672 0.250000 0.577030 0.045 Uiso 1 2 calc RS T P . . C2 C 0.3412(12) 0.250000 0.4560(11) 0.034(4) Uani 1 2 d S T P . . C3 C 0.2679(16) 0.250000 0.4022(14) 0.057(6) Uani 1 2 d S T P . . H3 H 0.278653 0.250000 0.344750 0.068 Uiso 1 2 calc RS T P . . C4 C 0.1708(15) 0.250000 0.5119(13) 0.048(5) Uani 1 2 d S T P . . H4 H 0.110795 0.250000 0.531764 0.057 Uiso 1 2 calc RS T P . . C9 C 0.3675(8) 0.5616(15) 0.7377(7) 0.026(2) Uani 1 1 d . . . . . C10 C 0.5524(7) 0.9400(17) 0.7929(8) 0.029(2) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0194(3) 0.0173(3) 0.0339(4) 0.000 -0.0008(3) 0.000 Fe1 0.0186(10) 0.0163(11) 0.0377(13) 0.000 0.0009(9) 0.000 N2 0.037(8) 0.015(7) 0.056(10) 0.000 -0.024(7) 0.000 N1 0.032(8) 0.033(9) 0.041(9) 0.000 -0.008(7) 0.000 N3 0.025(5) 0.029(6) 0.049(6) -0.004(5) -0.007(4) -0.001(4) N4 0.030(5) 0.022(5) 0.051(6) 0.000(5) -0.004(5) -0.012(4) N7 0.080(16) 0.089(18) 0.052(13) 0.000 0.032(12) 0.000 N8 0.14(3) 0.09(2) 0.10(2) 0.000 -0.07(2) 0.000 N5 0.036(10) 0.106(19) 0.047(11) 0.000 -0.010(8) 0.000 N6 0.040(11) 0.17(3) 0.044(11) 0.000 0.011(9) 0.000 C5 0.066(15) 0.043(13) 0.044(12) 0.000 0.001(11) 0.000 C6 0.11(2) 0.042(14) 0.044(13) 0.000 -0.017(14) 0.000 C7 0.13(3) 0.064(17) 0.029(11) 0.000 0.022(15) 0.000 C8 0.062(15) 0.057(15) 0.055(14) 0.000 0.022(12) 0.000 C1 0.029(9) 0.051(12) 0.034(10) 0.000 0.000(7) 0.000 C2 0.029(9) 0.046(11) 0.028(9) 0.000 0.004(7) 0.000 C3 0.054(14) 0.076(18) 0.039(12) 0.000 -0.006(10) 0.000 C4 0.040(11) 0.060(15) 0.043(11) 0.000 -0.002(9) 0.000 C9 0.026(5) 0.019(5) 0.034(6) 0.002(5) -0.005(5) -0.004(5) C10 0.018(5) 0.025(6) 0.043(6) 0.001(5) -0.005(4) 0.011(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C9 1.980(11) 7_575 ? Pt1 C9 1.980(11) . ? Pt1 C10 1.997(12) 7_575 ? Pt1 C10 1.997(12) . ? Fe1 N2 2.191(17) . ? Fe1 N1 2.189(16) . ? Fe1 N3 2.145(10) 7_565 ? Fe1 N3 2.145(10) . ? Fe1 N4 2.147(10) 6_547 ? Fe1 N4 2.147(10) 4_466 ? N2 C5 1.31(3) . ? N2 C8 1.39(3) . ? N1 C1 1.33(2) . ? N1 C4 1.34(3) . ? N3 C9 1.139(15) . ? N4 C10 1.120(15) . ? N7 C7 1.34(4) . ? N7 C8 1.32(3) . ? N8 C6 1.40(3) . ? N5 C3 1.34(3) . ? N5 C4 1.32(3) . ? N6 C2 1.37(2) . ? C5 C6 1.38(3) . ? C6 C7 1.37(4) . ? C1 C2 1.36(2) . ? C2 C3 1.37(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 Pt1 C9 89.0(7) 7_575 . ? C9 Pt1 C10 177.3(5) 7_575 7_575 ? C9 Pt1 C10 91.0(4) 7_575 . ? C9 Pt1 C10 91.0(4) . 7_575 ? C9 Pt1 C10 177.3(5) . . ? C10 Pt1 C10 88.9(6) . 7_575 ? N1 Fe1 N2 175.1(6) . . ? N3 Fe1 N2 86.8(4) 7_565 . ? N3 Fe1 N2 86.8(4) . . ? N3 Fe1 N1 89.7(4) 7_565 . ? N3 Fe1 N1 89.7(4) . . ? N3 Fe1 N3 89.8(6) 7_565 . ? N3 Fe1 N4 90.6(4) 7_565 6_547 ? N3 Fe1 N4 90.6(4) . 4_466 ? N3 Fe1 N4 176.5(4) . 6_547 ? N3 Fe1 N4 176.5(4) 7_565 4_466 ? N4 Fe1 N2 89.7(4) 6_547 . ? N4 Fe1 N2 89.7(4) 4_466 . ? N4 Fe1 N1 93.8(4) 4_466 . ? N4 Fe1 N1 93.8(4) 6_547 . ? N4 Fe1 N4 88.7(6) 6_547 4_466 ? C5 N2 Fe1 124.3(15) . . ? C5 N2 C8 113.6(19) . . ? C8 N2 Fe1 122.0(14) . . ? C1 N1 Fe1 121.7(12) . . ? C1 N1 C4 114.9(17) . . ? C4 N1 Fe1 123.4(14) . . ? C9 N3 Fe1 173.5(11) . . ? C10 N4 Fe1 168.0(11) . 6_667 ? C8 N7 C7 118(2) . . ? C4 N5 C3 116.0(19) . . ? N2 C5 C6 125(2) . . ? C5 C6 N8 123(3) . . ? C7 C6 N8 120(3) . . ? C7 C6 C5 117(3) . . ? N7 C7 C6 121(2) . . ? N7 C8 N2 125(2) . . ? N1 C1 C2 123.4(17) . . ? C1 C2 N6 121.7(18) . . ? C1 C2 C3 116.9(18) . . ? C3 C2 N6 121.5(18) . . ? N5 C3 C2 122(2) . . ? N5 C4 N1 127(2) . . ? N3 C9 Pt1 178.4(11) . . ? N4 C10 Pt1 176.9(12) . . ? _shelx_res_file ; TITL mo_rt327_5apmdpt_260kdes_0ma_a.res in Pnma mo_rt327_5apmdpt_260kdes_0ma.res created by SHELXL-2018/3 at 13:59:37 on 20-Nov-2019 REM Old TITL mo_RT327_5apmdPt_260Kdes_0ma in Pnma REM SHELXT solution in Pnma REM R1 0.116, Rweak 0.002, Alpha 0.035, Orientation as input REM Formula found by SHELXT: C10 N5 Fe Pt CELL 0.71073 14.5857 7.365 15.9543 90 90 90 ZERR 4 0.0006 0.0004 0.0008 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,-Z SYMM 0.5+X,0.5-Y,0.5-Z SFAC C H Fe N Pt UNIT 48 40 4 40 4 L.S. 20 0 0 PLAN 20 SIZE 0.1 0.18 0.18 TEMP -13.18 list 4 fmap 2 53 acta REM REM REM WGHT 0.052300 43.759800 FVAR 0.19156 PT1 5 0.458559 0.750000 0.767936 10.50000 0.01936 0.01726 = 0.03386 0.00000 -0.00084 0.00000 FE1 3 0.210951 0.250000 0.704990 10.50000 0.01856 0.01635 = 0.03769 0.00000 0.00091 0.00000 N2 4 0.197036 0.250000 0.841755 10.50000 0.03727 0.01511 = 0.05587 0.00000 -0.02393 0.00000 N1 4 0.237452 0.250000 0.569940 10.50000 0.03193 0.03331 = 0.04132 0.00000 -0.00759 0.00000 N3 4 0.313564 0.455602 0.721181 11.00000 0.02550 0.02871 = 0.04913 -0.00355 -0.00704 -0.00117 N4 4 0.606079 1.046266 0.803231 11.00000 0.02976 0.02191 = 0.05104 0.00033 -0.00355 -0.01175 N7 4 0.098437 0.250000 0.962936 10.50000 0.07994 0.08885 = 0.05185 0.00000 0.03155 0.00000 N8 4 0.334690 0.250000 1.034187 10.50000 0.13649 0.08871 = 0.09727 0.00000 -0.07117 0.00000 AFIX 7 H8A 2 0.358250 0.142840 1.035737 10.50000 -1.20000 H8B 2 0.374520 0.325131 1.014577 10.50000 -1.20000 AFIX 0 N5 4 0.181268 0.250000 0.429889 10.50000 0.03631 0.10636 = 0.04740 0.00000 -0.00995 0.00000 N6 4 0.429773 0.250000 0.426894 10.50000 0.03965 0.16790 = 0.04382 0.00000 0.01051 0.00000 AFIX 7 H6A 2 0.465833 0.191369 0.461203 10.50000 -1.20000 H6B 2 0.433403 0.197921 0.377793 10.50000 -1.20000 AFIX 0 C5 1 0.266427 0.250000 0.894342 10.50000 0.06611 0.04278 = 0.04419 0.00000 0.00062 0.00000 AFIX 43 H5 2 0.325205 0.250000 0.871749 10.50000 -1.20000 AFIX 0 C6 1 0.258616 0.250000 0.980552 10.50000 0.11153 0.04195 = 0.04352 0.00000 -0.01704 0.00000 C7 1 0.171952 0.250000 1.012949 10.50000 0.12831 0.06400 = 0.02932 0.00000 0.02176 0.00000 AFIX 43 H7 2 0.163953 0.250000 1.070780 10.50000 -1.20000 AFIX 0 C8 1 0.111688 0.250000 0.881044 10.50000 0.06210 0.05729 = 0.05468 0.00000 0.02184 0.00000 AFIX 43 H8 2 0.060003 0.250000 0.846909 10.50000 -1.20000 AFIX 0 C1 1 0.321949 0.250000 0.539429 10.50000 0.02869 0.05113 = 0.03389 0.00000 -0.00044 0.00000 AFIX 43 H1 2 0.370672 0.250000 0.577030 10.50000 -1.20000 AFIX 0 C2 1 0.341164 0.250000 0.455997 10.50000 0.02909 0.04595 = 0.02815 0.00000 0.00406 0.00000 C3 1 0.267866 0.250000 0.402201 10.50000 0.05414 0.07616 = 0.03950 0.00000 -0.00563 0.00000 AFIX 43 H3 2 0.278653 0.250000 0.344750 10.50000 -1.20000 AFIX 0 C4 1 0.170757 0.250000 0.511944 10.50000 0.03968 0.06046 = 0.04255 0.00000 -0.00160 0.00000 AFIX 43 H4 2 0.110795 0.250000 0.531764 10.50000 -1.20000 AFIX 0 C9 1 0.367491 0.561588 0.737717 11.00000 0.02572 0.01875 = 0.03442 0.00176 -0.00517 -0.00376 C10 1 0.552383 0.939960 0.792870 11.00000 0.01822 0.02547 = 0.04262 0.00087 -0.00470 0.01095 HKLF 4 REM mo_rt327_5apmdpt_260kdes_0ma_a.res in Pnma REM wR2 = 0.1557, GooF = S = 1.190, Restrained GooF = 1.190 for all data REM R1 = 0.0520 for 1596 Fo > 4sig(Fo) and 0.0854 for all 2164 data REM 135 parameters refined using 0 restraints END WGHT 0.0519 44.0294 REM Highest difference peak 7.441, deepest hole -3.285, 1-sigma level 0.292 Q1 1 0.4600 0.7500 0.6956 10.50000 0.05 7.44 Q2 1 0.2090 0.2500 0.7640 10.50000 0.05 1.93 Q3 1 0.4216 0.2500 0.2849 10.50000 0.05 1.43 Q4 1 0.4544 0.7500 0.8277 10.50000 0.05 1.42 Q5 1 0.4827 0.6144 0.7135 11.00000 0.05 1.30 Q6 1 0.5440 0.2500 0.3521 10.50000 0.05 1.29 Q7 1 0.4288 0.6229 0.7173 11.00000 0.05 1.24 Q8 1 0.5216 0.8260 0.7128 11.00000 0.05 1.20 Q9 1 0.5242 0.7500 0.7055 10.50000 0.05 1.18 Q10 1 0.5959 0.8302 0.7200 11.00000 0.05 1.14 Q11 1 0.3994 0.6865 0.7022 11.00000 0.05 1.08 Q12 1 0.3780 0.2500 0.7984 10.50000 0.05 1.03 Q13 1 0.5792 0.7500 0.8218 10.50000 0.05 1.03 Q14 1 0.2043 0.2500 0.3069 10.50000 0.05 1.03 Q15 1 0.3872 0.7500 0.7199 10.50000 0.05 1.03 Q16 1 0.3216 0.2500 0.2663 10.50000 0.05 1.00 Q17 1 0.6641 0.7756 0.8172 11.00000 0.05 1.00 Q18 1 0.6765 0.7500 0.7974 10.50000 0.05 0.99 Q19 1 0.3372 0.2054 0.2776 11.00000 0.05 0.96 Q20 1 0.4942 0.9151 0.7786 11.00000 0.05 0.95 ; _shelx_res_checksum 48806 _olex2_submission_special_instructions 'No special instructions were received' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_rt235_fe5apympd_180k_0m _database_code_depnum_ccdc_archive 'CCDC 2018392' loop_ _audit_author_name _audit_author_address 'Carlos Bartual-Murgui' ;Universitat de Valencia Spain ; _audit_update_record ; 2020-09-17 deposited with the CCDC. 2020-09-22 downloaded from the CCDC. ; # publcif _publ_body_element loop end _audit_creation_date 2020-09-09 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _shelx_SHELXL_version_number 2018/3 _publcif_funding_html ; ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C12 H10 Fe N10 Pd, H2 O' _chemical_formula_sum 'C12 H12 Fe N10 O Pd' _chemical_formula_weight 474.57 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_H-M_alt 'C 1 2/m 1' _space_group_name_Hall '-C 2y' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 21.454(3) _cell_length_b 7.1986(8) _cell_length_c 14.7221(16) _cell_angle_alpha 90 _cell_angle_beta 131.494(3) _cell_angle_gamma 90 _cell_volume 1703.0(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3862 _cell_measurement_temperature 180.01 _cell_measurement_theta_max 29.59 _cell_measurement_theta_min 2.53 _shelx_estimated_absorpt_T_max 0.910 _shelx_estimated_absorpt_T_min 0.699 _exptl_absorpt_coefficient_mu 1.932 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_correction_T_min 0.5121 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1086 before and 0.0724 after correction. The Ratio of minimum to maximum transmission is 0.6865. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.851 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 936 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_unetI/netI 0.0547 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.937 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 10741 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.937 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.971 _diffrn_reflns_theta_min 2.535 _diffrn_ambient_temperature 180.01 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.937 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1942 _reflns_number_total 2496 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _refine_diff_density_max 2.003 _refine_diff_density_min -1.608 _refine_diff_density_rms 0.230 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 156 _refine_ls_number_reflns 2496 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0564 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+42.1677P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1276 _refine_ls_wR_factor_ref 0.1593 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H,H) groups At 1.5 times of: All O(H,H) groups 2. Restrained distances O1-H1b 0.9 with sigma of 0.0001 H8b_$1-N8 0.9 with sigma of 0.0001 N8-H8a 0.9 with sigma of 0.0001 O1-H1a 0.9 with sigma of 0.0001 H3b-N3 0.9 with sigma of 0.0001 N3-H3a 0.9 with sigma of 0.0001 H8a-H8b_$1 1.5 with sigma of 0.0001 H8a-O1_$2 2.1 with sigma of 0.0001 H1b-H1a 1.45 with sigma of 0.0001 H1b-N2 2 with sigma of 0.0001 H3b-H3a 1.5 with sigma of 0.0001 3. Others Fixed Sof: O1(0.5) H1a(0.5) H1b(0.5) H3a(0.5) H3b(0.5) H8b(0.5) 4.a Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C4(H4), C7(H7), C9(H9), C10(H10) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.51479(4) 0.500000 0.77095(6) 0.02099(19) Uani 1 2 d S T P . . Fe1 Fe 0.500000 1.000000 1.000000 0.0193(3) Uani 1 4 d S T P . . Fe2 Fe 0.500000 0.000000 0.500000 0.0196(3) Uani 1 4 d S T P . . O1 O 0.22793(13) 1.1108(4) 1.01296(15) 0.079(4) Uiso 0.5 1 d D . P A -1 H1A H 0.2624(3) 1.2093(4) 1.0449(3) 0.119 Uiso 0.5 1 d D U P B -1 H1B H 0.21867(15) 1.0765(6) 0.94610(15) 0.119 Uiso 0.5 1 d D U P C -1 N1 N 0.3742(5) 1.000000 0.8817(7) 0.0268(15) Uani 1 2 d S T P . . N2 N 0.25173(17) 1.000000 0.8525(2) 0.044(2) Uani 1 2 d DS T P . . N3 N 0.19546(13) 1.000000 0.5612(2) 0.050(3) Uani 1 2 d DS T P . . H3A H 0.22641(11) 0.981(2) 0.5410(2) 0.060 Uiso 0.5 1 d D U P . . H3B H 0.14316(13) 0.9568(9) 0.5051(4) 0.060 Uiso 0.5 1 d D U P . . N4 N 0.4999(3) 0.8076(7) 0.9067(4) 0.0238(10) Uani 1 1 d . . . . . N5 N 0.5242(4) 0.2062(7) 0.6239(5) 0.0288(11) Uani 1 1 d . . . . . N6 N 0.3696(5) 0.000000 0.4201(7) 0.0284(16) Uani 1 2 d S T P . . N7 N 0.2710(6) 0.000000 0.4475(8) 0.045(2) Uani 1 2 d S T P . . N8 N 0.16163(12) 0.000000 0.1272(2) 0.059(3) Uani 1 2 d DS T P . . H8A H 0.18913(10) 0.000000 0.10048(15) 0.071 Uiso 1 2 d DS U P . . H8B H 0.12546(14) -0.0949(3) 0.0973(3) 0.071 Uiso 0.5 1 d . U P . . C1 C 0.3296(6) 1.000000 0.7633(8) 0.0285(18) Uani 1 2 d S T P . . H1 H 0.356889 1.000000 0.732386 0.034 Uiso 1 2 calc R U P . . C2 C 0.2415(7) 1.000000 0.6817(9) 0.036(2) Uani 1 2 d S T P . . C3 C 0.2045(7) 1.000000 0.7332(10) 0.038(2) Uani 1 2 d S T P . . H3 H 0.145606 1.000000 0.682033 0.046 Uiso 1 2 calc R U P . . C4 C 0.3343(7) 1.000000 0.9227(10) 0.037(2) Uani 1 2 d S T P . . H4 H 0.367113 1.000000 1.008049 0.044 Uiso 1 2 calc R U P . . C5 C 0.5044(4) 0.6969(7) 0.8557(5) 0.0205(11) Uani 1 1 d . . . . . C6 C 0.5224(4) 0.3088(8) 0.6813(5) 0.0222(11) Uani 1 1 d . . . . . C7 C 0.3086(7) 0.000000 0.3025(9) 0.034(2) Uani 1 2 d S T P . . H7 H 0.321339 0.000000 0.251853 0.041 Uiso 1 2 calc R U P . . C8 C 0.2242(6) 0.000000 0.2483(9) 0.034(2) Uani 1 2 d S T P . . C9 C 0.2099(7) 0.000000 0.3279(10) 0.040(2) Uani 1 2 d S T P . . H9 H 0.154054 0.000000 0.295068 0.048 Uiso 1 2 calc R U P . . C10 C 0.3491(7) 0.000000 0.4895(10) 0.041(2) Uani 1 2 d S T P . . H10 H 0.393544 0.000000 0.574957 0.049 Uiso 1 2 calc R U P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0312(4) 0.0134(3) 0.0246(3) 0.000 0.0211(3) 0.000 Fe1 0.0336(9) 0.0101(7) 0.0258(8) 0.000 0.0246(8) 0.000 Fe2 0.0350(9) 0.0096(7) 0.0270(8) 0.000 0.0259(8) 0.000 N1 0.035(4) 0.022(4) 0.032(4) 0.000 0.026(4) 0.000 N2 0.035(5) 0.053(6) 0.042(5) 0.000 0.025(4) 0.000 N3 0.036(5) 0.082(8) 0.035(5) 0.000 0.025(5) 0.000 N4 0.040(3) 0.014(2) 0.027(2) 0.0006(18) 0.027(2) -0.001(2) N5 0.044(3) 0.021(3) 0.033(3) -0.003(2) 0.030(3) -0.003(2) N6 0.026(4) 0.026(4) 0.032(4) 0.000 0.018(3) 0.000 N7 0.039(5) 0.064(7) 0.040(5) 0.000 0.030(5) 0.000 N8 0.044(6) 0.088(9) 0.045(6) 0.000 0.029(5) 0.000 C1 0.043(5) 0.020(4) 0.034(4) 0.000 0.030(4) 0.000 C2 0.039(6) 0.028(5) 0.033(5) 0.000 0.021(5) 0.000 C3 0.037(6) 0.043(6) 0.041(5) 0.000 0.028(5) 0.000 C4 0.046(6) 0.037(5) 0.041(5) 0.000 0.035(5) 0.000 C5 0.034(3) 0.013(2) 0.022(2) -0.0022(19) 0.021(3) -0.001(2) C6 0.032(3) 0.015(2) 0.028(3) 0.003(2) 0.024(3) 0.003(2) C7 0.051(6) 0.020(4) 0.039(5) 0.000 0.033(5) 0.000 C8 0.032(5) 0.032(5) 0.036(5) 0.000 0.022(5) 0.000 C9 0.034(5) 0.042(6) 0.044(6) 0.000 0.026(5) 0.000 C10 0.038(6) 0.045(6) 0.039(5) 0.000 0.025(5) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C5 1.997(5) 6_565 ? Pd1 C5 1.997(5) . ? Pd1 C6 1.987(6) 6_565 ? Pd1 C6 1.987(6) . ? Fe1 N1 2.022(8) 5_677 ? Fe1 N1 2.022(8) . ? Fe1 N4 1.950(5) 6_575 ? Fe1 N4 1.950(5) 2_657 ? Fe1 N4 1.950(5) . ? Fe1 N4 1.950(5) 5_677 ? Fe2 N5 2.132(5) 5_656 ? Fe2 N5 2.132(5) . ? Fe2 N5 2.132(5) 2_656 ? Fe2 N5 2.132(5) 6 ? Fe2 N6 2.203(8) 5_656 ? Fe2 N6 2.203(8) . ? O1 H1A 0.90000(15) . ? O1 H1B 0.90000(14) . ? N1 C1 1.321(11) . ? N1 C4 1.335(12) . ? N2 C3 1.324(11) . ? N2 C4 1.335(11) . ? N3 H3A 0.90003(18) 6_575 ? N3 H3A 0.90000(16) . ? N3 H3B 0.90000(15) . ? N3 H3B 0.90003(14) 6_575 ? N3 C2 1.342(10) . ? N4 C5 1.141(7) . ? N5 C6 1.142(8) . ? N6 C7 1.307(12) . ? N6 C10 1.352(13) . ? N7 C9 1.327(14) . ? N7 C10 1.349(14) . ? N8 H8A 0.90000(13) . ? N8 H8B 0.90000(13) 6 ? N8 H8B 0.90000(13) . ? N8 C8 1.345(10) . ? C1 H1 0.9500 . ? C1 C2 1.417(14) . ? C2 C3 1.414(15) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C7 H7 0.9500 . ? C7 C8 1.413(15) . ? C8 C9 1.395(14) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Pd1 C5 90.4(3) 6_565 . ? C6 Pd1 C5 178.0(2) . . ? C6 Pd1 C5 178.0(2) 6_565 6_565 ? C6 Pd1 C5 90.9(2) 6_565 . ? C6 Pd1 C5 90.9(2) . 6_565 ? C6 Pd1 C6 87.6(3) 6_565 . ? N1 Fe1 N1 180.0(4) 5_677 . ? N4 Fe1 N1 89.1(2) 6_575 5_677 ? N4 Fe1 N1 90.9(2) 5_677 5_677 ? N4 Fe1 N1 90.9(2) . . ? N4 Fe1 N1 89.1(2) 2_657 . ? N4 Fe1 N1 90.9(2) 2_657 5_677 ? N4 Fe1 N1 89.1(2) . 5_677 ? N4 Fe1 N1 90.9(2) 6_575 . ? N4 Fe1 N1 89.1(2) 5_677 . ? N4 Fe1 N4 89.5(3) 5_677 6_575 ? N4 Fe1 N4 180.0 6_575 2_657 ? N4 Fe1 N4 90.5(3) . 6_575 ? N4 Fe1 N4 90.5(3) 5_677 2_657 ? N4 Fe1 N4 89.5(3) . 2_657 ? N4 Fe1 N4 180.0(3) . 5_677 ? N5 Fe2 N5 180.0 6 2_656 ? N5 Fe2 N5 91.7(3) 5_656 6 ? N5 Fe2 N5 88.3(3) 5_656 2_656 ? N5 Fe2 N5 180.0 5_656 . ? N5 Fe2 N5 88.3(3) 6 . ? N5 Fe2 N5 91.7(3) 2_656 . ? N5 Fe2 N6 87.7(2) 5_656 5_656 ? N5 Fe2 N6 87.7(2) 2_656 5_656 ? N5 Fe2 N6 87.7(2) 6 . ? N5 Fe2 N6 92.3(2) 2_656 . ? N5 Fe2 N6 87.7(2) . . ? N5 Fe2 N6 92.3(2) . 5_656 ? N5 Fe2 N6 92.3(2) 6 5_656 ? N5 Fe2 N6 92.3(2) 5_656 . ? N6 Fe2 N6 180.0 5_656 . ? H1A O1 H1B 107.328(18) . . ? C1 N1 Fe1 121.6(6) . . ? C1 N1 C4 118.4(9) . . ? C4 N1 Fe1 120.0(7) . . ? C3 N2 C4 118.9(7) . . ? H3A N3 H3A 17(2) . 6_575 ? H3A N3 H3B 112.89(2) . . ? H3A N3 H3B 119.6(8) . 6_575 ? H3A N3 H3B 112.89(2) 6_575 6_575 ? H3B N3 H3A 119.6(8) . 6_575 ? H3B N3 H3B 40.5(9) . 6_575 ? C2 N3 H3A 112.3(5) . . ? C2 N3 H3A 112.3(5) . 6_575 ? C2 N3 H3B 126.2(6) . 6_575 ? C2 N3 H3B 126.2(6) . . ? C5 N4 Fe1 176.2(5) . . ? C6 N5 Fe2 167.1(5) . . ? C7 N6 Fe2 120.7(7) . . ? C7 N6 C10 117.3(9) . . ? C10 N6 Fe2 122.0(7) . . ? C9 N7 C10 116.3(9) . . ? H8A N8 H8B 112.89(2) . 6 ? H8A N8 H8B 112.89(2) . . ? H8B N8 H8B 98.8(5) . 6 ? C8 N8 H8A 102.2(5) . . ? C8 N8 H8B 115.4(3) . 6 ? C8 N8 H8B 115.4(3) . . ? N1 C1 H1 119.6 . . ? N1 C1 C2 120.8(9) . . ? C2 C1 H1 119.6 . . ? N3 C2 C1 121.3(9) . . ? N3 C2 C3 121.7(9) . . ? C3 C2 C1 116.9(9) . . ? N2 C3 C2 120.2(9) . . ? N2 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? N1 C4 N2 124.8(9) . . ? N1 C4 H4 117.6 . . ? N2 C4 H4 117.6 . . ? N4 C5 Pd1 178.4(6) . . ? N5 C6 Pd1 175.8(5) . . ? N6 C7 H7 118.9 . . ? N6 C7 C8 122.2(9) . . ? C8 C7 H7 118.9 . . ? N8 C8 C7 122.0(8) . . ? N8 C8 C9 122.1(9) . . ? C9 C8 C7 115.9(9) . . ? N7 C9 C8 122.8(10) . . ? N7 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? N6 C10 H10 117.3 . . ? N7 C10 N6 125.5(10) . . ? N7 C10 H10 117.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 N1 C1 C2 180.000(5) . . . . ? Fe1 N1 C4 N2 180.000(3) . . . . ? Fe2 N6 C7 C8 180.000(2) . . . . ? Fe2 N6 C10 N7 180.000(3) . . . . ? N1 C1 C2 N3 180.000(5) . . . . ? N1 C1 C2 C3 0.000(7) . . . . ? N3 C2 C3 N2 180.000(3) . . . . ? N6 C7 C8 N8 180.000(3) . . . . ? N6 C7 C8 C9 0.000(3) . . . . ? N8 C8 C9 N7 180.000(3) . . . . ? C1 N1 C4 N2 0.000(8) . . . . ? C1 C2 C3 N2 0.000(5) . . . . ? C3 N2 C4 N1 0.000(8) . . . . ? C4 N1 C1 C2 0.000(7) . . . . ? C4 N2 C3 C2 0.000(6) . . . . ? C7 N6 C10 N7 0.000(5) . . . . ? C7 C8 C9 N7 0.000(3) . . . . ? C9 N7 C10 N6 0.000(5) . . . . ? C10 N6 C7 C8 0.000(3) . . . . ? C10 N7 C9 C8 0.000(4) . . . . ? _shelx_res_file ; TITL rt235_fe5apympd_180k_0m_a.res in C2/m rt235_fe5apympd_180k_0m.res created by SHELXL-2018/3 at 00:51:17 on 09-Sep-2020 REM Old TITL RT235_Fe5apymPd_180K_0m in C2/m REM SHELXT solution in C2/m REM R1 0.164, Rweak 0.007, Alpha 0.046, Orientation as input REM Formula found by SHELXT: C20 N28 Fe Pd3 CELL 0.71073 21.4539 7.1986 14.7221 90 131.494 90 ZERR 4 0.0026 0.0008 0.0016 0 0.003 0 LATT 7 SYMM -X,+Y,-Z SFAC C H Fe N O Pd UNIT 48 48 4 40 4 4 EQIV $1 +X,-Y,+Z EQIV $2 +X,-1+Y,-1+Z DFIX 0.9 0.0001 O1 H1b DANG 1.5 0.0001 H8a H8b_$1 DFIX 0.9 0.0001 H8b_$1 N8 DFIX 0.9 0.0001 N8 H8a DANG 2.1 0.0001 H8a O1_$2 DANG 1.45 0.0001 H1b H1a DANG 2 0.0001 H1b N2 DFIX 0.9 0.0001 O1 H1a DANG 1.5 0.0001 H3b H3a DFIX 0.9 0.0001 H3b N3 DFIX 0.9 0.0001 N3 H3a L.S. 50 PLAN 10 SIZE 0.05 0.15 0.2 TEMP -93.14 CONF LIST 6 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.044500 42.167709 FVAR 0.24318 PD1 6 0.514793 0.500000 0.770948 10.50000 0.03120 0.01343 = 0.02458 0.00000 0.02113 0.00000 FE1 3 0.500000 1.000000 1.000000 10.25000 0.03365 0.01010 = 0.02578 0.00000 0.02461 0.00000 FE2 3 0.500000 0.000000 0.500000 10.25000 0.03503 0.00957 = 0.02696 0.00000 0.02591 0.00000 PART -1 O1 5 0.227935 1.110766 1.012965 10.50000 0.07913 H1A 2 0.262365 1.209339 1.044922 10.50000 -1.50000 H1B 2 0.218671 1.076502 0.946105 10.50000 -1.50000 PART 0 N1 4 0.374224 1.000000 0.881687 10.50000 0.03492 0.02243 = 0.03168 0.00000 0.02576 0.00000 N2 4 0.251727 1.000000 0.852505 10.50000 0.03475 0.05277 = 0.04248 0.00000 0.02514 0.00000 N3 4 0.195458 1.000000 0.561204 10.50000 0.03615 0.08180 = 0.03502 0.00000 0.02459 0.00000 H3A 2 0.226406 0.981039 0.540983 10.50000 -1.20000 H3B 2 0.143157 0.956751 0.505138 10.50000 -1.20000 N4 4 0.499901 0.807583 0.906684 11.00000 0.04003 0.01419 = 0.02739 0.00057 0.02661 -0.00082 N5 4 0.524193 0.206226 0.623851 11.00000 0.04416 0.02081 = 0.03262 -0.00269 0.03014 -0.00313 N6 4 0.369560 0.000000 0.420095 10.50000 0.02573 0.02565 = 0.03207 0.00000 0.01845 0.00000 N7 4 0.271016 0.000000 0.447530 10.50000 0.03910 0.06437 = 0.04007 0.00000 0.03009 0.00000 N8 4 0.161633 0.000000 0.127187 10.50000 0.04381 0.08821 = 0.04475 0.00000 0.02931 0.00000 H8A 2 0.189130 0.000000 0.100478 10.50000 -1.20000 H8B 2 0.125464 -0.094898 0.097306 10.50000 -1.20000 C1 1 0.329589 1.000000 0.763264 10.50000 0.04299 0.02027 = 0.03368 0.00000 0.03020 0.00000 AFIX 43 H1 2 0.356889 1.000000 0.732386 10.50000 -1.20000 AFIX 0 C2 1 0.241482 1.000000 0.681726 10.50000 0.03866 0.02845 = 0.03298 0.00000 0.02067 0.00000 C3 1 0.204494 1.000000 0.733195 10.50000 0.03682 0.04280 = 0.04052 0.00000 0.02812 0.00000 AFIX 43 H3 2 0.145606 1.000000 0.682033 10.50000 -1.20000 AFIX 0 C4 1 0.334332 1.000000 0.922699 10.50000 0.04566 0.03728 = 0.04148 0.00000 0.03516 0.00000 AFIX 43 H4 2 0.367113 1.000000 1.008049 10.50000 -1.20000 AFIX 0 C5 1 0.504365 0.696885 0.855723 11.00000 0.03417 0.01252 = 0.02161 -0.00218 0.02134 -0.00135 C6 1 0.522425 0.308823 0.681278 11.00000 0.03205 0.01520 = 0.02847 0.00261 0.02393 0.00268 C7 1 0.308566 0.000000 0.302526 10.50000 0.05068 0.01998 = 0.03890 0.00000 0.03257 0.00000 AFIX 43 H7 2 0.321339 0.000000 0.251853 10.50000 -1.20000 AFIX 0 C8 1 0.224229 0.000000 0.248260 10.50000 0.03241 0.03187 = 0.03554 0.00000 0.02199 0.00000 C9 1 0.209915 0.000000 0.327876 10.50000 0.03443 0.04177 = 0.04398 0.00000 0.02554 0.00000 AFIX 43 H9 2 0.154054 0.000000 0.295068 10.50000 -1.20000 AFIX 0 C10 1 0.349136 0.000000 0.489486 10.50000 0.03837 0.04497 = 0.03854 0.00000 0.02477 0.00000 AFIX 43 H10 2 0.393544 0.000000 0.574957 10.50000 -1.20000 AFIX 0 HKLF 4 REM rt235_fe5apympd_180k_0m_a.res in C2/m REM wR2 = 0.1593, GooF = S = 1.054, Restrained GooF = 1.051 for all data REM R1 = 0.0564 for 1942 Fo > 4sig(Fo) and 0.0887 for all 2496 data REM 156 parameters refined using 11 restraints END WGHT 0.0444 42.2275 REM Highest difference peak 2.003, deepest hole -1.608, 1-sigma level 0.230 Q1 1 0.5082 0.5000 0.7010 10.50000 0.05 2.00 Q2 1 0.4659 0.5000 0.7181 10.50000 0.05 1.53 Q3 1 0.2241 1.0000 0.9481 10.50000 0.05 1.13 Q4 1 0.5718 0.5000 0.6988 10.50000 0.05 1.06 Q5 1 0.4830 0.3829 0.6905 11.00000 0.05 1.05 Q6 1 0.3002 1.0000 0.8195 10.50000 0.05 0.99 Q7 1 0.2527 0.0000 0.1341 10.50000 0.05 0.96 Q8 1 0.5467 0.4387 0.7307 11.00000 0.05 0.96 Q9 1 0.3806 0.0000 0.3632 10.50000 0.05 0.95 Q10 1 0.5066 0.0000 0.4672 10.50000 0.05 0.93 ; _shelx_res_checksum 41849 _olex2_submission_special_instructions 'No special instructions were received' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_rt312_nh2pympdmeoh_100k _database_code_depnum_ccdc_archive 'CCDC 2018388' loop_ _audit_author_name _audit_author_address 'Carlos Bartual-Murgui' ;Universitat de Valencia Spain ; _audit_update_record ; 2020-09-17 deposited with the CCDC. 2020-09-22 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT971_rt312_nh2pympdmeoh_100k ; PROBLEM: Check Calcd Resid. Dens. 1.00A From Pd2 5.48 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_rt312_nh2pympdmeoh_100k_2 ; PROBLEM: Check Calcd Resid. Dens. 0.65A From Pd1 4.48 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt312_nh2pympdmeoh_100k ; PROBLEM: Check Calcd Resid. Dens. 1.34A From Pd2 -3.67 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT973_rt312_nh2pympdmeoh_100k ; PROBLEM: Check Calcd Positive Resid. Density on Fe1 3.92 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT973_rt312_nh2pympdmeoh_100k_2 ; PROBLEM: Check Calcd Positive Resid. Density on Pd2 3.21 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT973_rt312_nh2pympdmeoh_100k_3 ; PROBLEM: Check Calcd Positive Resid. Density on Fe2 3.14 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT097_rt312_nh2pympdmeoh_100k ; PROBLEM: Large Reported Max. (Positive) Residual Density 5.52 eA-3 RESPONSE: The crystal may be damaged during the dehydration process. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT342_rt312_nh2pympdmeoh_100k ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.025 Ang. RESPONSE: The crystal may be damaged during the dehydration process. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT910_rt312_nh2pympdmeoh_100k ; PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 12 Note RESPONSE: The unit cell is relatively large and Mo radiation was used. Therefore several reflections were probably stopped by the beam stop. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT971_rt312_nh2pympdmeoh_100k_3 ; PROBLEM: Check Calcd Resid. Dens. 1.26A From Pd1 2.54 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_rt312_nh2pympdmeoh_100k_4 ; PROBLEM: Check Calcd Resid. Dens. 0.98A From Pd1 2.53 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt312_nh2pympdmeoh_100k_2 ; PROBLEM: Check Calcd Resid. Dens. 1.28A From Pd1 -3.44 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt312_nh2pympdmeoh_100k_3 ; PROBLEM: Check Calcd Resid. Dens. 0.13A From N3 -3.41 eA-3 RESPONSE: The residual electronic density may be due to the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt312_nh2pympdmeoh_100k_4 ; PROBLEM: Check Calcd Resid. Dens. 0.63A From Pd2 -3.21 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt312_nh2pympdmeoh_100k_5 ; PROBLEM: Check Calcd Resid. Dens. 0.12A From N11 -2.78 eA-3 RESPONSE: The residual electronic density may be due to the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt312_nh2pympdmeoh_100k_6 ; PROBLEM: Check Calcd Resid. Dens. 0.07A From N2 -2.54 eA-3 RESPONSE: The residual electronic density may be due to the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; # Added during the CSD deposition process: Thursday 17 September 2020 12:29 PM # end Validation Reply Form _audit_creation_date 2020-09-09 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C12 H10 Fe N10 Pd, 0.5(C H4 O)' _chemical_formula_sum 'C12.50 H12 Fe N10 O0.50 Pd' _chemical_formula_weight 472.57 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system orthorhombic _space_group_IT_number 57 _space_group_name_H-M_alt 'P b c m' _space_group_name_Hall '-P 2c 2b' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y-1/2, z' _cell_length_a 14.9105(14) _cell_length_b 32.0213(19) _cell_length_c 7.1610(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3419.0(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 1130 _cell_measurement_temperature 100.00(14) _cell_measurement_theta_max 26.3910 _cell_measurement_theta_min 4.0460 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 1.922 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.97199 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'light orange' _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.836 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 1864 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_unetI/netI 0.0759 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.856 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_number 8760 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.856 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.807 _diffrn_reflns_theta_min 3.333 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(14) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0267 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.856 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -45.00 40.00 1.00 25.00 -- 15.83 -38.00 0.00 85 2 \w 30.00 80.00 1.00 25.00 -- 15.83 19.00-150.00 50 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0085941000 _diffrn_orient_matrix_UB_12 0.0162671000 _diffrn_orient_matrix_UB_13 0.0647607000 _diffrn_orient_matrix_UB_21 -0.0434155000 _diffrn_orient_matrix_UB_22 0.0027233000 _diffrn_orient_matrix_UB_23 -0.0388021000 _diffrn_orient_matrix_UB_31 -0.0175117000 _diffrn_orient_matrix_UB_32 -0.0147696000 _diffrn_orient_matrix_UB_33 0.0641131000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2486 _reflns_number_total 3757 _reflns_odcompleteness_completeness 99.43 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 24.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 5.519 _refine_diff_density_min -3.618 _refine_diff_density_rms 0.332 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 131 _refine_ls_number_reflns 3757 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1465 _refine_ls_R_factor_gt 0.1088 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0809P)^2^+178.4426P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2488 _refine_ls_wR_factor_ref 0.2765 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All N(H,H) groups, All O(H) groups 2. Restrained distances O2-C22 1.4 with sigma of 0.02 H3A-N3 0.9 with sigma of 0.0001 N3-H3B 0.9 with sigma of 0.0001 H8B_$1-N8_$1 0.9 with sigma of 0.0001 N8_$1-H8A_$1 0.9 with sigma of 0.0001 H14A_$2-N14_$2 0.9 with sigma of 0.0001 H14B_$2-N14_$2 0.9 with sigma of 0.0001 N11_$3-H11A_$3 0.9 with sigma of 0.0001 H11B_$3-N11_$3 0.9 with sigma of 0.0001 H3A-H3B 1.5 with sigma of 0.0001 H8B_$1-H8A_$1 1.5 with sigma of 0.0001 H14B_$2-H14A_$2 1.5 with sigma of 0.0001 H8A_$3-O1_$4 2.2 with sigma of 0.0001 H11A_$3-H11B_$3 1.5 with sigma of 0.0001 3. Uiso/Uaniso restraints and constraints Uanis(N3) = Uanis(C2) = Uanis(C3) = Uanis(N2) = Uanis(C4) = Uanis(N1) = Uanis(C1) = Uanis(Fe1) = Uanis(N9) = Uanis(C14) = Uanis(N10) = Uanis(C13) = Uanis(C12) = Uanis(C11) = Uanis(N11) Uanis(C9) = Uanis(N7) = Uanis(C10) = Uanis(N6) = Uanis(C7) = Uanis(C8) = Uanis(N8) = Uanis(N12) = Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(N13) = Uanis(C18) = Uanis(N14) Uanis(N4) = Uanis(C5) = Uanis(Pd1) = Uanis(C6) = Uanis(N5) = Uanis(Fe2) = Uanis(N15) = Uanis(C19) = Uanis(Pd2) = Uanis(N16) = Uanis(C20) Uiso(O2) = Uiso(C22) Uiso(O1) = Uiso(C21) 4. Others Fixed Sof: H8A(0.5) H14A(0.5) O1(0.25) H1A(0.25) C21(0.25) H21A(0.25) H21B(0.25) H21C(0.25) O2(0.25) H2(0.25) C22(0.25) H22A(0.25) H22B(0.25) H22C(0.25) Fixed X: O1(0.504549) C21(0.499149) Fixed Y: O1(0.232679) C21(0.239669) Fixed Z: O1(1.25) C21(1.056419) 5.a Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C4(H4), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18) 5.b Idealised Me refined as rotating group: C21(H21A,H21B,H21C), C22(H22A,H22B,H22C) 5.c Idealised tetrahedral OH refined as rotating group: O1(H1A), O2(H2) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.49849(8) 0.36641(4) 0.750000 0.0075(3) Uani 1 2 d S T P . . Pd2 Pd 0.01531(7) 0.38519(4) -0.250000 0.0075(3) Uani 1 2 d S T P . . Fe1 Fe 0.75738(15) 0.37430(8) 1.250000 0.0099(5) Uani 1 2 d S T P . . Fe2 Fe 0.25701(14) 0.37738(7) 0.250000 0.0075(3) Uani 1 2 d S T P . . N1 N 0.7671(9) 0.3063(4) 1.250000 0.0099(5) Uani 1 2 d S T P . . N2 N 0.6893(8) 0.2414(4) 1.250000 0.0099(5) Uani 1 2 d S T P . . N3 N 0.92736(18) 0.22251(7) 1.250000 0.0099(5) Uani 1 2 d DS T P . . H3A H 0.9309(3) 0.19445(6) 1.250000 0.015 Uiso 1 2 d DS U P . . H3B H 0.9815(2) 0.23492(10) 1.250000 0.015 Uiso 1 2 d DS U P . . N4 N 0.6544(6) 0.3716(3) 1.0436(13) 0.0075(3) Uani 1 1 d . . . . . N5 N 0.3489(6) 0.3692(3) 0.4426(13) 0.0075(3) Uani 1 1 d . . . . . N6 N 0.2232(11) 0.3161(5) 0.250000 0.0230(11) Uani 1 2 d S T P . . N7 N 0.1054(11) 0.2669(5) 0.250000 0.0230(11) Uani 1 2 d S T P . . N8 N 0.31901(18) 0.21415(8) 0.250000 0.0230(11) Uani 1 2 d S T P . . H8A H 0.36918(10) 0.20985(14) 0.3172(5) 0.034 Uiso 0.5 1 d . U P . . H8B H 0.28199(17) 0.19194(11) 0.250000 0.034 Uiso 1 2 d S U P . . N9 N 0.7441(9) 0.4431(4) 1.250000 0.0099(5) Uani 1 2 d S T P . . N10 N 0.8200(9) 0.5081(4) 1.250000 0.0099(5) Uani 1 2 d S T P . . N11 N 0.58372(18) 0.52785(7) 1.250000 0.0099(5) Uani 1 2 d S T P . . H11A H 0.5313(2) 0.51391(10) 1.250000 0.015 Uiso 1 2 d S U P . . H11B H 0.5765(4) 0.55575(6) 1.250000 0.015 Uiso 1 2 d S U P . . N12 N 0.2867(11) 0.4394(5) 0.250000 0.0230(11) Uani 1 2 d S T P . . N13 N 0.4047(11) 0.4903(5) 0.250000 0.0230(11) Uani 1 2 d S T P . . N14 N 0.18719(14) 0.54151(11) 0.250000 0.0230(11) Uani 1 2 d S T P . . H14A H 0.2098(2) 0.56318(11) 0.3148(8) 0.034 Uiso 0.5 1 d . U P . . H14B H 0.12684(15) 0.54097(17) 0.250000 0.034 Uiso 1 2 d S U P . . N15 N 0.1663(6) 0.3867(3) 0.0558(13) 0.0075(3) Uani 1 1 d . . . . . N16 N -0.1386(6) 0.3773(3) -0.5462(13) 0.0075(3) Uani 1 1 d . . . . . C1 C 0.8434(10) 0.2853(5) 1.250000 0.0099(5) Uani 1 2 d S T P . . H1 H 0.896669 0.300366 1.250000 0.012 Uiso 1 2 calc R U P . . C2 C 0.8488(10) 0.2409(5) 1.250000 0.0099(5) Uani 1 2 d S T P . . C3 C 0.7645(10) 0.2224(5) 1.250000 0.0099(5) Uani 1 2 d S T P . . H3 H 0.762766 0.193358 1.250000 0.012 Uiso 1 2 calc R U P . . C4 C 0.6915(10) 0.2838(5) 1.250000 0.0099(5) Uani 1 2 d S T P . . H4 H 0.637161 0.297986 1.250000 0.012 Uiso 1 2 calc R U P . . C5 C 0.5959(7) 0.3692(3) 0.9400(16) 0.0075(3) Uani 1 1 d . . . . . C6 C 0.4034(7) 0.3667(3) 0.5540(16) 0.0075(3) Uani 1 1 d . . . . . C7 C 0.2845(13) 0.2866(6) 0.250000 0.0230(11) Uani 1 2 d S T P . . H7 H 0.344992 0.293702 0.250000 0.028 Uiso 1 2 calc R U P . . C8 C 0.2588(12) 0.2448(6) 0.250000 0.0230(11) Uani 1 2 d S T P . . C9 C 0.1659(13) 0.2372(6) 0.250000 0.0230(11) Uani 1 2 d S T P . . H9 H 0.146351 0.209648 0.250000 0.028 Uiso 1 2 calc R U P . . C10 C 0.1351(13) 0.3058(6) 0.250000 0.0230(11) Uani 1 2 d S T P . . H10 H 0.093199 0.327293 0.250000 0.028 Uiso 1 2 calc R U P . . C11 C 0.6670(11) 0.4645(5) 1.250000 0.0099(5) Uani 1 2 d S T P . . H11 H 0.613894 0.449210 1.250000 0.012 Uiso 1 2 calc R U P . . C12 C 0.6604(10) 0.5081(5) 1.250000 0.0099(5) Uani 1 2 d S T P . . C13 C 0.7458(10) 0.5281(5) 1.250000 0.0099(5) Uani 1 2 d S T P . . H13 H 0.747638 0.557093 1.250000 0.012 Uiso 1 2 calc R U P . . C14 C 0.8192(10) 0.4660(5) 1.250000 0.0099(5) Uani 1 2 d S T P . . H14 H 0.873950 0.452136 1.250000 0.012 Uiso 1 2 calc R U P . . C15 C 0.2236(14) 0.4679(6) 0.250000 0.0230(11) Uani 1 2 d S T P . . H15 H 0.163448 0.460289 0.250000 0.028 Uiso 1 2 calc R U P . . C16 C 0.2489(13) 0.5105(6) 0.250000 0.0230(11) Uani 1 2 d S T P . . C17 C 0.3410(13) 0.5185(6) 0.250000 0.0230(11) Uani 1 2 d S T P . . H17 H 0.358722 0.546311 0.250000 0.028 Uiso 1 2 calc R U P . . C18 C 0.3710(13) 0.4514(6) 0.250000 0.0230(11) Uani 1 2 d S T P . . H18 H 0.413188 0.429957 0.250000 0.028 Uiso 1 2 calc R U P . . C19 C 0.1110(7) 0.3876(3) -0.0539(15) 0.0075(3) Uani 1 1 d . . . . . C20 C -0.0794(7) 0.3803(3) -0.4419(15) 0.0075(3) Uani 1 1 d . . . . . O1 O 0.504549 0.232679 1.250000 0.034(6) Uiso 0.25 1 d S . P A -1 H1A H 0.489748 0.253943 1.305869 0.050 Uiso 0.25 1 calc R U P A -1 C21 C 0.499149 0.239669 1.056419 0.034(6) Uiso 0.25 1 d . . P A -1 H21A H 0.544001 0.223332 0.993861 0.050 Uiso 0.25 1 calc R U P A -1 H21B H 0.508968 0.268743 1.030883 0.050 Uiso 0.25 1 calc R U P A -1 H21C H 0.440793 0.231703 1.012386 0.050 Uiso 0.25 1 calc R U P A -1 O2 O 1.002(2) 0.5163(10) 1.209(4) 0.020(7) Uiso 0.25 1 d D . P B -1 H2 H 1.004833 0.493214 1.159756 0.031 Uiso 0.25 1 calc R U P B -1 C22 C 1.004(4) 0.5116(16) 1.407(4) 0.020(7) Uiso 0.25 1 d D . P B -1 H22A H 0.998872 0.482536 1.438380 0.031 Uiso 0.25 1 calc R U P B -1 H22B H 0.955250 0.526777 1.461612 0.031 Uiso 0.25 1 calc R U P B -1 H22C H 1.059877 0.522255 1.454064 0.031 Uiso 0.25 1 calc R U P B -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0051(4) 0.0120(5) 0.0053(4) 0.000 0.000 -0.0012(3) Pd2 0.0051(4) 0.0120(5) 0.0053(4) 0.000 0.000 -0.0012(3) Fe1 0.0039(9) 0.0144(10) 0.0114(10) 0.000 0.000 -0.0026(7) Fe2 0.0051(4) 0.0120(5) 0.0053(4) 0.000 0.000 -0.0012(3) N1 0.0039(9) 0.0144(10) 0.0114(10) 0.000 0.000 -0.0026(7) N2 0.0039(9) 0.0144(10) 0.0114(10) 0.000 0.000 -0.0026(7) N3 0.0039(9) 0.0144(10) 0.0114(10) 0.000 0.000 -0.0026(7) N4 0.0051(4) 0.0120(5) 0.0053(4) 0.000 0.000 -0.0012(3) N5 0.0051(4) 0.0120(5) 0.0053(4) 0.000 0.000 -0.0012(3) N6 0.020(3) 0.019(2) 0.030(3) 0.000 0.000 -0.0061(19) N7 0.020(3) 0.019(2) 0.030(3) 0.000 0.000 -0.0061(19) N8 0.020(3) 0.019(2) 0.030(3) 0.000 0.000 -0.0061(19) N9 0.0039(9) 0.0144(10) 0.0114(10) 0.000 0.000 -0.0026(7) N10 0.0039(9) 0.0144(10) 0.0114(10) 0.000 0.000 -0.0026(7) N11 0.0039(9) 0.0144(10) 0.0114(10) 0.000 0.000 -0.0026(7) N12 0.020(3) 0.019(2) 0.030(3) 0.000 0.000 -0.0061(19) N13 0.020(3) 0.019(2) 0.030(3) 0.000 0.000 -0.0061(19) N14 0.020(3) 0.019(2) 0.030(3) 0.000 0.000 -0.0061(19) N15 0.0051(4) 0.0120(5) 0.0053(4) 0.000 0.000 -0.0012(3) N16 0.0051(4) 0.0120(5) 0.0053(4) 0.000 0.000 -0.0012(3) C1 0.0039(9) 0.0144(10) 0.0114(10) 0.000 0.000 -0.0026(7) C2 0.0039(9) 0.0144(10) 0.0114(10) 0.000 0.000 -0.0026(7) C3 0.0039(9) 0.0144(10) 0.0114(10) 0.000 0.000 -0.0026(7) C4 0.0039(9) 0.0144(10) 0.0114(10) 0.000 0.000 -0.0026(7) C5 0.0051(4) 0.0120(5) 0.0053(4) 0.000 0.000 -0.0012(3) C6 0.0051(4) 0.0120(5) 0.0053(4) 0.000 0.000 -0.0012(3) C7 0.020(3) 0.019(2) 0.030(3) 0.000 0.000 -0.0061(19) C8 0.020(3) 0.019(2) 0.030(3) 0.000 0.000 -0.0061(19) C9 0.020(3) 0.019(2) 0.030(3) 0.000 0.000 -0.0061(19) C10 0.020(3) 0.019(2) 0.030(3) 0.000 0.000 -0.0061(19) C11 0.0039(9) 0.0144(10) 0.0114(10) 0.000 0.000 -0.0026(7) C12 0.0039(9) 0.0144(10) 0.0114(10) 0.000 0.000 -0.0026(7) C13 0.0039(9) 0.0144(10) 0.0114(10) 0.000 0.000 -0.0026(7) C14 0.0039(9) 0.0144(10) 0.0114(10) 0.000 0.000 -0.0026(7) C15 0.020(3) 0.019(2) 0.030(3) 0.000 0.000 -0.0061(19) C16 0.020(3) 0.019(2) 0.030(3) 0.000 0.000 -0.0061(19) C17 0.020(3) 0.019(2) 0.030(3) 0.000 0.000 -0.0061(19) C18 0.020(3) 0.019(2) 0.030(3) 0.000 0.000 -0.0061(19) C19 0.0051(4) 0.0120(5) 0.0053(4) 0.000 0.000 -0.0012(3) C20 0.0051(4) 0.0120(5) 0.0053(4) 0.000 0.000 -0.0012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C5 1.993(11) . ? Pd1 C5 1.993(11) 6_557 ? Pd1 C6 1.995(11) 6_557 ? Pd1 C6 1.995(11) . ? Pd2 C19 2.003(11) . ? Pd2 C19 2.003(11) 6 ? Pd2 C20 1.977(11) 6 ? Pd2 C20 1.977(11) . ? Fe1 N1 2.181(14) . ? Fe1 N4 2.133(9) . ? Fe1 N4 2.133(9) 6_558 ? Fe1 N9 2.213(14) . ? Fe1 N16 2.132(9) 6_656 ? Fe1 N16 2.132(9) 1_657 ? Fe2 N5 1.961(9) . ? Fe2 N5 1.961(9) 6_556 ? Fe2 N6 2.027(16) . ? Fe2 N12 2.034(16) . ? Fe2 N15 1.962(9) 6_556 ? Fe2 N15 1.962(9) . ? N1 C1 1.32(2) . ? N1 C4 1.34(2) . ? N2 C3 1.28(2) . ? N2 C4 1.36(2) . ? N3 H3A 0.90000(11) . ? N3 H3B 0.90000(12) . ? N3 C2 1.312(16) . ? N4 C5 1.147(14) . ? N5 C6 1.142(14) . ? N6 C7 1.31(2) . ? N6 C10 1.35(2) . ? N7 C9 1.31(2) . ? N7 C10 1.32(2) . ? N8 H8A 0.90000(12) 6_556 ? N8 H8A 0.90000(12) . ? N8 H8B 0.90000(11) . ? N8 C8 1.33(2) . ? N9 C11 1.34(2) . ? N9 C14 1.34(2) . ? N10 C13 1.28(2) . ? N10 C14 1.35(2) . ? N11 H11A 0.90000(12) . ? N11 H11B 0.90000(11) . ? N11 C12 1.306(16) . ? N12 C15 1.31(3) . ? N12 C18 1.31(2) . ? N13 C17 1.31(3) . ? N13 C18 1.34(2) . ? N14 H14A 0.89997(11) 6_556 ? N14 H14A 0.90000(11) . ? N14 H14B 0.90000(13) . ? N14 C16 1.35(2) . ? N15 C19 1.140(14) . ? N16 C20 1.160(14) . ? C1 H1 0.9300 . ? C1 C2 1.42(2) . ? C2 C3 1.39(2) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C7 H7 0.9300 . ? C7 C8 1.39(3) . ? C8 C9 1.41(3) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C11 C12 1.40(2) . ? C12 C13 1.42(2) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C15 C16 1.42(3) . ? C16 C17 1.40(3) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? O1 H1A 0.8200 . ? O1 C21 1.40649(7) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? O2 H2 0.8200 . ? O2 C22 1.42(2) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Pd1 C5 86.1(6) . 6_557 ? C5 Pd1 C6 176.8(4) 6_557 6_557 ? C5 Pd1 C6 176.8(4) . . ? C5 Pd1 C6 92.2(4) . 6_557 ? C5 Pd1 C6 92.2(4) 6_557 . ? C6 Pd1 C6 89.4(6) . 6_557 ? C19 Pd2 C19 89.0(6) . 6 ? C20 Pd2 C19 91.4(4) 6 . ? C20 Pd2 C19 177.7(4) 6 6 ? C20 Pd2 C19 177.7(4) . . ? C20 Pd2 C19 91.4(4) . 6 ? C20 Pd2 C20 88.1(6) . 6 ? N1 Fe1 N9 178.7(5) . . ? N4 Fe1 N1 90.4(4) 6_558 . ? N4 Fe1 N1 90.4(4) . . ? N4 Fe1 N4 87.8(5) . 6_558 ? N4 Fe1 N9 88.6(3) . . ? N4 Fe1 N9 88.6(3) 6_558 . ? N16 Fe1 N1 89.8(4) 1_657 . ? N16 Fe1 N1 89.8(4) 6_656 . ? N16 Fe1 N4 92.9(3) 1_657 6_558 ? N16 Fe1 N4 179.3(4) 6_656 6_558 ? N16 Fe1 N4 179.3(4) 1_657 . ? N16 Fe1 N4 92.9(3) 6_656 . ? N16 Fe1 N9 91.2(4) 6_656 . ? N16 Fe1 N9 91.2(4) 1_657 . ? N16 Fe1 N16 86.4(5) 1_657 6_656 ? N5 Fe2 N5 89.4(5) . 6_556 ? N5 Fe2 N6 92.5(4) 6_556 . ? N5 Fe2 N6 92.5(4) . . ? N5 Fe2 N12 88.7(4) . . ? N5 Fe2 N12 88.7(4) 6_556 . ? N5 Fe2 N15 178.8(4) . . ? N5 Fe2 N15 90.2(4) 6_556 . ? N5 Fe2 N15 90.2(4) . 6_556 ? N5 Fe2 N15 178.8(4) 6_556 6_556 ? N6 Fe2 N12 178.2(7) . . ? N15 Fe2 N6 88.6(4) 6_556 . ? N15 Fe2 N6 88.6(4) . . ? N15 Fe2 N12 90.1(4) . . ? N15 Fe2 N12 90.1(4) 6_556 . ? N15 Fe2 N15 90.3(5) . 6_556 ? C1 N1 Fe1 124.5(11) . . ? C1 N1 C4 116.6(14) . . ? C4 N1 Fe1 118.9(11) . . ? C3 N2 C4 117.2(14) . . ? H3A N3 H3B 112.885(18) . . ? C2 N3 H3A 120.1(7) . . ? C2 N3 H3B 127.1(7) . . ? C5 N4 Fe1 176.2(9) . . ? C6 N5 Fe2 176.4(9) . . ? C7 N6 Fe2 121.5(13) . . ? C7 N6 C10 120.0(17) . . ? C10 N6 Fe2 118.4(13) . . ? C9 N7 C10 116.9(17) . . ? H8A N8 H8A 64.6(5) . 6_556 ? H8A N8 H8B 112.885(19) . . ? H8B N8 H8A 112.885(19) . 6_556 ? C8 N8 H8A 132.4(6) . . ? C8 N8 H8A 132.4(6) . 6_556 ? C8 N8 H8B 99.7(8) . . ? C11 N9 Fe1 125.8(11) . . ? C11 N9 C14 116.1(14) . . ? C14 N9 Fe1 118.1(11) . . ? C13 N10 C14 119.6(14) . . ? H11A N11 H11B 112.885(18) . . ? C12 N11 H11A 121.4(8) . . ? C12 N11 H11B 125.7(8) . . ? C15 N12 Fe2 121.6(13) . . ? C15 N12 C18 118.9(17) . . ? C18 N12 Fe2 119.6(14) . . ? C17 N13 C18 111.6(17) . . ? H14A N14 H14A 62.0(8) . 6_556 ? H14A N14 H14B 112.886(18) . . ? H14B N14 H14A 112.885(18) . 6_556 ? C16 N14 H14A 108.1(7) . 6_556 ? C16 N14 H14A 108.1(7) . . ? C16 N14 H14B 131.8(9) . . ? C19 N15 Fe2 172.5(9) . . ? C20 N16 Fe1 176.2(9) . 1_453 ? N1 C1 H1 118.0 . . ? N1 C1 C2 123.9(15) . . ? C2 C1 H1 118.0 . . ? N3 C2 C1 120.0(13) . . ? N3 C2 C3 127.9(14) . . ? C3 C2 C1 112.0(14) . . ? N2 C3 C2 126.1(16) . . ? N2 C3 H3 116.9 . . ? C2 C3 H3 116.9 . . ? N1 C4 N2 124.1(15) . . ? N1 C4 H4 118.0 . . ? N2 C4 H4 118.0 . . ? N4 C5 Pd1 177.0(10) . . ? N5 C6 Pd1 176.1(9) . . ? N6 C7 H7 120.0 . . ? N6 C7 C8 120.0(18) . . ? C8 C7 H7 120.0 . . ? N8 C8 C7 121.6(16) . . ? N8 C8 C9 122.6(16) . . ? C7 C8 C9 115.8(18) . . ? N7 C9 C8 123.7(17) . . ? N7 C9 H9 118.2 . . ? C8 C9 H9 118.2 . . ? N6 C10 H10 118.2 . . ? N7 C10 N6 123.7(19) . . ? N7 C10 H10 118.2 . . ? N9 C11 H11 117.6 . . ? N9 C11 C12 124.7(15) . . ? C12 C11 H11 117.6 . . ? N11 C12 C11 122.9(13) . . ? N11 C12 C13 124.4(14) . . ? C11 C12 C13 112.6(15) . . ? N10 C13 C12 123.3(16) . . ? N10 C13 H13 118.3 . . ? C12 C13 H13 118.3 . . ? N9 C14 N10 123.7(15) . . ? N9 C14 H14 118.1 . . ? N10 C14 H14 118.1 . . ? N12 C15 H15 120.6 . . ? N12 C15 C16 118.7(18) . . ? C16 C15 H15 120.6 . . ? N14 C16 C15 121.7(16) . . ? N14 C16 C17 122.4(16) . . ? C17 C16 C15 115.9(18) . . ? N13 C17 C16 126.0(18) . . ? N13 C17 H17 117.0 . . ? C16 C17 H17 117.0 . . ? N12 C18 N13 128.9(19) . . ? N12 C18 H18 115.5 . . ? N13 C18 H18 115.5 . . ? N15 C19 Pd2 176.1(10) . . ? N16 C20 Pd2 176.0(10) . . ? C21 O1 H1A 109.5 . . ? O1 C21 H21A 109.5 . . ? O1 C21 H21B 109.5 . . ? O1 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22 O2 H2 109.5 . . ? O2 C22 H22A 109.5 . . ? O2 C22 H22B 109.5 . . ? O2 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 N1 C1 C2 180.0 . . . . ? Fe1 N1 C4 N2 180.0 . . . . ? Fe1 N9 C11 C12 180.0 . . . . ? Fe1 N9 C14 N10 180.0 . . . . ? Fe2 N6 C7 C8 180.0 . . . . ? Fe2 N6 C10 N7 180.0 . . . . ? Fe2 N12 C15 C16 180.0 . . . . ? Fe2 N12 C18 N13 180.0 . . . . ? N1 C1 C2 N3 180.0 . . . . ? N1 C1 C2 C3 0.0 . . . . ? N3 C2 C3 N2 180.0 . . . . ? N6 C7 C8 N8 180.0 . . . . ? N6 C7 C8 C9 0.0 . . . . ? N8 C8 C9 N7 180.0 . . . . ? N9 C11 C12 N11 180.0 . . . . ? N9 C11 C12 C13 0.0 . . . . ? N11 C12 C13 N10 180.0 . . . . ? N12 C15 C16 N14 180.0 . . . . ? N12 C15 C16 C17 0.0 . . . . ? N14 C16 C17 N13 180.0 . . . . ? C1 N1 C4 N2 0.0 . . . . ? C1 C2 C3 N2 0.0 . . . . ? C3 N2 C4 N1 0.0 . . . . ? C4 N1 C1 C2 0.0 . . . . ? C4 N2 C3 C2 0.0 . . . . ? C7 N6 C10 N7 0.0 . . . . ? C7 C8 C9 N7 0.0 . . . . ? C9 N7 C10 N6 0.0 . . . . ? C10 N6 C7 C8 0.0 . . . . ? C10 N7 C9 C8 0.0 . . . . ? C11 N9 C14 N10 0.0 . . . . ? C11 C12 C13 N10 0.0 . . . . ? C13 N10 C14 N9 0.0 . . . . ? C14 N9 C11 C12 0.0 . . . . ? C14 N10 C13 C12 0.0 . . . . ? C15 N12 C18 N13 0.0 . . . . ? C15 C16 C17 N13 0.0 . . . . ? C17 N13 C18 N12 0.0 . . . . ? C18 N12 C15 C16 0.0 . . . . ? C18 N13 C17 C16 0.0 . . . . ? _shelx_res_file ; TITL rt312_nh2pympdmeoh_100k_a.res in Pbcm rt312_nh2pympdmeoh_100k.res created by SHELXL-2018/3 at 13:04:17 on 09-Sep-2020 REM Old TITL RT312_NH2pymPdMeOH_100K in Pbcm REM SHELXT solution in Pbcm: R1 0.148, Rweak 0.007, Alpha 0.105 REM 1.347 for 201 systematic absences, Orientation as input REM Formula found by SHELXT: C9 N27 Fe2 Pd2 CELL 0.71073 14.9105 32.0213 7.161 90 90 90 ZERR 8 0.0014 0.0019 0.0004 0 0 0 LATT 1 SYMM -X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM +X,0.5-Y,-Z SFAC C H Fe N O Pd UNIT 100 96 8 80 4 8 EQIV $1 +X,+Y,1.5-Z EQIV $2 1+X,+Y,1+Z EQIV $3 +X,+Y,0.5-Z EQIV $4 +X,+Y,-1+Z DFIX 1.4 O2 C22 EADP N3 C2 C3 N2 C4 N1 C1 Fe1 N9 C14 N10 C13 C12 C11 N11 EADP C9 N7 C10 N6 C7 C8 N8 N12 C15 C16 C17 N13 C18 N14 DANG 1.5 0.0001 H3a H3b DFIX 0.9 0.0001 H3a N3 EADP N4 C5 Pd1 C6 N5 Fe2 N15 C19 Pd2 N16 C20 DFIX 0.9 0.0001 N3 H3b EADP O2 C22 EADP O1 C21 DFIX 0.9 0.0001 H8b_$1 N8_$1 DFIX 0.9 0.0001 N8_$1 H8a_$1 DANG 1.5 0.0001 H8b_$1 H8a_$1 DFIX 0.9 0.0001 H14a_$2 N14_$2 DFIX 0.9 0.0001 H14b_$2 N14_$2 DANG 1.5 0.0001 H14b_$2 H14a_$2 DANG 2.2 0.0001 H8a_$3 O1_$4 DFIX 0.9 0.0001 N11_$3 H11a_$3 DFIX 0.9 0.0001 H11b_$3 N11_$3 DANG 1.5 0.0001 H11a_$3 H11b_$3 L.S. 50 PLAN 5 CONF list 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.080900 178.442551 FVAR 0.11886 PD1 6 0.498494 0.366408 0.750000 10.50000 0.00515 0.01198 = 0.00530 0.00000 0.00000 -0.00122 PD2 6 0.015314 0.385189 -0.250000 10.50000 0.00515 0.01198 = 0.00530 0.00000 0.00000 -0.00122 FE1 3 0.757378 0.374297 1.250000 10.50000 0.00388 0.01439 = 0.01141 0.00000 0.00000 -0.00261 FE2 3 0.257009 0.377375 0.250000 10.50000 0.00515 0.01198 = 0.00530 0.00000 0.00000 -0.00122 N1 4 0.767125 0.306350 1.250000 10.50000 0.00388 0.01439 = 0.01141 0.00000 0.00000 -0.00261 N2 4 0.689340 0.241446 1.250000 10.50000 0.00388 0.01439 = 0.01141 0.00000 0.00000 -0.00261 N3 4 0.927361 0.222507 1.250000 10.50000 0.00388 0.01439 = 0.01141 0.00000 0.00000 -0.00261 H3A 2 0.930851 0.194448 1.250000 10.50000 -1.50000 H3B 2 0.981519 0.234917 1.250000 10.50000 -1.50000 N4 4 0.654435 0.371580 1.043552 11.00000 0.00515 0.01198 = 0.00530 0.00000 0.00000 -0.00122 N5 4 0.348865 0.369208 0.442613 11.00000 0.00515 0.01198 = 0.00530 0.00000 0.00000 -0.00122 N6 4 0.223249 0.316067 0.250000 10.50000 0.02032 0.01901 = 0.02963 0.00000 0.00000 -0.00608 N7 4 0.105377 0.266900 0.250000 10.50000 0.02032 0.01901 = 0.02963 0.00000 0.00000 -0.00608 N8 4 0.319007 0.214146 0.250000 10.50000 0.02032 0.01901 = 0.02963 0.00000 0.00000 -0.00608 H8A 2 0.369180 0.209846 0.317173 10.50000 -1.50000 H8B 2 0.281992 0.191945 0.250000 10.50000 -1.50000 N9 4 0.744115 0.443131 1.250000 10.50000 0.00388 0.01439 = 0.01141 0.00000 0.00000 -0.00261 N10 4 0.819982 0.508076 1.250000 10.50000 0.00388 0.01439 = 0.01141 0.00000 0.00000 -0.00261 N11 4 0.583722 0.527845 1.250000 10.50000 0.00388 0.01439 = 0.01141 0.00000 0.00000 -0.00261 H11A 2 0.531298 0.513914 1.250000 10.50000 -1.50000 H11B 2 0.576547 0.555752 1.250000 10.50000 -1.50000 N12 4 0.286744 0.439379 0.250000 10.50000 0.02032 0.01901 = 0.02963 0.00000 0.00000 -0.00608 N13 4 0.404724 0.490290 0.250000 10.50000 0.02032 0.01901 = 0.02963 0.00000 0.00000 -0.00608 N14 4 0.187187 0.541508 0.250000 10.50000 0.02032 0.01901 = 0.02963 0.00000 0.00000 -0.00608 H14A 2 0.209769 0.563177 0.314773 10.50000 -1.50000 H14B 2 0.126838 0.540966 0.250000 10.50000 -1.50000 N15 4 0.166317 0.386652 0.055791 11.00000 0.00515 0.01198 = 0.00530 0.00000 0.00000 -0.00122 N16 4 -0.138628 0.377265 -0.546157 11.00000 0.00515 0.01198 = 0.00530 0.00000 0.00000 -0.00122 C1 1 0.843368 0.285283 1.250000 10.50000 0.00388 0.01439 = 0.01141 0.00000 0.00000 -0.00261 AFIX 43 H1 2 0.896669 0.300366 1.250000 10.50000 -1.20000 AFIX 0 C2 1 0.848797 0.240945 1.250000 10.50000 0.00388 0.01439 = 0.01141 0.00000 0.00000 -0.00261 C3 1 0.764533 0.222389 1.250000 10.50000 0.00388 0.01439 = 0.01141 0.00000 0.00000 -0.00261 AFIX 43 H3 2 0.762766 0.193358 1.250000 10.50000 -1.20000 AFIX 0 C4 1 0.691531 0.283754 1.250000 10.50000 0.00388 0.01439 = 0.01141 0.00000 0.00000 -0.00261 AFIX 43 H4 2 0.637161 0.297986 1.250000 10.50000 -1.20000 AFIX 0 C5 1 0.595932 0.369214 0.940025 11.00000 0.00515 0.01198 = 0.00530 0.00000 0.00000 -0.00122 C6 1 0.403387 0.366666 0.554041 11.00000 0.00515 0.01198 = 0.00530 0.00000 0.00000 -0.00122 C7 1 0.284493 0.286637 0.250000 10.50000 0.02032 0.01901 = 0.02963 0.00000 0.00000 -0.00608 AFIX 43 H7 2 0.344992 0.293702 0.250000 10.50000 -1.20000 AFIX 0 C8 1 0.258797 0.244754 0.250000 10.50000 0.02032 0.01901 = 0.02963 0.00000 0.00000 -0.00608 C9 1 0.165929 0.237223 0.250000 10.50000 0.02032 0.01901 = 0.02963 0.00000 0.00000 -0.00608 AFIX 43 H9 2 0.146351 0.209648 0.250000 10.50000 -1.20000 AFIX 0 C10 1 0.135119 0.305788 0.250000 10.50000 0.02032 0.01901 = 0.02963 0.00000 0.00000 -0.00608 AFIX 43 H10 2 0.093199 0.327293 0.250000 10.50000 -1.20000 AFIX 0 C11 1 0.666986 0.464453 1.250000 10.50000 0.00388 0.01439 = 0.01141 0.00000 0.00000 -0.00261 AFIX 43 H11 2 0.613894 0.449210 1.250000 10.50000 -1.20000 AFIX 0 C12 1 0.660411 0.508120 1.250000 10.50000 0.00388 0.01439 = 0.01141 0.00000 0.00000 -0.00261 C13 1 0.745784 0.528063 1.250000 10.50000 0.00388 0.01439 = 0.01141 0.00000 0.00000 -0.00261 AFIX 43 H13 2 0.747638 0.557093 1.250000 10.50000 -1.20000 AFIX 0 C14 1 0.819202 0.466050 1.250000 10.50000 0.00388 0.01439 = 0.01141 0.00000 0.00000 -0.00261 AFIX 43 H14 2 0.873950 0.452136 1.250000 10.50000 -1.20000 AFIX 0 C15 1 0.223637 0.467905 0.250000 10.50000 0.02032 0.01901 = 0.02963 0.00000 0.00000 -0.00608 AFIX 43 H15 2 0.163448 0.460289 0.250000 10.50000 -1.20000 AFIX 0 C16 1 0.248928 0.510530 0.250000 10.50000 0.02032 0.01901 = 0.02963 0.00000 0.00000 -0.00608 C17 1 0.340993 0.518466 0.250000 10.50000 0.02032 0.01901 = 0.02963 0.00000 0.00000 -0.00608 AFIX 43 H17 2 0.358722 0.546311 0.250000 10.50000 -1.20000 AFIX 0 C18 1 0.371037 0.451364 0.250000 10.50000 0.02032 0.01901 = 0.02963 0.00000 0.00000 -0.00608 AFIX 43 H18 2 0.413188 0.429957 0.250000 10.50000 -1.20000 AFIX 0 C19 1 0.110974 0.387619 -0.053916 11.00000 0.00515 0.01198 = 0.00530 0.00000 0.00000 -0.00122 C20 1 -0.079421 0.380314 -0.441915 11.00000 0.00515 0.01198 = 0.00530 0.00000 0.00000 -0.00122 PART -1 O1 5 10.504549 10.232679 11.250000 10.25000 0.03364 AFIX 147 H1A 2 0.489748 0.253943 1.305869 10.25000 -1.50000 AFIX 0 C21 1 10.499149 10.239669 11.056419 10.25000 0.03364 AFIX 137 H21A 2 0.544001 0.223332 0.993861 10.25000 -1.50000 H21B 2 0.508968 0.268743 1.030883 10.25000 -1.50000 H21C 2 0.440793 0.231703 1.012386 10.25000 -1.50000 AFIX 0 O2 5 1.001782 0.516264 1.209239 10.25000 0.02035 AFIX 147 H2 2 1.004833 0.493214 1.159756 10.25000 -1.50000 AFIX 0 C22 1 1.004137 0.511576 1.406928 10.25000 0.02035 AFIX 137 H22A 2 0.998872 0.482536 1.438380 10.25000 -1.50000 H22B 2 0.955250 0.526777 1.461612 10.25000 -1.50000 H22C 2 1.059877 0.522255 1.454064 10.25000 -1.50000 AFIX 0 HKLF 4 REM rt312_nh2pympdmeoh_100k_a.res in Pbcm REM wR2 = 0.2765, GooF = S = 1.043, Restrained GooF = 1.041 for all data REM R1 = 0.1088 for 2486 Fo > 4sig(Fo) and 0.1465 for all 3757 data REM 131 parameters refined using 14 restraints END WGHT 0.0812 178.5517 REM Highest difference peak 5.519, deepest hole -3.618, 1-sigma level 0.332 Q1 1 0.5395 0.3606 0.7500 10.50000 0.05 5.52 Q2 1 -0.0482 0.3871 -0.2500 10.50000 0.05 5.04 Q3 1 1.0000 0.5000 1.5000 10.50000 0.05 2.47 Q4 1 0.4978 0.3311 0.7500 10.50000 0.05 2.25 Q5 1 0.4933 0.2500 1.0000 10.50000 0.05 2.24 ; _shelx_res_checksum 74525 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.053 _oxdiff_exptl_absorpt_empirical_full_min 0.954 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_rt457_fenh2pymptetoh_100ka_2 _database_code_depnum_ccdc_archive 'CCDC 2018387' loop_ _audit_author_name _audit_author_address 'Carlos Bartual-Murgui' ;Universitat de Valencia Spain ; _audit_update_record ; 2020-09-17 deposited with the CCDC. 2020-09-22 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT971_rt457_fenh2pymptetoh_100ka_2 ; PROBLEM: Check Calcd Resid. Dens. 0.85A From Pt1 14.97 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_rt457_fenh2pymptetoh_100ka_2_2 ; PROBLEM: Check Calcd Resid. Dens. 1.04A From Pt1 13.74 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_rt457_fenh2pymptetoh_100ka_2_3 ; PROBLEM: Check Calcd Resid. Dens. 0.95A From Pt1 6.10 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_rt457_fenh2pymptetoh_100ka_2_4 ; PROBLEM: Check Calcd Resid. Dens. 0.98A From Pt1 4.19 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt457_fenh2pymptetoh_100ka_2 ; PROBLEM: Check Calcd Resid. Dens. 0.80A From Pt1 -5.48 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt457_fenh2pymptetoh_100ka_2_2 ; PROBLEM: Check Calcd Resid. Dens. 0.87A From Pt1 -5.25 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt457_fenh2pymptetoh_100ka_2_3 ; PROBLEM: Check Calcd Resid. Dens. 1.65A From Pt1 -4.19 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT097_rt457_fenh2pymptetoh_100ka_2 ; PROBLEM: Large Reported Max. (Positive) Residual Density 14.24 eA-3 RESPONSE: The crystal may be damaged during the dehydration/readsorption/SCO processes. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT342_rt457_fenh2pymptetoh_100ka_2 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0625 Ang. RESPONSE: The crystal may be damaged during the dehydration/readsorption/SCO processes. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT971_rt457_fenh2pymptetoh_100ka_2_5 ; PROBLEM: Check Calcd Resid. Dens. 0.81A From Fe2 2.73 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_rt457_fenh2pymptetoh_100ka_2_6 ; PROBLEM: Check Calcd Resid. Dens. 0.27A From Pt1 2.71 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_rt457_fenh2pymptetoh_100ka_2_7 ; PROBLEM: Check Calcd Resid. Dens. 0.79A From Fe2 2.69 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_rt457_fenh2pymptetoh_100ka_2_8 ; PROBLEM: Check Calcd Resid. Dens. 0.59A From Fe1 2.56 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT976_rt457_fenh2pymptetoh_100ka_2 ; PROBLEM: Check Calcd Resid. Dens. 0.62A From N3 -1.52 eA-3 RESPONSE: The residual electronic density may be due to the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; # Added during the CSD deposition process: Thursday 17 September 2020 12:29 PM # end Validation Reply Form _audit_creation_date 2020-09-09 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C12 H10 Fe N10 Pt, C0.8 O0.4' _chemical_formula_sum 'C12.80 H10 Fe N10 O0.40 Pt' _chemical_formula_weight 561.25 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_H-M_alt 'I 1 2/m 1' _space_group_name_Hall '-I 2y' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 14.8483(15) _cell_length_b 7.1717(7) _cell_length_c 15.880(3) _cell_angle_alpha 90 _cell_angle_beta 92.699(11) _cell_angle_gamma 90 _cell_volume 1689.2(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 1016 _cell_measurement_temperature 99.5(7) _cell_measurement_theta_max 27.1560 _cell_measurement_theta_min 4.0760 _shelx_estimated_absorpt_T_max 0.838 _shelx_estimated_absorpt_T_min 0.341 _exptl_absorpt_coefficient_mu 9.153 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.70140 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 2.207 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1056 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_unetI/netI 0.0928 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.862 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 3591 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.862 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.938 _diffrn_reflns_theta_min 3.672 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 99.5(7) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0267 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.862 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -90.00 -38.00 1.00 5.00 -- -18.04 178.00 60.00 52 2 \w -40.00 -1.00 1.00 5.00 -- -18.04 -77.00-150.00 39 3 \w 4.00 32.00 1.00 5.00 -- 18.82 77.00 120.00 28 4 \w -54.00 52.00 1.00 5.00 -- 18.82 -19.00-120.00 106 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0112584000 _diffrn_orient_matrix_UB_12 0.0862855000 _diffrn_orient_matrix_UB_13 0.0188818000 _diffrn_orient_matrix_UB_21 0.0167813000 _diffrn_orient_matrix_UB_22 -0.0333653000 _diffrn_orient_matrix_UB_23 0.0397051000 _diffrn_orient_matrix_UB_31 0.0433174000 _diffrn_orient_matrix_UB_32 0.0351333000 _diffrn_orient_matrix_UB_33 -0.0081398000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1857 _reflns_number_total 2079 _reflns_odcompleteness_completeness 99.41 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 14.244 _refine_diff_density_min -4.872 _refine_diff_density_rms 0.577 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.196 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 107 _refine_ls_number_reflns 2079 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1277 _refine_ls_R_factor_gt 0.1183 _refine_ls_restrained_S_all 1.194 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1097P)^2^+251.2023P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2800 _refine_ls_wR_factor_ref 0.2875 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All N(H,H) groups 2. Restrained distances N8-H8B 0.9 with sigma of 0.0001 N8-H8A 0.9 with sigma of 0.0001 N3-H3B 0.9 with sigma of 0.0001 H3A-N3 0.9 with sigma of 0.0001 H8B-O1 2.2 with sigma of 0.0001 H8A-H8B 1.5 with sigma of 0.0001 H3A-H3B 1.5 with sigma of 0.0001 3. Uiso/Uaniso restraints and constraints Uanis(N6) = Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(N7) = Uanis(C10) = Uanis(N8) Uanis(C4) = Uanis(N1) = Uanis(C2) = Uanis(C3) = Uanis(N2) = Uanis(N3) 4. Others Fixed Sof: H8B(0.5) O1(0.2) C11(0.4) 5.a Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C4(H4), C7(H7), C9(H9), C10(H10) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.74039(8) 0.500000 0.48186(8) 0.0229(4) Uani 1 2 d S T P . . Fe1 Fe 1.000000 1.000000 0.500000 0.0186(11) Uani 1 4 d S T P . . Fe2 Fe 0.500000 0.000000 0.500000 0.0170(11) Uani 1 4 d S T P . . N1 N 1.002(2) 1.000000 0.368(2) 0.045(3) Uani 1 2 d S T P . . N2 N 0.922(2) 1.000000 0.231(2) 0.045(3) Uani 1 2 d S T P . . N3 N 1.15281(18) 1.000000 0.19236(14) 0.045(3) Uani 1 2 d DS T P . . H3A H 1.1553(4) 1.000000 0.13585(13) 0.068 Uiso 1 2 d DS U P . . H3B H 1.2077(2) 1.000000 0.2190(2) 0.068 Uiso 1 2 d DS U P . . N4 N 0.8958(11) 0.798(3) 0.4938(11) 0.023(4) Uani 1 1 d . . . . . N5 N 0.5898(11) 0.195(2) 0.4814(11) 0.021(3) Uani 1 1 d . . . . . N6 N 0.459(2) 0.000000 0.376(2) 0.044(3) Uani 1 2 d S T P . . N7 N 0.335(2) 0.000000 0.273(2) 0.044(3) Uani 1 2 d S T P . . N8 N 0.5447(2) 0.000000 0.16772(15) 0.044(3) Uani 1 2 d DS T P . . H8A H 0.5226(3) 0.000000 0.11396(17) 0.066 Uiso 1 2 d DS U P . . H8B H 0.59174(16) 0.0779(5) 0.1763(2) 0.066 Uiso 0.5 1 d D U P . . C1 C 1.078(2) 1.000000 0.323(3) 0.036(8) Uani 1 2 d S T P . . H1 H 1.133440 1.000000 0.352464 0.043 Uiso 1 2 calc R U P . . C2 C 1.076(3) 1.000000 0.234(3) 0.045(3) Uani 1 2 d S T P . . C3 C 0.992(3) 1.000000 0.190(3) 0.045(3) Uani 1 2 d S T P . . H3 H 0.988486 1.000000 0.131655 0.054 Uiso 1 2 calc R U P . . C4 C 0.929(3) 1.000000 0.315(3) 0.045(3) Uani 1 2 d S T P . . H4 H 0.874476 1.000000 0.341273 0.054 Uiso 1 2 calc R U P . . C5 C 0.8366(15) 0.688(3) 0.4887(13) 0.025(4) Uani 1 1 d . . . . . C6 C 0.6433(12) 0.305(3) 0.4785(13) 0.020(4) Uani 1 1 d . . . . . C7 C 0.516(3) 0.000000 0.315(2) 0.044(3) Uani 1 2 d S T P . . H7 H 0.577700 0.000000 0.329561 0.053 Uiso 1 2 calc R U P . . C8 C 0.488(3) 0.000000 0.229(3) 0.044(3) Uani 1 2 d S T P . . C9 C 0.393(3) 0.000000 0.214(3) 0.044(3) Uani 1 2 d S T P . . H9 H 0.370181 0.000000 0.158247 0.053 Uiso 1 2 calc R U P . . C10 C 0.372(3) 0.000000 0.351(3) 0.044(3) Uani 1 2 d S T P . . H10 H 0.331643 0.000000 0.393747 0.053 Uiso 1 2 calc R U P . . O1 O 0.7259(2) 0.000000 0.2296(6) 0.08(3) Uiso 0.4 2 d DS . P . . C11 C 0.732(7) -0.176(15) 0.262(7) 0.08(3) Uiso 0.4 1 d . . P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0277(6) 0.0040(5) 0.0372(7) 0.000 0.0034(4) 0.000 Fe1 0.015(3) 0.004(2) 0.036(3) 0.000 -0.002(2) 0.000 Fe2 0.017(3) 0.005(2) 0.029(3) 0.000 -0.002(2) 0.000 N1 0.041(8) 0.043(9) 0.051(8) 0.000 -0.005(6) 0.000 N2 0.041(8) 0.043(9) 0.051(8) 0.000 -0.005(6) 0.000 N3 0.041(8) 0.043(9) 0.051(8) 0.000 -0.005(6) 0.000 N4 0.018(8) 0.013(8) 0.040(10) -0.001(7) 0.006(7) 0.002(7) N5 0.022(8) 0.010(8) 0.031(9) 0.000(7) -0.001(6) -0.005(7) N6 0.060(9) 0.027(7) 0.046(7) 0.000 0.011(6) 0.000 N7 0.060(9) 0.027(7) 0.046(7) 0.000 0.011(6) 0.000 N8 0.060(9) 0.027(7) 0.046(7) 0.000 0.011(6) 0.000 C1 0.026(16) 0.014(15) 0.07(2) 0.000 0.012(15) 0.000 C2 0.041(8) 0.043(9) 0.051(8) 0.000 -0.005(6) 0.000 C3 0.041(8) 0.043(9) 0.051(8) 0.000 -0.005(6) 0.000 C4 0.041(8) 0.043(9) 0.051(8) 0.000 -0.005(6) 0.000 C5 0.036(11) 0.014(9) 0.025(10) 0.005(8) 0.005(8) 0.014(9) C6 0.016(8) 0.013(9) 0.031(10) -0.003(8) 0.001(7) 0.002(8) C7 0.060(9) 0.027(7) 0.046(7) 0.000 0.011(6) 0.000 C8 0.060(9) 0.027(7) 0.046(7) 0.000 0.011(6) 0.000 C9 0.060(9) 0.027(7) 0.046(7) 0.000 0.011(6) 0.000 C10 0.060(9) 0.027(7) 0.046(7) 0.000 0.011(6) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C5 1.96(2) 6_565 ? Pt1 C5 1.96(2) . ? Pt1 C6 2.01(2) 6_565 ? Pt1 C6 2.01(2) . ? Fe1 N1 2.10(3) 5_776 ? Fe1 N1 2.10(3) . ? Fe1 N4 2.118(17) 2_756 ? Fe1 N4 2.118(17) . ? Fe1 N4 2.118(17) 6_575 ? Fe1 N4 2.118(17) 5_776 ? Fe2 N5 1.965(16) . ? Fe2 N5 1.965(16) 5_656 ? Fe2 N5 1.965(16) 2_656 ? Fe2 N5 1.965(16) 6 ? Fe2 N6 2.03(3) . ? Fe2 N6 2.03(3) 5_656 ? N1 C1 1.36(5) . ? N1 C4 1.34(5) . ? N2 C3 1.25(5) . ? N2 C4 1.34(5) . ? N3 H3A 0.90000(18) . ? N3 H3B 0.90000(13) . ? N3 C2 1.35(4) . ? N4 C5 1.18(3) . ? N5 C6 1.12(3) . ? N6 C7 1.31(5) . ? N6 C10 1.34(5) . ? N7 C9 1.30(5) . ? N7 C10 1.33(5) . ? N8 H8A 0.90000(18) . ? N8 H8B 0.90000(12) . ? N8 H8B 0.89999(12) 6 ? N8 C8 1.31(4) . ? C1 H1 0.9300 . ? C1 C2 1.41(6) . ? C2 C3 1.40(5) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C7 H7 0.9300 . ? C7 C8 1.42(6) . ? C8 C9 1.43(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? O1 C11 1.36(11) 6 ? O1 C11 1.36(11) . ? C11 C11 1.3(2) 7_645 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Pt1 C5 86.8(11) 6_565 . ? C5 Pt1 C6 178.2(8) 6_565 6_565 ? C5 Pt1 C6 92.5(8) . 6_565 ? C5 Pt1 C6 92.5(8) 6_565 . ? C5 Pt1 C6 178.2(8) . . ? C6 Pt1 C6 88.2(11) 6_565 . ? N1 Fe1 N1 180.0 5_776 . ? N1 Fe1 N4 90.2(8) 5_776 . ? N1 Fe1 N4 90.2(8) . 5_776 ? N1 Fe1 N4 89.8(8) 5_776 5_776 ? N1 Fe1 N4 89.8(8) . 6_575 ? N1 Fe1 N4 90.2(8) 5_776 6_575 ? N1 Fe1 N4 89.8(8) . . ? N1 Fe1 N4 89.8(8) 5_776 2_756 ? N1 Fe1 N4 90.2(8) . 2_756 ? N4 Fe1 N4 93.7(9) 5_776 6_575 ? N4 Fe1 N4 180.0 . 5_776 ? N4 Fe1 N4 86.3(9) 5_776 2_756 ? N4 Fe1 N4 86.3(9) . 6_575 ? N4 Fe1 N4 93.7(9) . 2_756 ? N4 Fe1 N4 180.0 6_575 2_756 ? N5 Fe2 N5 89.1(10) 5_656 6 ? N5 Fe2 N5 180.0(10) 6 2_656 ? N5 Fe2 N5 90.9(10) 5_656 2_656 ? N5 Fe2 N5 90.9(10) 6 . ? N5 Fe2 N5 180.0 5_656 . ? N5 Fe2 N5 89.1(10) 2_656 . ? N5 Fe2 N6 91.5(8) 5_656 5_656 ? N5 Fe2 N6 88.5(8) 2_656 . ? N5 Fe2 N6 91.5(8) 2_656 5_656 ? N5 Fe2 N6 88.5(8) 6 5_656 ? N5 Fe2 N6 88.5(8) 5_656 . ? N5 Fe2 N6 91.5(8) . . ? N5 Fe2 N6 88.5(8) . 5_656 ? N5 Fe2 N6 91.5(8) 6 . ? N6 Fe2 N6 180.0 . 5_656 ? C1 N1 Fe1 125(3) . . ? C4 N1 Fe1 126(3) . . ? C4 N1 C1 109(4) . . ? C3 N2 C4 119(4) . . ? H3A N3 H3B 112.89(2) . . ? C2 N3 H3A 124.6(17) . . ? C2 N3 H3B 122.5(17) . . ? C5 N4 Fe1 178.2(17) . . ? C6 N5 Fe2 173.5(17) . . ? C7 N6 Fe2 123(3) . . ? C7 N6 C10 115(4) . . ? C10 N6 Fe2 122(3) . . ? C9 N7 C10 114(4) . . ? H8A N8 H8B 112.89(2) . 6 ? H8A N8 H8B 112.89(2) . . ? H8B N8 H8B 76.8(6) . 6 ? C8 N8 H8A 119.0(19) . . ? C8 N8 H8B 114.0(14) . 6 ? C8 N8 H8B 114.0(14) . . ? N1 C1 H1 118.4 . . ? N1 C1 C2 123(3) . . ? C2 C1 H1 118.4 . . ? N3 C2 C1 121(3) . . ? N3 C2 C3 121(4) . . ? C3 C2 C1 118(4) . . ? N2 C3 C2 119(4) . . ? N2 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? N1 C4 N2 131(4) . . ? N1 C4 H4 114.5 . . ? N2 C4 H4 114.5 . . ? N4 C5 Pt1 178.3(18) . . ? N5 C6 Pt1 176.2(18) . . ? N6 C7 H7 118.5 . . ? N6 C7 C8 123(4) . . ? C8 C7 H7 118.5 . . ? N8 C8 C7 123(4) . . ? N8 C8 C9 123(3) . . ? C7 C8 C9 114(4) . . ? N7 C9 C8 124(4) . . ? N7 C9 H9 117.8 . . ? C8 C9 H9 117.8 . . ? N6 C10 H10 115.4 . . ? N7 C10 N6 129(4) . . ? N7 C10 H10 115.4 . . ? C11 O1 C11 135(9) 6 . ? C11 C11 O1 133(10) 7_645 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 N1 C1 C2 180.000(4) . . . . ? Fe1 N1 C4 N2 180.000(4) . . . . ? Fe2 N6 C7 C8 180.000(4) . . . . ? Fe2 N6 C10 N7 180.000(5) . . . . ? N1 C1 C2 N3 180.000(4) . . . . ? N1 C1 C2 C3 0.000(5) . . . . ? N3 C2 C3 N2 180.000(3) . . . . ? N6 C7 C8 N8 180.000(4) . . . . ? N6 C7 C8 C9 0.000(5) . . . . ? N8 C8 C9 N7 180.000(3) . . . . ? C1 N1 C4 N2 0.000(5) . . . . ? C1 C2 C3 N2 0.000(4) . . . . ? C3 N2 C4 N1 0.000(5) . . . . ? C4 N1 C1 C2 0.000(5) . . . . ? C4 N2 C3 C2 0.000(3) . . . . ? C7 N6 C10 N7 0.000(6) . . . . ? C7 C8 C9 N7 0.000(4) . . . . ? C9 N7 C10 N6 0.000(6) . . . . ? C10 N6 C7 C8 0.000(6) . . . . ? C10 N7 C9 C8 0.000(5) . . . . ? C11 O1 C11 C11 -139(12) 6 . . 7_645 ? _shelx_res_file ; TITL rt457_fenh2pymptetoh_100ka_2_a.res in I2/m rt457_fenh2pymptetoh_100ka_2.res created by SHELXL-2018/3 at 13:41:57 on 09-Sep-2020 REM Old TITL RT457_FeNH2PymPtEtOH_100Ka_2 in I2/m REM SHELXT solution in I2/m: R1 0.177, Rweak 0.033, Alpha 0.025 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C13 N3 Fe I CELL 0.71073 14.8483 7.1717 15.8801 90 92.699 90 ZERR 4 0.0015 0.0007 0.0026 0 0.011 0 LATT 2 SYMM -X,+Y,-Z SFAC C H Fe N O Pt UNIT 51.2 40 4 40 1.6 4 EADP N6 C7 C8 C9 N7 C10 N8 EADP C4 N1 C2 C3 N2 N3 DANG 2.2 0.0001 H8b O1 DFIX 0.9 0.0001 N8 H8b DFIX 0.9 0.0001 N8 H8a DANG 1.5 0.0001 H8a H8b DANG 1.5 0.0001 H3a H3b DFIX 0.9 0.0001 N3 H3b DFIX 0.9 0.0001 H3a N3 L.S. 50 PLAN 1 SIZE 0.15 0.15 0.02 CONF list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.109700 251.202301 FVAR 0.15659 PT1 6 0.740394 0.500000 0.481858 10.50000 0.02765 0.00404 = 0.03719 0.00000 0.00344 0.00000 FE1 3 1.000000 1.000000 0.500000 10.25000 0.01548 0.00376 = 0.03629 0.00000 -0.00165 0.00000 FE2 3 0.500000 0.000000 0.500000 10.25000 0.01697 0.00522 = 0.02858 0.00000 -0.00247 0.00000 N1 4 1.001775 1.000000 0.368044 10.50000 0.04091 0.04312 = 0.05138 0.00000 -0.00518 0.00000 N2 4 0.921605 1.000000 0.230604 10.50000 0.04091 0.04312 = 0.05138 0.00000 -0.00518 0.00000 N3 4 1.152814 1.000000 0.192364 10.50000 0.04091 0.04312 = 0.05138 0.00000 -0.00518 0.00000 H3A 2 1.155313 1.000000 0.135847 10.50000 -1.50000 H3B 2 1.207699 1.000000 0.218952 10.50000 -1.50000 N4 4 0.895834 0.797945 0.493824 11.00000 0.01757 0.01284 = 0.04023 -0.00064 0.00636 0.00220 N5 4 0.589771 0.195176 0.481356 11.00000 0.02154 0.01023 = 0.03097 -0.00015 -0.00061 -0.00513 N6 4 0.459290 0.000000 0.375938 10.50000 0.06014 0.02707 = 0.04606 0.00000 0.01096 0.00000 N7 4 0.334960 0.000000 0.272985 10.50000 0.06014 0.02707 = 0.04606 0.00000 0.01096 0.00000 N8 4 0.544691 0.000000 0.167722 10.50000 0.06014 0.02707 = 0.04606 0.00000 0.01096 0.00000 H8A 2 0.522613 0.000000 0.113960 10.50000 -1.50000 H8B 2 0.591742 0.077929 0.176290 10.50000 -1.50000 C1 1 1.077742 1.000000 0.323112 10.50000 0.02580 0.01444 = 0.06789 0.00000 0.01245 0.00000 AFIX 43 H1 2 1.133440 1.000000 0.352464 10.50000 -1.20000 AFIX 0 C2 1 1.075946 1.000000 0.234233 10.50000 0.04091 0.04312 = 0.05138 0.00000 -0.00518 0.00000 C3 1 0.991935 1.000000 0.190282 10.50000 0.04091 0.04312 = 0.05138 0.00000 -0.00518 0.00000 AFIX 43 H3 2 0.988486 1.000000 0.131655 10.50000 -1.20000 AFIX 0 C4 1 0.929180 1.000000 0.315058 10.50000 0.04091 0.04312 = 0.05138 0.00000 -0.00518 0.00000 AFIX 43 H4 2 0.874476 1.000000 0.341273 10.50000 -1.20000 AFIX 0 C5 1 0.836551 0.687995 0.488723 11.00000 0.03595 0.01378 = 0.02489 0.00491 0.00502 0.01359 C6 1 0.643255 0.305246 0.478534 11.00000 0.01590 0.01311 = 0.03077 -0.00316 0.00140 0.00216 C7 1 0.516258 0.000000 0.315168 10.50000 0.06014 0.02707 = 0.04606 0.00000 0.01096 0.00000 AFIX 43 H7 2 0.577700 0.000000 0.329561 10.50000 -1.20000 AFIX 0 C8 1 0.488287 0.000000 0.228675 10.50000 0.06014 0.02707 = 0.04606 0.00000 0.01096 0.00000 C9 1 0.392687 0.000000 0.213899 10.50000 0.06014 0.02707 = 0.04606 0.00000 0.01096 0.00000 AFIX 43 H9 2 0.370181 0.000000 0.158247 10.50000 -1.20000 AFIX 0 C10 1 0.372041 0.000000 0.350737 10.50000 0.06014 0.02707 = 0.04606 0.00000 0.01096 0.00000 AFIX 43 H10 2 0.331643 0.000000 0.393747 10.50000 -1.20000 AFIX 0 O1 5 0.725918 0.000000 0.229625 10.20000 0.08092 C11 1 0.731919 -0.175565 0.262182 10.40000 0.07658 HKLF 4 REM rt457_fenh2pymptetoh_100ka_2_a.res in I2/m REM wR2 = 0.2875, GooF = S = 1.196, Restrained GooF = 1.194 for all data REM R1 = 0.1183 for 1857 Fo > 4sig(Fo) and 0.1277 for all 2079 data REM 107 parameters refined using 7 restraints END WGHT 0.1098 251.1948 REM Highest difference peak 14.244, deepest hole -4.872, 1-sigma level 0.577 Q1 1 0.7990 0.5000 0.4823 10.50000 0.05 14.24 ; _shelx_res_checksum 90664 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.358 _oxdiff_exptl_absorpt_empirical_full_min 0.763 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mo_rt327_5apmdpt_120kdes_0ma _database_code_depnum_ccdc_archive 'CCDC 2018382' loop_ _audit_author_name _audit_author_address 'Carlos Bartual-Murgui' ;Universitat de Valencia Spain ; _audit_update_record ; 2020-07-22 deposited with the CCDC. 2020-09-22 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT971_mo_rt327_5apmdpt_120kdes_0ma ; PROBLEM: Check Calcd Resid. Dens. 0.67A From Pt1 4.68 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the dehydration/SCO processesand. ; _vrf_PLAT971_mo_rt327_5apmdpt_120kdes_0ma_2 ; PROBLEM: Check Calcd Resid. Dens. 1.44A From C9 3.83 eA-3 RESPONSE: The residual electronic density may be due to a strong absorption of the C and the deterioration of the crystal during the dehydration/SCO processes. ; _vrf_PLAT972_mo_rt327_5apmdpt_120kdes_0ma ; PROBLEM: Check Calcd Resid. Dens. 1.53A From C10 -5.51 eA-3 RESPONSE: The residual electronic density may be due to a strong absorption of the C and the deterioration of the crystal during the dehydration/SCO processes. ; _vrf_PLAT972_mo_rt327_5apmdpt_120kdes_0ma_2 ; PROBLEM: Check Calcd Resid. Dens. 1.41A From C10 -4.87 eA-3 RESPONSE: The residual electronic density may be due to a strong absorption of the C and the deterioration of the crystal during the dehydration/SCO processes. ; _vrf_PLAT934_mo_rt327_5apmdpt_120kdes_0ma ; PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers .. 2 Check RESPONSE: This alerts arises from 3 slighly disagreeable reflections in our refinements which were not omited as we believe that the difference between I(obs) and I(calc) was not two large. ; _vrf_PLAT971_mo_rt327_5apmdpt_120kdes_0ma_3 ; PROBLEM: Check Calcd Resid. Dens. 1.19A From Pt1 2.63 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the dehydration/SCO processes. ; _vrf_PLAT971_mo_rt327_5apmdpt_120kdes_0ma_4 ; PROBLEM: Check Calcd Resid. Dens. 1.05A From Pt1 2.54 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the dehydration/SCO processes. ; _vrf_PLAT972_mo_rt327_5apmdpt_120kdes_0ma_3 ; PROBLEM: Check Calcd Resid. Dens. 0.58A From Pt1 -3.11 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the dehydration/SCO processes. ; _vrf_PLAT972_mo_rt327_5apmdpt_120kdes_0ma_4 ; PROBLEM: Check Calcd Resid. Dens. 1.64A From N3 -2.74 eA-3 RESPONSE: The residual electronic density may be due to a strong absorption of the N atom and the deterioration of the crystal during the dehydration/SCO processes. ; _vrf_PLAT972_mo_rt327_5apmdpt_120kdes_0ma_5 ; PROBLEM: Check Calcd Resid. Dens. 0.71A From Pt1 -2.70 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the dehydration/SCO processes. ; # Added during the CSD deposition process: Wednesday 22 July 2020 04:49 PM # end Validation Reply Form _audit_creation_date 2020-07-01 _audit_creation_method ; Olex2 1.3 (compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C12 H10 Fe N10 Pt' _chemical_formula_sum 'C12 H10 Fe N10 Pt' _chemical_formula_weight 545.24 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_H-M_alt 'P n m a' _space_group_name_Hall '-P 2ac 2n' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.1282(6) _cell_length_b 7.1968(3) _cell_length_c 15.7460(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1601.02(12) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6154 _cell_measurement_temperature 120(1) _cell_measurement_theta_max 31.89 _cell_measurement_theta_min 2.88 _shelx_estimated_absorpt_T_max 0.445 _shelx_estimated_absorpt_T_min 0.275 _exptl_absorpt_coefficient_mu 9.651 _exptl_absorpt_correction_T_max 0.7463 _exptl_absorpt_correction_T_min 0.4608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1160 before and 0.0628 after correction. The Ratio of minimum to maximum transmission is 0.6174. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 2.262 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1024 _exptl_crystal_preparation ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.1 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_unetI/netI 0.0501 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.951 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 14492 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.951 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.978 _diffrn_reflns_theta_min 2.884 _diffrn_ambient_temperature 120(1) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.951 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2240 _reflns_number_total 2821 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 4.687 _refine_diff_density_min -5.113 _refine_diff_density_rms 0.361 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 135 _refine_ls_number_reflns 2821 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0470 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+52.1055P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1059 _refine_ls_wR_factor_ref 0.1169 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H,H) groups 2. Others Fixed Sof: H6A(0.5) H6B(0.5) H8A(0.5) H8B(0.5) 3.a Rotating group: N6(H6A,H6B), N8(H8A,H8B) 3.b Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.53026(3) 1.250000 0.23872(2) 0.01133(11) Uani 1 2 d S T P . . Fe1 Fe 0.77940(10) 0.750000 0.26990(9) 0.0114(3) Uani 1 2 d S T P . . N1 N 0.7672(7) 0.750000 0.3960(6) 0.0167(18) Uani 1 2 d S T P . . N2 N 0.7890(7) 0.750000 0.1430(6) 0.0169(18) Uani 1 2 d S T P . . N3 N 0.6841(4) 0.9405(9) 0.2618(4) 0.0129(11) Uani 1 1 d . . . . . C10 C 0.4328(5) 1.4452(10) 0.2284(5) 0.0132(13) Uani 1 1 d . . . . . N5 N 0.8417(9) 0.750000 0.5313(7) 0.030(3) Uani 1 2 d S T P . . N6 N 0.5852(9) 0.750000 0.5601(7) 0.036(3) Uani 1 2 d S T P . . H6A H 0.540981 0.703357 0.525192 0.043 Uiso 0.5 1 d R U P . . H6B H 0.585021 0.681173 0.607542 0.043 Uiso 0.5 1 d R U P . . N7 N 0.8858(10) 0.750000 0.0202(7) 0.032(3) Uani 1 2 d S T P . . N8 N 0.6402(11) 0.750000 -0.0461(9) 0.044(4) Uani 1 2 d S T P . . H8A H 0.626454 0.635159 -0.060928 0.053 Uiso 0.5 1 d R U P . . H8B H 0.592577 0.797867 -0.017582 0.053 Uiso 0.5 1 d R U P . . C1 C 0.6820(9) 0.750000 0.4343(7) 0.021(2) Uani 1 2 d S T P . . H1 H 0.626565 0.750000 0.400080 0.025 Uiso 1 2 calc R U P . . C2 C 0.6723(9) 0.750000 0.5226(8) 0.021(2) Uani 1 2 d S T P . . C3 C 0.7564(10) 0.750000 0.5688(8) 0.026(3) Uani 1 2 d S T P . . H3 H 0.753321 0.750000 0.629068 0.032 Uiso 1 2 calc R U P . . C4 C 0.8433(10) 0.750000 0.4475(8) 0.024(3) Uani 1 2 d S T P . . H4 H 0.903710 0.750000 0.421028 0.029 Uiso 1 2 calc R U P . . C5 C 0.7126(10) 0.750000 0.0934(8) 0.023(2) Uani 1 2 d S T P . . H5 H 0.651661 0.750000 0.119000 0.028 Uiso 1 2 calc R U P . . C6 C 0.7194(11) 0.750000 0.0055(8) 0.029(3) Uani 1 2 d S T P . . C7 C 0.8111(13) 0.750000 -0.0287(8) 0.037(4) Uani 1 2 d S T P . . H7 H 0.819026 0.750000 -0.088600 0.044 Uiso 1 2 calc R U P . . C8 C 0.8740(9) 0.750000 0.1038(8) 0.023(2) Uani 1 2 d S T P . . H8 H 0.929083 0.750000 0.138455 0.028 Uiso 1 2 calc R U P . . C9 C 0.6275(5) 1.0543(10) 0.2535(5) 0.0128(13) Uani 1 1 d . . . . . N4 N 0.3750(4) 1.5599(9) 0.2250(4) 0.0143(12) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.00870(16) 0.00822(17) 0.01706(19) 0.000 -0.00046(14) 0.000 Fe1 0.0083(6) 0.0079(6) 0.0180(7) 0.000 -0.0003(5) 0.000 N1 0.017(5) 0.015(5) 0.018(5) 0.000 -0.004(3) 0.000 N2 0.017(4) 0.014(4) 0.020(5) 0.000 0.003(3) 0.000 N3 0.012(3) 0.009(3) 0.018(3) 0.000(2) -0.001(2) -0.003(2) C10 0.009(3) 0.009(3) 0.022(4) -0.002(3) -0.001(2) 0.000(2) N5 0.031(6) 0.038(7) 0.021(5) 0.000 -0.010(4) 0.000 N6 0.036(7) 0.060(9) 0.011(5) 0.000 0.006(4) 0.000 N7 0.052(8) 0.025(6) 0.020(5) 0.000 0.013(5) 0.000 N8 0.062(10) 0.036(8) 0.035(7) 0.000 -0.023(7) 0.000 C1 0.022(6) 0.025(6) 0.015(5) 0.000 -0.001(4) 0.000 C2 0.026(6) 0.021(6) 0.017(5) 0.000 0.003(4) 0.000 C3 0.037(7) 0.025(7) 0.017(6) 0.000 -0.008(5) 0.000 C4 0.024(6) 0.022(6) 0.026(6) 0.000 -0.009(5) 0.000 C5 0.030(7) 0.016(6) 0.024(6) 0.000 -0.001(5) 0.000 C6 0.050(8) 0.020(6) 0.017(6) 0.000 -0.006(5) 0.000 C7 0.073(12) 0.028(7) 0.010(6) 0.000 0.009(6) 0.000 C8 0.025(6) 0.017(6) 0.028(6) 0.000 0.009(5) 0.000 C9 0.011(3) 0.009(3) 0.018(4) 0.001(3) -0.001(2) -0.001(2) N4 0.011(3) 0.011(3) 0.021(3) 0.000(2) 0.001(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C10 1.974(7) 7_585 ? Pt1 C10 1.974(7) . ? Pt1 C9 1.982(7) . ? Pt1 C9 1.982(7) 7_585 ? Fe1 N1 1.994(10) . ? Fe1 N2 2.003(10) . ? Fe1 N3 1.926(6) 7_575 ? Fe1 N3 1.926(6) . ? Fe1 N4 1.924(6) 6_646 ? Fe1 N4 1.924(6) 4_575 ? N1 C1 1.346(15) . ? N1 C4 1.346(15) . ? N2 C5 1.331(16) . ? N2 C8 1.351(15) . ? N3 C9 1.152(9) . ? C10 N4 1.162(9) . ? N5 C3 1.341(19) . ? N5 C4 1.320(17) . ? N6 H6A 0.90(11) 7_575 ? N6 H6A 0.8968 . ? N6 H6B 0.8966 . ? N6 H6B 0.90(14) 7_575 ? N6 C2 1.365(17) . ? N7 C7 1.31(2) . ? N7 C8 1.327(17) . ? N8 H8A 0.88(3) 7_575 ? N8 H8A 0.8805 . ? N8 H8B 0.8800 . ? N8 H8B 0.88(12) 7_575 ? N8 C6 1.383(19) . ? C1 H1 0.9500 . ? C1 C2 1.398(16) . ? C2 C3 1.394(18) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C5 C6 1.387(18) . ? C6 C7 1.40(2) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Pt1 C10 90.8(4) 7_585 . ? C10 Pt1 C9 89.3(3) 7_585 . ? C10 Pt1 C9 177.9(3) 7_585 7_585 ? C10 Pt1 C9 177.9(3) . . ? C10 Pt1 C9 89.3(3) . 7_585 ? C9 Pt1 C9 90.6(4) 7_585 . ? N1 Fe1 N2 178.9(4) . . ? N3 Fe1 N1 90.3(3) . . ? N3 Fe1 N1 90.3(3) 7_575 . ? N3 Fe1 N2 88.9(3) . . ? N3 Fe1 N2 88.9(3) 7_575 . ? N3 Fe1 N3 90.8(4) . 7_575 ? N4 Fe1 N1 91.1(3) 4_575 . ? N4 Fe1 N1 91.1(3) 6_646 . ? N4 Fe1 N2 89.7(3) 6_646 . ? N4 Fe1 N2 89.7(3) 4_575 . ? N4 Fe1 N3 89.3(2) 4_575 . ? N4 Fe1 N3 178.6(3) 6_646 . ? N4 Fe1 N3 89.3(2) 6_646 7_575 ? N4 Fe1 N3 178.6(3) 4_575 7_575 ? N4 Fe1 N4 90.6(4) 4_575 6_646 ? C1 N1 Fe1 121.6(8) . . ? C1 N1 C4 116.4(10) . . ? C4 N1 Fe1 122.0(9) . . ? C5 N2 Fe1 122.0(8) . . ? C5 N2 C8 117.0(11) . . ? C8 N2 Fe1 121.0(9) . . ? C9 N3 Fe1 177.3(6) . . ? N4 C10 Pt1 178.0(7) . . ? C4 N5 C3 117.1(12) . . ? H6A N6 H6A 44.0 . 7_575 ? H6A N6 H6B 107.6 . . ? H6A N6 H6B 107.6 7_575 7_575 ? H6A N6 H6B 135.7 . 7_575 ? H6B N6 H6A 135.7 . 7_575 ? H6B N6 H6B 67.1 . 7_575 ? C2 N6 H6A 111(3) . 7_575 ? C2 N6 H6A 111.3 . . ? C2 N6 H6B 111(4) . 7_575 ? C2 N6 H6B 111.3 . . ? C7 N7 C8 118.9(13) . . ? H8A N8 H8A 139.6 . 7_575 ? H8A N8 H8B 109.5 7_575 7_575 ? H8A N8 H8B 109.5 . . ? H8A N8 H8B 66.3 . 7_575 ? H8B N8 H8A 66.3 . 7_575 ? H8B N8 H8B 46.1 . 7_575 ? C6 N8 H8A 109.6(6) . 7_575 ? C6 N8 H8A 109.5 . . ? C6 N8 H8B 109(3) . 7_575 ? C6 N8 H8B 108.6 . . ? N1 C1 H1 118.9 . . ? N1 C1 C2 122.2(11) . . ? C2 C1 H1 118.9 . . ? N6 C2 C1 121.2(12) . . ? N6 C2 C3 122.9(11) . . ? C3 C2 C1 115.8(12) . . ? N5 C3 C2 122.4(11) . . ? N5 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? N1 C4 H4 117.0 . . ? N5 C4 N1 126.0(13) . . ? N5 C4 H4 117.0 . . ? N2 C5 H5 119.1 . . ? N2 C5 C6 121.8(13) . . ? C6 C5 H5 119.1 . . ? N8 C6 C5 122.0(15) . . ? N8 C6 C7 121.4(13) . . ? C5 C6 C7 116.6(13) . . ? N7 C7 C6 121.3(12) . . ? N7 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? N2 C8 H8 117.8 . . ? N7 C8 N2 124.3(13) . . ? N7 C8 H8 117.8 . . ? N3 C9 Pt1 179.7(7) . . ? C10 N4 Fe1 174.9(6) . 6_566 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 N1 C1 C2 180.000(2) . . . . ? Fe1 N1 C4 N5 180.000(2) . . . . ? Fe1 N2 C5 C6 180.000(1) . . . . ? Fe1 N2 C8 N7 180.000(1) . . . . ? N1 C1 C2 N6 180.000(2) . . . . ? N1 C1 C2 C3 0.000(3) . . . . ? N2 C5 C6 N8 180.000(1) . . . . ? N2 C5 C6 C7 0.000(1) . . . . ? N6 C2 C3 N5 180.000(2) . . . . ? N8 C6 C7 N7 180.0 . . . . ? C1 N1 C4 N5 0.000(2) . . . . ? C1 C2 C3 N5 0.000(3) . . . . ? C3 N5 C4 N1 0.000(3) . . . . ? C4 N1 C1 C2 0.000(2) . . . . ? C4 N5 C3 C2 0.000(3) . . . . ? C5 N2 C8 N7 0.000(1) . . . . ? C5 C6 C7 N7 0.000(1) . . . . ? C7 N7 C8 N2 0.000(1) . . . . ? C8 N2 C5 C6 0.000(1) . . . . ? C8 N7 C7 C6 0.000(1) . . . . ? _shelx_res_file ; TITL mo_rt327_5apmdpt_120kdes_0ma_a.res in Pnma mo_rt327_5apmdpt_120kdes_0ma.res created by SHELXL-2018/3 at 11:55:25 on 01-Jul-2020 REM Old TITL mo_RT327_5apmdPt_120Kdes_0ma in Pnma REM SHELXT solution in Pnma: R1 0.074, Rweak 0.004, Alpha 0.041 REM 0.919 for 138 systematic absences, Orientation as input REM Formula found by SHELXT: N4 N5 Fe Pt CELL 0.71073 14.1282 7.1968 15.746 90 90 90 ZERR 4 0.0006 0.0003 0.0007 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,-Z SYMM 0.5+X,0.5-Y,0.5-Z SFAC C H Fe N Pt UNIT 48 40 4 40 4 L.S. 20 0 0 PLAN 5 SIZE 0.1 0.18 0.18 TEMP -153.1(10) list 4 fmap 2 53 acta MORE -1 BOND $H CONF REM REM REM WGHT 0.000000 52.105499 FVAR 0.18822 PT1 5 0.530259 1.250000 0.238723 10.50000 0.00870 0.00822 = 0.01706 0.00000 -0.00046 0.00000 FE1 3 0.779404 0.750000 0.269898 10.50000 0.00831 0.00787 = 0.01804 0.00000 -0.00031 0.00000 N1 4 0.767159 0.750000 0.396036 10.50000 0.01700 0.01481 = 0.01844 0.00000 -0.00446 0.00000 N2 4 0.788954 0.750000 0.142963 10.50000 0.01675 0.01361 = 0.02029 0.00000 0.00274 0.00000 N3 4 0.684098 0.940511 0.261786 11.00000 0.01168 0.00947 = 0.01756 -0.00050 -0.00080 -0.00289 C10 1 0.432821 1.445238 0.228437 11.00000 0.00873 0.00932 = 0.02155 -0.00179 -0.00104 0.00002 N5 4 0.841655 0.750000 0.531288 10.50000 0.03069 0.03827 = 0.02086 0.00000 -0.01008 0.00000 N6 4 0.585171 0.750000 0.560081 10.50000 0.03610 0.06045 = 0.01052 0.00000 0.00578 0.00000 AFIX 7 H6A 2 0.540981 0.703357 0.525192 10.50000 -1.20000 H6B 2 0.585021 0.681173 0.607542 10.50000 -1.20000 AFIX 0 N7 4 0.885766 0.750000 0.020230 10.50000 0.05227 0.02533 = 0.01985 0.00000 0.01296 0.00000 N8 4 0.640246 0.750000 -0.046131 10.50000 0.06177 0.03634 = 0.03498 0.00000 -0.02298 0.00000 AFIX 7 H8A 2 0.626454 0.635159 -0.060928 10.50000 -1.20000 H8B 2 0.592577 0.797867 -0.017582 10.50000 -1.20000 AFIX 0 C1 1 0.681967 0.750000 0.434270 10.50000 0.02245 0.02536 = 0.01500 0.00000 -0.00071 0.00000 AFIX 43 H1 2 0.626565 0.750000 0.400080 10.50000 -1.20000 AFIX 0 C2 1 0.672289 0.750000 0.522599 10.50000 0.02639 0.02053 = 0.01745 0.00000 0.00273 0.00000 C3 1 0.756445 0.750000 0.568801 10.50000 0.03661 0.02532 = 0.01685 0.00000 -0.00796 0.00000 AFIX 43 H3 2 0.753321 0.750000 0.629068 10.50000 -1.20000 AFIX 0 C4 1 0.843278 0.750000 0.447483 10.50000 0.02418 0.02217 = 0.02593 0.00000 -0.00860 0.00000 AFIX 43 H4 2 0.903710 0.750000 0.421028 10.50000 -1.20000 AFIX 0 C5 1 0.712568 0.750000 0.093436 10.50000 0.03038 0.01598 = 0.02392 0.00000 -0.00115 0.00000 AFIX 43 H5 2 0.651661 0.750000 0.119000 10.50000 -1.20000 AFIX 0 C6 1 0.719434 0.750000 0.005547 10.50000 0.05013 0.01952 = 0.01725 0.00000 -0.00605 0.00000 C7 1 0.811101 0.750000 -0.028687 10.50000 0.07258 0.02792 = 0.01026 0.00000 0.00903 0.00000 AFIX 43 H7 2 0.819026 0.750000 -0.088600 10.50000 -1.20000 AFIX 0 C8 1 0.874016 0.750000 0.103831 10.50000 0.02486 0.01726 = 0.02824 0.00000 0.00926 0.00000 AFIX 43 H8 2 0.929083 0.750000 0.138455 10.50000 -1.20000 AFIX 0 C9 1 0.627521 1.054289 0.253548 11.00000 0.01121 0.00914 = 0.01814 0.00101 -0.00086 -0.00077 N4 4 0.375011 1.559865 0.224972 11.00000 0.01089 0.01096 = 0.02113 -0.00039 0.00134 -0.00240 HKLF 4 REM mo_rt327_5apmdpt_120kdes_0ma_a.res in Pnma REM wR2 = 0.1169, GooF = S = 1.124, Restrained GooF = 1.124 for all data REM R1 = 0.0470 for 2240 Fo > 4sig(Fo) and 0.0708 for all 2821 data REM 135 parameters refined using 0 restraints END WGHT 0.0000 52.0859 REM Highest difference peak 4.687, deepest hole -5.113, 1-sigma level 0.361 Q1 1 0.5313 1.2500 0.2827 10.50000 0.05 4.69 Q2 1 0.4595 1.2500 0.2776 10.50000 0.05 3.17 Q3 1 0.6557 1.2500 0.2702 10.50000 0.05 3.00 Q4 1 0.3571 1.2500 0.2782 10.50000 0.05 2.18 Q5 1 0.5360 1.2500 0.1649 10.50000 0.05 2.02 ; _shelx_res_checksum 12168 _olex2_submission_special_instructions 'No special instructions were received' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_rt457_fenh2pymptetoh_260ka_2 _database_code_depnum_ccdc_archive 'CCDC 2018386' loop_ _audit_author_name _audit_author_address 'Carlos Bartual-Murgui' ;Universitat de Valencia Spain ; _audit_update_record ; 2020-09-17 deposited with the CCDC. 2020-09-22 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT971_rt457_fenh2pymptetoh_260ka_2 ; PROBLEM: Check Calcd Resid. Dens. 0.95A From Pt1 8.54 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_rt457_fenh2pymptetoh_260ka_2_2 ; PROBLEM: Check Calcd Resid. Dens. 1.03A From Pt1 6.64 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_rt457_fenh2pymptetoh_260ka_2_3 ; PROBLEM: Check Calcd Resid. Dens. 0.76A From Pt1 5.19 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_rt457_fenh2pymptetoh_260ka_2_4 ; PROBLEM: Check Calcd Resid. Dens. 1.02A From Pt1 4.80 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt457_fenh2pymptetoh_260ka_2 ; PROBLEM: Check Calcd Resid. Dens. 0.91A From Pt1 -3.51 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT973_rt457_fenh2pymptetoh_260ka_2 ; PROBLEM: Check Calcd Positive Resid. Density on Pt1 3.72 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT342_rt457_fenh2pymptetoh_260ka_2 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.04 Ang. RESPONSE: The crystal may be damaged during the dehydration/readsorption/SCO processes. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT430_rt457_fenh2pymptetoh_260ka_2 ; PROBLEM: Short Inter D...A Contact N2 ..O1 . 2.80 Ang. RESPONSE: H of ethanol could not be located because of symetry. However the existence of H-bond interactions with the host framework are reported in the paper. ; _vrf_PLAT972_rt457_fenh2pymptetoh_260ka_2_2 ; PROBLEM: Check Calcd Resid. Dens. 0.80A From Pt1 -3.29 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; # Added during the CSD deposition process: Thursday 17 September 2020 12:29 PM # end Validation Reply Form _audit_creation_date 2020-09-09 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C12 H10 Fe N10 Pt, C0.8 O0.4' _chemical_formula_sum 'C12.80 H10 Fe N10 O0.40 Pt' _chemical_formula_weight 561.25 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_H-M_alt 'I 1 2/m 1' _space_group_name_Hall '-I 2y' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 14.9798(16) _cell_length_b 7.3662(6) _cell_length_c 16.181(2) _cell_angle_alpha 90 _cell_angle_beta 91.922(9) _cell_angle_gamma 90 _cell_volume 1784.5(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 1612 _cell_measurement_temperature 260.00(10) _cell_measurement_theta_max 28.6130 _cell_measurement_theta_min 3.9470 _shelx_estimated_absorpt_T_max 0.846 _shelx_estimated_absorpt_T_min 0.356 _exptl_absorpt_coefficient_mu 8.664 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.48136 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 2.089 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1056 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_unetI/netI 0.0606 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.852 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 4353 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.852 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.087 _diffrn_reflns_theta_min 3.647 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 260.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0267 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.852 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -93.00 -64.00 1.00 5.00 -- -17.88-178.00 150.00 29 2 \w 57.00 95.00 1.00 5.00 -- 18.67-173.00-120.00 38 3 \w 29.00 74.00 1.00 5.00 -- 18.67 0.00 -60.00 45 4 \w 11.00 85.00 1.00 5.00 -- 18.67 57.00 60.00 74 5 \w -52.00 12.00 1.00 5.00 -- 18.67 0.00 -60.00 64 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0117514000 _diffrn_orient_matrix_UB_12 0.0827287000 _diffrn_orient_matrix_UB_13 0.0191867000 _diffrn_orient_matrix_UB_21 0.0161214000 _diffrn_orient_matrix_UB_22 -0.0342897000 _diffrn_orient_matrix_UB_23 0.0386858000 _diffrn_orient_matrix_UB_31 0.0429663000 _diffrn_orient_matrix_UB_32 0.0353734000 _diffrn_orient_matrix_UB_33 -0.0077037000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1902 _reflns_number_total 2191 _reflns_odcompleteness_completeness 99.70 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 7.095 _refine_diff_density_min -3.452 _refine_diff_density_rms 0.392 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 103 _refine_ls_number_reflns 2191 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0693 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1006P)^2^+63.5736P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1773 _refine_ls_wR_factor_ref 0.1870 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All N(H,H) groups 2. Restrained distances N8-H8A 0.9 with sigma of 0.0001 N8-H8B 0.9 with sigma of 0.0001 N3-H3B 0.9 with sigma of 0.0001 H3A-N3 0.9 with sigma of 0.0001 H8A-H8B 1.5 with sigma of 0.0001 H8B-O1_$1 2.2 with sigma of 0.0001 H3A-H3B 1.5 with sigma of 0.0001 3. Uiso/Uaniso restraints and constraints Uanis(N1) = Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(N2) = Uanis(C4) = Uanis(N3) Uanis(N6) = Uanis(C10) = Uanis(N7) = Uanis(C9) = Uanis(C8) = Uanis(C7) = Uanis(N8) 4. Others Fixed Sof: H8B(0.5) O1(0.2) C11(0.4) 5.a Aromatic/amide H refined with riding coordinates: C9(H9), C1(H1), C3(H3), C7(H7), C4(H4), C10(H10) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.75216(4) 0.500000 0.51644(4) 0.0235(3) Uani 1 2 d S T P . . Fe2 Fe 1.000000 1.000000 0.500000 0.0246(7) Uani 1 4 d S T P . . Fe1 Fe 0.500000 0.000000 0.500000 0.0262(7) Uani 1 4 d S T P . . C6 C 0.8468(7) 0.6872(16) 0.5194(8) 0.028(2) Uani 1 1 d . . . . . C5 C 0.6579(8) 0.3130(17) 0.5099(8) 0.028(2) Uani 1 1 d . . . . . N5 N 0.9019(7) 0.7962(16) 0.5213(8) 0.039(3) Uani 1 1 d . . . . . N4 N 0.6023(7) 0.2039(16) 0.5048(9) 0.043(3) Uani 1 1 d . . . . . N6 N 1.0472(15) 1.000000 0.6323(14) 0.064(2) Uani 1 2 d S T P . . N1 N 0.4985(15) 0.000000 0.6358(15) 0.071(3) Uani 1 2 d S T P . . C8 C 1.0254(18) 1.000000 0.7721(17) 0.064(2) Uani 1 2 d S T P . . C9 C 1.1154(18) 1.000000 0.7891(18) 0.064(2) Uani 1 2 d S T P . . H9 H 1.137680 1.000000 0.843400 0.076 Uiso 1 2 calc R U P . . C1 C 0.4281(18) 0.000000 0.6764(18) 0.071(3) Uani 1 2 d S T P . . H1 H 0.373223 0.000000 0.647688 0.085 Uiso 1 2 calc R U P . . N3 N 0.35822(18) 0.000000 0.80582(14) 0.071(3) Uani 1 2 d DS T P . . H3A H 0.3564(3) 0.000000 0.86136(13) 0.107 Uiso 1 2 d DS U P . . H3B H 0.3036(2) 0.000000 0.7810(2) 0.107 Uiso 1 2 d DS U P . . N8 N 0.9667(2) 1.000000 0.83575(13) 0.064(2) Uani 1 2 d DS T P . . H8A H 0.9726(3) 1.000000 0.89128(14) 0.096 Uiso 1 2 d DS U P . . H8B H 0.91630(16) 1.0548(7) 0.8170(2) 0.096 Uiso 0.5 1 d D U P . . C2 C 0.4293(18) 0.000000 0.7676(18) 0.071(3) Uani 1 2 d S T P . . C3 C 0.5111(17) 0.000000 0.8072(19) 0.071(3) Uani 1 2 d S T P . . H3 H 0.515546 0.000000 0.864673 0.085 Uiso 1 2 calc R U P . . C7 C 0.9938(19) 1.000000 0.6900(17) 0.064(2) Uani 1 2 d S T P . . H7 H 0.932574 1.000000 0.678123 0.076 Uiso 1 2 calc R U P . . C4 C 0.5812(18) 0.000000 0.6811(18) 0.071(3) Uani 1 2 d S T P . . H4 H 0.633035 0.000000 0.651040 0.085 Uiso 1 2 calc R U P . . N7 N 1.1679(14) 1.000000 0.7293(14) 0.064(2) Uani 1 2 d S T P . . C10 C 1.1338(18) 1.000000 0.6528(17) 0.064(2) Uani 1 2 d S T P . . H10 H 1.173619 1.000000 0.609903 0.076 Uiso 1 2 calc R U P . . N2 N 0.5900(15) 0.000000 0.7599(15) 0.071(3) Uani 1 2 d S T P . . O1 O 0.7240(2) 0.500000 0.7192(8) 0.11(2) Uiso 0.4 2 d S . P . . C11 C 0.728(6) 0.676(14) 0.748(7) 0.15(3) Uiso 0.4 1 d . . P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0237(4) 0.0095(3) 0.0373(4) 0.000 -0.0003(2) 0.000 Fe2 0.0197(15) 0.0101(14) 0.044(2) 0.000 0.0019(13) 0.000 Fe1 0.0205(16) 0.0104(14) 0.048(2) 0.000 0.0015(13) 0.000 C6 0.022(5) 0.017(5) 0.044(7) -0.002(5) -0.002(5) -0.001(4) C5 0.026(6) 0.020(5) 0.038(6) -0.003(5) -0.006(4) -0.005(5) N5 0.024(5) 0.027(6) 0.067(8) 0.003(5) 0.001(5) -0.004(5) N4 0.028(5) 0.022(6) 0.078(9) -0.001(6) 0.002(5) -0.006(5) N6 0.062(5) 0.070(7) 0.059(5) 0.000 -0.001(4) 0.000 N1 0.052(5) 0.099(9) 0.062(6) 0.000 -0.004(4) 0.000 C8 0.062(5) 0.070(7) 0.059(5) 0.000 -0.001(4) 0.000 C9 0.062(5) 0.070(7) 0.059(5) 0.000 -0.001(4) 0.000 C1 0.052(5) 0.099(9) 0.062(6) 0.000 -0.004(4) 0.000 N3 0.052(5) 0.099(9) 0.062(6) 0.000 -0.004(4) 0.000 N8 0.062(5) 0.070(7) 0.059(5) 0.000 -0.001(4) 0.000 C2 0.052(5) 0.099(9) 0.062(6) 0.000 -0.004(4) 0.000 C3 0.052(5) 0.099(9) 0.062(6) 0.000 -0.004(4) 0.000 C7 0.062(5) 0.070(7) 0.059(5) 0.000 -0.001(4) 0.000 C4 0.052(5) 0.099(9) 0.062(6) 0.000 -0.004(4) 0.000 N7 0.062(5) 0.070(7) 0.059(5) 0.000 -0.001(4) 0.000 C10 0.062(5) 0.070(7) 0.059(5) 0.000 -0.001(4) 0.000 N2 0.052(5) 0.099(9) 0.062(6) 0.000 -0.004(4) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C6 1.977(12) 6_565 ? Pt1 C6 1.977(12) . ? Pt1 C5 1.973(12) . ? Pt1 C5 1.973(12) 6_565 ? Fe2 N5 2.137(11) 5_776 ? Fe2 N5 2.137(11) 6_575 ? Fe2 N5 2.137(11) 2_756 ? Fe2 N5 2.137(11) . ? Fe2 N6 2.23(2) . ? Fe2 N6 2.23(2) 5_776 ? Fe1 N4 2.146(11) 5_656 ? Fe1 N4 2.146(11) 6 ? Fe1 N4 2.146(11) 2_656 ? Fe1 N4 2.146(11) . ? Fe1 N1 2.20(2) . ? Fe1 N1 2.20(2) 5_656 ? C6 N5 1.152(17) . ? C5 N4 1.158(17) . ? N6 C7 1.25(3) . ? N6 C10 1.33(3) . ? N1 C1 1.26(3) . ? N1 C4 1.42(3) . ? C8 C9 1.37(4) . ? C8 N8 1.38(3) . ? C8 C7 1.40(4) . ? C9 H9 0.9300 . ? C9 N7 1.27(4) . ? C1 H1 0.9300 . ? C1 C2 1.47(4) . ? N3 H3A 0.90000(16) . ? N3 H3B 0.90000(14) . ? N3 C2 1.25(3) . ? N8 H8A 0.90000(16) . ? N8 H8B 0.90000(14) . ? N8 H8B 0.90003(15) 6_575 ? C2 C3 1.36(4) . ? C3 H3 0.9300 . ? C3 N2 1.43(4) . ? C7 H7 0.9300 . ? C4 H4 0.9300 . ? C4 N2 1.28(4) . ? N7 C10 1.32(3) . ? C10 H10 0.9300 . ? O1 C11 1.38(10) . ? O1 C11 1.38(10) 6_565 ? C11 C11 1.28(18) 7_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Pt1 C6 88.5(7) 6_565 . ? C5 Pt1 C6 178.4(5) 6_565 6_565 ? C5 Pt1 C6 91.5(5) 6_565 . ? C5 Pt1 C6 91.5(5) . 6_565 ? C5 Pt1 C6 178.4(5) . . ? C5 Pt1 C5 88.5(7) . 6_565 ? N5 Fe2 N5 180.0 . 5_776 ? N5 Fe2 N5 90.7(6) . 2_756 ? N5 Fe2 N5 180.0(7) 6_575 2_756 ? N5 Fe2 N5 90.7(6) 5_776 6_575 ? N5 Fe2 N5 89.3(6) 5_776 2_756 ? N5 Fe2 N5 89.3(6) . 6_575 ? N5 Fe2 N6 92.5(5) . . ? N5 Fe2 N6 92.5(5) 5_776 5_776 ? N5 Fe2 N6 87.5(5) 2_756 . ? N5 Fe2 N6 87.5(5) . 5_776 ? N5 Fe2 N6 92.5(5) 6_575 . ? N5 Fe2 N6 87.5(5) 6_575 5_776 ? N5 Fe2 N6 92.5(5) 2_756 5_776 ? N5 Fe2 N6 87.5(5) 5_776 . ? N6 Fe2 N6 180.0 . 5_776 ? N4 Fe1 N4 180.0 5_656 . ? N4 Fe1 N4 88.8(6) 5_656 2_656 ? N4 Fe1 N4 88.8(6) 6 . ? N4 Fe1 N4 180.0 6 2_656 ? N4 Fe1 N4 91.2(6) 5_656 6 ? N4 Fe1 N4 91.2(6) 2_656 . ? N4 Fe1 N1 90.3(6) 2_656 . ? N4 Fe1 N1 89.7(6) . . ? N4 Fe1 N1 89.7(6) 2_656 5_656 ? N4 Fe1 N1 90.3(6) 6 5_656 ? N4 Fe1 N1 89.7(6) 5_656 5_656 ? N4 Fe1 N1 90.3(6) . 5_656 ? N4 Fe1 N1 90.3(6) 5_656 . ? N4 Fe1 N1 89.7(6) 6 . ? N1 Fe1 N1 180.0 . 5_656 ? N5 C6 Pt1 179.9(15) . . ? N4 C5 Pt1 178.9(13) . . ? C6 N5 Fe2 169.2(12) . . ? C5 N4 Fe1 177.9(13) . . ? C7 N6 Fe2 121.8(19) . . ? C7 N6 C10 117(3) . . ? C10 N6 Fe2 121.0(18) . . ? C1 N1 Fe1 123.9(19) . . ? C1 N1 C4 118(3) . . ? C4 N1 Fe1 118.6(18) . . ? C9 C8 N8 120(2) . . ? C9 C8 C7 119(3) . . ? N8 C8 C7 120(2) . . ? C8 C9 H9 120.7 . . ? N7 C9 C8 119(3) . . ? N7 C9 H9 120.7 . . ? N1 C1 H1 118.7 . . ? N1 C1 C2 123(3) . . ? C2 C1 H1 118.7 . . ? H3A N3 H3B 112.89(2) . . ? C2 N3 H3A 123.3(13) . . ? C2 N3 H3B 123.8(13) . . ? C8 N8 H8A 134.7(12) . . ? C8 N8 H8B 107.4(11) . 6_575 ? C8 N8 H8B 107.4(10) . . ? H8A N8 H8B 112.89(2) . 6_575 ? H8A N8 H8B 112.89(2) . . ? H8B N8 H8B 53.3(8) . 6_575 ? N3 C2 C1 121(2) . . ? N3 C2 C3 122(3) . . ? C3 C2 C1 117(3) . . ? C2 C3 H3 120.2 . . ? C2 C3 N2 120(3) . . ? N2 C3 H3 120.2 . . ? N6 C7 C8 120(3) . . ? N6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? N1 C4 H4 117.4 . . ? N2 C4 N1 125(3) . . ? N2 C4 H4 117.4 . . ? C9 N7 C10 119(2) . . ? N6 C10 H10 117.4 . . ? N7 C10 N6 125(3) . . ? N7 C10 H10 117.4 . . ? C4 N2 C3 118(2) . . ? C11 O1 C11 140(9) 6_565 . ? C11 C11 O1 147(10) 7_666 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe2 N6 C7 C8 180.000(6) . . . . ? Fe2 N6 C10 N7 180.000(5) . . . . ? Fe1 N1 C1 C2 180.000(5) . . . . ? Fe1 N1 C4 N2 180.000(5) . . . . ? N1 C1 C2 N3 180.000(5) . . . . ? N1 C1 C2 C3 0.000(9) . . . . ? N1 C4 N2 C3 0.000(8) . . . . ? C8 C9 N7 C10 0.000(8) . . . . ? C9 C8 C7 N6 0.000(8) . . . . ? C9 N7 C10 N6 0.000(8) . . . . ? C1 N1 C4 N2 0.000(8) . . . . ? C1 C2 C3 N2 0.000(8) . . . . ? N3 C2 C3 N2 180.000(7) . . . . ? N8 C8 C9 N7 180.000(7) . . . . ? N8 C8 C7 N6 180.000(7) . . . . ? C2 C3 N2 C4 0.000(9) . . . . ? C7 N6 C10 N7 0.000(7) . . . . ? C7 C8 C9 N7 0.000(9) . . . . ? C4 N1 C1 C2 0.000(8) . . . . ? C10 N6 C7 C8 0.000(8) . . . . ? C11 O1 C11 C11 111(24) 6_565 . . 7_666 ? _shelx_res_file ; TITL rt457_fenh2pymptetoh_260ka_2_a.res in I2/m rt457_fenh2pymptetoh_260ka_2.res created by SHELXL-2018/3 at 13:29:36 on 09-Sep-2020 REM Old TITL RT457_FeNH2PymPtEtOH_260Ka_2 in I2/m REM SHELXT solution in I2/m: R1 0.143, Rweak 0.009, Alpha 0.016 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C9 N8 Fe Pt CELL 0.71073 14.9798 7.3662 16.1815 90 91.922 90 ZERR 4 0.0016 0.0006 0.0021 0 0.009 0 LATT 2 SYMM -X,+Y,-Z SFAC C H Fe N O Pt UNIT 51.2 40 4 40 1.6 4 EQIV $1 1.5-X,1.5-Y,1.5-Z DFIX 0.9 0.0001 N8 H8a EADP N1 C1 C2 C3 N2 C4 N3 DANG 1.5 0.0001 H8a H8b DFIX 0.9 0.0001 N8 H8b EADP N6 C10 N7 C9 C8 C7 N8 DANG 2.2 0.0001 H8b O1_$1 DANG 1.5 0.0001 H3a H3b DFIX 0.9 0.0001 N3 H3b DFIX 0.9 0.0001 H3a N3 L.S. 50 PLAN 3 SIZE 0.15 0.15 0.02 CONF list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.100600 63.573597 FVAR 0.17429 PT1 6 0.752164 0.500000 0.516439 10.50000 0.02370 0.00949 = 0.03732 0.00000 -0.00030 0.00000 FE2 3 1.000000 1.000000 0.500000 10.25000 0.01966 0.01010 = 0.04403 0.00000 0.00194 0.00000 FE1 3 0.500000 0.000000 0.500000 10.25000 0.02052 0.01036 = 0.04760 0.00000 0.00148 0.00000 C6 1 0.846753 0.687198 0.519447 11.00000 0.02157 0.01749 = 0.04419 -0.00227 -0.00161 -0.00141 C5 1 0.657872 0.313029 0.509946 11.00000 0.02576 0.01968 = 0.03825 -0.00255 -0.00649 -0.00526 N5 4 0.901936 0.796158 0.521259 11.00000 0.02396 0.02705 = 0.06663 0.00315 0.00107 -0.00442 N4 4 0.602349 0.203889 0.504790 11.00000 0.02762 0.02247 = 0.07769 -0.00071 0.00204 -0.00551 N6 4 1.047155 1.000000 0.632262 10.50000 0.06243 0.06966 = 0.05887 0.00000 -0.00077 0.00000 N1 4 0.498455 0.000000 0.635782 10.50000 0.05177 0.09896 = 0.06231 0.00000 -0.00411 0.00000 C8 1 1.025449 1.000000 0.772130 10.50000 0.06243 0.06966 = 0.05887 0.00000 -0.00077 0.00000 C9 1 1.115402 1.000000 0.789058 10.50000 0.06243 0.06966 = 0.05887 0.00000 -0.00077 0.00000 AFIX 43 H9 2 1.137680 1.000000 0.843400 10.50000 -1.20000 AFIX 0 C1 1 0.428072 0.000000 0.676370 10.50000 0.05177 0.09896 = 0.06231 0.00000 -0.00411 0.00000 AFIX 43 H1 2 0.373223 0.000000 0.647688 10.50000 -1.20000 AFIX 0 N3 4 0.358219 0.000000 0.805818 10.50000 0.05177 0.09896 = 0.06231 0.00000 -0.00411 0.00000 H3A 2 0.356424 0.000000 0.861356 10.50000 -1.50000 H3B 2 0.303559 0.000000 0.780971 10.50000 -1.50000 N8 4 0.966724 1.000000 0.835746 10.50000 0.06243 0.06966 = 0.05887 0.00000 -0.00077 0.00000 H8A 2 0.972584 1.000000 0.891282 10.50000 -1.50000 H8B 2 0.916302 1.054809 0.817017 10.50000 -1.50000 C2 1 0.429290 0.000000 0.767550 10.50000 0.05177 0.09896 = 0.06231 0.00000 -0.00411 0.00000 C3 1 0.511116 0.000000 0.807209 10.50000 0.05177 0.09896 = 0.06231 0.00000 -0.00411 0.00000 AFIX 43 H3 2 0.515546 0.000000 0.864673 10.50000 -1.20000 AFIX 0 C7 1 0.993757 1.000000 0.689960 10.50000 0.06243 0.06966 = 0.05887 0.00000 -0.00077 0.00000 AFIX 43 H7 2 0.932574 1.000000 0.678123 10.50000 -1.20000 AFIX 0 C4 1 0.581173 0.000000 0.681065 10.50000 0.05177 0.09896 = 0.06231 0.00000 -0.00411 0.00000 AFIX 43 H4 2 0.633035 0.000000 0.651040 10.50000 -1.20000 AFIX 0 N7 4 1.167886 1.000000 0.729264 10.50000 0.06243 0.06966 = 0.05887 0.00000 -0.00077 0.00000 C10 1 1.133765 1.000000 0.652751 10.50000 0.06243 0.06966 = 0.05887 0.00000 -0.00077 0.00000 AFIX 43 H10 2 1.173619 1.000000 0.609903 10.50000 -1.20000 AFIX 0 N2 4 0.590033 0.000000 0.759858 10.50000 0.05177 0.09896 = 0.06231 0.00000 -0.00411 0.00000 O1 5 0.723976 0.500000 0.719234 10.20000 0.10887 C11 1 0.728220 0.675620 0.748011 10.40000 0.14991 HKLF 4 REM rt457_fenh2pymptetoh_260ka_2_a.res in I2/m REM wR2 = 0.1870, GooF = S = 1.092, Restrained GooF = 1.090 for all data REM R1 = 0.0693 for 1902 Fo > 4sig(Fo) and 0.0793 for all 2191 data REM 103 parameters refined using 7 restraints END WGHT 0.1006 63.5761 REM Highest difference peak 7.095, deepest hole -3.452, 1-sigma level 0.392 Q1 1 0.6895 0.5000 0.5118 10.50000 0.05 7.09 Q2 1 0.7504 0.5000 0.4605 10.50000 0.05 6.54 Q3 1 0.8201 0.5000 0.5194 10.50000 0.05 5.13 ; _shelx_res_checksum 30658 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.710 _oxdiff_exptl_absorpt_empirical_full_min 0.583 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_rt174_nh2pymptmeoh_260k_2 _database_code_depnum_ccdc_archive 'CCDC 2018389' loop_ _audit_author_name _audit_author_address 'Carlos Bartual-Murgui' ;Universitat de Valencia Spain ; _audit_update_record ; 2020-09-17 deposited with the CCDC. 2020-09-22 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT971_rt174_nh2pymptmeoh_260k_2 ; PROBLEM: Check Calcd Resid. Dens. 0.72A From Pt2 3.73 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt174_nh2pymptmeoh_260k_2 ; PROBLEM: Check Calcd Resid. Dens. 0.17A From N11 -4.30 eA-3 RESPONSE: The residual electronic density may be due to the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt174_nh2pymptmeoh_260k_2_2 ; PROBLEM: Check Calcd Resid. Dens. 0.11A From N3 -4.13 eA-3 RESPONSE: The residual electronic density may be due to the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_rt174_nh2pymptmeoh_260k_2_3 ; PROBLEM: Check Calcd Resid. Dens. 0.08A From N2 -3.58 eA-3 RESPONSE: The residual electronic density may be due to the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT973_rt174_nh2pymptmeoh_260k_2 ; PROBLEM: Check Calcd Positive Resid. Density on Fe1 4.86 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; # Added during the CSD deposition process: Thursday 17 September 2020 12:29 PM # end Validation Reply Form _audit_creation_date 2020-09-09 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C12 H10 Fe N10 Pt, 0.25(C H3 O), 0.25(C H4 O)' _chemical_formula_sum 'C12.50 H11.75 Fe N10 O0.50 Pt' _chemical_formula_weight 561.01 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system orthorhombic _space_group_IT_number 57 _space_group_name_H-M_alt 'P b c m' _space_group_name_Hall '-P 2c 2b' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y-1/2, z' _cell_length_a 14.9943(8) _cell_length_b 32.6263(19) _cell_length_c 7.3615(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3601.3(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used 3011 _cell_measurement_temperature 260.00(10) _cell_measurement_theta_max 27.5970 _cell_measurement_theta_min 3.9060 _shelx_estimated_absorpt_T_max 0.847 _shelx_estimated_absorpt_T_min 0.481 _exptl_absorpt_coefficient_mu 8.587 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.27350 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 2.069 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 2118 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_unetI/netI 0.0555 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.887 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 19370 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.887 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.092 _diffrn_reflns_theta_min 3.326 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 260.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0267 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.887 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -59.00 58.00 1.00 5.00 -- -14.97 19.00 -60.00 117 2 \w -14.00 42.00 1.00 5.00 -- 15.83 77.00 150.00 56 3 \w -6.00 19.00 1.00 5.00 -- 15.83 57.00 -90.00 25 4 \w -42.00 46.00 1.00 5.00 -- 15.83 -77.00 120.00 88 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0400310677 _diffrn_orient_matrix_UB_12 0.0113676126 _diffrn_orient_matrix_UB_13 0.0190743162 _diffrn_orient_matrix_UB_21 -0.0875870030 _diffrn_orient_matrix_UB_22 0.0049998293 _diffrn_orient_matrix_UB_23 0.0088222772 _diffrn_orient_matrix_UB_31 0.0004575283 _diffrn_orient_matrix_UB_32 -0.0455539532 _diffrn_orient_matrix_UB_33 0.0057650418 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2751 _reflns_number_total 4199 _reflns_odcompleteness_completeness 99.48 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 24.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 5.181 _refine_diff_density_min -4.383 _refine_diff_density_rms 0.335 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 133 _refine_ls_number_reflns 4199 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1250 _refine_ls_R_factor_gt 0.0869 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+253.2535P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1624 _refine_ls_wR_factor_ref 0.1846 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All N(H,H) groups, All O(H) groups 2. Restrained distances H8B-N8 0.9 with sigma of 0.0001 O2-C22 1.4 with sigma of 0.02 H8A-N8 0.9 with sigma of 0.0001 H14A-N14 0.9 with sigma of 0.0001 N14-H14B 0.9 with sigma of 0.0001 N11-H11B 0.9 with sigma of 0.0001 H11A-N11 0.9 with sigma of 0.0001 H8B-H8A 1.5 with sigma of 0.0001 H14A-H14B 1.5 with sigma of 0.0001 H14B-O2_$1 2.2 with sigma of 0.0001 H3B-N3 0.9 with sigma of 0.0001 H3A-H3B 1.5 with sigma of 0.0001 N3_$2-H3A_$2 0.9 with sigma of 0.0001 H11A-H11B 1.5 with sigma of 0.0001 H8B_$2-O1_$3 2 with sigma of 0.0001 3. Uiso/Uaniso restraints and constraints Uanis(N8) = Uanis(C8) = Uanis(C7) = Uanis(N6) = Uanis(C10) = Uanis(N7) = Uanis(C9) = Uanis(N12) = Uanis(C15) = Uanis(C17) = Uanis(N13) = Uanis(C18) = Uanis(C16) = Uanis(N14) Uanis(N3) = Uanis(C2) = Uanis(C1) = Uanis(N1) = Uanis(C3) = Uanis(N2) = Uanis(C4) = Uanis(Fe1) = Uanis(N9) = Uanis(C14) = Uanis(N10) = Uanis(C13) = Uanis(C12) = Uanis(C11) = Uanis(N11) Uanis(N16) = Uanis(C20) = Uanis(Pt2) = Uanis(C19) = Uanis(N15) = Uanis(N4) = Uanis(C5) = Uanis(Pt1) = Uanis(C6) = Uanis(N5) 4. Others Fixed Sof: H8A(0.5) H14A(0.5) H14B(0.5) O2(0.25) O1(0.25) H1A(0.25) C21(0.25) H21A(0.25) H21B(0.25) H21C(0.25) C22(0.25) H22A(0.25) H22B(0.25) H22C(0.25) Fixed X: O2(0.99566) O1(0.489029) C21(0.489469) Fixed Y: O2(0.736329) O1(0.51052) C21(0.51225) Fixed Z: O2(1.25) O1(1.25) C21(1.069429) 5.a Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C4(H4), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18) 5.b Tetrahedral OH refined with riding coordinates: O1(H1A) 5.c Idealised Me refined as rotating group: C21(H21A,H21B,H21C), C22(H22A,H22B,H22C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.50820(5) 0.61784(3) 1.250000 0.01524(19) Uani 1 2 d S T P . . Pt2 Pt 1.00612(5) 0.63305(3) 0.250000 0.01524(19) Uani 1 2 d S T P . . Fe1 Fe 0.2568(2) 0.62705(10) 1.750000 0.0209(6) Uani 1 2 d S T P . . Fe2 Fe 0.75746(18) 0.62415(10) 0.750000 0.0156(6) Uani 1 2 d S T P . . N1 N 0.2509(11) 0.5576(6) 1.750000 0.0209(6) Uani 1 2 d S T P . . N2 N 0.3296(11) 0.4944(6) 1.750000 0.0209(6) Uani 1 2 d S T P . . N3 N 0.09421(18) 0.47169(7) 1.750000 0.0209(6) Uani 1 2 d DS T P . . H3A H 0.0421(2) 0.48537(9) 1.750000 0.031 Uiso 1 2 d DS U P . . H3B H 0.0870(4) 0.44430(6) 1.750000 0.031 Uiso 1 2 d DS U P . . N4 N 0.3597(7) 0.6249(4) 1.5467(16) 0.01524(19) Uani 1 1 d . . . . . N5 N 0.6580(7) 0.6136(4) 0.9551(16) 0.01524(19) Uani 1 1 d . . . . . N6 N 0.7951(16) 0.5592(8) 0.750000 0.0505(18) Uani 1 2 d S T P . . N7 N 0.9125(16) 0.5086(8) 0.750000 0.0505(18) Uani 1 2 d S T P . . N8 N 0.69281(6) 0.45920(8) 0.750000 0.0505(18) Uani 1 2 d DS T P . . H8A H 0.6977(3) 0.43412(8) 0.7999(9) 0.076 Uiso 0.5 1 d D U P . . H8B H 0.63645(8) 0.46869(10) 0.750000 0.076 Uiso 1 2 d DS U P . . N9 N 0.2635(11) 0.6952(6) 1.750000 0.0209(6) Uani 1 2 d S T P . . N10 N 0.1819(11) 0.7555(6) 1.750000 0.0209(6) Uani 1 2 d S T P . . N11 N 0.4159(2) 0.77706(7) 1.750000 0.0209(6) Uani 1 2 d DS T P . . H11A H 0.4331(4) 0.80349(6) 1.750000 0.031 Uiso 1 2 d DS U P . . H11B H 0.4622(2) 0.75949(8) 1.750000 0.031 Uiso 1 2 d DS U P . . N12 N 0.7147(16) 0.6897(8) 0.750000 0.0505(18) Uani 1 2 d S T P . . N13 N 0.5982(15) 0.7381(7) 0.750000 0.0505(18) Uani 1 2 d S T P . . N14 N 0.8069(2) 0.79214(13) 0.750000 0.0505(18) Uani 1 2 d DS T P . . H14A H 0.77509(16) 0.81029(11) 0.8154(7) 0.076 Uiso 0.5 1 d D U P . . H14B H 0.85936(10) 0.78570(13) 0.8021(6) 0.076 Uiso 0.5 1 d D U P . . N15 N 0.8563(7) 0.6342(4) 0.5455(16) 0.01524(19) Uani 1 1 d . . . . . N16 N 1.1571(7) 0.6292(4) -0.0455(16) 0.01524(19) Uani 1 1 d . . . . . C1 C 0.1720(13) 0.5367(7) 1.750000 0.0209(6) Uani 1 2 d S T P . . H1 H 0.118764 0.551379 1.750000 0.025 Uiso 1 2 calc R U P . . C2 C 0.1692(13) 0.4940(7) 1.750000 0.0209(6) Uani 1 2 d S T P . . C3 C 0.2551(13) 0.4743(7) 1.750000 0.0209(6) Uani 1 2 d S T P . . H3 H 0.257235 0.445788 1.750000 0.025 Uiso 1 2 calc R U P . . C4 C 0.3246(13) 0.5354(7) 1.750000 0.0209(6) Uani 1 2 d S T P . . H4 H 0.378338 0.549593 1.750000 0.025 Uiso 1 2 calc R U P . . C5 C 0.4156(8) 0.6218(4) 1.4369(19) 0.01524(19) Uani 1 1 d . . . . . C6 C 0.6034(8) 0.6146(4) 1.0617(19) 0.01524(19) Uani 1 1 d . . . . . C7 C 0.735(2) 0.5294(9) 0.750000 0.0505(18) Uani 1 2 d S T P . . H7 H 0.674419 0.536310 0.750000 0.061 Uiso 1 2 calc R U P . . C8 C 0.7588(19) 0.4877(9) 0.750000 0.0505(18) Uani 1 2 d S T P . . C9 C 0.8469(19) 0.4812(10) 0.750000 0.0505(18) Uani 1 2 d S T P . . H9 H 0.864559 0.453906 0.750000 0.061 Uiso 1 2 calc R U P . . C10 C 0.8789(19) 0.5479(9) 0.750000 0.0505(18) Uani 1 2 d S T P . . H10 H 0.920757 0.568899 0.750000 0.061 Uiso 1 2 calc R U P . . C11 C 0.3362(13) 0.7149(7) 1.750000 0.0209(6) Uani 1 2 d S T P . . H11 H 0.389484 0.700310 1.750000 0.025 Uiso 1 2 calc R U P . . C12 C 0.3400(13) 0.7596(7) 1.750000 0.0209(6) Uani 1 2 d S T P . . C13 C 0.2592(13) 0.7754(7) 1.750000 0.0209(6) Uani 1 2 d S T P . . H13 H 0.255844 0.803863 1.750000 0.025 Uiso 1 2 calc R U P . . C14 C 0.1870(13) 0.7142(7) 1.750000 0.0209(6) Uani 1 2 d S T P . . H14 H 0.134712 0.698870 1.750000 0.025 Uiso 1 2 calc R U P . . C15 C 0.772(2) 0.7207(9) 0.750000 0.0505(18) Uani 1 2 d S T P . . H15 H 0.832925 0.714865 0.750000 0.061 Uiso 1 2 calc R U P . . C16 C 0.7460(19) 0.7609(9) 0.750000 0.0505(18) Uani 1 2 d S T P . . C17 C 0.6572(19) 0.7688(10) 0.750000 0.0505(18) Uani 1 2 d S T P . . H17 H 0.637186 0.795766 0.750000 0.061 Uiso 1 2 calc R U P . . C18 C 0.628(2) 0.6994(9) 0.750000 0.0505(18) Uani 1 2 d S T P . . H18 H 0.585886 0.678279 0.750000 0.061 Uiso 1 2 calc R U P . . C19 C 0.9133(8) 0.6341(4) 0.4383(19) 0.01524(19) Uani 1 1 d . . . . . C20 C 1.1006(8) 0.6302(4) 0.0569(19) 0.01524(19) Uani 1 1 d . . . . . O2 O 0.995660 0.736329 1.250000 0.11(2) Uiso 0.25 1 d DS . P A -1 O1 O 0.489029 0.510520 1.250000 0.092(19) Uiso 0.25 1 d S . P B -1 H1A H 0.488720 0.533839 1.291549 0.138 Uiso 0.25 1 calc R U P B -1 C21 C 0.489469 0.512250 1.069429 0.014(11) Uiso 0.25 1 d . . P B -1 H21A H 0.533218 0.531809 1.030043 0.021 Uiso 0.25 1 calc R U P B -1 H21B H 0.431640 0.520453 1.026880 0.021 Uiso 0.25 1 calc R U P B -1 H21C H 0.503864 0.485736 1.021076 0.021 Uiso 0.25 1 calc R U P B -1 C22 C 0.987(4) 0.747(3) 1.066(4) 0.038(17) Uiso 0.25 1 d D . P A -1 H22A H 0.962871 0.724272 0.999745 0.057 Uiso 0.25 1 calc R U P A -1 H22B H 1.045076 0.753679 1.017838 0.057 Uiso 0.25 1 calc R U P A -1 H22C H 0.948601 0.770234 1.054614 0.057 Uiso 0.25 1 calc R U P A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0102(3) 0.0270(3) 0.0085(2) 0.000 0.000 -0.0010(2) Pt2 0.0102(3) 0.0270(3) 0.0085(2) 0.000 0.000 -0.0010(2) Fe1 0.0152(12) 0.0284(15) 0.0190(12) 0.000 0.000 -0.0018(10) Fe2 0.0063(12) 0.0352(17) 0.0052(11) 0.000 0.000 -0.0023(11) N1 0.0152(12) 0.0284(15) 0.0190(12) 0.000 0.000 -0.0018(10) N2 0.0152(12) 0.0284(15) 0.0190(12) 0.000 0.000 -0.0018(10) N3 0.0152(12) 0.0284(15) 0.0190(12) 0.000 0.000 -0.0018(10) N4 0.0102(3) 0.0270(3) 0.0085(2) 0.000 0.000 -0.0010(2) N5 0.0102(3) 0.0270(3) 0.0085(2) 0.000 0.000 -0.0010(2) N6 0.043(4) 0.044(4) 0.064(4) 0.000 0.000 -0.002(3) N7 0.043(4) 0.044(4) 0.064(4) 0.000 0.000 -0.002(3) N8 0.043(4) 0.044(4) 0.064(4) 0.000 0.000 -0.002(3) N9 0.0152(12) 0.0284(15) 0.0190(12) 0.000 0.000 -0.0018(10) N10 0.0152(12) 0.0284(15) 0.0190(12) 0.000 0.000 -0.0018(10) N11 0.0152(12) 0.0284(15) 0.0190(12) 0.000 0.000 -0.0018(10) N12 0.043(4) 0.044(4) 0.064(4) 0.000 0.000 -0.002(3) N13 0.043(4) 0.044(4) 0.064(4) 0.000 0.000 -0.002(3) N14 0.043(4) 0.044(4) 0.064(4) 0.000 0.000 -0.002(3) N15 0.0102(3) 0.0270(3) 0.0085(2) 0.000 0.000 -0.0010(2) N16 0.0102(3) 0.0270(3) 0.0085(2) 0.000 0.000 -0.0010(2) C1 0.0152(12) 0.0284(15) 0.0190(12) 0.000 0.000 -0.0018(10) C2 0.0152(12) 0.0284(15) 0.0190(12) 0.000 0.000 -0.0018(10) C3 0.0152(12) 0.0284(15) 0.0190(12) 0.000 0.000 -0.0018(10) C4 0.0152(12) 0.0284(15) 0.0190(12) 0.000 0.000 -0.0018(10) C5 0.0102(3) 0.0270(3) 0.0085(2) 0.000 0.000 -0.0010(2) C6 0.0102(3) 0.0270(3) 0.0085(2) 0.000 0.000 -0.0010(2) C7 0.043(4) 0.044(4) 0.064(4) 0.000 0.000 -0.002(3) C8 0.043(4) 0.044(4) 0.064(4) 0.000 0.000 -0.002(3) C9 0.043(4) 0.044(4) 0.064(4) 0.000 0.000 -0.002(3) C10 0.043(4) 0.044(4) 0.064(4) 0.000 0.000 -0.002(3) C11 0.0152(12) 0.0284(15) 0.0190(12) 0.000 0.000 -0.0018(10) C12 0.0152(12) 0.0284(15) 0.0190(12) 0.000 0.000 -0.0018(10) C13 0.0152(12) 0.0284(15) 0.0190(12) 0.000 0.000 -0.0018(10) C14 0.0152(12) 0.0284(15) 0.0190(12) 0.000 0.000 -0.0018(10) C15 0.043(4) 0.044(4) 0.064(4) 0.000 0.000 -0.002(3) C16 0.043(4) 0.044(4) 0.064(4) 0.000 0.000 -0.002(3) C17 0.043(4) 0.044(4) 0.064(4) 0.000 0.000 -0.002(3) C18 0.043(4) 0.044(4) 0.064(4) 0.000 0.000 -0.002(3) C19 0.0102(3) 0.0270(3) 0.0085(2) 0.000 0.000 -0.0010(2) C20 0.0102(3) 0.0270(3) 0.0085(2) 0.000 0.000 -0.0010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C5 1.959(13) 6_558 ? Pt1 C5 1.959(13) . ? Pt1 C6 1.993(13) . ? Pt1 C6 1.993(13) 6_558 ? Pt2 C19 1.965(13) . ? Pt2 C19 1.965(13) 6_556 ? Pt2 C20 2.009(13) . ? Pt2 C20 2.009(13) 6_556 ? Fe1 N1 2.267(19) . ? Fe1 N4 2.151(11) 6_559 ? Fe1 N4 2.151(11) . ? Fe1 N9 2.226(19) . ? Fe1 N16 2.123(11) 1_457 ? Fe1 N16 2.123(11) 6_457 ? Fe2 N5 2.150(11) 6_557 ? Fe2 N5 2.150(11) . ? Fe2 N6 2.19(2) . ? Fe2 N12 2.23(2) . ? Fe2 N15 2.138(11) 6_557 ? Fe2 N15 2.138(11) . ? N1 C1 1.37(3) . ? N1 C4 1.32(3) . ? N2 C3 1.30(3) . ? N2 C4 1.34(3) . ? N3 H3A 0.90000(11) . ? N3 H3B 0.90000(12) . ? N3 C2 1.34(2) . ? N4 C5 1.169(17) . ? N5 C6 1.134(17) . ? N6 C7 1.33(4) . ? N6 C10 1.31(4) . ? N7 C9 1.33(4) . ? N7 C10 1.38(4) . ? N8 H8A 0.90009(11) 6_557 ? N8 H8A 0.90000(12) . ? N8 H8B 0.90000(11) . ? N8 C8 1.36(3) . ? N9 C11 1.27(3) . ? N9 C14 1.30(3) . ? N10 C13 1.33(3) . ? N10 C14 1.35(3) . ? N11 H11A 0.90000(11) . ? N11 H11B 0.90000(11) . ? N11 C12 1.27(2) . ? N12 C15 1.33(4) . ? N12 C18 1.35(4) . ? N13 C17 1.34(3) . ? N13 C18 1.34(4) . ? N14 H14A 0.90000(11) . ? N14 H14A 0.89998(11) 6_557 ? N14 H14B 0.90000(13) . ? N14 H14B 0.90001(13) 6_557 ? N14 C16 1.37(3) . ? N15 C19 1.163(17) . ? N16 C20 1.135(17) . ? C1 H1 0.9300 . ? C1 C2 1.40(3) . ? C2 C3 1.44(3) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C7 H7 0.9300 . ? C7 C8 1.41(4) . ? C8 C9 1.34(4) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C11 C12 1.46(3) . ? C12 C13 1.32(3) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C15 C16 1.37(4) . ? C16 C17 1.36(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? O2 C22 1.40(2) . ? O1 H1A 0.8200 . ? O1 C21 1.33048(5) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Pt1 C5 89.3(8) 6_558 . ? C5 Pt1 C6 91.3(6) 6_558 . ? C5 Pt1 C6 179.1(6) 6_558 6_558 ? C5 Pt1 C6 179.1(6) . . ? C5 Pt1 C6 91.3(6) . 6_558 ? C6 Pt1 C6 88.1(8) 6_558 . ? C19 Pt2 C19 89.7(8) 6_556 . ? C19 Pt2 C20 90.1(6) . 6_556 ? C19 Pt2 C20 90.1(6) 6_556 . ? C19 Pt2 C20 178.4(6) . . ? C19 Pt2 C20 178.4(6) 6_556 6_556 ? C20 Pt2 C20 90.1(8) 6_556 . ? N4 Fe1 N1 89.8(4) 6_559 . ? N4 Fe1 N1 89.8(4) . . ? N4 Fe1 N4 88.2(6) . 6_559 ? N4 Fe1 N9 90.0(5) 6_559 . ? N4 Fe1 N9 90.0(5) . . ? N9 Fe1 N1 179.6(6) . . ? N16 Fe1 N1 90.3(4) 6_457 . ? N16 Fe1 N1 90.3(4) 1_457 . ? N16 Fe1 N4 178.9(5) 6_457 6_559 ? N16 Fe1 N4 90.8(4) 6_457 . ? N16 Fe1 N4 178.9(5) 1_457 . ? N16 Fe1 N4 90.8(4) 1_457 6_559 ? N16 Fe1 N9 90.0(5) 1_457 . ? N16 Fe1 N9 90.0(5) 6_457 . ? N16 Fe1 N16 90.3(6) 6_457 1_457 ? N5 Fe2 N5 89.2(6) . 6_557 ? N5 Fe2 N6 91.4(6) . . ? N5 Fe2 N6 91.4(6) 6_557 . ? N5 Fe2 N12 87.4(5) 6_557 . ? N5 Fe2 N12 87.4(5) . . ? N6 Fe2 N12 178.2(9) . . ? N15 Fe2 N5 90.6(4) 6_557 . ? N15 Fe2 N5 179.7(5) 6_557 6_557 ? N15 Fe2 N5 179.7(5) . . ? N15 Fe2 N5 90.6(4) . 6_557 ? N15 Fe2 N6 88.3(5) . . ? N15 Fe2 N6 88.3(5) 6_557 . ? N15 Fe2 N12 92.9(5) 6_557 . ? N15 Fe2 N12 92.9(5) . . ? N15 Fe2 N15 89.5(6) . 6_557 ? C1 N1 Fe1 122.1(14) . . ? C4 N1 Fe1 121.1(14) . . ? C4 N1 C1 116.8(19) . . ? C3 N2 C4 117.2(19) . . ? H3A N3 H3B 112.885(19) . . ? C2 N3 H3A 117.4(10) . . ? C2 N3 H3B 129.7(10) . . ? C5 N4 Fe1 176.8(12) . . ? C6 N5 Fe2 169.2(12) . . ? C7 N6 Fe2 122(2) . . ? C10 N6 Fe2 121(2) . . ? C10 N6 C7 117(3) . . ? C9 N7 C10 111(3) . . ? H8A N8 H8A 48.2(9) . 6_557 ? H8A N8 H8B 112.885(19) . . ? H8B N8 H8A 112.886(19) . 6_557 ? C8 N8 H8A 124.3(11) . . ? C8 N8 H8A 124.3(11) . 6_557 ? C8 N8 H8B 116.7(13) . . ? C11 N9 Fe1 123.2(15) . . ? C11 N9 C14 121(2) . . ? C14 N9 Fe1 115.8(14) . . ? C13 N10 C14 116.0(18) . . ? H11A N11 H11B 112.885(19) . . ? C12 N11 H11A 133.2(10) . . ? C12 N11 H11B 113.9(10) . . ? C15 N12 Fe2 123(2) . . ? C15 N12 C18 117(3) . . ? C18 N12 Fe2 120(2) . . ? C17 N13 C18 119(3) . . ? H14A N14 H14A 64.7(8) . 6_557 ? H14A N14 H14B 147.6(6) . 6_557 ? H14A N14 H14B 112.885(18) . . ? H14A N14 H14B 112.881(18) 6_557 6_557 ? H14B N14 H14A 147.6(6) . 6_557 ? H14B N14 H14B 50.4(6) . 6_557 ? C16 N14 H14A 97.9(11) . . ? C16 N14 H14A 97.9(11) . 6_557 ? C16 N14 H14B 114.1(12) . 6_557 ? C16 N14 H14B 114.1(12) . . ? C19 N15 Fe2 170.5(12) . . ? C20 N16 Fe1 176.5(11) . 1_653 ? N1 C1 H1 119.2 . . ? N1 C1 C2 121.6(19) . . ? C2 C1 H1 119.2 . . ? N3 C2 C1 124.6(18) . . ? N3 C2 C3 120.6(19) . . ? C1 C2 C3 114.8(19) . . ? N2 C3 C2 123(2) . . ? N2 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? N1 C4 N2 126.5(19) . . ? N1 C4 H4 116.7 . . ? N2 C4 H4 116.7 . . ? N4 C5 Pt1 178.5(13) . . ? N5 C6 Pt1 178.4(13) . . ? N6 C7 H7 119.0 . . ? N6 C7 C8 122(3) . . ? C8 C7 H7 119.0 . . ? N8 C8 C7 118(2) . . ? C9 C8 N8 128(3) . . ? C9 C8 C7 114(3) . . ? N7 C9 C8 129(3) . . ? N7 C9 H9 115.6 . . ? C8 C9 H9 115.6 . . ? N6 C10 N7 128(3) . . ? N6 C10 H10 116.0 . . ? N7 C10 H10 116.0 . . ? N9 C11 H11 118.6 . . ? N9 C11 C12 123(2) . . ? C12 C11 H11 118.6 . . ? N11 C12 C11 118.8(17) . . ? N11 C12 C13 130(2) . . ? C13 C12 C11 110.8(19) . . ? N10 C13 H13 116.2 . . ? C12 C13 N10 128(2) . . ? C12 C13 H13 116.2 . . ? N9 C14 N10 121.6(19) . . ? N9 C14 H14 119.2 . . ? N10 C14 H14 119.2 . . ? N12 C15 H15 118.5 . . ? N12 C15 C16 123(3) . . ? C16 C15 H15 118.5 . . ? C15 C16 N14 122(3) . . ? C17 C16 N14 121(3) . . ? C17 C16 C15 118(3) . . ? N13 C17 C16 120(3) . . ? N13 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? N12 C18 H18 118.6 . . ? N13 C18 N12 123(3) . . ? N13 C18 H18 118.6 . . ? N15 C19 Pt2 177.7(12) . . ? N16 C20 Pt2 176.5(12) . . ? C21 O1 H1A 109.5 . . ? O1 C21 H21A 109.5 . . ? O1 C21 H21B 109.5 . . ? O1 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O2 C22 H22A 109.5 . . ? O2 C22 H22B 109.5 . . ? O2 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 N1 C1 C2 180.0 . . . . ? Fe1 N1 C4 N2 180.0 . . . . ? Fe1 N9 C11 C12 180.0 . . . . ? Fe1 N9 C14 N10 180.0 . . . . ? Fe2 N6 C7 C8 180.0 . . . . ? Fe2 N6 C10 N7 180.0 . . . . ? Fe2 N12 C15 C16 180.0 . . . . ? Fe2 N12 C18 N13 180.0 . . . . ? N1 C1 C2 N3 180.0 . . . . ? N1 C1 C2 C3 0.0 . . . . ? N3 C2 C3 N2 180.0 . . . . ? N6 C7 C8 N8 180.0 . . . . ? N6 C7 C8 C9 0.0 . . . . ? N8 C8 C9 N7 180.0 . . . . ? N9 C11 C12 N11 180.0 . . . . ? N9 C11 C12 C13 0.0 . . . . ? N11 C12 C13 N10 180.0 . . . . ? N12 C15 C16 N14 180.0 . . . . ? N12 C15 C16 C17 0.0 . . . . ? N14 C16 C17 N13 180.0 . . . . ? C1 N1 C4 N2 0.0 . . . . ? C1 C2 C3 N2 0.0 . . . . ? C3 N2 C4 N1 0.0 . . . . ? C4 N1 C1 C2 0.0 . . . . ? C4 N2 C3 C2 0.0 . . . . ? C7 N6 C10 N7 0.0 . . . . ? C7 C8 C9 N7 0.0 . . . . ? C9 N7 C10 N6 0.0 . . . . ? C10 N6 C7 C8 0.0 . . . . ? C10 N7 C9 C8 0.0 . . . . ? C11 N9 C14 N10 0.0 . . . . ? C11 C12 C13 N10 0.0 . . . . ? C13 N10 C14 N9 0.0 . . . . ? C14 N9 C11 C12 0.0 . . . . ? C14 N10 C13 C12 0.0 . . . . ? C15 N12 C18 N13 0.0 . . . . ? C15 C16 C17 N13 0.0 . . . . ? C17 N13 C18 N12 0.0 . . . . ? C18 N12 C15 C16 0.0 . . . . ? C18 N13 C17 C16 0.0 . . . . ? _shelx_res_file ; TITL rt174_nh2pymptmeoh_260k_2_a.res in Pbcm rt174_nh2pymptmeoh_260k_2.res created by SHELXL-2018/3 at 11:12:39 on 09-Sep-2020 REM Old TITL RT174_NH2PymPtMeOH_260K_2 in Pbn21 #33 REM SHELXT solution in Pbcm: R1 0.179, Rweak 0.001, Alpha 0.056 REM 1.449 for 218 systematic absences, Orientation as input REM Formula found by SHELXT: C10 N21 Fe2 Pt2 CELL 0.71073 14.9943 32.6263 7.3615 90 90 90 ZERR 8 0.0008 0.0019 0.0003 0 0 0 LATT 1 SYMM -X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM +X,0.5-Y,-Z SFAC C H Fe N O Pt UNIT 100 94 8 80 4 8 EQIV $1 +X,1.5-Y,-0.5+Z EQIV $2 +X,+Y,1+Z EQIV $3 1-X,1-Y,0.5+Z EADP N8 C8 C7 N6 C10 N7 C9 N12 C15 C17 N13 C18 C16 N14 EADP N3 C2 C1 N1 C3 N2 C4 Fe1 N9 C14 N10 C13 C12 C11 N11 DFIX 0.9 0.0001 H8b N8 DANG 1.5 0.0001 H8b H8a EADP N16 C20 Pt2 C19 N15 N4 C5 Pt1 C6 N5 DFIX 1.4 O2 C22 DFIX 0.9 0.0001 H8a N8 DFIX 0.9 0.0001 H14a N14 DFIX 0.9 0.0001 N14 H14b DANG 1.5 0.0001 H14a H14b DANG 2.2 0.0001 H14b O2_$1 DANG 0.9 0.0001 H3b N3 DANG 1.5 0.0001 H3a H3b DANG 0.9 0.0001 N3_$2 H3a_$2 DFIX 0.9 0.0001 N11 H11b DANG 1.5 0.0001 H11a H11b DFIX 0.9 0.0001 H11a N11 DANG 2 0.0001 H8b_$2 O1_$3 L.S. 50 PLAN 5 SIZE 0.1 0.1 0.02 CONF list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.033300 253.253525 FVAR 0.09326 PT1 6 0.508201 0.617836 1.250000 10.50000 0.01022 0.02699 = 0.00853 0.00000 0.00000 -0.00105 PT2 6 1.006120 0.633054 0.250000 10.50000 0.01022 0.02699 = 0.00853 0.00000 0.00000 -0.00105 FE1 3 0.256802 0.627047 1.750000 10.50000 0.01523 0.02836 = 0.01897 0.00000 0.00000 -0.00180 FE2 3 0.757461 0.624148 0.750000 10.50000 0.00634 0.03520 = 0.00518 0.00000 0.00000 -0.00232 N1 4 0.250937 0.557624 1.750000 10.50000 0.01523 0.02836 = 0.01897 0.00000 0.00000 -0.00180 N2 4 0.329579 0.494388 1.750000 10.50000 0.01523 0.02836 = 0.01897 0.00000 0.00000 -0.00180 N3 4 0.094208 0.471690 1.750000 10.50000 0.01523 0.02836 = 0.01897 0.00000 0.00000 -0.00180 H3A 2 0.042092 0.485375 1.750000 10.50000 -1.50000 H3B 2 0.087043 0.444303 1.750000 10.50000 -1.50000 N4 4 0.359727 0.624935 1.546728 11.00000 0.01022 0.02699 = 0.00853 0.00000 0.00000 -0.00105 N5 4 0.658004 0.613624 0.955102 11.00000 0.01022 0.02699 = 0.00853 0.00000 0.00000 -0.00105 N6 4 0.795058 0.559214 0.750000 10.50000 0.04304 0.04421 = 0.06430 0.00000 0.00000 -0.00234 N7 4 0.912535 0.508611 0.750000 10.50000 0.04304 0.04421 = 0.06430 0.00000 0.00000 -0.00234 N8 4 0.692805 0.459196 0.750000 10.50000 0.04304 0.04421 = 0.06430 0.00000 0.00000 -0.00234 H8A 2 0.697670 0.434116 0.799940 10.50000 -1.50000 H8B 2 0.636447 0.468686 0.750000 10.50000 -1.50000 N9 4 0.263539 0.695191 1.750000 10.50000 0.01523 0.02836 = 0.01897 0.00000 0.00000 -0.00180 N10 4 0.181896 0.755454 1.750000 10.50000 0.01523 0.02836 = 0.01897 0.00000 0.00000 -0.00180 N11 4 0.415920 0.777064 1.750000 10.50000 0.01523 0.02836 = 0.01897 0.00000 0.00000 -0.00180 H11A 2 0.433150 0.803489 1.750000 10.50000 -1.50000 H11B 2 0.462191 0.759493 1.750000 10.50000 -1.50000 N12 4 0.714738 0.689671 0.750000 10.50000 0.04304 0.04421 = 0.06430 0.00000 0.00000 -0.00234 N13 4 0.598178 0.738094 0.750000 10.50000 0.04304 0.04421 = 0.06430 0.00000 0.00000 -0.00234 N14 4 0.806894 0.792139 0.750000 10.50000 0.04304 0.04421 = 0.06430 0.00000 0.00000 -0.00234 H14A 2 0.775091 0.810286 0.815439 10.50000 -1.50000 H14B 2 0.859360 0.785695 0.802063 10.50000 -1.50000 N15 4 0.856318 0.634243 0.545466 11.00000 0.01022 0.02699 = 0.00853 0.00000 0.00000 -0.00105 N16 4 1.157076 0.629183 -0.045508 11.00000 0.01022 0.02699 = 0.00853 0.00000 0.00000 -0.00105 C1 1 0.171984 0.536741 1.750000 10.50000 0.01523 0.02836 = 0.01897 0.00000 0.00000 -0.00180 AFIX 43 H1 2 0.118764 0.551379 1.750000 10.50000 -1.20000 AFIX 0 C2 1 0.169186 0.493962 1.750000 10.50000 0.01523 0.02836 = 0.01897 0.00000 0.00000 -0.00180 C3 1 0.255104 0.474275 1.750000 10.50000 0.01523 0.02836 = 0.01897 0.00000 0.00000 -0.00180 AFIX 43 H3 2 0.257235 0.445788 1.750000 10.50000 -1.20000 AFIX 0 C4 1 0.324590 0.535367 1.750000 10.50000 0.01523 0.02836 = 0.01897 0.00000 0.00000 -0.00180 AFIX 43 H4 2 0.378338 0.549593 1.750000 10.50000 -1.20000 AFIX 0 C5 1 0.415644 0.621783 1.436934 11.00000 0.01022 0.02699 = 0.00853 0.00000 0.00000 -0.00105 C6 1 0.603414 0.614562 1.061707 11.00000 0.01022 0.02699 = 0.00853 0.00000 0.00000 -0.00105 C7 1 0.734592 0.529399 0.750000 10.50000 0.04304 0.04421 = 0.06430 0.00000 0.00000 -0.00234 AFIX 43 H7 2 0.674419 0.536310 0.750000 10.50000 -1.20000 AFIX 0 C8 1 0.758797 0.487662 0.750000 10.50000 0.04304 0.04421 = 0.06430 0.00000 0.00000 -0.00234 C9 1 0.846851 0.481224 0.750000 10.50000 0.04304 0.04421 = 0.06430 0.00000 0.00000 -0.00234 AFIX 43 H9 2 0.864559 0.453906 0.750000 10.50000 -1.20000 AFIX 0 C10 1 0.878890 0.547869 0.750000 10.50000 0.04304 0.04421 = 0.06430 0.00000 0.00000 -0.00234 AFIX 43 H10 2 0.920757 0.568899 0.750000 10.50000 -1.20000 AFIX 0 C11 1 0.336223 0.714917 1.750000 10.50000 0.01523 0.02836 = 0.01897 0.00000 0.00000 -0.00180 AFIX 43 H11 2 0.389484 0.700310 1.750000 10.50000 -1.20000 AFIX 0 C12 1 0.339984 0.759629 1.750000 10.50000 0.01523 0.02836 = 0.01897 0.00000 0.00000 -0.00180 C13 1 0.259238 0.775401 1.750000 10.50000 0.01523 0.02836 = 0.01897 0.00000 0.00000 -0.00180 AFIX 43 H13 2 0.255844 0.803863 1.750000 10.50000 -1.20000 AFIX 0 C14 1 0.187045 0.714169 1.750000 10.50000 0.01523 0.02836 = 0.01897 0.00000 0.00000 -0.00180 AFIX 43 H14 2 0.134712 0.698870 1.750000 10.50000 -1.20000 AFIX 0 C15 1 0.772224 0.720719 0.750000 10.50000 0.04304 0.04421 = 0.06430 0.00000 0.00000 -0.00234 AFIX 43 H15 2 0.832925 0.714865 0.750000 10.50000 -1.20000 AFIX 0 C16 1 0.746041 0.760853 0.750000 10.50000 0.04304 0.04421 = 0.06430 0.00000 0.00000 -0.00234 C17 1 0.657156 0.768779 0.750000 10.50000 0.04304 0.04421 = 0.06430 0.00000 0.00000 -0.00234 AFIX 43 H17 2 0.637186 0.795766 0.750000 10.50000 -1.20000 AFIX 0 C18 1 0.627552 0.699393 0.750000 10.50000 0.04304 0.04421 = 0.06430 0.00000 0.00000 -0.00234 AFIX 43 H18 2 0.585886 0.678279 0.750000 10.50000 -1.20000 AFIX 0 C19 1 0.913263 0.634119 0.438256 11.00000 0.01022 0.02699 = 0.00853 0.00000 0.00000 -0.00105 C20 1 1.100587 0.630226 0.056937 11.00000 0.01022 0.02699 = 0.00853 0.00000 0.00000 -0.00105 PART -1 O2 5 10.995660 10.736329 11.250000 10.25000 0.10720 O1 5 10.489029 10.510520 11.250000 10.25000 0.09211 AFIX 83 H1A 2 0.488720 0.533839 1.291549 10.25000 -1.50000 AFIX 0 C21 1 10.489469 10.512250 11.069429 10.25000 0.01423 AFIX 137 H21A 2 0.533218 0.531809 1.030043 10.25000 -1.50000 H21B 2 0.431640 0.520453 1.026880 10.25000 -1.50000 H21C 2 0.503864 0.485736 1.021076 10.25000 -1.50000 AFIX 0 C22 1 0.987399 0.746969 1.066010 10.25000 0.03805 AFIX 137 H22A 2 0.962871 0.724272 0.999745 10.25000 -1.50000 H22B 2 1.045076 0.753679 1.017838 10.25000 -1.50000 H22C 2 0.948601 0.770234 1.054614 10.25000 -1.50000 AFIX 0 HKLF 4 REM rt174_nh2pymptmeoh_260k_2_a.res in Pbcm REM wR2 = 0.1846, GooF = S = 1.058, Restrained GooF = 1.056 for all data REM R1 = 0.0869 for 2751 Fo > 4sig(Fo) and 0.1250 for all 4199 data REM 133 parameters refined using 15 restraints END WGHT 0.0333 253.2347 REM Highest difference peak 5.181, deepest hole -4.383, 1-sigma level 0.335 Q1 1 1.0196 0.6029 0.2500 10.50000 0.05 2.97 Q2 1 0.9737 0.6265 0.1760 11.00000 0.05 2.89 Q3 1 0.4733 0.6222 1.1826 11.00000 0.05 2.66 Q4 1 0.4420 0.6231 1.2500 10.50000 0.05 2.25 Q5 1 0.5094 0.6367 1.2500 10.50000 0.05 2.04 ; _shelx_res_checksum 92435 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 4.184 _oxdiff_exptl_absorpt_empirical_full_min 0.606 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mo_rt327_5apmdpth2o_187k_0m _database_code_depnum_ccdc_archive 'CCDC 2018391' loop_ _audit_author_name _audit_author_address 'Carlos Bartual-Murgui' ;Universitat de Valencia Spain ; _audit_update_record ; 2020-09-17 deposited with the CCDC. 2020-09-22 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT971_mo_rt327_5apmdpth2o_187k_0m ; PROBLEM: Check Calcd Resid. Dens. 0.75A From Pt1 12.50 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_mo_rt327_5apmdpth2o_187k_0m_2 ; PROBLEM: Check Calcd Resid. Dens. 0.98A From Pt1 8.26 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT971_mo_rt327_5apmdpth2o_187k_0m_3 ; PROBLEM: Check Calcd Resid. Dens. 0.96A From Pt1 3.70 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_mo_rt327_5apmdpth2o_187k_0m ; PROBLEM: Check Calcd Resid. Dens. 0.70A From Pt1 -5.13 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_mo_rt327_5apmdpth2o_187k_0m_2 ; PROBLEM: Check Calcd Resid. Dens. 1.42A From Pt1 -4.83 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT097_mo_rt327_5apmdpth2o_187k_0m ; PROBLEM: Large Reported Max. (Positive) Residual Density 12.34 eA-3 RESPONSE: The crystal may be damaged during the dehydration/readsorption/SCO processes. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT342_mo_rt327_5apmdpth2o_187k_0m ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.045 Ang. RESPONSE: The crystal may be damaged during the dehydration/readsorption/SCO processes. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT971_mo_rt327_5apmdpth2o_187k_0m_4 ; PROBLEM: Check Calcd Resid. Dens. 1.70A From Pt1 3.45 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT972_mo_rt327_5apmdpth2o_187k_0m_3 ; PROBLEM: Check Calcd Resid. Dens. 0.77A From Pt1 -3.32 eA-3 RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO/dehydration/readsorption processes. ; _vrf_PLAT977_mo_rt327_5apmdpth2o_187k_0m ; PROBLEM: Check Negative Difference Density on H4 -1.65 eA-3 RESPONSE: The crystal may be damaged during the dehydration process. Nevertheless, this has not represented a problem to obtain good quality structural data. ; # Added during the CSD deposition process: Thursday 17 September 2020 12:29 PM # end Validation Reply Form _audit_creation_date 2020-09-09 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C12 H10 Fe N10 Pt, 0.8(H2 O)' _chemical_formula_sum 'C12 H11.60 Fe N10 O0.80 Pt' _chemical_formula_weight 559.65 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_H-M_alt 'C 1 2/m 1' _space_group_name_Hall '-C 2y' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 21.488(3) _cell_length_b 7.1993(8) _cell_length_c 14.6712(16) _cell_angle_alpha 90 _cell_angle_beta 131.584(3) _cell_angle_gamma 90 _cell_volume 1697.6(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6022 _cell_measurement_temperature 187(2) _cell_measurement_theta_max 30.80 _cell_measurement_theta_min 2.53 _shelx_estimated_absorpt_T_max 0.463 _shelx_estimated_absorpt_T_min 0.291 _exptl_absorpt_coefficient_mu 9.109 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_correction_T_min 0.4109 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1298 before and 0.0847 after correction. The Ratio of minimum to maximum transmission is 0.5507. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 2.190 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1056 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.1 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0843 _diffrn_reflns_av_unetI/netI 0.0666 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.969 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 14692 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.969 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.216 _diffrn_reflns_theta_min 2.534 _diffrn_ambient_temperature 186.99 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.969 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2407 _reflns_number_total 2871 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 12.343 _refine_diff_density_min -5.083 _refine_diff_density_rms 0.421 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 155 _refine_ls_number_reflns 2871 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0737 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+170.7754P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1674 _refine_ls_wR_factor_ref 0.1783 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All N(H,H) groups, All O(H,H) groups 2. Restrained distances H8B-N8 0.9 with sigma of 0.001 N8-H8A 0.9 with sigma of 0.001 N3-H3B 0.9 with sigma of 0.001 N3-H3A 0.9 with sigma of 0.001 O1-H1A 0.9 with sigma of 0.0001 H1B-O1 0.9 with sigma of 0.0001 H8A-O1 2.18 with sigma of 0.0001 H8B-H8A 1.5 with sigma of 0.0001 H3B-H3A 1.5 with sigma of 0.001 H3A-N7_$1 2.18 with sigma of 0.001 H1B-H1A 1.45 with sigma of 0.0001 3. Others Fixed Sof: O1(0.4) H1A(0.4) H1B(0.4) H3B(0.5) H8B(0.5) 4.a Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C4(H4), C7(H7), C9(H9), C10(H10) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.51405(4) 0.500000 0.76973(6) 0.01907(18) Uani 1 2 d S T P . . Fe1 Fe 0.500000 1.000000 1.000000 0.0177(6) Uani 1 4 d S T P . . Fe2 Fe 0.500000 0.000000 0.500000 0.0181(6) Uani 1 4 d S T P . . O1 O 0.23469(13) 0.1277(4) 0.01888(17) 0.063(9) Uiso 0.4 1 d D . P A -1 H1A H 0.2583(5) 0.0204(4) 0.0598(3) 0.095 Uiso 0.4 1 d D U P B -1 H1B H 0.2262(2) 0.1198(9) -0.04985(17) 0.095 Uiso 0.4 1 d D U P C -1 N1 N 0.3749(11) 1.000000 0.8793(16) 0.031(3) Uani 1 2 d S T P . . N2 N 0.2529(13) 1.000000 0.851(2) 0.056(5) Uani 1 2 d S T P . . N3 N 0.1974(8) 1.000000 0.5634(14) 0.050(5) Uani 1 2 d DS T P . . H3A H 0.2374(8) 1.000000 0.5594(14) 0.076 Uiso 1 2 d DS U P . . H3B H 0.1501(13) 1.055(7) 0.499(3) 0.076 Uiso 0.5 1 d D U P . . N4 N 0.5021(7) 0.8083(13) 0.9089(9) 0.026(2) Uani 1 1 d . . . . . N5 N 0.5213(8) 0.2046(15) 0.6205(11) 0.035(3) Uani 1 1 d . . . . . N6 N 0.3689(11) 0.000000 0.4179(15) 0.032(3) Uani 1 2 d S T P . . N7 N 0.2711(10) 0.000000 0.4482(14) 0.051(5) Uani 1 2 d S T P . . N8 N 0.1665(6) 0.000000 0.1299(7) 0.068(7) Uani 1 2 d DS T P . . H8A H 0.17270(13) 0.000000 0.0750(2) 0.101 Uiso 1 2 d DS U P . . H8B H 0.1453(2) 0.1072(8) 0.1307(3) 0.101 Uiso 0.5 1 d D U P . . C1 C 0.3302(14) 1.000000 0.7628(19) 0.035(4) Uani 1 2 d S T P . . H1 H 0.357532 1.000000 0.731934 0.042 Uiso 1 2 calc R U P . . C2 C 0.2408(13) 1.000000 0.6777(18) 0.035(4) Uani 1 2 d S T P . . C3 C 0.2013(16) 1.000000 0.730(2) 0.041(5) Uani 1 2 d S T P . . H3 H 0.142635 1.000000 0.680784 0.050 Uiso 1 2 calc R U P . . C4 C 0.3328(15) 1.000000 0.920(2) 0.040(5) Uani 1 2 d S T P . . H4 H 0.365118 1.000000 1.005524 0.048 Uiso 1 2 calc R U P . . C5 C 0.5062(7) 0.6955(15) 0.8570(10) 0.020(2) Uani 1 1 d . . . . . C6 C 0.5197(8) 0.3100(16) 0.6782(11) 0.024(2) Uani 1 1 d . . . . . C7 C 0.3075(18) 0.000000 0.303(2) 0.047(6) Uani 1 2 d S T P . . H7 H 0.320729 0.000000 0.253227 0.056 Uiso 1 2 calc R U P . . C8 C 0.2265(14) 0.000000 0.246(2) 0.043(5) Uani 1 2 d S T P . . C9 C 0.2106(14) 0.000000 0.327(2) 0.040(5) Uani 1 2 d S T P . . H9 H 0.154515 0.000000 0.293130 0.048 Uiso 1 2 calc R U P . . C10 C 0.3487(14) 0.000000 0.490(2) 0.041(5) Uani 1 2 d S T P . . H10 H 0.393344 0.000000 0.575363 0.049 Uiso 1 2 calc R U P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0276(3) 0.0100(2) 0.0226(3) 0.000 0.0180(3) 0.000 Fe1 0.0305(17) 0.0065(11) 0.0230(15) 0.000 0.0207(14) 0.000 Fe2 0.0289(16) 0.0093(12) 0.0236(15) 0.000 0.0206(14) 0.000 N1 0.042(9) 0.021(7) 0.042(9) 0.000 0.033(8) 0.000 N2 0.045(12) 0.060(14) 0.056(13) 0.000 0.031(11) 0.000 N3 0.047(11) 0.077(15) 0.046(11) 0.000 0.039(10) 0.000 N4 0.047(6) 0.013(4) 0.025(5) 0.000(3) 0.027(5) -0.006(4) N5 0.060(8) 0.019(5) 0.051(7) 0.004(5) 0.047(7) 0.006(5) N6 0.042(9) 0.024(7) 0.037(9) 0.000 0.029(8) 0.000 N7 0.036(10) 0.073(15) 0.053(12) 0.000 0.034(10) 0.000 N8 0.10(2) 0.071(17) 0.068(16) 0.000 0.071(16) 0.000 C1 0.059(13) 0.012(7) 0.042(11) 0.000 0.036(11) 0.000 C2 0.033(10) 0.024(8) 0.032(10) 0.000 0.015(8) 0.000 C3 0.054(13) 0.034(10) 0.053(13) 0.000 0.043(12) 0.000 C4 0.057(13) 0.031(10) 0.065(14) 0.000 0.054(13) 0.000 C5 0.037(6) 0.014(4) 0.019(5) 0.000(4) 0.023(5) -0.004(4) C6 0.030(6) 0.016(5) 0.031(6) 0.003(4) 0.022(5) 0.002(4) C7 0.092(19) 0.021(9) 0.043(12) 0.000 0.051(14) 0.000 C8 0.036(11) 0.026(9) 0.055(14) 0.000 0.025(11) 0.000 C9 0.031(10) 0.043(11) 0.044(11) 0.000 0.024(9) 0.000 C10 0.036(11) 0.051(13) 0.049(12) 0.000 0.034(10) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C5 1.983(10) . ? Pt1 C5 1.983(10) 6_565 ? Pt1 C6 1.976(12) 6_565 ? Pt1 C6 1.976(12) . ? Fe1 N1 2.010(17) 5_677 ? Fe1 N1 2.010(17) . ? Fe1 N4 1.942(10) 6_575 ? Fe1 N4 1.942(10) 2_657 ? Fe1 N4 1.942(10) 5_677 ? Fe1 N4 1.942(10) . ? Fe2 N5 2.105(11) 2_656 ? Fe2 N5 2.105(11) 6 ? Fe2 N5 2.105(11) 5_656 ? Fe2 N5 2.105(11) . ? Fe2 N6 2.210(17) . ? Fe2 N6 2.210(17) 5_656 ? O1 H1A 0.90000(13) . ? O1 H1B 0.90000(15) . ? N1 C1 1.29(3) . ? N1 C4 1.37(2) . ? N2 C3 1.33(3) . ? N2 C4 1.29(3) . ? N3 H3A 0.9000(10) . ? N3 H3B 0.9000(10) . ? N3 H3B 0.9000(11) 6_575 ? N3 C2 1.27(2) . ? N4 C5 1.157(14) . ? N5 C6 1.155(16) . ? N6 C7 1.27(3) . ? N6 C10 1.38(3) . ? N7 C9 1.33(3) . ? N7 C10 1.34(2) . ? N8 H8A 0.9000(10) . ? N8 H8B 0.9000(10) . ? N8 H8B 0.9000(10) 6 ? N8 C8 1.28(3) . ? C1 H1 0.9500 . ? C1 C2 1.44(3) . ? C2 C3 1.48(3) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C7 H7 0.9500 . ? C7 C8 1.34(4) . ? C8 C9 1.45(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Pt1 C5 90.4(6) . 6_565 ? C6 Pt1 C5 91.0(4) . 6_565 ? C6 Pt1 C5 91.0(4) 6_565 . ? C6 Pt1 C5 178.2(5) 6_565 6_565 ? C6 Pt1 C5 178.2(5) . . ? C6 Pt1 C6 87.6(7) . 6_565 ? N1 Fe1 N1 180.0 . 5_677 ? N4 Fe1 N1 88.8(5) 2_657 . ? N4 Fe1 N1 91.2(5) 5_677 5_677 ? N4 Fe1 N1 88.8(5) 5_677 . ? N4 Fe1 N1 91.2(5) 2_657 5_677 ? N4 Fe1 N1 91.2(5) 6_575 . ? N4 Fe1 N1 91.2(5) . . ? N4 Fe1 N1 88.8(5) . 5_677 ? N4 Fe1 N1 88.8(5) 6_575 5_677 ? N4 Fe1 N4 180.0 6_575 2_657 ? N4 Fe1 N4 90.6(5) 6_575 . ? N4 Fe1 N4 180.0(8) 5_677 . ? N4 Fe1 N4 90.6(5) 5_677 2_657 ? N4 Fe1 N4 89.4(5) 2_657 . ? N4 Fe1 N4 89.4(5) 5_677 6_575 ? N5 Fe2 N5 180.0(4) . 5_656 ? N5 Fe2 N5 91.2(6) . 2_656 ? N5 Fe2 N5 91.2(6) 5_656 6 ? N5 Fe2 N5 180.0 6 2_656 ? N5 Fe2 N5 88.8(6) 5_656 2_656 ? N5 Fe2 N5 88.8(6) . 6 ? N5 Fe2 N6 93.1(5) . 5_656 ? N5 Fe2 N6 86.9(5) 6 . ? N5 Fe2 N6 93.1(5) 5_656 . ? N5 Fe2 N6 86.9(5) 5_656 5_656 ? N5 Fe2 N6 93.1(5) 2_656 . ? N5 Fe2 N6 86.9(5) 2_656 5_656 ? N5 Fe2 N6 86.9(5) . . ? N5 Fe2 N6 93.1(5) 6 5_656 ? N6 Fe2 N6 180.0 . 5_656 ? H1A O1 H1B 107.328(17) . . ? C1 N1 Fe1 123.5(15) . . ? C1 N1 C4 117(2) . . ? C4 N1 Fe1 119.9(15) . . ? C4 N2 C3 123(2) . . ? H3A N3 H3B 112.89(18) . 6_575 ? H3A N3 H3B 112.88(19) . . ? H3B N3 H3B 53(8) . 6_575 ? C2 N3 H3A 101.0(19) . . ? C2 N3 H3B 136(3) . 6_575 ? C2 N3 H3B 136(3) . . ? C5 N4 Fe1 177.6(10) . . ? C6 N5 Fe2 168.5(12) . . ? C7 N6 Fe2 123.3(16) . . ? C7 N6 C10 116(2) . . ? C10 N6 Fe2 121.2(14) . . ? C9 N7 C10 115.0(17) . . ? H8A N8 H8B 112.88(14) . 6 ? H8A N8 H8B 112.89(14) . . ? H8B N8 H8B 118.0(14) . 6 ? C8 N8 H8A 124.8(14) . . ? C8 N8 H8B 93.2(7) . 6 ? C8 N8 H8B 93.2(7) . . ? N1 C1 H1 118.6 . . ? N1 C1 C2 123(2) . . ? C2 C1 H1 118.6 . . ? N3 C2 C1 122(2) . . ? N3 C2 C3 121.2(19) . . ? C1 C2 C3 116.5(19) . . ? N2 C3 C2 116(2) . . ? N2 C3 H3 122.0 . . ? C2 C3 H3 122.0 . . ? N1 C4 H4 117.4 . . ? N2 C4 N1 125(2) . . ? N2 C4 H4 117.4 . . ? N4 C5 Pt1 179.3(8) . . ? N5 C6 Pt1 176.9(11) . . ? N6 C7 H7 116.2 . . ? N6 C7 C8 128(2) . . ? C8 C7 H7 116.2 . . ? N8 C8 C7 126(2) . . ? N8 C8 C9 121.0(19) . . ? C7 C8 C9 113(2) . . ? N7 C9 C8 123.0(19) . . ? N7 C9 H9 118.5 . . ? C8 C9 H9 118.5 . . ? N6 C10 H10 117.2 . . ? N7 C10 N6 126(2) . . ? N7 C10 H10 117.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 N1 C1 C2 180.000(10) . . . . ? Fe1 N1 C4 N2 180.000(14) . . . . ? Fe2 N6 C7 C8 180.000(5) . . . . ? Fe2 N6 C10 N7 180.000(5) . . . . ? N1 C1 C2 N3 180.000(8) . . . . ? N1 C1 C2 C3 0.000(16) . . . . ? N3 C2 C3 N2 180.000(13) . . . . ? N6 C7 C8 N8 180.000(7) . . . . ? N6 C7 C8 C9 0.000(8) . . . . ? N8 C8 C9 N7 180.000(5) . . . . ? C1 N1 C4 N2 0.00(2) . . . . ? C1 C2 C3 N2 0.000(14) . . . . ? C3 N2 C4 N1 0.00(2) . . . . ? C4 N1 C1 C2 0.000(15) . . . . ? C4 N2 C3 C2 0.000(17) . . . . ? C7 N6 C10 N7 0.000(9) . . . . ? C7 C8 C9 N7 0.000(6) . . . . ? C9 N7 C10 N6 0.000(9) . . . . ? C10 N6 C7 C8 0.000(7) . . . . ? C10 N7 C9 C8 0.000(8) . . . . ? _shelx_res_file ; TITL mo_rt327_5apmdpth2o_187k_0m_a.res in C2/m mo_rt327_5apmdpth2o_187k_0m.res created by SHELXL-2018/3 at 02:09:57 on 09-Sep-2020 REM Old TITL mo_RT327_5apmdPtH2O_187K_0m in C2/m REM SHELXT solution in C2/m: R1 0.118, Rweak 0.021, Alpha 0.017 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C13 N7 Fe Pt CELL 0.71073 21.4877 7.1993 14.6712 90 131.584 90 ZERR 4 0.0025 0.0008 0.0016 0 0.003 0 LATT 7 SYMM -X,+Y,-Z SFAC C H Fe N O Pt UNIT 48 46.4 4 40 3.2 4 EQIV $1 +X,1-Y,+Z DFIX 0.9 0.001 H8b N8 DANG 2.18 0.0001 H8a O1 DFIX 0.9 0.001 N8 H8a DANG 1.5 0.0001 H8b H8a DANG 1.5 0.001 H3b H3a DFIX 0.9 0.001 N3 H3b DFIX 0.9 0.001 N3 H3a DANG 2.18 0.001 H3a N7_$1 DFIX 0.9 0.0001 O1 H1a DFIX 0.9 0.0001 H1b O1 DANG 1.45 0.0001 H1b H1a L.S. 50 PLAN 50 SIZE 0.1 0.18 0.18 TEMP -86.16 CONF list 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.026500 170.775406 FVAR 0.18003 PT1 6 0.514047 0.500000 0.769732 10.50000 0.02762 0.01003 = 0.02261 0.00000 0.01796 0.00000 FE1 3 0.500000 1.000000 1.000000 10.25000 0.03055 0.00647 = 0.02300 0.00000 0.02071 0.00000 FE2 3 0.500000 0.000000 0.500000 10.25000 0.02887 0.00929 = 0.02361 0.00000 0.02059 0.00000 PART -1 O1 5 0.234689 0.127703 0.018878 10.40000 0.06327 H1A 2 0.258306 0.020414 0.059780 10.40000 -1.50000 H1B 2 0.226240 0.119784 -0.049852 10.40000 -1.50000 PART 0 N1 4 0.374936 1.000000 0.879310 10.50000 0.04227 0.02058 = 0.04222 0.00000 0.03293 0.00000 N2 4 0.252891 1.000000 0.851004 10.50000 0.04497 0.05969 = 0.05572 0.00000 0.03080 0.00000 N3 4 0.197361 1.000000 0.563424 10.50000 0.04747 0.07683 = 0.04638 0.00000 0.03926 0.00000 H3A 2 0.237355 1.000000 0.559364 10.50000 -1.50000 H3B 2 0.150150 1.055387 0.498835 10.50000 -1.50000 N4 4 0.502079 0.808301 0.908939 11.00000 0.04706 0.01281 = 0.02481 -0.00026 0.02727 -0.00559 N5 4 0.521349 0.204635 0.620501 11.00000 0.06039 0.01867 = 0.05068 0.00351 0.04690 0.00585 N6 4 0.368895 0.000000 0.417906 10.50000 0.04188 0.02438 = 0.03745 0.00000 0.02907 0.00000 N7 4 0.271078 0.000000 0.448220 10.50000 0.03619 0.07290 = 0.05315 0.00000 0.03413 0.00000 N8 4 0.166486 0.000000 0.129907 10.50000 0.10025 0.07060 = 0.06828 0.00000 0.07116 0.00000 H8A 2 0.172697 0.000000 0.074979 10.50000 -1.50000 H8B 2 0.145279 0.107157 0.130703 10.50000 -1.50000 C1 1 0.330211 1.000000 0.762796 10.50000 0.05895 0.01160 = 0.04172 0.00000 0.03606 0.00000 AFIX 43 H1 2 0.357532 1.000000 0.731934 10.50000 -1.20000 AFIX 0 C2 1 0.240797 1.000000 0.677729 10.50000 0.03310 0.02389 = 0.03214 0.00000 0.01501 0.00000 C3 1 0.201346 1.000000 0.730371 10.50000 0.05373 0.03404 = 0.05311 0.00000 0.04252 0.00000 AFIX 43 H3 2 0.142635 1.000000 0.680784 10.50000 -1.20000 AFIX 0 C4 1 0.332823 1.000000 0.919897 10.50000 0.05683 0.03147 = 0.06477 0.00000 0.05442 0.00000 AFIX 43 H4 2 0.365118 1.000000 1.005524 10.50000 -1.20000 AFIX 0 C5 1 0.506207 0.695451 0.857000 11.00000 0.03714 0.01361 = 0.01938 -0.00049 0.02274 -0.00359 C6 1 0.519681 0.310019 0.678206 11.00000 0.02982 0.01632 = 0.03115 0.00318 0.02214 0.00236 C7 1 0.307510 0.000000 0.303490 10.50000 0.09170 0.02095 = 0.04287 0.00000 0.05105 0.00000 AFIX 43 H7 2 0.320729 0.000000 0.253227 10.50000 -1.20000 AFIX 0 C8 1 0.226498 0.000000 0.245720 10.50000 0.03617 0.02647 = 0.05461 0.00000 0.02537 0.00000 C9 1 0.210623 0.000000 0.327308 10.50000 0.03094 0.04304 = 0.04379 0.00000 0.02379 0.00000 AFIX 43 H9 2 0.154515 0.000000 0.293130 10.50000 -1.20000 AFIX 0 C10 1 0.348663 0.000000 0.489539 10.50000 0.03629 0.05086 = 0.04878 0.00000 0.03367 0.00000 AFIX 43 H10 2 0.393344 0.000000 0.575363 10.50000 -1.20000 AFIX 0 HKLF 4 REM mo_rt327_5apmdpth2o_187k_0m_a.res in C2/m REM wR2 = 0.1783, GooF = S = 1.142, Restrained GooF = 1.139 for all data REM R1 = 0.0737 for 2407 Fo > 4sig(Fo) and 0.0935 for all 2871 data REM 155 parameters refined using 11 restraints END WGHT 0.0265 170.6903 REM Highest difference peak 12.343, deepest hole -5.083, 1-sigma level 0.421 Q1 1 0.5144 0.5000 0.7207 10.50000 0.05 12.34 Q2 1 0.4540 0.5000 0.7215 10.50000 0.05 7.70 Q3 1 0.5733 0.5000 0.8400 10.50000 0.05 3.25 Q4 1 0.5030 0.5776 0.8223 11.00000 0.05 1.83 Q5 1 0.5600 0.5961 0.7742 11.00000 0.05 1.79 Q6 1 0.4984 1.0000 1.0506 10.50000 0.05 1.63 Q7 1 0.2756 1.0000 0.5997 10.50000 0.05 1.63 Q8 1 0.5158 0.0000 0.4691 10.50000 0.05 1.56 Q9 1 0.5566 0.7995 0.9717 11.00000 0.05 1.51 Q10 1 0.3899 1.0000 0.8380 10.50000 0.05 1.45 Q11 1 0.4044 0.0000 0.3584 10.50000 0.05 1.41 Q12 1 0.2465 0.0000 0.0875 10.50000 0.05 1.41 Q13 1 0.6216 0.5000 0.9109 10.50000 0.05 1.39 Q14 1 0.4994 0.2990 0.6081 11.00000 0.05 1.38 Q15 1 0.4574 0.4040 0.6686 11.00000 0.05 1.33 Q16 1 0.5594 0.5000 0.8847 10.50000 0.05 1.33 Q17 1 0.2883 1.0000 0.6762 10.50000 0.05 1.33 Q18 1 0.3904 0.0000 0.2373 10.50000 0.05 1.33 Q19 1 0.2505 0.0000 0.1605 10.50000 0.05 1.32 Q20 1 0.5199 0.6614 0.8230 11.00000 0.05 1.31 Q21 1 0.4220 1.0000 0.9292 10.50000 0.05 1.31 Q22 1 0.5375 0.7898 0.9036 11.00000 0.05 1.28 Q23 1 0.2206 0.0000 0.1879 10.50000 0.05 1.27 Q24 1 0.2986 0.0000 0.1253 10.50000 0.05 1.24 Q25 1 0.5039 0.3500 0.7207 11.00000 0.05 1.22 Q26 1 0.0914 1.0000 0.5786 10.50000 0.05 1.15 Q27 1 0.4576 0.5000 0.6081 10.50000 0.05 1.11 Q28 1 0.3231 0.0000 0.3731 10.50000 0.05 1.09 Q29 1 0.2928 1.0000 0.8488 10.50000 0.05 1.09 Q30 1 0.4938 0.2034 0.5404 11.00000 0.05 1.07 Q31 1 0.4321 0.0000 0.5086 10.50000 0.05 1.02 Q32 1 0.4736 0.5000 0.8484 10.50000 0.05 0.99 Q33 1 0.4375 0.0740 0.4289 11.00000 0.05 0.99 Q34 1 0.5607 0.0000 0.7199 10.50000 0.05 0.97 Q35 1 0.5589 0.6110 0.8587 11.00000 0.05 0.91 Q36 1 0.4610 0.5000 0.5595 10.50000 0.05 0.91 Q37 1 0.4723 0.3043 0.6384 11.00000 0.05 0.91 Q38 1 0.4909 0.1848 0.6383 11.00000 0.05 0.91 Q39 1 0.3135 1.0000 0.8111 10.50000 0.05 0.90 Q40 1 0.4369 0.7934 0.7838 11.00000 0.05 0.89 Q41 1 0.1955 0.0000 0.3776 10.50000 0.05 0.89 Q42 1 0.3726 1.0000 0.7054 10.50000 0.05 0.88 Q43 1 0.4331 1.0000 0.8318 10.50000 0.05 0.87 Q44 1 0.4383 0.2084 0.5586 11.00000 0.05 0.86 Q45 1 0.2128 0.0000 0.0086 10.50000 0.05 0.86 Q46 1 0.5181 0.1075 0.5687 11.00000 0.05 0.86 Q47 1 0.5594 0.6738 0.9115 11.00000 0.05 0.85 Q48 1 0.1288 1.1169 0.4409 11.00000 0.05 0.85 Q49 1 0.1172 0.0000 0.2007 10.50000 0.05 0.85 Q50 1 0.5000 -0.1080 0.5000 10.50000 0.05 0.84 ; _shelx_res_checksum 46365 _olex2_submission_special_instructions 'No special instructions were received' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_rt312_nh2pympdmeoh_260k _database_code_depnum_ccdc_archive 'CCDC 2018393' loop_ _audit_author_name _audit_author_address 'Carlos Bartual-Murgui' ;Universitat de Valencia Spain ; _audit_update_record ; 2020-09-17 deposited with the CCDC. 2020-09-22 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT342_rt312_nh2pympdmeoh_260k ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.02375 Ang. RESPONSE: The crystal may be damaged during the dehydration process. Nevertheless, this has not represented a problem to obtain good quality structural data. ; _vrf_PLAT910_rt312_nh2pympdmeoh_260k ; PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 12 Note RESPONSE: The unit cell is relatively large and Mo radiation was used. Therefore several reflections were probably stopped by the beam stop. Nevertheless, this has not represented a problem to obtain good quality structural data. ; # Added during the CSD deposition process: Thursday 17 September 2020 12:29 PM # end Validation Reply Form _audit_creation_date 2020-09-09 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C12 H10 Fe N10 Pd, 0.5(C H4 O)' _chemical_formula_sum 'C12.50 H12 Fe N10 O0.50 Pd' _chemical_formula_weight 472.57 _chemical_melting_point ? _chemical_oxdiff_formula 'C11 H10 N O' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system orthorhombic _space_group_IT_number 57 _space_group_name_H-M_alt 'P b c m' _space_group_name_Hall '-P 2c 2b' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y-1/2, z' _cell_length_a 15.0184(12) _cell_length_b 32.5156(18) _cell_length_c 7.3514(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3589.9(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 911 _cell_measurement_temperature 260.0(2) _cell_measurement_theta_max 26.7370 _cell_measurement_theta_min 3.9600 _shelx_estimated_absorpt_T_max 0.947 _shelx_estimated_absorpt_T_min 0.810 _exptl_absorpt_coefficient_mu 1.830 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.93558 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1864 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_unetI/netI 0.0845 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.835 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 9664 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.835 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.982 _diffrn_reflns_theta_min 3.300 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 260.0(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0267 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.835 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -88.00 -62.00 1.00 30.00 -- -14.81-178.00 60.00 26 2 \w -57.00 57.00 1.00 30.00 -- -14.81 19.00-180.00 114 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0162461000 _diffrn_orient_matrix_UB_12 0.0133803000 _diffrn_orient_matrix_UB_13 0.0685554000 _diffrn_orient_matrix_UB_21 -0.0422743000 _diffrn_orient_matrix_UB_22 0.0003913000 _diffrn_orient_matrix_UB_23 -0.0430863000 _diffrn_orient_matrix_UB_31 -0.0135657000 _diffrn_orient_matrix_UB_32 -0.0172113000 _diffrn_orient_matrix_UB_33 0.0523726000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1884 _reflns_number_total 3897 _reflns_odcompleteness_completeness 99.48 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 24.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 2.012 _refine_diff_density_min -1.507 _refine_diff_density_rms 0.187 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 195 _refine_ls_number_reflns 3897 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1491 _refine_ls_R_factor_gt 0.0816 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0848P)^2^+25.2612P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2037 _refine_ls_wR_factor_ref 0.2498 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, {H3A,H3B} of N3 At 1.5 times of: All C(H,H,H) groups, {H11A,H11B} of N11, {H14A,H14B} of N14, {H8A,H8B} of N8, All O(H) groups 2. Restrained distances O1-C21 1.4 with sigma of 0.02 N14-H14A_$1 0.9 with sigma of 0.0001 H14B_$1-N14 0.9 with sigma of 0.0001 N8-H8B 0.9 with sigma of 0.0001 N8-H8A 0.9 with sigma of 0.0001 H14B_$1-H14A_$1 1.5 with sigma of 0.0001 H14A-O2_$2 2.2 with sigma of 0.0001 N11_$1-H11A_$1 0.9 with sigma of 0.0001 H11A_$1-H11B_$1 1.5 with sigma of 0.0001 N11_$1-H11B_$1 0.9 with sigma of 0.0001 H8A-H8B 1.5 with sigma of 0.0001 3. Uiso/Uaniso restraints and constraints Uanis(N11) = Uanis(C12) = Uanis(C13) = Uanis(N10) = Uanis(C14) = Uanis(N9) = Uanis(C11) Uanis(N8) = Uanis(C8) = Uanis(C9) = Uanis(N7) = Uanis(C10) = Uanis(N6) = Uanis(C7) Uanis(N14) = Uanis(C16) = Uanis(C15) = Uanis(N12) = Uanis(C18) = Uanis(N13) = Uanis(C17) Uanis(N1) = Uanis(C4) = Uanis(N2) = Uanis(C3) = Uanis(C2) = Uanis(C1) = Uanis(N3) 4. Others Fixed Sof: H8B(0.5) H11B(0.5) H14A(0.5) O2(0.25) H2(0.25) C22(0.25) H22A(0.25) H22B(0.25) H22C(0.25) O1(0.25) H1A(0.25) C21(0.25) H21A(0.25) H21B(0.25) H21C(0.25) Fixed X: O2(0.496119) C22(0.484519) O1(1.01363) Fixed Y: O2(0.7643) C22(0.762381) O1(0.484839) Fixed Z: O2(1.25) C22(1.05867) O1(1.25) 5.a Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C4(H4), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18) 5.b X=CH2 refined with riding coordinates: N3(H3A,H3B) 5.c Idealised Me refined as rotating group: C22(H22A,H22B,H22C), C21(H21A,H21B,H21C) 5.d Idealised tetrahedral OH refined as rotating group: O2(H2), O1(H1A) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.50601(7) 0.63272(3) 0.750000 0.0156(4) Uani 1 2 d S T P . . Pd2 Pd 0.00788(6) 0.61627(3) -0.250000 0.0146(4) Uani 1 2 d S T P . . Fe1 Fe 0.75721(13) 0.62579(6) 1.250000 0.0146(5) Uani 1 2 d S T P . . Fe2 Fe 0.25661(13) 0.62264(6) 0.250000 0.0157(5) Uani 1 2 d S T P . . N1 N 0.7478(9) 0.5579(4) 1.250000 0.0495(19) Uani 1 2 d S T P . . N2 N 0.8303(9) 0.4944(4) 1.250000 0.0495(19) Uani 1 2 d S T P . . N3 N 0.5980(9) 0.4736(4) 1.250000 0.0495(19) Uani 1 2 d S T P . . H3A H 0.598126 0.447136 1.250000 0.059 Uiso 1 2 calc R U P . . H3B H 0.548296 0.486746 1.250000 0.059 Uiso 1 2 calc R U P . . N4 N 0.6556(6) 0.6278(3) 1.0447(14) 0.029(2) Uani 1 1 d . . . . . N5 N 0.3572(6) 0.6318(3) 0.4543(14) 0.026(2) Uani 1 1 d . . . . . N6 N 0.2947(10) 0.5567(4) 0.250000 0.0455(17) Uani 1 2 d S T P . . N7 N 0.4086(10) 0.5065(4) 0.250000 0.0455(17) Uani 1 2 d S T P . . N8 N 0.1979(2) 0.45679(7) 0.250000 0.0455(17) Uani 1 2 d DS T P . . H8A H 0.2065(3) 0.42940(7) 0.250000 0.068 Uiso 1 2 d DS U P . . H8B H 0.1529(2) 0.46465(11) 0.3228(6) 0.068 Uiso 0.5 1 d D U P . . N9 N 0.7630(10) 0.6941(4) 1.250000 0.052(2) Uani 1 2 d S T P . . N10 N 0.6805(10) 0.7565(4) 1.250000 0.052(2) Uani 1 2 d S T P . . N11 N 0.9138(5) 0.77719(6) 1.250000 0.052(2) Uani 1 2 d S T P . . H11A H 0.9097(7) 0.80480(7) 1.250000 0.078 Uiso 1 2 d S U P . . H11B H 0.9342(5) 0.76704(11) 1.1440(4) 0.078 Uiso 0.5 1 d . U P . . N12 N 0.2135(11) 0.6883(4) 0.250000 0.054(2) Uani 1 2 d S T P . . N13 N 0.0965(10) 0.7368(4) 0.250000 0.054(2) Uani 1 2 d S T P . . N14 N 0.30975(18) 0.78857(7) 0.250000 0.054(2) Uani 1 2 d DS T P . . H14A H 0.36212(10) 0.78809(12) 0.3095(5) 0.081 Uiso 0.5 1 d D U P . . H14B H 0.2841(2) 0.81359(9) 0.250000 0.081 Uiso 1 2 d S U P . . N15 N 0.1583(6) 0.6113(3) 0.0444(14) 0.030(2) Uani 1 1 d . . . . . N16 N -0.1399(6) 0.6231(3) -0.5452(13) 0.027(2) Uani 1 1 d . . . . . C1 C 0.6730(12) 0.5368(5) 1.250000 0.0495(19) Uani 1 2 d S T P . . H1 H 0.619017 0.550816 1.250000 0.059 Uiso 1 2 calc R U P . . C2 C 0.6726(12) 0.4936(5) 1.250000 0.0495(19) Uani 1 2 d S T P . . C3 C 0.7553(11) 0.4745(5) 1.250000 0.0495(19) Uani 1 2 d S T P . . H3 H 0.757045 0.445954 1.250000 0.059 Uiso 1 2 calc R U P . . C4 C 0.8240(12) 0.5350(5) 1.250000 0.0495(19) Uani 1 2 d S T P . . H4 H 0.877308 0.549583 1.250000 0.059 Uiso 1 2 calc R U P . . C5 C 0.6018(7) 0.6305(3) 0.9400(16) 0.020(3) Uani 1 1 d . . . . . C6 C 0.4123(7) 0.6327(3) 0.5590(17) 0.023(3) Uani 1 1 d . . . . . C7 C 0.2324(12) 0.5274(5) 0.250000 0.0455(17) Uani 1 2 d S T P . . H7 H 0.172389 0.534332 0.250000 0.055 Uiso 1 2 calc R U P . . C8 C 0.2584(12) 0.4862(5) 0.250000 0.0455(17) Uani 1 2 d S T P . . C9 C 0.3514(12) 0.4785(5) 0.250000 0.0455(17) Uani 1 2 d S T P . . H9 H 0.370859 0.451376 0.250000 0.055 Uiso 1 2 calc R U P . . C10 C 0.3794(12) 0.5455(5) 0.250000 0.0455(17) Uani 1 2 d S T P . . H10 H 0.422042 0.566252 0.250000 0.055 Uiso 1 2 calc R U P . . C11 C 0.8373(13) 0.7142(5) 1.250000 0.052(2) Uani 1 2 d S T P . . H11 H 0.891179 0.700078 1.250000 0.063 Uiso 1 2 calc R U P . . C12 C 0.8364(13) 0.7581(5) 1.250000 0.052(2) Uani 1 2 d S T P . . C13 C 0.7564(12) 0.7761(5) 1.250000 0.052(2) Uani 1 2 d S T P . . H13 H 0.754601 0.804653 1.250000 0.063 Uiso 1 2 calc R U P . . C14 C 0.6863(13) 0.7149(5) 1.250000 0.052(2) Uani 1 2 d S T P . . H14 H 0.633603 0.699885 1.250000 0.063 Uiso 1 2 calc R U P . . C15 C 0.2744(13) 0.7184(5) 0.250000 0.054(2) Uani 1 2 d S T P . . H15 H 0.334773 0.711964 0.250000 0.065 Uiso 1 2 calc R U P . . C16 C 0.2476(12) 0.7590(5) 0.250000 0.054(2) Uani 1 2 d S T P . . C17 C 0.1577(13) 0.7658(5) 0.250000 0.054(2) Uani 1 2 d S T P . . H17 H 0.138343 0.792961 0.250000 0.065 Uiso 1 2 calc R U P . . C18 C 0.1291(13) 0.6988(5) 0.250000 0.054(2) Uani 1 2 d S T P . . H18 H 0.087881 0.677500 0.250000 0.065 Uiso 1 2 calc R U P . . C19 C 0.1020(7) 0.6135(3) -0.0596(16) 0.023(3) Uani 1 1 d . . . . . C20 C -0.0841(7) 0.6209(3) -0.4378(15) 0.019(2) Uani 1 1 d . . . . . O2 O 0.496119 0.764300 1.250000 0.082(11) Uiso 0.25 1 d S . P A -1 H2 H 0.492002 0.788255 1.283841 0.123 Uiso 0.25 1 calc R U P A -1 C22 C 0.484519 0.762381 1.058670 0.048(15) Uiso 0.25 1 d . . P A -1 H22A H 0.529569 0.778624 1.000178 0.071 Uiso 0.25 1 calc R U P A -1 H22B H 0.426783 0.772882 1.027314 0.071 Uiso 0.25 1 calc R U P A -1 H22C H 0.489356 0.734337 1.019047 0.071 Uiso 0.25 1 calc R U P A -1 O1 O 1.013630 0.484839 1.250000 0.090(11) Uiso 0.25 1 d DS . P B -1 H1A H 0.997818 0.461913 1.283404 0.135 Uiso 0.25 1 calc R U P B -1 C21 C 1.011(4) 0.4868(14) 1.063(3) 0.040(13) Uiso 0.25 1 d D . P B -1 H21A H 1.066170 0.476834 1.014465 0.060 Uiso 0.25 1 calc R U P B -1 H21B H 1.002155 0.514824 1.026140 0.060 Uiso 0.25 1 calc R U P B -1 H21C H 0.962807 0.470195 1.019183 0.060 Uiso 0.25 1 calc R U P B -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0116(7) 0.0257(6) 0.0094(9) 0.000 0.000 0.0025(4) Pd2 0.0082(6) 0.0263(6) 0.0093(9) 0.000 0.000 0.0030(4) Fe1 0.0088(10) 0.0262(10) 0.0089(10) 0.000 0.000 0.0038(8) Fe2 0.0081(10) 0.0313(11) 0.0077(10) 0.000 0.000 0.0040(8) N1 0.034(4) 0.038(3) 0.076(5) 0.000 0.000 0.003(3) N2 0.034(4) 0.038(3) 0.076(5) 0.000 0.000 0.003(3) N3 0.034(4) 0.038(3) 0.076(5) 0.000 0.000 0.003(3) N4 0.018(5) 0.048(6) 0.020(6) -0.009(5) -0.001(5) 0.014(4) N5 0.011(5) 0.055(6) 0.013(6) 0.000(5) -0.007(4) 0.004(4) N6 0.047(4) 0.039(4) 0.050(4) 0.000 0.000 0.000(3) N7 0.047(4) 0.039(4) 0.050(4) 0.000 0.000 0.000(3) N8 0.047(4) 0.039(4) 0.050(4) 0.000 0.000 0.000(3) N9 0.045(4) 0.042(4) 0.070(6) 0.000 0.000 0.001(3) N10 0.045(4) 0.042(4) 0.070(6) 0.000 0.000 0.001(3) N11 0.045(4) 0.042(4) 0.070(6) 0.000 0.000 0.001(3) N12 0.045(4) 0.042(4) 0.075(6) 0.000 0.000 0.001(3) N13 0.045(4) 0.042(4) 0.075(6) 0.000 0.000 0.001(3) N14 0.045(4) 0.042(4) 0.075(6) 0.000 0.000 0.001(3) N15 0.014(5) 0.052(6) 0.025(7) -0.005(5) -0.002(5) 0.008(4) N16 0.029(6) 0.044(5) 0.007(6) 0.006(4) 0.000(5) -0.001(4) C1 0.034(4) 0.038(3) 0.076(5) 0.000 0.000 0.003(3) C2 0.034(4) 0.038(3) 0.076(5) 0.000 0.000 0.003(3) C3 0.034(4) 0.038(3) 0.076(5) 0.000 0.000 0.003(3) C4 0.034(4) 0.038(3) 0.076(5) 0.000 0.000 0.003(3) C5 0.014(6) 0.040(6) 0.007(6) 0.001(5) -0.003(5) 0.005(4) C6 0.013(6) 0.034(6) 0.022(8) 0.004(5) 0.005(5) 0.000(4) C7 0.047(4) 0.039(4) 0.050(4) 0.000 0.000 0.000(3) C8 0.047(4) 0.039(4) 0.050(4) 0.000 0.000 0.000(3) C9 0.047(4) 0.039(4) 0.050(4) 0.000 0.000 0.000(3) C10 0.047(4) 0.039(4) 0.050(4) 0.000 0.000 0.000(3) C11 0.045(4) 0.042(4) 0.070(6) 0.000 0.000 0.001(3) C12 0.045(4) 0.042(4) 0.070(6) 0.000 0.000 0.001(3) C13 0.045(4) 0.042(4) 0.070(6) 0.000 0.000 0.001(3) C14 0.045(4) 0.042(4) 0.070(6) 0.000 0.000 0.001(3) C15 0.045(4) 0.042(4) 0.075(6) 0.000 0.000 0.001(3) C16 0.045(4) 0.042(4) 0.075(6) 0.000 0.000 0.001(3) C17 0.045(4) 0.042(4) 0.075(6) 0.000 0.000 0.001(3) C18 0.045(4) 0.042(4) 0.075(6) 0.000 0.000 0.001(3) C19 0.015(6) 0.046(7) 0.009(7) 0.005(5) 0.008(5) 0.008(5) C20 0.014(5) 0.030(5) 0.012(6) 0.006(5) 0.001(5) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C5 2.007(11) 6_557 ? Pd1 C5 2.007(11) . ? Pd1 C6 1.989(12) . ? Pd1 C6 1.989(12) 6_557 ? Pd2 C19 1.991(12) . ? Pd2 C19 1.991(12) 6 ? Pd2 C20 1.959(11) . ? Pd2 C20 1.959(11) 6 ? Fe1 N1 2.213(13) . ? Fe1 N4 2.147(10) 6_558 ? Fe1 N4 2.147(10) . ? Fe1 N9 2.224(14) . ? Fe1 N16 2.159(10) 6_656 ? Fe1 N16 2.159(10) 1_657 ? Fe2 N5 2.151(10) 6_556 ? Fe2 N5 2.151(10) . ? Fe2 N6 2.219(14) . ? Fe2 N12 2.229(14) . ? Fe2 N15 2.145(10) 6_556 ? Fe2 N15 2.145(10) . ? N1 C1 1.317(19) . ? N1 C4 1.363(19) . ? N2 C3 1.30(2) . ? N2 C4 1.33(2) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? N3 C2 1.30(2) . ? N4 C5 1.120(13) . ? N5 C6 1.130(14) . ? N6 C7 1.34(2) . ? N6 C10 1.32(2) . ? N7 C9 1.25(2) . ? N7 C10 1.34(2) . ? N8 H8A 0.90000(11) . ? N8 H8B 0.90000(11) . ? N8 H8B 0.89997(11) 6_556 ? N8 C8 1.318(18) . ? N9 C11 1.29(2) . ? N9 C14 1.34(2) . ? N10 C13 1.31(2) . ? N10 C14 1.35(2) . ? N11 H11A 0.90000(12) . ? N11 H11B 0.89995(11) 6_558 ? N11 H11B 0.90000(11) . ? N11 C12 1.318(19) . ? N12 C15 1.34(2) . ? N12 C18 1.31(2) . ? N13 C17 1.32(2) . ? N13 C18 1.33(2) . ? N14 H14A 0.90000(13) . ? N14 H14A 0.90000(13) 6_556 ? N14 H14B 0.90000(12) . ? N14 C16 1.341(18) . ? N15 C19 1.142(13) . ? N16 C20 1.154(13) . ? C1 H1 0.9300 . ? C1 C2 1.40(2) . ? C2 C3 1.39(2) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C7 H7 0.9300 . ? C7 C8 1.39(2) . ? C8 C9 1.42(2) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C11 C12 1.43(2) . ? C12 C13 1.34(2) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C15 C16 1.38(2) . ? C16 C17 1.37(2) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? O2 H2 0.8200 . ? O2 C22 1.41867(7) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? O1 H1A 0.8200 . ? O1 C21 1.374(19) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Pd1 C5 88.2(6) 6_557 . ? C6 Pd1 C5 177.8(4) 6_557 6_557 ? C6 Pd1 C5 90.9(5) . 6_557 ? C6 Pd1 C5 90.9(5) 6_557 . ? C6 Pd1 C5 177.8(4) . . ? C6 Pd1 C6 89.9(6) 6_557 . ? C19 Pd2 C19 89.4(6) 6 . ? C20 Pd2 C19 178.1(4) . . ? C20 Pd2 C19 90.5(5) . 6 ? C20 Pd2 C19 90.5(5) 6 . ? C20 Pd2 C19 178.1(4) 6 6 ? C20 Pd2 C20 89.6(6) 6 . ? N1 Fe1 N9 178.6(6) . . ? N4 Fe1 N1 89.1(4) 6_558 . ? N4 Fe1 N1 89.1(4) . . ? N4 Fe1 N4 89.3(5) 6_558 . ? N4 Fe1 N9 89.9(4) . . ? N4 Fe1 N9 89.9(4) 6_558 . ? N4 Fe1 N16 179.3(4) 6_558 6_656 ? N4 Fe1 N16 91.1(3) . 6_656 ? N4 Fe1 N16 91.1(3) 6_558 1_657 ? N4 Fe1 N16 179.3(4) . 1_657 ? N16 Fe1 N1 90.3(4) 1_657 . ? N16 Fe1 N1 90.3(4) 6_656 . ? N16 Fe1 N9 90.7(4) 1_657 . ? N16 Fe1 N9 90.7(4) 6_656 . ? N16 Fe1 N16 88.5(5) 1_657 6_656 ? N5 Fe2 N5 88.6(5) . 6_556 ? N5 Fe2 N6 87.3(4) 6_556 . ? N5 Fe2 N6 87.3(4) . . ? N5 Fe2 N12 94.0(4) 6_556 . ? N5 Fe2 N12 94.0(4) . . ? N6 Fe2 N12 178.1(6) . . ? N15 Fe2 N5 90.9(3) . 6_556 ? N15 Fe2 N5 177.9(4) 6_556 6_556 ? N15 Fe2 N5 90.9(3) 6_556 . ? N15 Fe2 N5 177.9(4) . . ? N15 Fe2 N6 90.7(4) . . ? N15 Fe2 N6 90.7(4) 6_556 . ? N15 Fe2 N12 88.0(4) 6_556 . ? N15 Fe2 N12 88.0(4) . . ? N15 Fe2 N15 89.6(5) . 6_556 ? C1 N1 Fe1 125.0(12) . . ? C1 N1 C4 115.6(14) . . ? C4 N1 Fe1 119.3(11) . . ? C3 N2 C4 115.7(15) . . ? H3A N3 H3B 120.0 . . ? C2 N3 H3A 120.0 . . ? C2 N3 H3B 120.0 . . ? C5 N4 Fe1 176.9(9) . . ? C6 N5 Fe2 173.2(9) . . ? C7 N6 Fe2 120.6(12) . . ? C10 N6 Fe2 121.0(12) . . ? C10 N6 C7 118.4(15) . . ? C9 N7 C10 117.6(17) . . ? H8A N8 H8B 112.891(18) . 6_556 ? H8A N8 H8B 112.885(18) . . ? H8B N8 H8B 73.0(7) . 6_556 ? C8 N8 H8A 128.2(9) . . ? C8 N8 H8B 108.2(7) . . ? C8 N8 H8B 108.2(7) . 6_556 ? C11 N9 Fe1 122.6(12) . . ? C11 N9 C14 119.4(15) . . ? C14 N9 Fe1 118.1(12) . . ? C13 N10 C14 115.5(16) . . ? H11A N11 H11B 112.878(19) . 6_558 ? H11A N11 H11B 112.885(19) . . ? H11B N11 H11B 120.0(8) . 6_558 ? C12 N11 H11A 114.1(11) . . ? C12 N11 H11B 97.3(6) . . ? C12 N11 H11B 97.3(6) . 6_558 ? C15 N12 Fe2 120.1(13) . . ? C18 N12 Fe2 122.0(12) . . ? C18 N12 C15 117.8(16) . . ? C17 N13 C18 114.1(17) . . ? H14A N14 H14A 58.1(5) . 6_556 ? H14A N14 H14B 112.886(18) . . ? H14B N14 H14A 112.886(19) . 6_556 ? C16 N14 H14A 126.6(7) . . ? C16 N14 H14A 126.6(7) . 6_556 ? C16 N14 H14B 110.5(8) . . ? C19 N15 Fe2 166.0(9) . . ? C20 N16 Fe1 178.4(10) . 1_453 ? N1 C1 H1 119.2 . . ? N1 C1 C2 121.6(16) . . ? C2 C1 H1 119.2 . . ? N3 C2 C1 120.4(16) . . ? N3 C2 C3 123.3(16) . . ? C3 C2 C1 116.3(16) . . ? N2 C3 C2 123.7(16) . . ? N2 C3 H3 118.2 . . ? C2 C3 H3 118.2 . . ? N1 C4 H4 116.5 . . ? N2 C4 N1 127.1(16) . . ? N2 C4 H4 116.5 . . ? N4 C5 Pd1 177.4(10) . . ? N5 C6 Pd1 177.5(10) . . ? N6 C7 H7 120.3 . . ? N6 C7 C8 119.4(17) . . ? C8 C7 H7 120.3 . . ? N8 C8 C7 120.3(16) . . ? N8 C8 C9 123.4(15) . . ? C7 C8 C9 116.3(16) . . ? N7 C9 C8 123.2(17) . . ? N7 C9 H9 118.4 . . ? C8 C9 H9 118.4 . . ? N6 C10 N7 125.1(17) . . ? N6 C10 H10 117.5 . . ? N7 C10 H10 117.5 . . ? N9 C11 H11 120.1 . . ? N9 C11 C12 119.7(17) . . ? C12 C11 H11 120.1 . . ? N11 C12 C11 117.5(16) . . ? N11 C12 C13 126.0(16) . . ? C13 C12 C11 116.5(18) . . ? N10 C13 C12 124.9(18) . . ? N10 C13 H13 117.6 . . ? C12 C13 H13 117.6 . . ? N9 C14 N10 124.0(17) . . ? N9 C14 H14 118.0 . . ? N10 C14 H14 118.0 . . ? N12 C15 H15 120.0 . . ? N12 C15 C16 120.0(18) . . ? C16 C15 H15 120.0 . . ? N14 C16 C15 118.8(16) . . ? N14 C16 C17 124.8(15) . . ? C17 C16 C15 116.3(17) . . ? N13 C17 C16 124.9(18) . . ? N13 C17 H17 117.5 . . ? C16 C17 H17 117.5 . . ? N12 C18 N13 126.8(18) . . ? N12 C18 H18 116.6 . . ? N13 C18 H18 116.6 . . ? N15 C19 Pd2 177.2(10) . . ? N16 C20 Pd2 178.1(10) . . ? C22 O2 H2 109.5 . . ? O2 C22 H22A 109.5 . . ? O2 C22 H22B 109.5 . . ? O2 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 O1 H1A 109.5 . . ? O1 C21 H21A 109.5 . . ? O1 C21 H21B 109.5 . . ? O1 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 N1 C1 C2 180.0 . . . . ? Fe1 N1 C4 N2 180.0 . . . . ? Fe1 N9 C11 C12 180.0 . . . . ? Fe1 N9 C14 N10 180.0 . . . . ? Fe2 N6 C7 C8 180.0 . . . . ? Fe2 N6 C10 N7 180.0 . . . . ? Fe2 N12 C15 C16 180.0 . . . . ? Fe2 N12 C18 N13 180.0 . . . . ? N1 C1 C2 N3 180.0 . . . . ? N1 C1 C2 C3 0.0 . . . . ? N3 C2 C3 N2 180.0 . . . . ? N6 C7 C8 N8 180.0 . . . . ? N6 C7 C8 C9 0.0 . . . . ? N8 C8 C9 N7 180.0 . . . . ? N9 C11 C12 N11 180.0 . . . . ? N9 C11 C12 C13 0.0 . . . . ? N11 C12 C13 N10 180.0 . . . . ? N12 C15 C16 N14 180.0 . . . . ? N12 C15 C16 C17 0.0 . . . . ? N14 C16 C17 N13 180.0 . . . . ? C1 N1 C4 N2 0.0 . . . . ? C1 C2 C3 N2 0.0 . . . . ? C3 N2 C4 N1 0.0 . . . . ? C4 N1 C1 C2 0.0 . . . . ? C4 N2 C3 C2 0.0 . . . . ? C7 N6 C10 N7 0.0 . . . . ? C7 C8 C9 N7 0.0 . . . . ? C9 N7 C10 N6 0.0 . . . . ? C10 N6 C7 C8 0.0 . . . . ? C10 N7 C9 C8 0.0 . . . . ? C11 N9 C14 N10 0.0 . . . . ? C11 C12 C13 N10 0.0 . . . . ? C13 N10 C14 N9 0.0 . . . . ? C14 N9 C11 C12 0.0 . . . . ? C14 N10 C13 C12 0.0 . . . . ? C15 N12 C18 N13 0.0 . . . . ? C15 C16 C17 N13 0.0 . . . . ? C17 N13 C18 N12 0.0 . . . . ? C18 N12 C15 C16 0.0 . . . . ? C18 N13 C17 C16 0.0 . . . . ? _shelx_res_file ; TITL rt312_nh2pympdmeoh_260k_a.res in Pbcm rt312_nh2pympdmeoh_260k.res created by SHELXL-2018/3 at 12:38:46 on 09-Sep-2020 REM Old TITL RT312_NH2pymPdMeOH_260K in Pbc21 #29 REM SHELXT solution in Pbcm: R1 0.244, Rweak 0.002, Alpha 0.073 REM 0.844 for 207 systematic absences, Orientation as input REM Formula found by SHELXT: C16 N8 Pd2 CELL 0.71073 15.0184 32.5156 7.3514 90 90 90 ZERR 8 0.0012 0.0018 0.0004 0 0 0 LATT 1 SYMM -X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM +X,0.5-Y,-Z SFAC C H Fe N O Pd UNIT 100 96 8 80 4 8 EQIV $1 +X,+Y,0.5-Z EQIV $2 +X,+Y,-1+Z EADP N11 C12 C13 N10 C14 N9 C11 DFIX 1.4 O1 C21 DANG 1.5 0.0001 H14b_$1 H14a_$1 DFIX 0.9 0.0001 N14 H14a_$1 DFIX 0.9 0.0001 H14b_$1 N14 DANG 2.2 0.0001 H14a O2_$2 DANG 0.9 0.0001 N11_$1 H11a_$1 DANG 1.5 0.0001 H11a_$1 H11b_$1 DANG 0.9 0.0001 N11_$1 H11b_$1 DFIX 0.9 0.0001 N8 H8b DANG 1.5 0.0001 H8a H8b DFIX 0.9 0.0001 N8 H8a EADP N8 C8 C9 N7 C10 N6 C7 EADP N14 C16 C15 N12 C18 N13 C17 EADP N1 C4 N2 C3 C2 C1 N3 L.S. 50 PLAN 1 SIZE 0.12 0.12 0.03 CONF list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.084800 25.261200 FVAR 0.11868 PD1 6 0.506011 0.632717 0.750000 10.50000 0.01160 0.02574 = 0.00936 0.00000 0.00000 0.00248 PD2 6 0.007879 0.616273 -0.250000 10.50000 0.00818 0.02631 = 0.00929 0.00000 0.00000 0.00297 FE1 3 0.757208 0.625789 1.250000 10.50000 0.00881 0.02623 = 0.00887 0.00000 0.00000 0.00376 FE2 3 0.256610 0.622642 0.250000 10.50000 0.00806 0.03134 = 0.00771 0.00000 0.00000 0.00402 N1 4 0.747839 0.557860 1.250000 10.50000 0.03423 0.03831 = 0.07600 0.00000 0.00000 0.00265 N2 4 0.830306 0.494374 1.250000 10.50000 0.03423 0.03831 = 0.07600 0.00000 0.00000 0.00265 N3 4 0.597967 0.473585 1.250000 10.50000 0.03423 0.03831 = 0.07600 0.00000 0.00000 0.00265 AFIX 93 H3A 2 0.598126 0.447136 1.250000 10.50000 -1.20000 H3B 2 0.548296 0.486746 1.250000 10.50000 -1.20000 AFIX 0 N4 4 0.655632 0.627755 1.044729 11.00000 0.01767 0.04821 = 0.01977 -0.00930 -0.00101 0.01376 N5 4 0.357163 0.631847 0.454261 11.00000 0.01139 0.05484 = 0.01311 -0.00038 -0.00744 0.00373 N6 4 0.294742 0.556712 0.250000 10.50000 0.04698 0.03943 = 0.05012 0.00000 0.00000 0.00031 N7 4 0.408607 0.506547 0.250000 10.50000 0.04698 0.03943 = 0.05012 0.00000 0.00000 0.00031 N8 4 0.197937 0.456793 0.250000 10.50000 0.04698 0.03943 = 0.05012 0.00000 0.00000 0.00031 H8A 2 0.206548 0.429401 0.250000 10.50000 -1.50000 H8B 2 0.152863 0.464647 0.322812 10.50000 -1.50000 N9 4 0.763041 0.694146 1.250000 10.50000 0.04473 0.04171 = 0.07009 0.00000 0.00000 0.00054 N10 4 0.680515 0.756470 1.250000 10.50000 0.04473 0.04171 = 0.07009 0.00000 0.00000 0.00054 N11 4 0.913831 0.777189 1.250000 10.50000 0.04473 0.04171 = 0.07009 0.00000 0.00000 0.00054 H11A 2 0.909739 0.804804 1.250000 10.50000 -1.50000 H11B 2 0.934202 0.767044 1.143969 10.50000 -1.50000 N12 4 0.213547 0.688252 0.250000 10.50000 0.04544 0.04169 = 0.07479 0.00000 0.00000 0.00121 N13 4 0.096523 0.736774 0.250000 10.50000 0.04544 0.04169 = 0.07479 0.00000 0.00000 0.00121 N14 4 0.309745 0.788566 0.250000 10.50000 0.04544 0.04169 = 0.07479 0.00000 0.00000 0.00121 H14A 2 0.362115 0.788094 0.309474 10.50000 -1.50000 H14B 2 0.284135 0.813590 0.250000 10.50000 -1.50000 N15 4 0.158295 0.611309 0.044357 11.00000 0.01361 0.05199 = 0.02520 -0.00521 -0.00156 0.00817 N16 4 -0.139948 0.623145 -0.545162 11.00000 0.02907 0.04367 = 0.00737 0.00578 -0.00006 -0.00135 C1 1 0.672957 0.536768 1.250000 10.50000 0.03423 0.03831 = 0.07600 0.00000 0.00000 0.00265 AFIX 43 H1 2 0.619017 0.550816 1.250000 10.50000 -1.20000 AFIX 0 C2 1 0.672612 0.493619 1.250000 10.50000 0.03423 0.03831 = 0.07600 0.00000 0.00000 0.00265 C3 1 0.755293 0.474544 1.250000 10.50000 0.03423 0.03831 = 0.07600 0.00000 0.00000 0.00265 AFIX 43 H3 2 0.757045 0.445954 1.250000 10.50000 -1.20000 AFIX 0 C4 1 0.823987 0.535039 1.250000 10.50000 0.03423 0.03831 = 0.07600 0.00000 0.00000 0.00265 AFIX 43 H4 2 0.877308 0.549583 1.250000 10.50000 -1.20000 AFIX 0 C5 1 0.601826 0.630525 0.940045 11.00000 0.01382 0.03952 = 0.00684 0.00105 -0.00279 0.00484 C6 1 0.412258 0.632739 0.558970 11.00000 0.01302 0.03359 = 0.02249 0.00360 0.00510 -0.00041 C7 1 0.232446 0.527361 0.250000 10.50000 0.04698 0.03943 = 0.05012 0.00000 0.00000 0.00031 AFIX 43 H7 2 0.172389 0.534332 0.250000 10.50000 -1.20000 AFIX 0 C8 1 0.258380 0.486180 0.250000 10.50000 0.04698 0.03943 = 0.05012 0.00000 0.00000 0.00031 C9 1 0.351419 0.478532 0.250000 10.50000 0.04698 0.03943 = 0.05012 0.00000 0.00000 0.00031 AFIX 43 H9 2 0.370859 0.451376 0.250000 10.50000 -1.20000 AFIX 0 C10 1 0.379446 0.545492 0.250000 10.50000 0.04698 0.03943 = 0.05012 0.00000 0.00000 0.00031 AFIX 43 H10 2 0.422042 0.566252 0.250000 10.50000 -1.20000 AFIX 0 C11 1 0.837318 0.714191 1.250000 10.50000 0.04473 0.04171 = 0.07009 0.00000 0.00000 0.00054 AFIX 43 H11 2 0.891179 0.700078 1.250000 10.50000 -1.20000 AFIX 0 C12 1 0.836371 0.758124 1.250000 10.50000 0.04473 0.04171 = 0.07009 0.00000 0.00000 0.00054 C13 1 0.756389 0.776064 1.250000 10.50000 0.04473 0.04171 = 0.07009 0.00000 0.00000 0.00054 AFIX 43 H13 2 0.754601 0.804653 1.250000 10.50000 -1.20000 AFIX 0 C14 1 0.686309 0.714900 1.250000 10.50000 0.04473 0.04171 = 0.07009 0.00000 0.00000 0.00054 AFIX 43 H14 2 0.633603 0.699885 1.250000 10.50000 -1.20000 AFIX 0 C15 1 0.274436 0.718398 0.250000 10.50000 0.04544 0.04169 = 0.07479 0.00000 0.00000 0.00121 AFIX 43 H15 2 0.334773 0.711964 0.250000 10.50000 -1.20000 AFIX 0 C16 1 0.247555 0.758981 0.250000 10.50000 0.04544 0.04169 = 0.07479 0.00000 0.00000 0.00121 C17 1 0.157704 0.765793 0.250000 10.50000 0.04544 0.04169 = 0.07479 0.00000 0.00000 0.00121 AFIX 43 H17 2 0.138343 0.792961 0.250000 10.50000 -1.20000 AFIX 0 C18 1 0.129129 0.698833 0.250000 10.50000 0.04544 0.04169 = 0.07479 0.00000 0.00000 0.00121 AFIX 43 H18 2 0.087881 0.677500 0.250000 10.50000 -1.20000 AFIX 0 C19 1 0.101958 0.613516 -0.059574 11.00000 0.01475 0.04616 = 0.00908 0.00482 0.00774 0.00806 C20 1 -0.084089 0.620931 -0.437801 11.00000 0.01375 0.03035 = 0.01151 0.00632 0.00100 -0.00308 PART -1 O2 5 10.496119 10.764300 11.250000 10.25000 0.08221 AFIX 147 H2 2 0.492002 0.788255 1.283841 10.25000 -1.50000 AFIX 0 C22 1 10.484519 10.762381 11.058670 10.25000 0.04761 AFIX 137 H22A 2 0.529569 0.778624 1.000178 10.25000 -1.50000 H22B 2 0.426783 0.772882 1.027314 10.25000 -1.50000 H22C 2 0.489356 0.734337 1.019047 10.25000 -1.50000 AFIX 0 O1 5 11.013630 10.484839 11.250000 10.25000 0.08997 AFIX 147 H1A 2 0.997818 0.461913 1.283404 10.25000 -1.50000 AFIX 0 C21 1 1.010992 0.486822 1.063392 10.25000 0.04014 AFIX 137 H21A 2 1.066170 0.476834 1.014465 10.25000 -1.50000 H21B 2 1.002155 0.514824 1.026140 10.25000 -1.50000 H21C 2 0.962807 0.470195 1.019183 10.25000 -1.50000 AFIX 0 HKLF 4 REM rt312_nh2pympdmeoh_260k_a.res in Pbcm REM wR2 = 0.2498, GooF = S = 1.051, Restrained GooF = 1.050 for all data REM R1 = 0.0816 for 1884 Fo > 4sig(Fo) and 0.1491 for all 3897 data REM 195 parameters refined using 11 restraints END WGHT 0.0852 23.9103 REM Highest difference peak 2.012, deepest hole -1.507, 1-sigma level 0.187 Q1 1 -0.0443 0.6197 -0.2500 10.50000 0.05 2.01 ; _shelx_res_checksum 6336 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.212 _oxdiff_exptl_absorpt_empirical_full_min 0.853