# Electronic Supplementary Material (ESI) for Chemical Science. # This journal is © The Royal Society of Chemistry 2021 ####################################################################### # # 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_ln585 _database_code_depnum_ccdc_archive 'CCDC 2044409' loop_ _audit_author_name _audit_author_address 'Benjamin S. Gelfand' ;University of Calgary Canada ; _audit_update_record ; 2020-11-14 deposited with the CCDC. 2020-12-22 downloaded from the CCDC. ; _audit_creation_date 2019-06-04 _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 'C31 H32 B2 Fe N10, C6 H6' _chemical_formula_sum 'C37 H38 B2 Fe N10' _chemical_formula_weight 700.24 _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 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 '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 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.6461(14) _cell_length_b 17.2299(16) _cell_length_c 24.132(2) _cell_angle_alpha 90 _cell_angle_beta 102.636(4) _cell_angle_gamma 90 _cell_volume 6753.7(10) _cell_formula_units_Z 8 _cell_measurement_reflns_used 8710 _cell_measurement_temperature 173 _cell_measurement_theta_max 68.226 _cell_measurement_theta_min 3.740 _shelx_estimated_absorpt_T_max 0.602 _shelx_estimated_absorpt_T_min 0.405 _exptl_absorpt_coefficient_mu 3.928 _exptl_absorpt_correction_T_max 0.6554 _exptl_absorpt_correction_T_min 0.4822 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0908 before and 0.0370 after correction. The Ratio of minimum to maximum transmission is 0.7357. 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 1.377 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 2928 _exptl_crystal_size_max 0.281 _exptl_crystal_size_mid 0.236 _exptl_crystal_size_min 0.144 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_unetI/netI 0.0778 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 18406 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.291 _diffrn_reflns_theta_min 3.740 _diffrn_ambient_temperature 173 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source ? _diffrn_special_details ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4514 _reflns_number_total 6138 _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 v8.37A (Bruker, 2015)' _computing_data_collection ? _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _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 0.591 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.077 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 496 _refine_ls_number_reflns 6138 _refine_ls_number_restraints 162 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0441 _refine_ls_restrained_S_all 1.044 _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^)+(0.0818P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1222 _refine_ls_wR_factor_ref 0.1395 _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 2. Restrained distances N10-H10A = N10-H10B = N10-H10C 0.91 with sigma of 0.02 H10A-H10C 1.49 with sigma of 0.04 H10C-H10B 1.49 with sigma of 0.04 H10B-H10A 1.49 with sigma of 0.04 C1S-C2S \\sim C1T-C2T with sigma of 0.02 C1S-C6S \\sim C1T-C6T with sigma of 0.02 C2S-C3S \\sim C2T-C3T with sigma of 0.02 C3S-C4S \\sim C3T-C4T with sigma of 0.02 C4S-C5S \\sim C4T-C5T with sigma of 0.02 C5S-C6S \\sim C5T-C6T with sigma of 0.02 C1S-C3S \\sim C1T-C3T with sigma of 0.04 C1S-C5S \\sim C1T-C5T with sigma of 0.04 C2S-C4S \\sim C2T-C4T with sigma of 0.04 C2S-C6S \\sim C2T-C6T with sigma of 0.04 C3S-C5S \\sim C3T-C5T with sigma of 0.04 C4S-C6S \\sim C4T-C6T with sigma of 0.04 3. Uiso/Uaniso restraints and constraints C6S \\sim C1S \\sim C2S \\sim C3S \\sim C5S \\sim C4S: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C1T \\sim C6T \\sim C2T \\sim C5T \\sim C3T \\sim C4T: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 4. Rigid body (RIGU) restrains C1T, C6T, C2T, C5T, C3T, C4T with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C6S, C1S, C2S, C3S, C5S, C4S with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(C6T)=Sof(H6T)=Sof(C1T)=Sof(H1T)=Sof(C2T)=Sof(H2T)=Sof(C3T)=Sof(H3T)= Sof(C4T)=Sof(H4T)=Sof(C5T)=Sof(H5T)=1-FVAR(1) Sof(C1S)=Sof(H1S)=Sof(C2S)=Sof(H2S)=Sof(C3S)=Sof(H3S)=Sof(C4S)=Sof(H4S)= Sof(C5S)=Sof(H5S)=Sof(C6S)=Sof(H6S)=FVAR(1) 6.a Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C29(H29), C30(H30), C1S(H1S), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S), C6T(H6T), C1T(H1T), C2T(H2T), C3T(H3T), C4T(H4T), C5T(H5T) 6.b Fitted hexagon refined as free rotating group: C1S(C2S,C3S,C4S,C5S,C6S), C6T(C1T,C2T,C3T,C4T,C5T) 6.c Idealised Me refined as rotating group: C13(H13A,H13B,H13C), C31(H31A,H31B,H31C) ; _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 Fe1 Fe 0.35808(2) 0.35593(2) 0.30219(2) 0.02893(14) Uani 1 1 d . . . . . N1 N 0.27355(12) 0.27391(13) 0.27439(8) 0.0329(5) Uani 1 1 d . . . . . N2 N 0.19844(12) 0.27712(13) 0.28896(8) 0.0320(5) Uani 1 1 d . . . . . N3 N 0.26617(12) 0.43179(13) 0.27786(8) 0.0322(5) Uani 1 1 d . . . . . N4 N 0.19154(12) 0.41870(13) 0.29163(8) 0.0318(5) Uani 1 1 d . . . . . N5 N 0.33752(12) 0.35206(11) 0.37943(8) 0.0288(5) Uani 1 1 d . . . . . N6 N 0.43954(12) 0.43837(13) 0.32672(7) 0.0312(5) Uani 1 1 d . . . . . N7 N 0.49746(12) 0.42888(13) 0.37602(8) 0.0310(5) Uani 1 1 d . . . . . N8 N 0.44590(12) 0.27663(13) 0.32583(8) 0.0325(5) Uani 1 1 d . . . . . N9 N 0.50198(12) 0.28324(13) 0.37657(8) 0.0325(5) Uani 1 1 d . . . . . N10 N 0.38194(15) 0.35994(15) 0.22149(9) 0.0385(6) Uani 1 1 d D . . . . C1 C 0.26475(16) 0.22107(17) 0.23266(10) 0.0391(6) Uani 1 1 d . . . . . H1 H 0.307321 0.206338 0.214222 0.047 Uiso 1 1 calc R . . . . C2 C 0.18580(17) 0.19070(18) 0.21984(11) 0.0439(7) Uani 1 1 d . . . . . H2 H 0.164309 0.152226 0.192390 0.053 Uiso 1 1 calc R . . . . C3 C 0.14564(16) 0.22886(16) 0.25582(10) 0.0388(6) Uani 1 1 d . . . . . H3 H 0.089408 0.222102 0.257028 0.047 Uiso 1 1 calc R . . . . C4 C 0.25355(16) 0.48886(17) 0.23938(10) 0.0393(6) Uani 1 1 d . . . . . H4 H 0.295078 0.510494 0.222631 0.047 Uiso 1 1 calc R . . . . C5 C 0.17146(16) 0.51246(18) 0.22707(11) 0.0422(7) Uani 1 1 d . . . . . H5 H 0.146627 0.551838 0.201414 0.051 Uiso 1 1 calc R . . . . C6 C 0.13483(15) 0.46611(16) 0.26029(10) 0.0381(6) Uani 1 1 d . . . . . H6 H 0.078060 0.467120 0.261179 0.046 Uiso 1 1 calc R . . . . C7 C 0.09616(15) 0.33780(16) 0.34639(10) 0.0333(6) Uani 1 1 d . . . . . C8 C 0.04780(16) 0.40045(18) 0.35612(10) 0.0393(6) Uani 1 1 d . . . . . H8 H 0.064512 0.451364 0.348543 0.047 Uiso 1 1 calc R . . . . C9 C -0.02390(17) 0.3916(2) 0.37644(11) 0.0445(7) Uani 1 1 d . . . . . H9 H -0.054924 0.436109 0.381995 0.053 Uiso 1 1 calc R . . . . C10 C -0.05042(16) 0.31837(19) 0.38866(11) 0.0426(7) Uani 1 1 d . . . . . C11 C -0.00209(16) 0.25520(18) 0.38136(10) 0.0419(7) Uani 1 1 d . . . . . H11 H -0.017952 0.204593 0.390368 0.050 Uiso 1 1 calc R . . . . C12 C 0.06943(15) 0.26495(17) 0.36098(10) 0.0380(6) Uani 1 1 d . . . . . H12 H 0.101327 0.220476 0.356825 0.046 Uiso 1 1 calc R . . . . C13 C -0.12782(18) 0.3073(2) 0.41044(14) 0.0633(9) Uani 1 1 d . . . . . H13A H -0.164507 0.351774 0.399170 0.095 Uiso 1 1 calc GR . . . . H13B H -0.113713 0.303384 0.451948 0.095 Uiso 1 1 calc GR . . . . H13C H -0.155612 0.259675 0.394356 0.095 Uiso 1 1 calc GR . . . . C14 C 0.25800(15) 0.34661(14) 0.38531(10) 0.0298(6) Uani 1 1 d . . . . . C15 C 0.24222(15) 0.33906(15) 0.43967(10) 0.0339(6) Uani 1 1 d . . . . . H15 H 0.186933 0.337628 0.444129 0.041 Uiso 1 1 calc R . . . . C16 C 0.30576(16) 0.33368(17) 0.48671(10) 0.0384(6) Uani 1 1 d . . . . . H16 H 0.294964 0.327425 0.523507 0.046 Uiso 1 1 calc R . . . . C17 C 0.38533(16) 0.33755(16) 0.47934(10) 0.0340(6) Uani 1 1 d . . . . . H17 H 0.429890 0.331502 0.511194 0.041 Uiso 1 1 calc R . . . . C18 C 0.40141(15) 0.35021(14) 0.42586(10) 0.0300(6) Uani 1 1 d . . . . . C19 C 0.45559(15) 0.50725(16) 0.30559(10) 0.0362(6) Uani 1 1 d . . . . . H19 H 0.424438 0.529178 0.271474 0.043 Uiso 1 1 calc R . . . . C20 C 0.52367(16) 0.54234(17) 0.34005(10) 0.0394(6) Uani 1 1 d . . . . . H20 H 0.547799 0.590857 0.334405 0.047 Uiso 1 1 calc R . . . . C21 C 0.54840(15) 0.49086(16) 0.38437(10) 0.0370(6) Uani 1 1 d . . . . . H21 H 0.593742 0.497870 0.415571 0.044 Uiso 1 1 calc R . . . . C22 C 0.45852(15) 0.20641(17) 0.30532(11) 0.0386(6) Uani 1 1 d . . . . . H22 H 0.428440 0.186369 0.270198 0.046 Uiso 1 1 calc R . . . . C23 C 0.52095(17) 0.16672(18) 0.34177(12) 0.0447(7) Uani 1 1 d . . . . . H23 H 0.541718 0.116404 0.336930 0.054 Uiso 1 1 calc R . . . . C24 C 0.54603(16) 0.21705(17) 0.38669(11) 0.0400(6) Uani 1 1 d . . . . . H24 H 0.587746 0.206718 0.419566 0.048 Uiso 1 1 calc R . . . . C25 C 0.56993(15) 0.36625(16) 0.46862(10) 0.0340(6) Uani 1 1 d . . . . . C26 C 0.65064(15) 0.34169(15) 0.46953(10) 0.0355(6) Uani 1 1 d . . . . . H26 H 0.660524 0.311806 0.438609 0.043 Uiso 1 1 calc R . . . . C27 C 0.71630(16) 0.35931(15) 0.51368(11) 0.0373(6) Uani 1 1 d . . . . . H27 H 0.769439 0.339801 0.512965 0.045 Uiso 1 1 calc R . . . . C28 C 0.70602(16) 0.40501(17) 0.55908(10) 0.0381(6) Uani 1 1 d . . . . . C29 C 0.62710(15) 0.43135(16) 0.55904(10) 0.0370(6) Uani 1 1 d . . . . . H29 H 0.618080 0.462755 0.589466 0.044 Uiso 1 1 calc R . . . . C30 C 0.56146(15) 0.41232(16) 0.51512(10) 0.0362(6) Uani 1 1 d . . . . . H30 H 0.508314 0.431228 0.516462 0.043 Uiso 1 1 calc R . . . . C31 C 0.77698(17) 0.42726(19) 0.60630(11) 0.0484(7) Uani 1 1 d . . . . . H31A H 0.804617 0.380265 0.623789 0.073 Uiso 1 1 calc GR . . . . H31B H 0.756610 0.457183 0.634922 0.073 Uiso 1 1 calc GR . . . . H31C H 0.816057 0.458856 0.591021 0.073 Uiso 1 1 calc GR . . . . B1 B 0.18408(18) 0.34592(17) 0.32892(12) 0.0312(6) Uani 1 1 d . . . . . B2 B 0.49421(18) 0.35610(18) 0.41428(11) 0.0327(7) Uani 1 1 d . . . . . C1S C 0.0984(4) 0.4386(4) 0.51585(15) 0.0536(19) Uani 0.648(12) 1 d D U P A 1 H1S H 0.055483 0.450271 0.483978 0.064 Uiso 0.648(12) 1 calc R . P A 1 C2S C 0.1606(6) 0.4924(2) 0.5348(3) 0.060(2) Uani 0.648(12) 1 d DG U P A 1 H2S H 0.160127 0.540835 0.515904 0.072 Uiso 0.648(12) 1 calc R . P A 1 C3S C 0.2234(3) 0.4754(4) 0.5815(3) 0.059(2) Uani 0.648(12) 1 d DG U P A 1 H3S H 0.265922 0.512164 0.594419 0.071 Uiso 0.648(12) 1 calc R . P A 1 C4S C 0.2241(3) 0.4046(5) 0.60913(18) 0.051(2) Uani 0.648(12) 1 d DG U P A 1 H4S H 0.267076 0.392929 0.641007 0.061 Uiso 0.648(12) 1 calc R . P A 1 C5S C 0.1620(5) 0.3508(2) 0.5902(2) 0.051(2) Uani 0.648(12) 1 d DG U P A 1 H5S H 0.162433 0.302363 0.609081 0.061 Uiso 0.648(12) 1 calc R . P A 1 C6S C 0.0991(3) 0.3678(3) 0.5435(3) 0.0533(18) Uani 0.648(12) 1 d DG U P A 1 H6S H 0.056636 0.331033 0.530567 0.064 Uiso 0.648(12) 1 calc R . P A 1 H10A H 0.3359(13) 0.3567(15) 0.1926(11) 0.052(9) Uiso 1 1 d D . . . . H10B H 0.4150(18) 0.3209(15) 0.2124(15) 0.090(13) Uiso 1 1 d D . . . . H10C H 0.4107(19) 0.4025(15) 0.2151(16) 0.100(15) Uiso 1 1 d 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 Fe1 0.0291(2) 0.0335(3) 0.0248(2) 0.00053(15) 0.00718(16) 0.00009(16) N1 0.0327(11) 0.0364(13) 0.0289(9) -0.0001(9) 0.0053(8) 0.0036(9) N2 0.0313(10) 0.0315(13) 0.0322(9) -0.0012(9) 0.0049(8) -0.0029(9) N3 0.0311(10) 0.0358(13) 0.0295(9) 0.0013(9) 0.0061(8) -0.0024(9) N4 0.0302(10) 0.0351(13) 0.0295(9) 0.0016(9) 0.0056(8) 0.0002(9) N5 0.0314(11) 0.0274(13) 0.0279(9) 0.0000(8) 0.0071(8) 0.0001(8) N6 0.0324(10) 0.0352(13) 0.0272(9) 0.0020(9) 0.0092(8) 0.0013(9) N7 0.0298(10) 0.0349(13) 0.0288(9) -0.0006(9) 0.0074(8) -0.0011(9) N8 0.0324(10) 0.0378(14) 0.0272(9) -0.0020(9) 0.0059(8) 0.0004(9) N9 0.0306(10) 0.0356(13) 0.0310(9) 0.0004(9) 0.0064(8) 0.0030(9) N10 0.0410(13) 0.0468(17) 0.0293(10) 0.0000(10) 0.0109(10) 0.0006(11) C1 0.0392(14) 0.0426(18) 0.0341(11) -0.0064(12) 0.0047(11) 0.0009(12) C2 0.0443(15) 0.0435(19) 0.0413(13) -0.0065(13) 0.0033(12) -0.0034(13) C3 0.0347(13) 0.0407(17) 0.0393(12) -0.0029(12) 0.0040(11) -0.0050(12) C4 0.0402(14) 0.0415(17) 0.0346(12) 0.0092(12) 0.0051(11) -0.0014(12) C5 0.0418(14) 0.0433(18) 0.0394(13) 0.0124(13) 0.0044(12) 0.0023(13) C6 0.0326(13) 0.0401(17) 0.0401(12) 0.0048(12) 0.0045(11) 0.0040(12) C7 0.0303(13) 0.0367(16) 0.0323(11) 0.0024(11) 0.0055(10) -0.0020(11) C8 0.0388(14) 0.0409(18) 0.0395(13) 0.0036(12) 0.0115(11) 0.0044(12) C9 0.0415(15) 0.051(2) 0.0412(13) 0.0011(14) 0.0105(12) 0.0071(14) C10 0.0344(14) 0.056(2) 0.0388(13) -0.0016(14) 0.0105(11) -0.0065(13) C11 0.0403(14) 0.0469(19) 0.0388(13) 0.0011(13) 0.0095(11) -0.0110(13) C12 0.0355(13) 0.0403(17) 0.0391(12) -0.0004(12) 0.0100(11) -0.0017(12) C13 0.0510(18) 0.080(3) 0.0686(19) -0.0092(19) 0.0339(16) -0.0076(18) C14 0.0332(13) 0.0248(14) 0.0321(12) -0.0009(10) 0.0087(10) 0.0006(10) C15 0.0330(13) 0.0363(16) 0.0338(12) -0.0003(11) 0.0102(11) -0.0007(11) C16 0.0442(15) 0.0437(18) 0.0295(11) 0.0007(11) 0.0127(11) -0.0053(13) C17 0.0361(13) 0.0358(16) 0.0293(11) 0.0016(11) 0.0056(10) -0.0018(11) C18 0.0341(13) 0.0274(15) 0.0277(11) 0.0008(10) 0.0049(10) -0.0001(10) C19 0.0394(13) 0.0366(17) 0.0338(12) 0.0028(11) 0.0106(10) -0.0008(12) C20 0.0424(15) 0.0370(17) 0.0412(13) -0.0019(12) 0.0141(12) -0.0063(12) C21 0.0342(13) 0.0408(17) 0.0371(12) -0.0045(12) 0.0104(10) -0.0039(12) C22 0.0341(13) 0.0414(18) 0.0397(12) -0.0075(12) 0.0068(11) 0.0019(12) C23 0.0406(15) 0.0355(17) 0.0543(16) -0.0066(14) 0.0023(13) 0.0077(13) C24 0.0369(14) 0.0381(17) 0.0422(13) 0.0004(13) 0.0025(11) 0.0044(12) C25 0.0334(13) 0.0372(16) 0.0311(11) 0.0015(11) 0.0066(10) -0.0010(11) C26 0.0349(14) 0.0391(17) 0.0326(11) -0.0024(11) 0.0073(11) 0.0005(11) C27 0.0300(13) 0.0411(18) 0.0411(13) 0.0018(12) 0.0080(11) 0.0046(11) C28 0.0385(14) 0.0392(17) 0.0347(12) 0.0018(12) 0.0041(11) -0.0028(12) C29 0.0389(14) 0.0379(17) 0.0345(11) -0.0037(12) 0.0089(11) 0.0003(12) C30 0.0327(13) 0.0406(17) 0.0358(12) -0.0011(12) 0.0087(10) 0.0022(12) C31 0.0411(15) 0.055(2) 0.0434(13) -0.0044(14) -0.0019(12) 0.0008(14) B1 0.0313(14) 0.0296(18) 0.0324(13) 0.0009(12) 0.0066(11) 0.0005(12) B2 0.0332(15) 0.0370(19) 0.0284(12) -0.0005(12) 0.0078(12) 0.0005(12) C1S 0.080(4) 0.031(5) 0.051(3) -0.003(3) 0.016(3) -0.003(3) C2S 0.087(6) 0.042(4) 0.054(4) -0.002(3) 0.022(4) -0.016(4) C3S 0.067(4) 0.052(5) 0.063(6) -0.009(4) 0.026(3) -0.008(4) C4S 0.062(4) 0.036(5) 0.056(3) -0.016(3) 0.017(3) -0.002(3) C5S 0.055(6) 0.050(4) 0.050(4) -0.005(3) 0.016(4) -0.003(3) C6S 0.060(4) 0.038(4) 0.064(5) 0.007(3) 0.019(3) 0.002(3) C6T 0.054(10) 0.050(7) 0.082(12) -0.003(6) 0.024(7) -0.007(6) C1T 0.074(7) 0.052(11) 0.071(8) -0.002(7) 0.021(6) -0.014(7) C2T 0.083(8) 0.051(9) 0.054(6) -0.003(6) 0.020(5) -0.010(6) C3T 0.088(9) 0.048(7) 0.056(9) 0.014(5) 0.010(6) -0.013(6) C4T 0.062(6) 0.040(9) 0.061(6) 0.007(6) 0.023(5) -0.009(6) C5T 0.058(8) 0.037(8) 0.066(8) 0.010(7) 0.032(6) -0.002(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 Fe1 N1 2.003(2) . ? Fe1 N3 2.000(2) . ? Fe1 N5 1.9686(19) . ? Fe1 N6 1.964(2) . ? Fe1 N8 1.991(2) . ? Fe1 N10 2.072(2) . ? N1 N2 1.372(3) . ? N1 C1 1.342(3) . ? N2 C3 1.340(3) . ? N2 B1 1.579(3) . ? N3 N4 1.373(3) . ? N3 C4 1.337(3) . ? N4 C6 1.348(3) . ? N4 B1 1.564(3) . ? N5 C14 1.365(3) . ? N5 C18 1.366(3) . ? N6 N7 1.367(3) . ? N6 C19 1.342(3) . ? N7 C21 1.351(3) . ? N7 B2 1.565(4) . ? N8 N9 1.372(3) . ? N8 C22 1.341(3) . ? N9 C24 1.349(3) . ? N9 B2 1.572(3) . ? C1 C2 1.385(4) . ? C2 C3 1.374(4) . ? C4 C5 1.394(4) . ? C5 C6 1.366(4) . ? C7 C8 1.397(4) . ? C7 C12 1.402(4) . ? C7 B1 1.615(3) . ? C8 C9 1.395(4) . ? C9 C10 1.390(4) . ? C10 C11 1.387(4) . ? C10 C13 1.506(3) . ? C11 C12 1.394(3) . ? C14 C15 1.399(3) . ? C14 B1 1.623(4) . ? C15 C16 1.375(3) . ? C16 C17 1.376(3) . ? C17 C18 1.391(3) . ? C18 B2 1.632(4) . ? C19 C20 1.389(3) . ? C20 C21 1.381(4) . ? C22 C23 1.386(4) . ? C23 C24 1.380(4) . ? C25 C26 1.404(3) . ? C25 C30 1.407(3) . ? C25 B2 1.617(4) . ? C26 C27 1.383(4) . ? C27 C28 1.390(4) . ? C28 C29 1.390(3) . ? C28 C31 1.501(3) . ? C29 C30 1.385(3) . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C2S C3S 1.3900 . ? C3S C4S 1.3900 . ? C4S C5S 1.3900 . ? C5S C6S 1.3900 . ? C6T C1T 1.3900 . ? C6T C5T 1.3900 . ? C1T C2T 1.3900 . ? C2T C3T 1.3900 . ? C3T C4T 1.3900 . ? C4T C5T 1.3900 . ? 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 N1 Fe1 N10 88.50(9) . . ? N3 Fe1 N1 85.79(9) . . ? N3 Fe1 N10 89.65(9) . . ? N5 Fe1 N1 92.20(8) . . ? N5 Fe1 N3 91.14(8) . . ? N5 Fe1 N8 88.52(8) . . ? N5 Fe1 N10 178.99(9) . . ? N6 Fe1 N1 177.85(8) . . ? N6 Fe1 N3 92.82(9) . . ? N6 Fe1 N5 89.46(8) . . ? N6 Fe1 N8 89.70(9) . . ? N6 Fe1 N10 89.86(9) . . ? N8 Fe1 N1 91.71(9) . . ? N8 Fe1 N3 177.46(8) . . ? N8 Fe1 N10 90.72(9) . . ? N2 N1 Fe1 119.89(16) . . ? C1 N1 Fe1 133.11(18) . . ? C1 N1 N2 105.3(2) . . ? N1 N2 B1 117.1(2) . . ? C3 N2 N1 109.72(19) . . ? C3 N2 B1 131.5(2) . . ? N4 N3 Fe1 119.74(15) . . ? C4 N3 Fe1 132.71(17) . . ? C4 N3 N4 106.0(2) . . ? N3 N4 B1 117.44(19) . . ? C6 N4 N3 108.92(19) . . ? C6 N4 B1 132.4(2) . . ? C14 N5 Fe1 118.30(15) . . ? C14 N5 C18 120.8(2) . . ? C18 N5 Fe1 120.79(16) . . ? N7 N6 Fe1 119.00(15) . . ? C19 N6 Fe1 135.00(17) . . ? C19 N6 N7 106.0(2) . . ? N6 N7 B2 120.01(19) . . ? C21 N7 N6 109.6(2) . . ? C21 N7 B2 130.3(2) . . ? N9 N8 Fe1 120.82(16) . . ? C22 N8 Fe1 132.67(17) . . ? C22 N8 N9 105.9(2) . . ? N8 N9 B2 117.15(19) . . ? C24 N9 N8 109.1(2) . . ? C24 N9 B2 132.9(2) . . ? N1 C1 C2 111.5(2) . . ? C3 C2 C1 104.3(2) . . ? N2 C3 C2 109.1(2) . . ? N3 C4 C5 111.1(2) . . ? C6 C5 C4 104.3(2) . . ? N4 C6 C5 109.6(2) . . ? C8 C7 C12 115.0(2) . . ? C8 C7 B1 124.4(2) . . ? C12 C7 B1 119.9(2) . . ? C9 C8 C7 122.9(3) . . ? C10 C9 C8 120.6(3) . . ? C9 C10 C13 121.6(3) . . ? C11 C10 C9 117.7(2) . . ? C11 C10 C13 120.6(3) . . ? C10 C11 C12 120.9(3) . . ? C11 C12 C7 122.6(3) . . ? N5 C14 C15 119.3(2) . . ? N5 C14 B1 119.2(2) . . ? C15 C14 B1 121.5(2) . . ? C16 C15 C14 120.8(2) . . ? C15 C16 C17 118.6(2) . . ? C16 C17 C18 120.9(2) . . ? N5 C18 C17 119.4(2) . . ? N5 C18 B2 117.0(2) . . ? C17 C18 B2 123.4(2) . . ? N6 C19 C20 111.2(2) . . ? C21 C20 C19 104.5(2) . . ? N7 C21 C20 108.7(2) . . ? N8 C22 C23 111.5(2) . . ? C24 C23 C22 104.2(3) . . ? N9 C24 C23 109.3(2) . . ? C26 C25 C30 114.8(2) . . ? C26 C25 B2 123.6(2) . . ? C30 C25 B2 120.8(2) . . ? C27 C26 C25 122.5(2) . . ? C26 C27 C28 121.3(2) . . ? C27 C28 C31 122.1(2) . . ? C29 C28 C27 117.6(2) . . ? C29 C28 C31 120.3(2) . . ? C30 C29 C28 120.7(2) . . ? C29 C30 C25 123.0(2) . . ? N2 B1 C7 111.2(2) . . ? N2 B1 C14 109.2(2) . . ? N4 B1 N2 102.06(19) . . ? N4 B1 C7 114.2(2) . . ? N4 B1 C14 109.6(2) . . ? C7 B1 C14 110.24(19) . . ? N7 B2 N9 106.30(19) . . ? N7 B2 C18 107.9(2) . . ? N7 B2 C25 105.7(2) . . ? N9 B2 C18 104.5(2) . . ? N9 B2 C25 114.0(2) . . ? C25 B2 C18 117.8(2) . . ? C2S C1S C6S 120.0 . . ? C3S C2S C1S 120.0 . . ? C2S C3S C4S 120.0 . . ? C3S C4S C5S 120.0 . . ? C4S C5S C6S 120.0 . . ? C5S C6S C1S 120.0 . . ? C1T C6T C5T 120.0 . . ? C2T C1T C6T 120.0 . . ? C3T C2T C1T 120.0 . . ? C2T C3T C4T 120.0 . . ? C5T C4T C3T 120.0 . . ? C4T C5T C6T 120.0 . . ? _shelx_res_file ; TITL ln585_a.res in C2/c ln585.res created by SHELXL-2018/3 at 08:33:10 on 04-Jun-2019 REM Old TITL LN585 in C2/c REM SHELXT solution in C2/c: R1 0.154, Rweak 0.027, Alpha 0.055 REM 0.522 for 212 systematic absences, Orientation as input REM Formula found by SHELXT: C38 B N10 Fe CELL 1.54178 16.6461 17.2299 24.1321 90 102.636 90 ZERR 8 0.0014 0.0016 0.002 0 0.004 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H B Fe N UNIT 296 304 16 8 80 DFIX 0.91 N10 H10a N10 H10b N10 H10c SADI C1S C2S C1T C2T SADI C1S C6S C1T C6T SADI C2S C3S C2T C3T SADI C3S C4S C3T C4T SADI C4S C5S C4T C5T SADI C5S C6S C5T C6T SADI 0.04 C1S C3S C1T C3T SADI 0.04 C1S C5S C1T C5T SADI 0.04 C2S C4S C2T C4T SADI 0.04 C2S C6S C2T C6T SADI 0.04 C3S C5S C3T C5T SADI 0.04 C4S C6S C4T C6T DANG 1.49 H10a H10c DANG 1.49 H10c H10b DANG 1.49 H10b H10a SIMU C6S C1S C2S C3S C5S C4S SIMU C1T C6T C2T C5T C3T C4T RIGU C1T C6T C2T C5T C3T C4T RIGU C6S C1S C2S C3S C5S C4S L.S. 30 PLAN 20 SIZE 0.144 0.236 0.281 TEMP -100.15 BOND list 4 fmap 2 ACTA REM REM REM WGHT 0.081800 FVAR 0.15697 0.64771 FE1 4 0.358081 0.355927 0.302188 11.00000 0.02909 0.03349 = 0.02480 0.00053 0.00718 0.00009 N1 5 0.273554 0.273910 0.274389 11.00000 0.03270 0.03642 = 0.02885 -0.00015 0.00527 0.00363 N2 5 0.198436 0.277122 0.288964 11.00000 0.03132 0.03153 = 0.03216 -0.00117 0.00487 -0.00287 N3 5 0.266169 0.431789 0.277858 11.00000 0.03108 0.03576 = 0.02952 0.00130 0.00608 -0.00242 N4 5 0.191535 0.418697 0.291631 11.00000 0.03024 0.03507 = 0.02950 0.00155 0.00556 0.00023 N5 5 0.337519 0.352055 0.379431 11.00000 0.03140 0.02735 = 0.02789 0.00003 0.00711 0.00006 N6 5 0.439543 0.438371 0.326724 11.00000 0.03235 0.03522 = 0.02718 0.00200 0.00918 0.00125 N7 5 0.497457 0.428884 0.376023 11.00000 0.02978 0.03492 = 0.02877 -0.00065 0.00743 -0.00113 N8 5 0.445900 0.276632 0.325835 11.00000 0.03236 0.03776 = 0.02722 -0.00202 0.00594 0.00036 N9 5 0.501983 0.283236 0.376575 11.00000 0.03065 0.03556 = 0.03102 0.00044 0.00640 0.00296 N10 5 0.381937 0.359935 0.221491 11.00000 0.04102 0.04676 = 0.02929 -0.00003 0.01088 0.00065 C1 1 0.264754 0.221074 0.232661 11.00000 0.03917 0.04256 = 0.03413 -0.00644 0.00466 0.00090 AFIX 43 H1 2 0.307321 0.206338 0.214222 11.00000 -1.20000 AFIX 0 C2 1 0.185801 0.190701 0.219837 11.00000 0.04426 0.04346 = 0.04129 -0.00652 0.00330 -0.00343 AFIX 43 H2 2 0.164309 0.152226 0.192390 11.00000 -1.20000 AFIX 0 C3 1 0.145641 0.228856 0.255825 11.00000 0.03467 0.04067 = 0.03933 -0.00293 0.00402 -0.00501 AFIX 43 H3 2 0.089408 0.222102 0.257028 11.00000 -1.20000 AFIX 0 C4 1 0.253548 0.488864 0.239382 11.00000 0.04023 0.04155 = 0.03464 0.00917 0.00513 -0.00136 AFIX 43 H4 2 0.295078 0.510494 0.222631 11.00000 -1.20000 AFIX 0 C5 1 0.171456 0.512464 0.227073 11.00000 0.04185 0.04333 = 0.03936 0.01244 0.00437 0.00235 AFIX 43 H5 2 0.146627 0.551838 0.201414 11.00000 -1.20000 AFIX 0 C6 1 0.134826 0.466107 0.260293 11.00000 0.03258 0.04008 = 0.04006 0.00478 0.00448 0.00404 AFIX 43 H6 2 0.078060 0.467120 0.261179 11.00000 -1.20000 AFIX 0 C7 1 0.096164 0.337797 0.346385 11.00000 0.03035 0.03671 = 0.03227 0.00244 0.00554 -0.00205 C8 1 0.047803 0.400451 0.356115 11.00000 0.03878 0.04094 = 0.03955 0.00362 0.01151 0.00441 AFIX 43 H8 2 0.064512 0.451364 0.348543 11.00000 -1.20000 AFIX 0 C9 1 -0.023900 0.391620 0.376444 11.00000 0.04147 0.05140 = 0.04123 0.00111 0.01045 0.00712 AFIX 43 H9 2 -0.054924 0.436109 0.381995 11.00000 -1.20000 AFIX 0 C10 1 -0.050420 0.318367 0.388664 11.00000 0.03442 0.05586 = 0.03877 -0.00164 0.01049 -0.00649 C11 1 -0.002086 0.255201 0.381359 11.00000 0.04031 0.04687 = 0.03875 0.00111 0.00948 -0.01098 AFIX 43 H11 2 -0.017952 0.204593 0.390368 11.00000 -1.20000 AFIX 0 C12 1 0.069434 0.264953 0.360984 11.00000 0.03554 0.04029 = 0.03913 -0.00041 0.01002 -0.00173 AFIX 43 H12 2 0.101327 0.220476 0.356825 11.00000 -1.20000 AFIX 0 C13 1 -0.127823 0.307336 0.410436 11.00000 0.05096 0.07994 = 0.06864 -0.00924 0.03395 -0.00763 AFIX 137 H13A 2 -0.164507 0.351774 0.399170 11.00000 -1.50000 H13B 2 -0.113713 0.303384 0.451948 11.00000 -1.50000 H13C 2 -0.155612 0.259675 0.394356 11.00000 -1.50000 AFIX 0 C14 1 0.257999 0.346613 0.385306 11.00000 0.03321 0.02477 = 0.03207 -0.00088 0.00872 0.00058 C15 1 0.242218 0.339059 0.439665 11.00000 0.03300 0.03628 = 0.03383 -0.00031 0.01018 -0.00068 AFIX 43 H15 2 0.186933 0.337628 0.444129 11.00000 -1.20000 AFIX 0 C16 1 0.305764 0.333681 0.486706 11.00000 0.04416 0.04374 = 0.02953 0.00065 0.01275 -0.00526 AFIX 43 H16 2 0.294964 0.327425 0.523507 11.00000 -1.20000 AFIX 0 C17 1 0.385334 0.337552 0.479337 11.00000 0.03614 0.03580 = 0.02932 0.00158 0.00563 -0.00184 AFIX 43 H17 2 0.429890 0.331502 0.511194 11.00000 -1.20000 AFIX 0 C18 1 0.401413 0.350209 0.425859 11.00000 0.03407 0.02736 = 0.02774 0.00082 0.00491 -0.00011 C19 1 0.455591 0.507252 0.305585 11.00000 0.03943 0.03658 = 0.03376 0.00280 0.01060 -0.00081 AFIX 43 H19 2 0.424438 0.529178 0.271474 11.00000 -1.20000 AFIX 0 C20 1 0.523669 0.542344 0.340049 11.00000 0.04240 0.03696 = 0.04120 -0.00189 0.01405 -0.00626 AFIX 43 H20 2 0.547799 0.590857 0.334405 11.00000 -1.20000 AFIX 0 C21 1 0.548401 0.490860 0.384371 11.00000 0.03421 0.04081 = 0.03710 -0.00449 0.01042 -0.00394 AFIX 43 H21 2 0.593742 0.497870 0.415571 11.00000 -1.20000 AFIX 0 C22 1 0.458522 0.206406 0.305317 11.00000 0.03413 0.04140 = 0.03975 -0.00753 0.00681 0.00193 AFIX 43 H22 2 0.428440 0.186369 0.270198 11.00000 -1.20000 AFIX 0 C23 1 0.520954 0.166725 0.341769 11.00000 0.04058 0.03550 = 0.05434 -0.00661 0.00235 0.00773 AFIX 43 H23 2 0.541718 0.116404 0.336930 11.00000 -1.20000 AFIX 0 C24 1 0.546025 0.217052 0.386687 11.00000 0.03686 0.03813 = 0.04216 0.00042 0.00251 0.00442 AFIX 43 H24 2 0.587746 0.206718 0.419566 11.00000 -1.20000 AFIX 0 C25 1 0.569933 0.366253 0.468616 11.00000 0.03341 0.03716 = 0.03108 0.00146 0.00661 -0.00102 C26 1 0.650639 0.341688 0.469525 11.00000 0.03488 0.03908 = 0.03260 -0.00245 0.00726 0.00053 AFIX 43 H26 2 0.660524 0.311806 0.438609 11.00000 -1.20000 AFIX 0 C27 1 0.716295 0.359307 0.513680 11.00000 0.02995 0.04109 = 0.04105 0.00176 0.00796 0.00456 AFIX 43 H27 2 0.769439 0.339801 0.512965 11.00000 -1.20000 AFIX 0 C28 1 0.706016 0.405006 0.559084 11.00000 0.03853 0.03916 = 0.03474 0.00176 0.00406 -0.00277 C29 1 0.627101 0.431353 0.559044 11.00000 0.03895 0.03791 = 0.03453 -0.00371 0.00887 0.00031 AFIX 43 H29 2 0.618080 0.462755 0.589466 11.00000 -1.20000 AFIX 0 C30 1 0.561464 0.412317 0.515121 11.00000 0.03272 0.04062 = 0.03582 -0.00112 0.00875 0.00221 AFIX 43 H30 2 0.508314 0.431228 0.516462 11.00000 -1.20000 AFIX 0 C31 1 0.776980 0.427257 0.606299 11.00000 0.04115 0.05549 = 0.04339 -0.00443 -0.00191 0.00078 AFIX 137 H31A 2 0.804617 0.380265 0.623789 11.00000 -1.50000 H31B 2 0.756610 0.457183 0.634922 11.00000 -1.50000 H31C 2 0.816057 0.458856 0.591021 11.00000 -1.50000 AFIX 0 B1 3 0.184084 0.345922 0.328920 11.00000 0.03130 0.02957 = 0.03244 0.00094 0.00658 0.00052 B2 3 0.494207 0.356103 0.414275 11.00000 0.03316 0.03702 = 0.02836 -0.00046 0.00777 0.00048 PART 1 AFIX 66 C1S 1 0.098435 0.438631 0.515853 21.00000 0.07997 0.03058 = 0.05096 -0.00258 0.01582 -0.00262 AFIX 43 H1S 2 0.055483 0.450271 0.483978 21.00000 -1.20000 AFIX 65 C2S 1 0.160595 0.492428 0.534818 21.00000 0.08744 0.04229 = 0.05413 -0.00182 0.02231 -0.01553 AFIX 43 H2S 2 0.160127 0.540835 0.515904 21.00000 -1.20000 AFIX 65 C3S 1 0.223439 0.475396 0.581457 21.00000 0.06739 0.05181 = 0.06309 -0.00876 0.02555 -0.00757 AFIX 43 H3S 2 0.265922 0.512164 0.594419 21.00000 -1.20000 AFIX 65 C4S 1 0.224124 0.404568 0.609132 21.00000 0.06221 0.03597 = 0.05620 -0.01633 0.01676 -0.00209 AFIX 43 H4S 2 0.267076 0.392929 0.641007 21.00000 -1.20000 AFIX 65 C5S 1 0.161964 0.350771 0.590167 21.00000 0.05493 0.05035 = 0.04960 -0.00539 0.01644 -0.00287 AFIX 43 H5S 2 0.162433 0.302363 0.609081 21.00000 -1.20000 AFIX 65 C6S 1 0.099120 0.367801 0.543528 21.00000 0.06018 0.03834 = 0.06404 0.00703 0.01906 0.00152 AFIX 43 H6S 2 0.056636 0.331033 0.530567 21.00000 -1.20000 AFIX 66 PART 0 PART 2 C6T 1 0.125940 0.353632 0.571830 -21.00000 0.05416 0.05028 = 0.08220 -0.00335 0.02377 -0.00750 AFIX 43 H6T 2 0.096868 0.307380 0.576179 -21.00000 -1.20000 AFIX 65 C1T 1 0.093736 0.405461 0.528520 -21.00000 0.07444 0.05159 = 0.07093 -0.00241 0.02060 -0.01425 AFIX 43 H1T 2 0.042655 0.394631 0.503267 -21.00000 -1.20000 AFIX 65 C2T 1 0.136273 0.473134 0.522157 -21.00000 0.08302 0.05137 = 0.05360 -0.00332 0.02002 -0.00986 AFIX 43 H2T 2 0.114263 0.508557 0.492556 -21.00000 -1.20000 AFIX 65 C3T 1 0.211014 0.488980 0.559105 -21.00000 0.08808 0.04788 = 0.05600 0.01424 0.00993 -0.01262 AFIX 43 H3T 2 0.240086 0.535232 0.554756 -21.00000 -1.20000 AFIX 65 C4T 1 0.243218 0.437152 0.602416 -21.00000 0.06186 0.04003 = 0.06075 0.00734 0.02341 -0.00939 AFIX 43 H4T 2 0.294300 0.447982 0.627668 -21.00000 -1.20000 AFIX 65 C5T 1 0.200682 0.369478 0.608779 -21.00000 0.05821 0.03668 = 0.06624 0.00969 0.03189 -0.00183 AFIX 43 H5T 2 0.222693 0.334056 0.638381 -21.00000 -1.20000 AFIX 0 PART 0 H10A 2 0.335865 0.356719 0.192619 11.00000 0.05192 H10B 2 0.414966 0.320871 0.212414 11.00000 0.09008 H10C 2 0.410653 0.402471 0.215107 11.00000 0.09984 HKLF 4 REM ln585_a.res in C2/c REM wR2 = 0.1395, GooF = S = 1.057, Restrained GooF = 1.044 for all data REM R1 = 0.0441 for 4514 Fo > 4sig(Fo) and 0.0937 for all 6138 data REM 496 parameters refined using 162 restraints END WGHT 0.0818 0.0000 REM Highest difference peak 0.591, deepest hole -0.482, 1-sigma level 0.077 Q1 1 0.1421 0.4649 0.1988 11.00000 0.05 0.59 Q2 1 0.3591 0.3569 0.2618 11.00000 0.05 0.49 Q3 1 0.3539 0.3175 0.3017 11.00000 0.05 0.45 Q4 1 0.3237 0.3550 0.3319 11.00000 0.05 0.38 Q5 1 0.3518 0.3577 0.3431 11.00000 0.05 0.37 Q6 1 0.1350 0.3407 0.3287 11.00000 0.05 0.31 Q7 1 0.2963 0.3494 0.3819 11.00000 0.05 0.30 Q8 1 0.3534 0.4368 0.2678 11.00000 0.05 0.30 Q9 1 -0.1272 0.2502 0.4354 11.00000 0.05 0.30 Q10 1 0.5438 0.4995 0.3541 11.00000 0.05 0.30 Q11 1 0.2619 0.3897 0.2246 11.00000 0.05 0.29 Q12 1 0.4756 0.4292 0.3549 11.00000 0.05 0.29 Q13 1 0.3014 0.4870 0.2170 11.00000 0.05 0.29 Q14 1 0.5224 0.4607 0.3833 11.00000 0.05 0.29 Q15 1 0.5397 0.4114 0.3593 11.00000 0.05 0.28 Q16 1 0.4197 0.4045 0.2785 11.00000 0.05 0.28 Q17 1 0.4225 0.3042 0.2763 11.00000 0.05 0.28 Q18 1 0.5166 0.2481 0.3796 11.00000 0.05 0.28 Q19 1 -0.0240 0.3607 0.3778 11.00000 0.05 0.28 Q20 1 0.4558 0.4988 0.2782 11.00000 0.05 0.28 ; _shelx_res_checksum 67301 _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_ln634 _database_code_depnum_ccdc_archive 'CCDC 2044414' loop_ _audit_author_name _audit_author_address 'Benjamin S. Gelfand' ;University of Calgary Canada ; _audit_update_record ; 2020-11-14 deposited with the CCDC. 2020-12-22 downloaded from the CCDC. ; _audit_creation_date 2019-08-23 _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 'C62 H60 B4 Fe2 N20, C3 H3' _chemical_formula_sum 'C65 H63 B4 Fe2 N20' _chemical_formula_weight 1279.29 _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 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 '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 triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5636(9) _cell_length_b 13.6840(10) _cell_length_c 20.5835(17) _cell_angle_alpha 98.128(5) _cell_angle_beta 100.359(5) _cell_angle_gamma 115.218(5) _cell_volume 3053.3(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3745 _cell_measurement_temperature 173 _cell_measurement_theta_max 69.99 _cell_measurement_theta_min 3.68 _shelx_estimated_absorpt_T_max 0.847 _shelx_estimated_absorpt_T_min 0.413 _exptl_absorpt_coefficient_mu 4.291 _exptl_absorpt_correction_T_max 0.7533 _exptl_absorpt_correction_T_min 0.6144 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1073 before and 0.0372 after correction. The Ratio of minimum to maximum transmission is 0.8156. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour blue _exptl_crystal_colour_primary blue _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plank _exptl_crystal_F_000 1330 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_unetI/netI 0.0660 _diffrn_reflns_Laue_measured_fraction_full 0.977 _diffrn_reflns_Laue_measured_fraction_max 0.973 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 10913 _diffrn_reflns_point_group_measured_fraction_full 0.977 _diffrn_reflns_point_group_measured_fraction_max 0.973 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.355 _diffrn_reflns_theta_min 2.251 _diffrn_ambient_temperature 173.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source ? _diffrn_special_details ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 7603 _reflns_number_total 10913 _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 v8.37A (Bruker, 2015)' _computing_data_collection ? _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _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 0.573 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.073 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 830 _refine_ls_number_reflns 10913 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0546 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0815P)^2^+0.1435P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1325 _refine_ls_wR_factor_ref 0.1502 _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) groups, All C(H,H,H) groups 2. Restrained distances N10-H10 \\sim N11-H11 with sigma of 0.02 H10-N11 \\sim N10-H11 with sigma of 0.02 3.a Aromatic/amide H refined with riding coordinates: C53(H53), C35(H35), C19(H19), C17(H17), C3(H3), C15(H15), C46(H46), C20(H20), C1(H1), C48(H48), C26(H26), C4(H4), C50(H50), C32(H32), C55(H55), C54(H54), C52(H52), C22(H22), C24(H24), C21(H21), C58(H58), C8(H8), C5(H5), C57(H57), C43(H43), C47(H47), C16(H16), C37(H37), C6(H6), C30(H30), C33(H33), C42(H42), C34(H34), C61(H61), C51(H51), C23(H23), C2(H2), C27(H27), C36(H36), C60(H60), C39(H39), C29(H29), C9(H9), C12(H12), C40(H40), C11(H11A), C1S(H1S), C3S(H3S), C2S(H2S) 3.b Idealised Me refined as rotating group: C44(H44A,H44B,H44C), C62(H62A,H62B,H62C), C13(H13A,H13B,H13C), C31(H31A,H31B, H31C) ; _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 Fe1 Fe 0.44005(4) 0.49152(4) 0.30321(3) 0.01777(14) Uani 1 1 d . . . . . Fe2 Fe 0.75259(4) 0.47176(4) 0.20894(3) 0.01800(14) Uani 1 1 d . . . . . N17 N 0.8863(2) 0.6276(2) 0.25564(15) 0.0216(6) Uani 1 1 d . . . . . N7 N 0.3637(3) 0.3720(2) 0.40524(16) 0.0218(6) Uani 1 1 d . . . . . N19 N 0.7331(3) 0.5350(2) 0.12828(15) 0.0209(6) Uani 1 1 d . . . . . N5 N 0.3146(2) 0.5299(2) 0.33372(15) 0.0202(6) Uani 1 1 d . . . . . N14 N 0.7783(2) 0.4105(2) 0.28936(16) 0.0210(6) Uani 1 1 d . . . . . N18 N 0.9670(2) 0.6867(2) 0.22173(16) 0.0218(6) Uani 1 1 d . . . . . N11 N 0.6371(2) 0.5084(2) 0.24180(15) 0.0203(6) Uani 1 1 d D . . . . N3 N 0.5669(3) 0.6421(2) 0.35123(15) 0.0203(6) Uani 1 1 d . . . . . N13 N 0.6308(3) 0.2278(2) 0.16487(16) 0.0220(6) Uani 1 1 d . . . . . N8 N 0.3064(3) 0.3341(2) 0.25886(15) 0.0221(6) Uani 1 1 d . . . . . N12 N 0.6224(2) 0.3224(2) 0.15811(15) 0.0213(6) Uani 1 1 d . . . . . N10 N 0.5527(3) 0.4555(2) 0.27002(15) 0.0205(6) Uani 1 1 d D . . . . N1 N 0.4110(2) 0.5518(2) 0.22206(16) 0.0214(6) Uani 1 1 d . . . . . N16 N 0.8725(2) 0.4310(2) 0.17905(15) 0.0197(6) Uani 1 1 d . . . . . N4 N 0.5475(3) 0.7318(2) 0.34772(16) 0.0230(6) Uani 1 1 d . . . . . N20 N 0.8328(3) 0.5934(2) 0.10621(16) 0.0223(6) Uani 1 1 d . . . . . N6 N 0.4635(2) 0.4335(2) 0.38439(16) 0.0210(6) Uani 1 1 d . . . . . N9 N 0.2197(2) 0.2780(2) 0.29088(16) 0.0241(6) Uani 1 1 d . . . . . N2 N 0.4141(3) 0.6542(2) 0.22900(16) 0.0233(6) Uani 1 1 d . . . . . N15 N 0.7663(3) 0.3049(2) 0.28233(16) 0.0241(6) Uani 1 1 d . . . . . C45 C 0.8670(3) 0.3300(3) 0.18432(18) 0.0211(7) Uani 1 1 d . . . . . C14 C 0.3101(3) 0.6246(3) 0.32206(18) 0.0226(7) Uani 1 1 d . . . . . C56 C 1.0663(3) 0.6911(3) 0.11544(19) 0.0214(7) Uani 1 1 d . . . . . C18 C 0.2213(3) 0.4510(3) 0.35042(18) 0.0219(7) Uani 1 1 d . . . . . C49 C 0.9658(3) 0.5075(3) 0.16018(18) 0.0199(7) Uani 1 1 d . . . . . C53 C 0.6394(3) 0.5405(3) 0.08948(19) 0.0253(8) Uani 1 1 d . . . . . H53 H 0.558238 0.506857 0.093637 0.030 Uiso 1 1 calc R . . . . C35 C 0.7965(3) 0.4499(3) 0.35516(19) 0.0269(8) Uani 1 1 d . . . . . H35 H 0.809144 0.522435 0.374707 0.032 Uiso 1 1 calc R . . . . C19 C 0.5591(3) 0.4367(3) 0.42733(19) 0.0252(8) Uani 1 1 d . . . . . H19 H 0.640921 0.473819 0.424549 0.030 Uiso 1 1 calc R . . . . C17 C 0.1138(3) 0.4596(3) 0.3486(2) 0.0267(8) Uani 1 1 d . . . . . H17 H 0.047374 0.403019 0.358999 0.032 Uiso 1 1 calc R . . . . C3 C 0.3867(3) 0.6722(3) 0.1675(2) 0.0255(8) Uani 1 1 d . . . . . H3 H 0.381700 0.736746 0.158956 0.031 Uiso 1 1 calc R . . . . C7 C 0.4311(3) 0.8375(3) 0.30808(19) 0.0247(8) Uani 1 1 d . . . . . C15 C 0.2024(3) 0.6327(3) 0.3196(2) 0.0269(8) Uani 1 1 d . . . . . H15 H 0.197357 0.696371 0.309267 0.032 Uiso 1 1 calc R . . . . C46 C 0.9596(3) 0.3071(3) 0.1715(2) 0.0277(8) Uani 1 1 d . . . . . H46 H 0.954658 0.236283 0.173281 0.033 Uiso 1 1 calc R . . . . C20 C 0.5243(3) 0.3797(3) 0.4761(2) 0.0280(8) Uani 1 1 d . . . . . H20 H 0.574796 0.370537 0.512451 0.034 Uiso 1 1 calc R . . . . C1 C 0.3829(3) 0.5098(3) 0.15510(19) 0.0241(8) Uani 1 1 d . . . . . H1 H 0.374697 0.439083 0.135179 0.029 Uiso 1 1 calc R . . . . C48 C 1.0609(3) 0.4853(3) 0.1498(2) 0.0264(8) Uani 1 1 d . . . . . H48 H 1.127574 0.539375 0.138089 0.032 Uiso 1 1 calc R . . . . C26 C 0.1106(3) 0.3293(3) 0.4555(2) 0.0283(8) Uani 1 1 d . . . . . H26 H 0.152897 0.408415 0.467069 0.034 Uiso 1 1 calc R . . . . C25 C 0.1379(3) 0.2711(3) 0.4046(2) 0.0265(8) Uani 1 1 d . . . . . C4 C 0.6797(3) 0.6826(3) 0.39165(19) 0.0245(8) Uani 1 1 d . . . . . H4 H 0.718046 0.638309 0.403135 0.029 Uiso 1 1 calc R . . . . C50 C 0.9003(3) 0.7006(3) 0.3104(2) 0.0272(8) Uani 1 1 d . . . . . H50 H 0.855489 0.682428 0.343305 0.033 Uiso 1 1 calc R . . . . C32 C 0.5095(3) 0.2882(3) 0.1183(2) 0.0261(8) Uani 1 1 d . . . . . H32 H 0.478384 0.336588 0.104748 0.031 Uiso 1 1 calc R . . . . C55 C 0.7992(3) 0.6338(3) 0.05486(19) 0.0274(8) Uani 1 1 d . . . . . H55 H 0.852002 0.677650 0.030977 0.033 Uiso 1 1 calc R . . . . C54 C 0.6763(3) 0.6018(3) 0.0424(2) 0.0302(8) Uani 1 1 d . . . . . H54 H 0.627682 0.617988 0.009010 0.036 Uiso 1 1 calc R . . . . C52 C 1.0271(3) 0.7944(3) 0.2562(2) 0.0341(9) Uani 1 1 d . . . . . H52 H 1.086854 0.852720 0.242787 0.041 Uiso 1 1 calc R . . . . C22 C 0.2791(3) 0.2649(3) 0.1990(2) 0.0261(8) Uani 1 1 d . . . . . H22 H 0.325711 0.281038 0.166775 0.031 Uiso 1 1 calc R . . . . C24 C 0.1392(3) 0.1786(3) 0.2486(2) 0.0279(8) Uani 1 1 d . . . . . H24 H 0.068981 0.125162 0.257962 0.033 Uiso 1 1 calc R . . . . C21 C 0.3993(3) 0.3389(3) 0.4598(2) 0.0283(8) Uani 1 1 d . . . . . H21 H 0.346681 0.294499 0.483567 0.034 Uiso 1 1 calc R . . . . C58 C 1.2630(3) 0.8357(3) 0.1122(2) 0.0296(8) Uani 1 1 d . . . . . H58 H 1.334668 0.903209 0.135143 0.036 Uiso 1 1 calc R . . . . C8 C 0.4908(3) 0.9101(3) 0.2703(2) 0.0296(8) Uani 1 1 d . . . . . H8 H 0.529226 0.887160 0.240042 0.036 Uiso 1 1 calc R . . . . C5 C 0.7336(3) 0.7972(3) 0.4146(2) 0.0289(8) Uani 1 1 d . . . . . H5 H 0.812787 0.845587 0.444006 0.035 Uiso 1 1 calc R . . . . C38 C 0.7562(3) 0.1239(3) 0.2052(2) 0.0265(8) Uani 1 1 d . . . . . C57 C 1.1762(3) 0.7876(3) 0.1471(2) 0.0271(8) Uani 1 1 d . . . . . H57 H 1.192269 0.821320 0.193800 0.033 Uiso 1 1 calc R . . . . C43 C 0.8173(3) 0.0987(3) 0.2591(2) 0.0309(9) Uani 1 1 d . . . . . H43 H 0.866187 0.156043 0.299371 0.037 Uiso 1 1 calc R . . . . C47 C 1.0590(3) 0.3857(3) 0.1563(2) 0.0301(9) Uani 1 1 d . . . . . H47 H 1.124782 0.371429 0.150331 0.036 Uiso 1 1 calc R . . . . C16 C 0.1038(3) 0.5499(3) 0.3318(2) 0.0295(8) Uani 1 1 d . . . . . H16 H 0.029836 0.554600 0.328735 0.035 Uiso 1 1 calc R . . . . C37 C 0.7742(4) 0.2809(3) 0.3432(2) 0.0309(9) Uani 1 1 d . . . . . H37 H 0.766755 0.212043 0.351659 0.037 Uiso 1 1 calc R . . . . C6 C 0.6469(3) 0.8254(3) 0.3854(2) 0.0289(8) Uani 1 1 d . . . . . H6 H 0.655687 0.898823 0.390860 0.035 Uiso 1 1 calc R . . . . C30 C 0.0809(4) 0.1558(3) 0.3953(2) 0.0319(9) Uani 1 1 d . . . . . H30 H 0.100689 0.111983 0.364362 0.038 Uiso 1 1 calc R . . . . C33 C 0.4451(3) 0.1736(3) 0.0998(2) 0.0312(9) Uani 1 1 d . . . . . H33 H 0.364048 0.128883 0.071664 0.037 Uiso 1 1 calc R . . . . C42 C 0.8096(3) -0.0055(3) 0.2563(2) 0.0315(9) Uani 1 1 d . . . . . H42 H 0.850632 -0.018246 0.295113 0.038 Uiso 1 1 calc R . . . . C34 C 0.5232(3) 0.1381(3) 0.1307(2) 0.0275(8) Uani 1 1 d . . . . . H34 H 0.504837 0.062584 0.128476 0.033 Uiso 1 1 calc R . . . . C59 C 1.2479(3) 0.7881(3) 0.0455(2) 0.0293(8) Uani 1 1 d . . . . . C61 C 1.0529(3) 0.6461(3) 0.0472(2) 0.0314(9) Uani 1 1 d . . . . . H61 H 0.979116 0.581483 0.022839 0.038 Uiso 1 1 calc R . . . . C51 C 0.9886(4) 0.8070(3) 0.3135(2) 0.0352(10) Uani 1 1 d . . . . . H51 H 1.016177 0.873329 0.347646 0.042 Uiso 1 1 calc R . . . . C10 C 0.4422(4) 1.0524(3) 0.3189(2) 0.0344(9) Uani 1 1 d . . . . . C41 C 0.7438(3) -0.0919(3) 0.1986(2) 0.0306(9) Uani 1 1 d . . . . . C23 C 0.1740(4) 0.1662(3) 0.1899(2) 0.0328(9) Uani 1 1 d . . . . . H23 H 0.134935 0.104079 0.151513 0.039 Uiso 1 1 calc R . . . . C2 C 0.3670(3) 0.5822(3) 0.1183(2) 0.0274(8) Uani 1 1 d . . . . . H2 H 0.347155 0.572159 0.070251 0.033 Uiso 1 1 calc R . . . . C27 C 0.0252(3) 0.2772(3) 0.4896(2) 0.0340(9) Uani 1 1 d . . . . . H27 H 0.009515 0.320674 0.523133 0.041 Uiso 1 1 calc R . . . . C36 C 0.7949(4) 0.3722(3) 0.3920(2) 0.0345(9) Uani 1 1 d . . . . . H36 H 0.805479 0.379972 0.439601 0.041 Uiso 1 1 calc R . . . . C60 C 1.1411(4) 0.6906(3) 0.0135(2) 0.0330(9) Uani 1 1 d . . . . . H60 H 1.128603 0.654078 -0.032069 0.040 Uiso 1 1 calc R . . . . C39 C 0.6998(4) 0.0387(3) 0.1451(2) 0.0339(9) Uani 1 1 d . . . . . H39 H 0.664948 0.053111 0.104921 0.041 Uiso 1 1 calc R . . . . C29 C -0.0043(4) 0.1026(3) 0.4301(2) 0.0374(10) Uani 1 1 d . . . . . H29 H -0.040184 0.023817 0.422707 0.045 Uiso 1 1 calc R . . . . C9 C 0.4964(4) 1.0147(3) 0.2752(2) 0.0332(9) Uani 1 1 d . . . . . H9 H 0.537990 1.060973 0.248308 0.040 Uiso 1 1 calc R . . . . C28 C -0.0377(4) 0.1618(3) 0.4751(2) 0.0357(9) Uani 1 1 d . . . . . C12 C 0.3863(4) 0.8815(3) 0.3554(2) 0.0386(10) Uani 1 1 d . . . . . H12 H 0.351021 0.838480 0.385386 0.046 Uiso 1 1 calc R . . . . C40 C 0.6931(4) -0.0661(3) 0.1419(2) 0.0366(10) Uani 1 1 d . . . . . H40 H 0.652900 -0.121367 0.100032 0.044 Uiso 1 1 calc R . . . . C44 C 0.7260(4) -0.2087(3) 0.1976(3) 0.0416(11) Uani 1 1 d . . . . . H44A H 0.783703 -0.221783 0.175911 0.062 Uiso 1 1 calc GR . . . . H44B H 0.642303 -0.262710 0.171766 0.062 Uiso 1 1 calc GR . . . . H44C H 0.740520 -0.217165 0.244339 0.062 Uiso 1 1 calc GR . . . . C62 C 1.3456(4) 0.8355(4) 0.0091(2) 0.0439(11) Uani 1 1 d . . . . . H62A H 1.367934 0.914168 0.011828 0.066 Uiso 1 1 calc GR . . . . H62B H 1.314497 0.794119 -0.038843 0.066 Uiso 1 1 calc GR . . . . H62C H 1.417646 0.828897 0.030516 0.066 Uiso 1 1 calc GR . . . . B2 B 0.2315(4) 0.3408(3) 0.3636(2) 0.0237(9) Uani 1 1 d . . . . . C11 C 0.3913(4) 0.9859(3) 0.3603(3) 0.0446(12) Uani 1 1 d . . . . . H11A H 0.358682 1.011728 0.393065 0.054 Uiso 1 1 calc R . . . . B1 B 0.4241(4) 0.7157(3) 0.3028(2) 0.0231(9) Uani 1 1 d . . . . . B3 B 0.7562(4) 0.2439(3) 0.2088(2) 0.0261(9) Uani 1 1 d . . . . . C13 C 0.4427(5) 1.1634(3) 0.3205(3) 0.0519(13) Uani 1 1 d . . . . . H13A H 0.526415 1.221427 0.327358 0.078 Uiso 1 1 calc GR . . . . H13B H 0.410522 1.181505 0.357872 0.078 Uiso 1 1 calc GR . . . . H13C H 0.391363 1.159192 0.277164 0.078 Uiso 1 1 calc GR . . . . B4 B 0.9629(4) 0.6229(3) 0.1510(2) 0.0232(9) Uani 1 1 d . . . . . C31 C -0.1402(4) 0.1043(4) 0.5067(3) 0.0541(13) Uani 1 1 d . . . . . H31A H -0.131187 0.155670 0.548112 0.081 Uiso 1 1 calc GR . . . . H31B H -0.136987 0.038417 0.518371 0.081 Uiso 1 1 calc GR . . . . H31C H -0.218744 0.081571 0.474265 0.081 Uiso 1 1 calc GR . . . . C1S C -0.0876(4) 0.0229(4) 0.0201(3) 0.0548(14) Uani 1 1 d . . . . . H1S H -0.148016 0.038538 0.034024 0.066 Uiso 1 1 calc R . . . . C3S C 0.0211(5) -0.0841(4) 0.0193(3) 0.0540(14) Uani 1 1 d . . . . . H3S H 0.035462 -0.142067 0.032671 0.065 Uiso 1 1 calc R . . . . C2S C -0.0664(5) -0.0610(4) 0.0391(3) 0.0578(14) Uani 1 1 d . . . . . H2S H -0.112463 -0.103354 0.066205 0.069 Uiso 1 1 calc R . . . . H10 H 0.546(5) 0.394(4) 0.272(3) 0.087 Uiso 1 1 d DR . . . . H11 H 0.638(5) 0.565(4) 0.234(3) 0.087 Uiso 1 1 d DR . . . . 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 Fe1 0.0167(3) 0.0168(3) 0.0217(3) 0.0038(2) 0.0055(2) 0.0096(2) Fe2 0.0164(3) 0.0166(3) 0.0226(3) 0.0037(2) 0.0059(2) 0.0091(2) N17 0.0203(14) 0.0227(15) 0.0225(16) 0.0025(12) 0.0034(12) 0.0125(12) N7 0.0241(15) 0.0181(14) 0.0249(17) 0.0069(12) 0.0101(12) 0.0094(12) N19 0.0203(14) 0.0199(14) 0.0241(16) 0.0049(12) 0.0079(12) 0.0101(12) N5 0.0194(14) 0.0201(14) 0.0224(16) 0.0035(12) 0.0051(11) 0.0112(12) N14 0.0177(13) 0.0223(15) 0.0271(17) 0.0087(12) 0.0066(11) 0.0119(12) N18 0.0181(13) 0.0159(14) 0.0300(18) 0.0030(12) 0.0061(12) 0.0076(12) N11 0.0188(14) 0.0179(14) 0.0226(16) 0.0058(12) 0.0051(12) 0.0069(12) N3 0.0246(14) 0.0185(14) 0.0192(15) 0.0055(11) 0.0064(11) 0.0107(12) N13 0.0203(14) 0.0150(14) 0.0308(18) 0.0043(12) 0.0089(12) 0.0077(12) N8 0.0220(14) 0.0217(15) 0.0240(16) 0.0033(12) 0.0088(12) 0.0110(12) N12 0.0200(14) 0.0205(15) 0.0253(17) 0.0042(12) 0.0071(12) 0.0110(12) N10 0.0212(14) 0.0206(15) 0.0204(16) 0.0051(12) 0.0037(11) 0.0110(13) N1 0.0176(13) 0.0212(15) 0.0267(17) 0.0041(12) 0.0043(12) 0.0114(12) N16 0.0185(13) 0.0191(14) 0.0224(16) 0.0035(11) 0.0044(11) 0.0106(12) N4 0.0231(15) 0.0151(14) 0.0288(17) 0.0034(12) 0.0065(12) 0.0078(12) N20 0.0198(14) 0.0209(15) 0.0271(17) 0.0057(12) 0.0089(12) 0.0093(12) N6 0.0197(14) 0.0186(14) 0.0269(17) 0.0071(12) 0.0061(12) 0.0103(12) N9 0.0166(13) 0.0233(15) 0.0286(18) 0.0060(13) 0.0052(12) 0.0064(12) N2 0.0225(14) 0.0222(15) 0.0287(18) 0.0077(13) 0.0080(12) 0.0126(13) N15 0.0229(15) 0.0209(15) 0.0316(18) 0.0102(13) 0.0083(12) 0.0113(13) C45 0.0192(16) 0.0193(17) 0.0257(19) 0.0052(14) 0.0051(14) 0.0103(14) C14 0.0252(17) 0.0252(18) 0.0208(19) 0.0033(14) 0.0045(14) 0.0161(15) C56 0.0210(16) 0.0174(17) 0.028(2) 0.0087(14) 0.0071(14) 0.0101(14) C18 0.0214(16) 0.0212(17) 0.0226(19) 0.0028(14) 0.0079(14) 0.0094(15) C49 0.0180(16) 0.0200(17) 0.0210(18) 0.0031(13) 0.0061(13) 0.0084(14) C53 0.0188(16) 0.0291(19) 0.028(2) 0.0060(15) 0.0043(14) 0.0123(15) C35 0.0277(18) 0.0289(19) 0.026(2) 0.0041(15) 0.0066(15) 0.0159(16) C19 0.0244(18) 0.0239(18) 0.029(2) 0.0050(15) 0.0027(15) 0.0148(16) C17 0.0219(17) 0.030(2) 0.030(2) 0.0056(16) 0.0103(15) 0.0131(16) C3 0.0248(17) 0.0234(18) 0.033(2) 0.0112(15) 0.0084(15) 0.0137(15) C7 0.0258(18) 0.0214(18) 0.028(2) 0.0037(15) 0.0040(15) 0.0140(15) C15 0.0290(19) 0.0262(19) 0.033(2) 0.0082(16) 0.0111(16) 0.0186(16) C46 0.0288(19) 0.0271(19) 0.036(2) 0.0100(16) 0.0117(16) 0.0193(17) C20 0.0269(18) 0.029(2) 0.029(2) 0.0060(16) 0.0031(15) 0.0152(16) C1 0.0233(17) 0.0249(18) 0.024(2) -0.0005(14) 0.0041(14) 0.0134(15) C48 0.0195(17) 0.0272(19) 0.034(2) 0.0073(16) 0.0102(15) 0.0111(15) C26 0.0290(19) 0.0254(19) 0.028(2) 0.0065(15) 0.0059(15) 0.0110(16) C25 0.0213(17) 0.0277(19) 0.030(2) 0.0066(16) 0.0062(15) 0.0108(16) C4 0.0208(17) 0.0246(18) 0.030(2) 0.0083(15) 0.0069(15) 0.0117(15) C50 0.0287(19) 0.0279(19) 0.027(2) 0.0029(15) 0.0083(15) 0.0158(17) C32 0.0244(18) 0.0274(19) 0.030(2) 0.0054(15) 0.0087(15) 0.0154(16) C55 0.0316(19) 0.0253(19) 0.028(2) 0.0105(15) 0.0122(16) 0.0124(17) C54 0.0270(19) 0.031(2) 0.030(2) 0.0081(16) 0.0035(16) 0.0131(17) C52 0.0258(19) 0.0204(19) 0.047(3) 0.0015(17) 0.0121(17) 0.0041(16) C22 0.0306(19) 0.0243(18) 0.026(2) 0.0043(15) 0.0100(15) 0.0149(16) C24 0.0211(17) 0.0204(18) 0.035(2) 0.0037(15) 0.0050(15) 0.0055(15) C21 0.033(2) 0.028(2) 0.029(2) 0.0104(16) 0.0117(16) 0.0165(17) C58 0.0230(18) 0.0232(19) 0.037(2) 0.0108(16) 0.0079(16) 0.0046(16) C8 0.0294(19) 0.028(2) 0.034(2) 0.0053(16) 0.0112(16) 0.0152(17) C5 0.0228(18) 0.0231(19) 0.030(2) 0.0034(15) 0.0030(15) 0.0032(16) C38 0.0274(18) 0.0205(18) 0.039(2) 0.0131(16) 0.0167(16) 0.0132(16) C57 0.0259(18) 0.0284(19) 0.025(2) 0.0051(15) 0.0061(15) 0.0120(16) C43 0.0232(18) 0.0227(19) 0.044(2) 0.0027(16) 0.0041(16) 0.0114(16) C47 0.0199(17) 0.033(2) 0.041(2) 0.0073(17) 0.0092(16) 0.0155(16) C16 0.0249(18) 0.038(2) 0.035(2) 0.0086(17) 0.0104(16) 0.0220(17) C37 0.038(2) 0.034(2) 0.034(2) 0.0166(17) 0.0174(17) 0.0230(18) C6 0.0316(19) 0.0203(18) 0.029(2) 0.0041(15) 0.0034(16) 0.0088(16) C30 0.035(2) 0.027(2) 0.032(2) 0.0064(16) 0.0100(17) 0.0126(17) C33 0.0218(18) 0.028(2) 0.034(2) -0.0022(16) 0.0052(16) 0.0057(16) C42 0.0270(19) 0.030(2) 0.040(2) 0.0096(17) 0.0043(16) 0.0166(17) C34 0.0254(18) 0.0180(18) 0.035(2) 0.0038(15) 0.0116(16) 0.0057(15) C59 0.0252(18) 0.032(2) 0.034(2) 0.0156(17) 0.0111(16) 0.0132(17) C61 0.0229(18) 0.026(2) 0.037(2) 0.0005(16) 0.0049(16) 0.0071(16) C51 0.030(2) 0.024(2) 0.042(3) -0.0049(17) 0.0092(18) 0.0083(17) C10 0.033(2) 0.0206(19) 0.048(3) 0.0057(17) 0.0054(18) 0.0145(17) C41 0.0304(19) 0.027(2) 0.041(2) 0.0086(17) 0.0118(17) 0.0177(17) C23 0.031(2) 0.0235(19) 0.034(2) -0.0020(16) 0.0044(17) 0.0087(17) C2 0.0298(19) 0.036(2) 0.0205(19) 0.0069(15) 0.0090(15) 0.0177(17) C27 0.0282(19) 0.043(2) 0.024(2) 0.0032(17) 0.0051(16) 0.0122(18) C36 0.044(2) 0.046(2) 0.025(2) 0.0136(18) 0.0125(17) 0.028(2) C60 0.033(2) 0.033(2) 0.028(2) 0.0004(16) 0.0114(17) 0.0118(18) C39 0.042(2) 0.038(2) 0.034(2) 0.0119(18) 0.0141(18) 0.027(2) C29 0.038(2) 0.023(2) 0.038(2) 0.0071(17) 0.0075(18) 0.0035(18) C9 0.039(2) 0.026(2) 0.034(2) 0.0103(16) 0.0100(17) 0.0138(18) C28 0.029(2) 0.039(2) 0.030(2) 0.0085(18) 0.0084(17) 0.0065(18) C12 0.049(2) 0.030(2) 0.044(3) 0.0109(18) 0.026(2) 0.018(2) C40 0.043(2) 0.034(2) 0.039(2) 0.0030(18) 0.0090(19) 0.0254(19) C44 0.045(2) 0.025(2) 0.056(3) 0.0037(19) 0.003(2) 0.022(2) C62 0.039(2) 0.053(3) 0.040(3) 0.018(2) 0.020(2) 0.016(2) B2 0.0215(19) 0.021(2) 0.027(2) 0.0043(16) 0.0045(16) 0.0094(17) C11 0.047(3) 0.028(2) 0.065(3) 0.002(2) 0.030(2) 0.020(2) B1 0.0230(19) 0.022(2) 0.029(2) 0.0061(16) 0.0067(16) 0.0144(17) B3 0.024(2) 0.026(2) 0.036(3) 0.0121(18) 0.0122(18) 0.0151(18) C13 0.055(3) 0.028(2) 0.079(4) 0.012(2) 0.014(3) 0.027(2) B4 0.0213(19) 0.021(2) 0.027(2) 0.0029(16) 0.0062(16) 0.0106(17) C31 0.048(3) 0.051(3) 0.044(3) 0.007(2) 0.019(2) 0.003(2) C1S 0.043(3) 0.045(3) 0.073(4) 0.004(3) 0.010(2) 0.022(2) C3S 0.049(3) 0.032(2) 0.076(4) 0.014(2) 0.006(3) 0.019(2) C2S 0.049(3) 0.051(3) 0.067(4) 0.019(3) 0.016(3) 0.015(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 Fe1 N5 2.030(3) . ? Fe1 N3 1.955(3) . ? Fe1 N8 2.026(3) . ? Fe1 N10 1.887(3) . ? Fe1 N1 2.008(3) . ? Fe1 N6 1.977(3) . ? Fe2 N17 2.020(3) . ? Fe2 N19 2.001(3) . ? Fe2 N14 1.994(3) . ? Fe2 N11 1.921(3) . ? Fe2 N12 1.970(3) . ? Fe2 N16 1.978(3) . ? N17 N18 1.373(4) . ? N17 C50 1.327(5) . ? N7 N6 1.364(4) . ? N7 C21 1.343(5) . ? N7 B2 1.567(5) . ? N19 N20 1.367(4) . ? N19 C53 1.335(4) . ? N5 C14 1.373(4) . ? N5 C18 1.353(4) . ? N14 N15 1.371(4) . ? N14 C35 1.325(5) . ? N18 C52 1.345(5) . ? N18 B4 1.569(5) . ? N11 N10 1.293(4) . ? N3 N4 1.359(4) . ? N3 C4 1.336(4) . ? N13 N12 1.366(4) . ? N13 C34 1.353(4) . ? N13 B3 1.576(5) . ? N8 N9 1.377(4) . ? N8 C22 1.332(5) . ? N12 C32 1.346(4) . ? N1 N2 1.372(4) . ? N1 C1 1.335(5) . ? N16 C45 1.374(4) . ? N16 C49 1.362(4) . ? N4 C6 1.345(4) . ? N4 B1 1.562(5) . ? N20 C55 1.344(5) . ? N20 B4 1.573(5) . ? N6 C19 1.337(4) . ? N9 C24 1.345(4) . ? N9 B2 1.565(5) . ? N2 C3 1.336(5) . ? N2 B1 1.585(5) . ? N15 C37 1.338(5) . ? N15 B3 1.578(5) . ? C45 C46 1.386(5) . ? C45 B3 1.613(5) . ? C14 C15 1.397(5) . ? C14 B1 1.608(5) . ? C56 C57 1.398(5) . ? C56 C61 1.401(5) . ? C56 B4 1.611(5) . ? C18 C17 1.399(5) . ? C18 B2 1.623(5) . ? C49 C48 1.395(5) . ? C49 B4 1.632(5) . ? C53 C54 1.385(5) . ? C35 C36 1.385(5) . ? C19 C20 1.376(5) . ? C17 C16 1.377(5) . ? C3 C2 1.378(5) . ? C7 C8 1.395(5) . ? C7 C12 1.396(5) . ? C7 B1 1.618(5) . ? C15 C16 1.371(5) . ? C46 C47 1.381(5) . ? C20 C21 1.379(5) . ? C1 C2 1.387(5) . ? C48 C47 1.379(5) . ? C26 C25 1.406(5) . ? C26 C27 1.382(5) . ? C25 C30 1.393(5) . ? C25 B2 1.622(5) . ? C4 C5 1.383(5) . ? C50 C51 1.388(5) . ? C32 C33 1.378(5) . ? C55 C54 1.375(5) . ? C52 C51 1.369(6) . ? C22 C23 1.386(5) . ? C24 C23 1.369(6) . ? C58 C57 1.393(5) . ? C58 C59 1.375(6) . ? C8 C9 1.391(5) . ? C5 C6 1.373(5) . ? C38 C43 1.402(5) . ? C38 C39 1.402(5) . ? C38 B3 1.632(5) . ? C43 C42 1.380(5) . ? C37 C36 1.383(6) . ? C30 C29 1.396(5) . ? C33 C34 1.369(5) . ? C42 C41 1.381(5) . ? C59 C60 1.387(5) . ? C59 C62 1.511(5) . ? C61 C60 1.378(5) . ? C10 C9 1.389(6) . ? C10 C11 1.372(6) . ? C10 C13 1.511(5) . ? C41 C40 1.390(6) . ? C41 C44 1.513(5) . ? C27 C28 1.387(6) . ? C39 C40 1.392(5) . ? C29 C28 1.381(6) . ? C28 C31 1.511(6) . ? C12 C11 1.392(5) . ? C1S C3S 1.377(7) 2 ? C1S C2S 1.377(7) . ? C3S C2S 1.377(7) . ? 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 N3 Fe1 N5 89.12(11) . . ? N3 Fe1 N8 176.55(13) . . ? N3 Fe1 N1 87.92(12) . . ? N3 Fe1 N6 92.10(12) . . ? N8 Fe1 N5 89.13(11) . . ? N10 Fe1 N5 176.92(13) . . ? N10 Fe1 N3 92.03(12) . . ? N10 Fe1 N8 89.87(12) . . ? N10 Fe1 N1 90.20(12) . . ? N10 Fe1 N6 92.17(12) . . ? N1 Fe1 N5 86.99(12) . . ? N1 Fe1 N8 94.95(12) . . ? N6 Fe1 N5 90.63(12) . . ? N6 Fe1 N8 84.94(12) . . ? N6 Fe1 N1 177.62(12) . . ? N19 Fe2 N17 84.79(12) . . ? N14 Fe2 N17 94.09(12) . . ? N14 Fe2 N19 177.93(11) . . ? N11 Fe2 N17 89.76(12) . . ? N11 Fe2 N19 91.70(12) . . ? N11 Fe2 N14 90.03(12) . . ? N11 Fe2 N12 91.19(12) . . ? N11 Fe2 N16 177.19(13) . . ? N12 Fe2 N17 176.53(13) . . ? N12 Fe2 N19 91.85(12) . . ? N12 Fe2 N14 89.25(12) . . ? N12 Fe2 N16 88.74(11) . . ? N16 Fe2 N17 90.47(11) . . ? N16 Fe2 N19 91.11(12) . . ? N16 Fe2 N14 87.16(12) . . ? N18 N17 Fe2 120.2(2) . . ? C50 N17 Fe2 131.8(3) . . ? C50 N17 N18 106.1(3) . . ? N6 N7 B2 121.3(3) . . ? C21 N7 N6 109.2(3) . . ? C21 N7 B2 129.3(3) . . ? N20 N19 Fe2 119.8(2) . . ? C53 N19 Fe2 133.8(3) . . ? C53 N19 N20 106.2(3) . . ? C14 N5 Fe1 118.8(2) . . ? C18 N5 Fe1 119.1(2) . . ? C18 N5 C14 120.4(3) . . ? N15 N14 Fe2 121.8(2) . . ? C35 N14 Fe2 131.8(2) . . ? C35 N14 N15 106.1(3) . . ? N17 N18 B4 117.4(3) . . ? C52 N18 N17 108.8(3) . . ? C52 N18 B4 133.4(3) . . ? N10 N11 Fe2 131.8(2) . . ? N4 N3 Fe1 120.9(2) . . ? C4 N3 Fe1 133.3(2) . . ? C4 N3 N4 105.8(3) . . ? N12 N13 B3 116.8(3) . . ? C34 N13 N12 109.0(3) . . ? C34 N13 B3 134.2(3) . . ? N9 N8 Fe1 121.4(2) . . ? C22 N8 Fe1 132.5(3) . . ? C22 N8 N9 106.1(3) . . ? N13 N12 Fe2 122.0(2) . . ? C32 N12 Fe2 131.6(2) . . ? C32 N12 N13 106.1(3) . . ? N11 N10 Fe1 132.0(2) . . ? N2 N1 Fe1 121.6(2) . . ? C1 N1 Fe1 132.7(2) . . ? C1 N1 N2 105.6(3) . . ? C45 N16 Fe2 119.1(2) . . ? C49 N16 Fe2 119.4(2) . . ? C49 N16 C45 121.2(3) . . ? N3 N4 B1 119.9(3) . . ? C6 N4 N3 109.8(3) . . ? C6 N4 B1 130.2(3) . . ? N19 N20 B4 118.5(3) . . ? C55 N20 N19 109.1(3) . . ? C55 N20 B4 130.9(3) . . ? N7 N6 Fe1 118.8(2) . . ? C19 N6 Fe1 135.3(3) . . ? C19 N6 N7 105.9(3) . . ? N8 N9 B2 116.8(3) . . ? C24 N9 N8 108.6(3) . . ? C24 N9 B2 134.5(3) . . ? N1 N2 B1 116.8(3) . . ? C3 N2 N1 109.6(3) . . ? C3 N2 B1 132.5(3) . . ? N14 N15 B3 115.9(3) . . ? C37 N15 N14 109.3(3) . . ? C37 N15 B3 134.7(3) . . ? N16 C45 C46 119.2(3) . . ? N16 C45 B3 119.0(3) . . ? C46 C45 B3 121.7(3) . . ? N5 C14 C15 119.2(3) . . ? N5 C14 B1 118.1(3) . . ? C15 C14 B1 122.2(3) . . ? C57 C56 C61 114.6(3) . . ? C57 C56 B4 126.8(3) . . ? C61 C56 B4 118.3(3) . . ? N5 C18 C17 119.9(3) . . ? N5 C18 B2 118.3(3) . . ? C17 C18 B2 121.4(3) . . ? N16 C49 C48 119.2(3) . . ? N16 C49 B4 118.6(3) . . ? C48 C49 B4 122.2(3) . . ? N19 C53 C54 111.1(3) . . ? N14 C35 C36 111.7(3) . . ? N6 C19 C20 111.6(3) . . ? C16 C17 C18 120.3(3) . . ? N2 C3 C2 109.2(3) . . ? C8 C7 C12 114.7(3) . . ? C8 C7 B1 123.2(3) . . ? C12 C7 B1 121.9(3) . . ? C16 C15 C14 120.8(3) . . ? C47 C46 C45 120.9(3) . . ? C19 C20 C21 104.0(3) . . ? N1 C1 C2 111.5(3) . . ? C47 C48 C49 120.8(3) . . ? C27 C26 C25 123.3(4) . . ? C26 C25 B2 119.0(3) . . ? C30 C25 C26 114.8(4) . . ? C30 C25 B2 126.2(3) . . ? N3 C4 C5 111.3(3) . . ? N17 C50 C51 111.4(4) . . ? N12 C32 C33 110.9(3) . . ? N20 C55 C54 109.1(3) . . ? C55 C54 C53 104.4(3) . . ? N18 C52 C51 109.4(3) . . ? N8 C22 C23 111.2(4) . . ? N9 C24 C23 109.6(3) . . ? N7 C21 C20 109.2(3) . . ? C59 C58 C57 121.9(3) . . ? C9 C8 C7 122.8(4) . . ? C6 C5 C4 104.4(3) . . ? C43 C38 B3 124.1(3) . . ? C39 C38 C43 114.1(3) . . ? C39 C38 B3 121.7(3) . . ? C58 C57 C56 121.9(4) . . ? C42 C43 C38 123.0(4) . . ? C48 C47 C46 118.7(3) . . ? C15 C16 C17 118.8(3) . . ? N15 C37 C36 109.0(3) . . ? N4 C6 C5 108.6(3) . . ? C25 C30 C29 122.0(4) . . ? C34 C33 C32 105.0(3) . . ? C43 C42 C41 121.8(4) . . ? N13 C34 C33 109.0(3) . . ? C58 C59 C60 117.3(3) . . ? C58 C59 C62 122.1(4) . . ? C60 C59 C62 120.6(4) . . ? C60 C61 C56 123.5(3) . . ? C52 C51 C50 104.2(3) . . ? C9 C10 C13 120.2(4) . . ? C11 C10 C9 117.1(3) . . ? C11 C10 C13 122.7(4) . . ? C42 C41 C40 116.4(3) . . ? C42 C41 C44 121.8(4) . . ? C40 C41 C44 121.8(4) . . ? C24 C23 C22 104.4(3) . . ? C3 C2 C1 104.1(3) . . ? C26 C27 C28 120.5(4) . . ? C37 C36 C35 103.9(4) . . ? C61 C60 C59 120.6(4) . . ? C40 C39 C38 122.5(4) . . ? C28 C29 C30 121.5(4) . . ? C10 C9 C8 121.0(4) . . ? C27 C28 C31 120.7(4) . . ? C29 C28 C27 117.4(4) . . ? C29 C28 C31 121.8(4) . . ? C11 C12 C7 122.5(4) . . ? C41 C40 C39 121.5(4) . . ? N7 B2 C18 111.0(3) . . ? N7 B2 C25 107.3(3) . . ? N9 B2 N7 104.1(3) . . ? N9 B2 C18 103.1(3) . . ? N9 B2 C25 117.0(3) . . ? C25 B2 C18 113.9(3) . . ? C10 C11 C12 121.5(4) . . ? N4 B1 N2 104.4(3) . . ? N4 B1 C14 110.9(3) . . ? N4 B1 C7 107.7(3) . . ? N2 B1 C14 102.6(3) . . ? N2 B1 C7 114.4(3) . . ? C14 B1 C7 116.2(3) . . ? N13 B3 N15 103.4(3) . . ? N13 B3 C45 109.7(3) . . ? N13 B3 C38 110.6(3) . . ? N15 B3 C45 106.4(3) . . ? N15 B3 C38 113.6(3) . . ? C45 B3 C38 112.6(3) . . ? N18 B4 N20 102.4(3) . . ? N18 B4 C56 116.3(3) . . ? N18 B4 C49 107.9(3) . . ? N20 B4 C56 110.2(3) . . ? N20 B4 C49 108.7(3) . . ? C56 B4 C49 110.8(3) . . ? C3S C1S C2S 119.8(5) 2 . ? C1S C3S C2S 119.7(5) 2 . ? C1S C2S C3S 120.5(5) . . ? _shelx_res_file ; TITL ln634-partial_a.res in P-1 ln634.res created by SHELXL-2018/3 at 14:47:16 on 23-Aug-2019 REM Old TITL LN634-partial in P-1 REM SHELXT solution in P-1: R1 0.134, Rweak 0.005, Alpha 0.065 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C65 B4 N20 Fe2 CELL 1.54178 12.5636 13.684 20.5835 98.128 100.359 115.218 ZERR 2 0.0009 0.001 0.0017 0.005 0.005 0.005 LATT 1 SFAC C H B Fe N UNIT 130 126 8 4 40 SADI N10 H10 N11 H11 SADI H10 N11 N10 H11 L.S. 10 PLAN 5 SIZE 0.04 0.06 0.25 TEMP -100.15 BOND list 4 fmap 2 53 acta REM REM REM WGHT 0.081500 0.143500 FVAR 0.11074 FE1 4 0.440046 0.491524 0.303210 11.00000 0.01669 0.01684 = 0.02166 0.00383 0.00551 0.00959 FE2 4 0.752595 0.471756 0.208940 11.00000 0.01642 0.01661 = 0.02258 0.00373 0.00592 0.00914 N17 5 0.886313 0.627612 0.255641 11.00000 0.02026 0.02271 = 0.02247 0.00254 0.00335 0.01247 N7 5 0.363683 0.371954 0.405240 11.00000 0.02408 0.01813 = 0.02489 0.00688 0.01008 0.00936 N19 5 0.733087 0.534956 0.128283 11.00000 0.02030 0.01988 = 0.02407 0.00493 0.00788 0.01014 N5 5 0.314580 0.529890 0.333719 11.00000 0.01940 0.02013 = 0.02242 0.00348 0.00514 0.01117 N14 5 0.778345 0.410534 0.289363 11.00000 0.01768 0.02232 = 0.02712 0.00875 0.00655 0.01192 N18 5 0.967004 0.686715 0.221730 11.00000 0.01805 0.01589 = 0.03001 0.00303 0.00606 0.00763 N11 5 0.637107 0.508437 0.241798 11.00000 0.01882 0.01788 = 0.02256 0.00582 0.00514 0.00691 N3 5 0.566909 0.642085 0.351234 11.00000 0.02460 0.01848 = 0.01925 0.00552 0.00643 0.01068 N13 5 0.630847 0.227839 0.164866 11.00000 0.02026 0.01502 = 0.03078 0.00425 0.00894 0.00773 N8 5 0.306356 0.334099 0.258865 11.00000 0.02200 0.02171 = 0.02396 0.00330 0.00880 0.01104 N12 5 0.622402 0.322356 0.158107 11.00000 0.01997 0.02051 = 0.02530 0.00422 0.00712 0.01103 N10 5 0.552703 0.455498 0.270021 11.00000 0.02119 0.02064 = 0.02036 0.00508 0.00367 0.01099 N1 5 0.410995 0.551830 0.222064 11.00000 0.01759 0.02119 = 0.02672 0.00408 0.00426 0.01135 N16 5 0.872505 0.430994 0.179046 11.00000 0.01847 0.01912 = 0.02243 0.00348 0.00437 0.01059 N4 5 0.547494 0.731845 0.347715 11.00000 0.02313 0.01513 = 0.02879 0.00337 0.00652 0.00777 N20 5 0.832754 0.593361 0.106209 11.00000 0.01984 0.02090 = 0.02714 0.00574 0.00888 0.00927 N6 5 0.463478 0.433461 0.384387 11.00000 0.01965 0.01858 = 0.02691 0.00713 0.00615 0.01033 N9 5 0.219747 0.278048 0.290876 11.00000 0.01661 0.02330 = 0.02857 0.00595 0.00517 0.00639 N2 5 0.414086 0.654247 0.228999 11.00000 0.02254 0.02217 = 0.02871 0.00773 0.00803 0.01256 N15 5 0.766276 0.304930 0.282330 11.00000 0.02288 0.02092 = 0.03161 0.01019 0.00832 0.01131 C45 1 0.866996 0.330023 0.184317 11.00000 0.01918 0.01930 = 0.02568 0.00518 0.00510 0.01027 C14 1 0.310073 0.624604 0.322057 11.00000 0.02521 0.02520 = 0.02082 0.00327 0.00448 0.01612 C56 1 1.066321 0.691143 0.115444 11.00000 0.02102 0.01743 = 0.02823 0.00868 0.00706 0.01015 C18 1 0.221260 0.450999 0.350417 11.00000 0.02140 0.02121 = 0.02255 0.00281 0.00788 0.00939 C49 1 0.965831 0.507525 0.160180 11.00000 0.01797 0.01996 = 0.02104 0.00309 0.00614 0.00844 C53 1 0.639448 0.540507 0.089482 11.00000 0.01876 0.02909 = 0.02826 0.00598 0.00433 0.01228 AFIX 43 H53 2 0.558238 0.506857 0.093637 11.00000 -1.20000 AFIX 0 C35 1 0.796524 0.449888 0.355165 11.00000 0.02774 0.02888 = 0.02609 0.00407 0.00665 0.01586 AFIX 43 H35 2 0.809144 0.522435 0.374707 11.00000 -1.20000 AFIX 0 C19 1 0.559095 0.436723 0.427329 11.00000 0.02436 0.02391 = 0.02887 0.00497 0.00267 0.01482 AFIX 43 H19 2 0.640921 0.473819 0.424549 11.00000 -1.20000 AFIX 0 C17 1 0.113766 0.459650 0.348596 11.00000 0.02194 0.03007 = 0.03023 0.00558 0.01030 0.01311 AFIX 43 H17 2 0.047374 0.403019 0.358999 11.00000 -1.20000 AFIX 0 C3 1 0.386742 0.672186 0.167458 11.00000 0.02479 0.02337 = 0.03273 0.01117 0.00837 0.01365 AFIX 43 H3 2 0.381700 0.736746 0.158956 11.00000 -1.20000 AFIX 0 C7 1 0.431140 0.837459 0.308078 11.00000 0.02579 0.02137 = 0.02814 0.00371 0.00395 0.01403 C15 1 0.202359 0.632684 0.319565 11.00000 0.02897 0.02622 = 0.03339 0.00818 0.01114 0.01863 AFIX 43 H15 2 0.197357 0.696371 0.309267 11.00000 -1.20000 AFIX 0 C46 1 0.959604 0.307055 0.171524 11.00000 0.02880 0.02709 = 0.03625 0.01002 0.01167 0.01930 AFIX 43 H46 2 0.954658 0.236283 0.173281 11.00000 -1.20000 AFIX 0 C20 1 0.524327 0.379700 0.476055 11.00000 0.02694 0.02883 = 0.02860 0.00598 0.00306 0.01524 AFIX 43 H20 2 0.574796 0.370537 0.512451 11.00000 -1.20000 AFIX 0 C1 1 0.382850 0.509767 0.155100 11.00000 0.02326 0.02486 = 0.02365 -0.00049 0.00405 0.01340 AFIX 43 H1 2 0.374697 0.439083 0.135179 11.00000 -1.20000 AFIX 0 C48 1 1.060851 0.485285 0.149772 11.00000 0.01949 0.02724 = 0.03411 0.00728 0.01024 0.01111 AFIX 43 H48 2 1.127574 0.539375 0.138089 11.00000 -1.20000 AFIX 0 C26 1 0.110555 0.329301 0.455504 11.00000 0.02903 0.02540 = 0.02788 0.00649 0.00588 0.01096 AFIX 43 H26 2 0.152897 0.408415 0.467069 11.00000 -1.20000 AFIX 0 C25 1 0.137856 0.271057 0.404575 11.00000 0.02129 0.02768 = 0.02954 0.00660 0.00622 0.01084 C4 1 0.679736 0.682574 0.391648 11.00000 0.02079 0.02456 = 0.03011 0.00833 0.00693 0.01170 AFIX 43 H4 2 0.718046 0.638309 0.403135 11.00000 -1.20000 AFIX 0 C50 1 0.900282 0.700635 0.310409 11.00000 0.02868 0.02792 = 0.02710 0.00293 0.00831 0.01582 AFIX 43 H50 2 0.855489 0.682428 0.343305 11.00000 -1.20000 AFIX 0 C32 1 0.509492 0.288190 0.118279 11.00000 0.02444 0.02739 = 0.03019 0.00536 0.00865 0.01539 AFIX 43 H32 2 0.478384 0.336588 0.104748 11.00000 -1.20000 AFIX 0 C55 1 0.799217 0.633850 0.054859 11.00000 0.03160 0.02531 = 0.02761 0.01050 0.01219 0.01244 AFIX 43 H55 2 0.852002 0.677650 0.030977 11.00000 -1.20000 AFIX 0 C54 1 0.676319 0.601773 0.042395 11.00000 0.02705 0.03139 = 0.03022 0.00812 0.00354 0.01314 AFIX 43 H54 2 0.627682 0.617988 0.009010 11.00000 -1.20000 AFIX 0 C52 1 1.027065 0.794418 0.256170 11.00000 0.02584 0.02040 = 0.04725 0.00149 0.01206 0.00409 AFIX 43 H52 2 1.086854 0.852720 0.242787 11.00000 -1.20000 AFIX 0 C22 1 0.279128 0.264885 0.199010 11.00000 0.03056 0.02428 = 0.02638 0.00429 0.00996 0.01494 AFIX 43 H22 2 0.325711 0.281038 0.166775 11.00000 -1.20000 AFIX 0 C24 1 0.139221 0.178614 0.248566 11.00000 0.02105 0.02040 = 0.03550 0.00366 0.00503 0.00550 AFIX 43 H24 2 0.068981 0.125162 0.257962 11.00000 -1.20000 AFIX 0 C21 1 0.399292 0.338928 0.459846 11.00000 0.03303 0.02826 = 0.02890 0.01040 0.01173 0.01652 AFIX 43 H21 2 0.346681 0.294499 0.483567 11.00000 -1.20000 AFIX 0 C58 1 1.262995 0.835659 0.112221 11.00000 0.02301 0.02316 = 0.03689 0.01077 0.00789 0.00455 AFIX 43 H58 2 1.334668 0.903209 0.135143 11.00000 -1.20000 AFIX 0 C8 1 0.490816 0.910100 0.270347 11.00000 0.02937 0.02843 = 0.03350 0.00534 0.01120 0.01518 AFIX 43 H8 2 0.529226 0.887160 0.240042 11.00000 -1.20000 AFIX 0 C5 1 0.733623 0.797240 0.414622 11.00000 0.02285 0.02307 = 0.02956 0.00342 0.00300 0.00315 AFIX 43 H5 2 0.812787 0.845587 0.444006 11.00000 -1.20000 AFIX 0 C38 1 0.756164 0.123930 0.205189 11.00000 0.02742 0.02050 = 0.03920 0.01313 0.01674 0.01323 C57 1 1.176249 0.787586 0.147125 11.00000 0.02593 0.02840 = 0.02546 0.00509 0.00613 0.01202 AFIX 43 H57 2 1.192269 0.821320 0.193800 11.00000 -1.20000 AFIX 0 C43 1 0.817260 0.098732 0.259085 11.00000 0.02319 0.02273 = 0.04375 0.00268 0.00409 0.01135 AFIX 43 H43 2 0.866187 0.156043 0.299371 11.00000 -1.20000 AFIX 0 C47 1 1.059012 0.385682 0.156251 11.00000 0.01992 0.03305 = 0.04093 0.00733 0.00922 0.01554 AFIX 43 H47 2 1.124782 0.371429 0.150331 11.00000 -1.20000 AFIX 0 C16 1 0.103771 0.549857 0.331795 11.00000 0.02489 0.03757 = 0.03516 0.00858 0.01039 0.02196 AFIX 43 H16 2 0.029836 0.554600 0.328735 11.00000 -1.20000 AFIX 0 C37 1 0.774172 0.280853 0.343239 11.00000 0.03783 0.03420 = 0.03394 0.01664 0.01739 0.02305 AFIX 43 H37 2 0.766755 0.212043 0.351659 11.00000 -1.20000 AFIX 0 C6 1 0.646916 0.825438 0.385389 11.00000 0.03165 0.02034 = 0.02851 0.00408 0.00337 0.00878 AFIX 43 H6 2 0.655687 0.898823 0.390860 11.00000 -1.20000 AFIX 0 C30 1 0.080902 0.155755 0.395318 11.00000 0.03455 0.02741 = 0.03207 0.00643 0.00997 0.01264 AFIX 43 H30 2 0.100689 0.111983 0.364362 11.00000 -1.20000 AFIX 0 C33 1 0.445071 0.173560 0.099766 11.00000 0.02182 0.02774 = 0.03352 -0.00223 0.00517 0.00573 AFIX 43 H33 2 0.364048 0.128883 0.071664 11.00000 -1.20000 AFIX 0 C42 1 0.809573 -0.005533 0.256289 11.00000 0.02695 0.02985 = 0.03973 0.00957 0.00434 0.01659 AFIX 43 H42 2 0.850632 -0.018246 0.295113 11.00000 -1.20000 AFIX 0 C34 1 0.523215 0.138085 0.130676 11.00000 0.02541 0.01797 = 0.03487 0.00378 0.01157 0.00568 AFIX 43 H34 2 0.504837 0.062584 0.128476 11.00000 -1.20000 AFIX 0 C59 1 1.247852 0.788141 0.045542 11.00000 0.02525 0.03214 = 0.03426 0.01555 0.01115 0.01316 C61 1 1.052941 0.646137 0.047201 11.00000 0.02289 0.02624 = 0.03653 0.00050 0.00488 0.00710 AFIX 43 H61 2 0.979116 0.581483 0.022839 11.00000 -1.20000 AFIX 0 C51 1 0.988634 0.806961 0.313513 11.00000 0.02989 0.02428 = 0.04214 -0.00491 0.00915 0.00833 AFIX 43 H51 2 1.016177 0.873329 0.347646 11.00000 -1.20000 AFIX 0 C10 1 0.442166 1.052441 0.318925 11.00000 0.03305 0.02060 = 0.04847 0.00573 0.00538 0.01455 C41 1 0.743825 -0.091861 0.198597 11.00000 0.03036 0.02656 = 0.04100 0.00861 0.01179 0.01769 C23 1 0.174017 0.166241 0.189858 11.00000 0.03112 0.02348 = 0.03444 -0.00204 0.00443 0.00875 AFIX 43 H23 2 0.134935 0.104079 0.151513 11.00000 -1.20000 AFIX 0 C2 1 0.367019 0.582224 0.118291 11.00000 0.02980 0.03561 = 0.02052 0.00685 0.00897 0.01768 AFIX 43 H2 2 0.347155 0.572159 0.070251 11.00000 -1.20000 AFIX 0 C27 1 0.025192 0.277193 0.489576 11.00000 0.02819 0.04290 = 0.02365 0.00316 0.00505 0.01217 AFIX 43 H27 2 0.009515 0.320674 0.523133 11.00000 -1.20000 AFIX 0 C36 1 0.794865 0.372245 0.391952 11.00000 0.04411 0.04563 = 0.02534 0.01360 0.01253 0.02832 AFIX 43 H36 2 0.805479 0.379972 0.439601 11.00000 -1.20000 AFIX 0 C60 1 1.141086 0.690593 0.013519 11.00000 0.03332 0.03311 = 0.02758 0.00041 0.01141 0.01179 AFIX 43 H60 2 1.128603 0.654078 -0.032069 11.00000 -1.20000 AFIX 0 C39 1 0.699842 0.038728 0.145051 11.00000 0.04180 0.03818 = 0.03366 0.01189 0.01414 0.02669 AFIX 43 H39 2 0.664948 0.053111 0.104921 11.00000 -1.20000 AFIX 0 C29 1 -0.004338 0.102563 0.430123 11.00000 0.03764 0.02347 = 0.03796 0.00706 0.00748 0.00354 AFIX 43 H29 2 -0.040184 0.023817 0.422707 11.00000 -1.20000 AFIX 0 C9 1 0.496438 1.014681 0.275234 11.00000 0.03937 0.02588 = 0.03400 0.01029 0.01004 0.01383 AFIX 43 H9 2 0.537990 1.060973 0.248308 11.00000 -1.20000 AFIX 0 C28 1 -0.037749 0.161816 0.475099 11.00000 0.02901 0.03857 = 0.02963 0.00846 0.00839 0.00646 C12 1 0.386292 0.881468 0.355392 11.00000 0.04866 0.02952 = 0.04390 0.01086 0.02636 0.01789 AFIX 43 H12 2 0.351021 0.838480 0.385386 11.00000 -1.20000 AFIX 0 C40 1 0.693086 -0.066147 0.141886 11.00000 0.04258 0.03356 = 0.03929 0.00301 0.00900 0.02536 AFIX 43 H40 2 0.652900 -0.121367 0.100032 11.00000 -1.20000 AFIX 0 C44 1 0.726020 -0.208667 0.197562 11.00000 0.04473 0.02473 = 0.05561 0.00371 0.00349 0.02213 AFIX 137 H44A 2 0.783703 -0.221783 0.175911 11.00000 -1.50000 H44B 2 0.642303 -0.262710 0.171766 11.00000 -1.50000 H44C 2 0.740520 -0.217165 0.244339 11.00000 -1.50000 AFIX 0 C62 1 1.345564 0.835490 0.009057 11.00000 0.03880 0.05333 = 0.03960 0.01823 0.02014 0.01551 AFIX 137 H62A 2 1.367934 0.914168 0.011828 11.00000 -1.50000 H62B 2 1.314497 0.794119 -0.038843 11.00000 -1.50000 H62C 2 1.417646 0.828897 0.030516 11.00000 -1.50000 AFIX 0 B2 3 0.231513 0.340776 0.363642 11.00000 0.02155 0.02114 = 0.02654 0.00433 0.00447 0.00942 C11 1 0.391277 0.985914 0.360301 11.00000 0.04681 0.02849 = 0.06498 0.00177 0.02993 0.02036 AFIX 43 H11A 2 0.358682 1.011728 0.393065 11.00000 -1.20000 AFIX 0 B1 3 0.424103 0.715669 0.302821 11.00000 0.02295 0.02174 = 0.02890 0.00605 0.00667 0.01438 B3 3 0.756211 0.243861 0.208766 11.00000 0.02429 0.02569 = 0.03558 0.01214 0.01216 0.01515 C13 1 0.442660 1.163395 0.320465 11.00000 0.05512 0.02822 = 0.07878 0.01180 0.01440 0.02682 AFIX 137 H13A 2 0.526415 1.221427 0.327358 11.00000 -1.50000 H13B 2 0.410522 1.181505 0.357872 11.00000 -1.50000 H13C 2 0.391363 1.159192 0.277164 11.00000 -1.50000 AFIX 0 B4 3 0.962866 0.622899 0.150953 11.00000 0.02133 0.02148 = 0.02652 0.00293 0.00621 0.01063 C31 1 -0.140162 0.104318 0.506741 11.00000 0.04775 0.05054 = 0.04367 0.00655 0.01891 0.00343 AFIX 137 H31A 2 -0.131187 0.155670 0.548112 11.00000 -1.50000 H31B 2 -0.136987 0.038417 0.518371 11.00000 -1.50000 H31C 2 -0.218744 0.081571 0.474265 11.00000 -1.50000 AFIX 0 C1S 1 -0.087646 0.022922 0.020072 11.00000 0.04283 0.04502 = 0.07291 0.00414 0.01005 0.02236 AFIX 43 H1S 2 -0.148016 0.038538 0.034024 11.00000 -1.20000 AFIX 0 C3S 1 0.021096 -0.084149 0.019279 11.00000 0.04929 0.03192 = 0.07625 0.01420 0.00625 0.01853 AFIX 43 H3S 2 0.035462 -0.142067 0.032671 11.00000 -1.20000 AFIX 0 C2S 1 -0.066393 -0.061032 0.039134 11.00000 0.04854 0.05090 = 0.06700 0.01925 0.01635 0.01501 AFIX 43 H2S 2 -0.112463 -0.103354 0.066205 11.00000 -1.20000 AFIX 0 H10 2 0.545857 0.393823 0.272457 11.00000 -1.50000 H11 2 0.638274 0.565396 0.234286 11.00000 -1.50000 HKLF 4 REM ln634-partial_a.res in P-1 REM wR2 = 0.1502, GooF = S = 1.036, Restrained GooF = 1.036 for all data REM R1 = 0.0546 for 7603 Fo > 4sig(Fo) and 0.0888 for all 10913 data REM 830 parameters refined using 2 restraints END WGHT 0.0816 0.1321 REM Highest difference peak 0.573, deepest hole -0.485, 1-sigma level 0.073 Q1 1 0.1127 0.2646 0.1955 11.00000 0.05 0.57 Q2 1 0.4289 0.2342 0.1016 11.00000 0.05 0.50 Q3 1 0.7565 0.5410 0.1961 11.00000 0.05 0.41 Q4 1 0.7680 0.4739 0.2583 11.00000 0.05 0.41 Q5 1 0.8277 0.2925 0.1992 11.00000 0.05 0.40 ; _shelx_res_checksum 4357 _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_ln582red _database_code_depnum_ccdc_archive 'CCDC 2044411' loop_ _audit_author_name _audit_author_address 'Benjamin S. Gelfand' ;University of Calgary Canada ; _audit_update_record ; 2020-11-14 deposited with the CCDC. 2020-12-22 downloaded from the CCDC. ; _audit_creation_date 2019-04-24 _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 'F6 Sb, C31 H32 B2 Fe N10, C6 H6' _chemical_formula_sum 'C37 H38 B2 F6 Fe N10 Sb' _chemical_formula_weight 935.99 _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 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.0562 5.8946 '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 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.9800(2) _cell_length_b 25.1657(5) _cell_length_c 14.4893(3) _cell_angle_alpha 90 _cell_angle_beta 114.2040(10) _cell_angle_gamma 90 _cell_volume 3984.29(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9945 _cell_measurement_temperature 173 _cell_measurement_theta_max 71.811 _cell_measurement_theta_min 3.777 _shelx_estimated_absorpt_T_max 0.701 _shelx_estimated_absorpt_T_min 0.559 _exptl_absorpt_coefficient_mu 8.900 _exptl_absorpt_correction_T_max 0.7535 _exptl_absorpt_correction_T_min 0.6567 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0512 before and 0.0406 after correction. The Ratio of minimum to maximum transmission is 0.8715. 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 1.560 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1884 _exptl_crystal_size_max 0.074 _exptl_crystal_size_mid 0.059 _exptl_crystal_size_min 0.043 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_unetI/netI 0.0373 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 28060 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 70.065 _diffrn_reflns_theta_min 3.512 _diffrn_ambient_temperature 173 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source ? _diffrn_special_details ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6088 _reflns_number_total 7559 _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 1.416 _refine_diff_density_min -0.975 _refine_diff_density_rms 0.086 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 517 _refine_ls_number_reflns 7559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0447 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+4.0072P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1117 _refine_ls_wR_factor_ref 0.1195 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C1S(H1S), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S) 2.b Idealised Me refined as rotating group: N10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C) ; _atom_sites_solution_hydrogens geom _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 Sb1 Sb 0.78407(3) 0.49568(2) 0.63254(2) 0.04816(11) Uani 1 1 d . . . . . Fe1 Fe 0.46218(5) 0.66219(2) 0.69340(4) 0.02523(13) Uani 1 1 d . . . . . F1 F 0.7873(4) 0.52468(15) 0.7528(3) 0.0973(13) Uani 1 1 d . . . . . F2 F 0.6407(3) 0.53399(16) 0.5650(3) 0.0899(12) Uani 1 1 d . . . . . F3 F 0.8705(3) 0.55325(13) 0.6194(3) 0.0900(12) Uani 1 1 d . . . . . F4 F 0.6954(5) 0.43856(15) 0.6470(4) 0.131(2) Uani 1 1 d . . . . . F5 F 0.9272(4) 0.45824(19) 0.7021(3) 0.1125(16) Uani 1 1 d . . . . . F6 F 0.7741(3) 0.46670(11) 0.5105(2) 0.0578(7) Uani 1 1 d . . . . . N1 N 0.5738(3) 0.63795(11) 0.8275(2) 0.0284(6) Uani 1 1 d . . . . . N2 N 0.5507(3) 0.65098(12) 0.9089(2) 0.0290(6) Uani 1 1 d . . . . . N3 N 0.3251(3) 0.63810(12) 0.7281(2) 0.0305(6) Uani 1 1 d . . . . . N4 N 0.3236(3) 0.65091(12) 0.8190(2) 0.0297(6) Uani 1 1 d . . . . . N5 N 0.4479(3) 0.73419(11) 0.7475(2) 0.0268(6) Uani 1 1 d . . . . . N6 N 0.3534(3) 0.68642(12) 0.5547(2) 0.0292(6) Uani 1 1 d . . . . . N7 N 0.3651(3) 0.73572(12) 0.5203(2) 0.0302(6) Uani 1 1 d . . . . . N8 N 0.5962(3) 0.68560(12) 0.6608(2) 0.0297(6) Uani 1 1 d . . . . . N9 N 0.5915(3) 0.73502(12) 0.6211(2) 0.0304(6) Uani 1 1 d . . . . . N10 N 0.4665(3) 0.58951(12) 0.6374(2) 0.0329(7) Uani 1 1 d . . . . . H10A H 0.390937 0.581259 0.589571 0.039 Uiso 1 1 calc GR . . . . H10B H 0.488740 0.565175 0.688285 0.039 Uiso 1 1 calc GR . . . . H10C H 0.521630 0.589200 0.609089 0.039 Uiso 1 1 calc GR . . . . C1 C 0.6742(3) 0.60748(15) 0.8613(3) 0.0337(8) Uani 1 1 d . . . . . H1 H 0.710117 0.592212 0.819983 0.040 Uiso 1 1 calc R . . . . C2 C 0.7180(4) 0.60147(16) 0.9651(3) 0.0375(9) Uani 1 1 d . . . . . H2 H 0.788551 0.582388 1.008241 0.045 Uiso 1 1 calc R . . . . C3 C 0.6365(3) 0.62936(15) 0.9924(3) 0.0345(8) Uani 1 1 d . . . . . H3 H 0.640643 0.632611 1.059063 0.041 Uiso 1 1 calc R . . . . C4 C 0.2190(3) 0.61375(16) 0.6744(3) 0.0380(9) Uani 1 1 d . . . . . H4 H 0.196468 0.599566 0.608392 0.046 Uiso 1 1 calc R . . . . C5 C 0.1467(4) 0.61204(18) 0.7278(3) 0.0433(10) Uani 1 1 d . . . . . H5 H 0.066984 0.597346 0.706462 0.052 Uiso 1 1 calc R . . . . C6 C 0.2150(3) 0.63621(16) 0.8186(3) 0.0364(8) Uani 1 1 d . . . . . H6 H 0.190001 0.641674 0.872164 0.044 Uiso 1 1 calc R . . . . C7 C 0.4411(3) 0.69102(15) 1.0085(3) 0.0340(8) Uani 1 1 d . . . . . C8 C 0.3932(4) 0.65553(17) 1.0567(3) 0.0405(9) Uani 1 1 d . . . . . H8 H 0.340560 0.627892 1.018421 0.049 Uiso 1 1 calc R . . . . C9 C 0.4206(4) 0.65960(19) 1.1597(3) 0.0486(11) Uani 1 1 d . . . . . H9 H 0.384009 0.635470 1.189426 0.058 Uiso 1 1 calc R . . . . C10 C 0.4998(5) 0.6979(2) 1.2194(3) 0.0525(12) Uani 1 1 d . . . . . C11 C 0.5503(4) 0.73334(19) 1.1729(4) 0.0505(11) Uani 1 1 d . . . . . H11 H 0.605567 0.759949 1.212232 0.061 Uiso 1 1 calc R . . . . C12 C 0.5208(4) 0.73016(17) 1.0701(3) 0.0408(9) Uani 1 1 d . . . . . H12 H 0.555438 0.755174 1.040249 0.049 Uiso 1 1 calc R . . . . C13 C 0.5327(6) 0.7008(3) 1.3326(4) 0.0767(18) Uani 1 1 d . . . . . H13A H 0.458698 0.695929 1.344681 0.115 Uiso 1 1 calc GR . . . . H13B H 0.569011 0.735497 1.358508 0.115 Uiso 1 1 calc GR . . . . H13C H 0.591722 0.672678 1.367314 0.115 Uiso 1 1 calc GR . . . . C14 C 0.4268(3) 0.73740(14) 0.8326(3) 0.0287(7) Uani 1 1 d . . . . . C15 C 0.3855(4) 0.78542(15) 0.8554(3) 0.0366(8) Uani 1 1 d . . . . . H15 H 0.368696 0.787921 0.913931 0.044 Uiso 1 1 calc R . . . . C16 C 0.3687(4) 0.82911(16) 0.7943(3) 0.0401(9) Uani 1 1 d . . . . . H16 H 0.335729 0.861075 0.807564 0.048 Uiso 1 1 calc R . . . . C17 C 0.4006(3) 0.82564(15) 0.7131(3) 0.0352(8) Uani 1 1 d . . . . . H17 H 0.393845 0.856065 0.672302 0.042 Uiso 1 1 calc R . . . . C18 C 0.4427(3) 0.77791(14) 0.6904(3) 0.0287(7) Uani 1 1 d . . . . . C19 C 0.5007(3) 0.82491(14) 0.5455(3) 0.0319(8) Uani 1 1 d . . . . . C20 C 0.5720(4) 0.86471(16) 0.6115(3) 0.0402(9) Uani 1 1 d . . . . . H20 H 0.598839 0.859595 0.682372 0.048 Uiso 1 1 calc R . . . . C21 C 0.6044(4) 0.91083(16) 0.5775(4) 0.0437(10) Uani 1 1 d . . . . . H21 H 0.653167 0.936461 0.625036 0.052 Uiso 1 1 calc R . . . . C22 C 0.5670(4) 0.92046(15) 0.4750(3) 0.0389(9) Uani 1 1 d . . . . . C23 C 0.4985(4) 0.88149(16) 0.4082(3) 0.0388(9) Uani 1 1 d . . . . . H23 H 0.472062 0.886856 0.337501 0.047 Uiso 1 1 calc R . . . . C24 C 0.4680(3) 0.83500(15) 0.4429(3) 0.0348(8) Uani 1 1 d . . . . . H24 H 0.422967 0.808758 0.394969 0.042 Uiso 1 1 calc R . . . . C25 C 0.6024(5) 0.97115(18) 0.4386(4) 0.0555(12) Uani 1 1 d . . . . . H25A H 0.597101 0.966009 0.369904 0.083 Uiso 1 1 calc GR . . . . H25B H 0.686442 0.980710 0.483901 0.083 Uiso 1 1 calc GR . . . . H25C H 0.546696 0.999710 0.438421 0.083 Uiso 1 1 calc GR . . . . C26 C 0.2580(3) 0.66343(15) 0.4807(3) 0.0348(8) Uani 1 1 d . . . . . H26 H 0.230652 0.628199 0.482768 0.042 Uiso 1 1 calc R . . . . C27 C 0.2052(4) 0.69795(17) 0.4011(3) 0.0396(9) Uani 1 1 d . . . . . H27 H 0.135481 0.691689 0.339888 0.048 Uiso 1 1 calc R . . . . C28 C 0.2746(3) 0.74359(16) 0.4289(3) 0.0354(8) Uani 1 1 d . . . . . H28 H 0.260600 0.775201 0.389889 0.042 Uiso 1 1 calc R . . . . C29 C 0.6994(4) 0.66253(16) 0.6652(3) 0.0371(8) Uani 1 1 d . . . . . H29 H 0.725374 0.627580 0.689138 0.045 Uiso 1 1 calc R . . . . C30 C 0.7619(4) 0.69716(18) 0.6297(3) 0.0434(10) Uani 1 1 d . . . . . H30 H 0.837667 0.691060 0.624954 0.052 Uiso 1 1 calc R . . . . C31 C 0.6916(3) 0.74235(17) 0.6027(3) 0.0388(9) Uani 1 1 d . . . . . H31 H 0.710616 0.773671 0.575510 0.047 Uiso 1 1 calc R . . . . C1S C 0.3557(7) 0.4963(3) 0.8377(7) 0.085(2) Uani 1 1 d . . . . . H1S H 0.329227 0.509957 0.886459 0.102 Uiso 1 1 calc R . . . . C2S C 0.2731(7) 0.4751(3) 0.7505(7) 0.091(2) Uani 1 1 d . . . . . H2S H 0.188784 0.474115 0.737730 0.110 Uiso 1 1 calc R . . . . C3S C 0.3132(8) 0.4544(3) 0.6794(6) 0.094(2) Uani 1 1 d . . . . . H3S H 0.257046 0.439190 0.617897 0.112 Uiso 1 1 calc R . . . . C4S C 0.4376(7) 0.4569(2) 0.7016(6) 0.0806(19) Uani 1 1 d . . . . . H4S H 0.466622 0.443403 0.654335 0.097 Uiso 1 1 calc R . . . . C5S C 0.5177(6) 0.4783(2) 0.7893(6) 0.0750(17) Uani 1 1 d . . . . . H5S H 0.602544 0.479077 0.803841 0.090 Uiso 1 1 calc R . . . . C6S C 0.4774(7) 0.4984(2) 0.8559(6) 0.0774(17) Uani 1 1 d . . . . . H6S H 0.534013 0.514230 0.916498 0.093 Uiso 1 1 calc R . . . . B1 B 0.4337(4) 0.68381(17) 0.8961(3) 0.0313(9) Uani 1 1 d . . . . . B2 B 0.4743(4) 0.77076(17) 0.5924(3) 0.0313(9) 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 Sb1 0.05538(19) 0.03814(16) 0.05467(19) -0.01426(13) 0.02633(15) -0.00335(13) Fe1 0.0230(3) 0.0224(3) 0.0279(3) -0.0013(2) 0.0080(2) -0.0012(2) F1 0.152(4) 0.084(2) 0.072(2) -0.030(2) 0.063(2) 0.017(2) F2 0.0552(19) 0.097(3) 0.107(3) -0.019(2) 0.0225(19) 0.0250(18) F3 0.089(2) 0.062(2) 0.134(3) -0.033(2) 0.060(2) -0.0422(18) F4 0.208(5) 0.056(2) 0.210(5) -0.034(3) 0.170(5) -0.051(3) F5 0.122(3) 0.136(4) 0.064(2) 0.002(2) 0.023(2) 0.077(3) F6 0.0770(19) 0.0495(15) 0.0492(15) -0.0177(13) 0.0282(14) -0.0032(14) N1 0.0261(14) 0.0250(14) 0.0312(15) -0.0007(12) 0.0090(13) -0.0008(12) N2 0.0278(15) 0.0261(15) 0.0297(15) -0.0016(12) 0.0083(12) -0.0008(12) N3 0.0299(16) 0.0276(15) 0.0337(16) -0.0025(13) 0.0128(13) -0.0023(12) N4 0.0270(15) 0.0311(15) 0.0312(15) -0.0011(13) 0.0121(13) -0.0019(12) N5 0.0232(14) 0.0235(14) 0.0301(15) -0.0032(12) 0.0070(12) -0.0010(11) N6 0.0304(15) 0.0268(15) 0.0271(14) -0.0025(12) 0.0084(13) -0.0012(12) N7 0.0300(16) 0.0270(15) 0.0294(15) 0.0025(12) 0.0080(13) -0.0009(12) N8 0.0259(15) 0.0258(15) 0.0364(16) 0.0014(13) 0.0118(13) -0.0002(12) N9 0.0293(16) 0.0277(15) 0.0333(16) -0.0007(13) 0.0119(13) -0.0030(12) N10 0.0316(16) 0.0276(15) 0.0361(16) -0.0026(13) 0.0105(14) 0.0013(12) C1 0.0305(18) 0.0282(18) 0.039(2) 0.0012(16) 0.0109(16) 0.0037(14) C2 0.032(2) 0.0322(19) 0.039(2) 0.0029(17) 0.0057(17) 0.0064(15) C3 0.034(2) 0.0325(19) 0.0314(19) 0.0014(15) 0.0079(16) 0.0009(15) C4 0.032(2) 0.041(2) 0.036(2) -0.0056(17) 0.0100(17) -0.0109(17) C5 0.033(2) 0.050(2) 0.046(2) -0.002(2) 0.0148(19) -0.0103(18) C6 0.0297(19) 0.039(2) 0.042(2) 0.0007(17) 0.0162(17) -0.0029(16) C7 0.0328(19) 0.0342(19) 0.0333(19) 0.0005(16) 0.0120(16) 0.0078(16) C8 0.040(2) 0.040(2) 0.040(2) 0.0017(18) 0.0153(18) 0.0051(18) C9 0.057(3) 0.051(3) 0.043(2) 0.013(2) 0.026(2) 0.016(2) C10 0.059(3) 0.060(3) 0.035(2) 0.000(2) 0.015(2) 0.027(2) C11 0.055(3) 0.044(2) 0.042(2) -0.010(2) 0.008(2) 0.011(2) C12 0.042(2) 0.038(2) 0.037(2) -0.0004(17) 0.0100(18) 0.0054(17) C13 0.100(5) 0.091(4) 0.036(3) -0.006(3) 0.026(3) 0.027(4) C14 0.0227(17) 0.0297(18) 0.0300(17) -0.0047(15) 0.0072(15) -0.0012(13) C15 0.034(2) 0.036(2) 0.041(2) -0.0021(17) 0.0157(17) 0.0049(16) C16 0.041(2) 0.031(2) 0.046(2) 0.0003(17) 0.0150(19) 0.0100(16) C17 0.0328(19) 0.0283(18) 0.036(2) 0.0038(16) 0.0057(16) 0.0036(15) C18 0.0222(16) 0.0257(17) 0.0299(17) -0.0015(14) 0.0022(14) -0.0029(13) C19 0.0307(19) 0.0278(18) 0.0363(19) 0.0032(15) 0.0128(16) 0.0007(14) C20 0.041(2) 0.036(2) 0.041(2) 0.0023(18) 0.0136(18) -0.0026(17) C21 0.045(2) 0.032(2) 0.053(2) -0.0068(19) 0.020(2) -0.0075(17) C22 0.042(2) 0.0283(19) 0.056(3) 0.0088(18) 0.031(2) 0.0072(16) C23 0.036(2) 0.045(2) 0.042(2) 0.0062(18) 0.0217(18) 0.0077(17) C24 0.0347(19) 0.0321(19) 0.039(2) -0.0025(16) 0.0162(17) 0.0000(16) C25 0.068(3) 0.038(2) 0.076(3) 0.009(2) 0.046(3) 0.002(2) C26 0.033(2) 0.0307(19) 0.0338(19) -0.0045(16) 0.0069(16) -0.0025(15) C27 0.033(2) 0.042(2) 0.034(2) -0.0049(17) 0.0035(17) -0.0019(17) C28 0.032(2) 0.036(2) 0.0334(19) 0.0027(16) 0.0082(16) 0.0038(16) C29 0.035(2) 0.035(2) 0.043(2) 0.0016(17) 0.0171(18) 0.0038(16) C30 0.032(2) 0.050(2) 0.055(3) 0.001(2) 0.023(2) 0.0015(18) C31 0.0305(19) 0.041(2) 0.044(2) 0.0040(18) 0.0140(18) -0.0060(16) C1S 0.091(5) 0.072(4) 0.112(6) -0.005(4) 0.062(5) -0.002(4) C2S 0.067(4) 0.072(4) 0.135(7) 0.023(5) 0.041(5) -0.001(3) C3S 0.115(6) 0.050(4) 0.087(5) 0.014(3) 0.012(4) -0.024(4) C4S 0.115(6) 0.051(3) 0.093(5) 0.010(3) 0.060(5) 0.001(4) C5S 0.075(4) 0.061(3) 0.101(5) 0.021(4) 0.049(4) 0.007(3) C6S 0.090(5) 0.062(4) 0.084(4) 0.003(3) 0.040(4) -0.012(3) B1 0.029(2) 0.030(2) 0.034(2) -0.0027(17) 0.0117(18) 0.0009(16) B2 0.027(2) 0.030(2) 0.032(2) 0.0007(17) 0.0073(17) -0.0016(16) _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 Sb1 F1 1.875(3) . ? Sb1 F2 1.860(3) . ? Sb1 F3 1.835(3) . ? Sb1 F4 1.850(3) . ? Sb1 F5 1.851(4) . ? Sb1 F6 1.871(3) . ? Fe1 N1 1.951(3) . ? Fe1 N3 1.999(3) . ? Fe1 N5 2.009(3) . ? Fe1 N6 1.991(3) . ? Fe1 N8 1.942(3) . ? Fe1 N10 2.010(3) . ? N1 N2 1.357(4) . ? N1 C1 1.339(5) . ? N2 C3 1.340(5) . ? N2 B1 1.572(5) . ? N3 N4 1.363(4) . ? N3 C4 1.337(5) . ? N4 C6 1.350(5) . ? N4 B1 1.570(5) . ? N5 C14 1.359(5) . ? N5 C18 1.362(5) . ? N6 N7 1.366(4) . ? N6 C26 1.336(5) . ? N7 C28 1.338(5) . ? N7 B2 1.568(5) . ? N8 N9 1.362(4) . ? N8 C29 1.344(5) . ? N9 C31 1.344(5) . ? N9 B2 1.573(5) . ? C1 C2 1.383(6) . ? C2 C3 1.386(6) . ? C4 C5 1.379(6) . ? C5 C6 1.374(6) . ? C7 C8 1.394(6) . ? C7 C12 1.407(6) . ? C7 B1 1.605(5) . ? C8 C9 1.394(6) . ? C9 C10 1.380(7) . ? C10 C11 1.396(7) . ? C10 C13 1.523(6) . ? C11 C12 1.385(6) . ? C14 C15 1.397(5) . ? C14 B1 1.616(6) . ? C15 C16 1.374(6) . ? C16 C17 1.381(6) . ? C17 C18 1.393(5) . ? C18 B2 1.623(6) . ? C19 C20 1.406(5) . ? C19 C24 1.397(6) . ? C19 B2 1.611(5) . ? C20 C21 1.378(6) . ? C21 C22 1.385(6) . ? C22 C23 1.386(6) . ? C22 C25 1.506(6) . ? C23 C24 1.380(5) . ? C26 C27 1.373(6) . ? C27 C28 1.378(6) . ? C29 C30 1.379(6) . ? C30 C31 1.373(6) . ? C1S C2S 1.355(11) . ? C1S C6S 1.372(9) . ? C2S C3S 1.403(11) . ? C3S C4S 1.391(10) . ? C4S C5S 1.351(10) . ? C5S C6S 1.341(9) . ? 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 F2 Sb1 F1 87.13(18) . . ? F2 Sb1 F6 90.98(15) . . ? F3 Sb1 F1 89.52(19) . . ? F3 Sb1 F2 88.57(19) . . ? F3 Sb1 F4 178.82(17) . . ? F3 Sb1 F5 91.3(2) . . ? F3 Sb1 F6 91.72(15) . . ? F4 Sb1 F1 89.5(2) . . ? F4 Sb1 F2 90.7(2) . . ? F4 Sb1 F5 89.4(3) . . ? F4 Sb1 F6 89.25(17) . . ? F5 Sb1 F1 91.78(18) . . ? F5 Sb1 F2 178.89(17) . . ? F5 Sb1 F6 90.11(15) . . ? F6 Sb1 F1 177.72(17) . . ? N1 Fe1 N3 87.28(13) . . ? N1 Fe1 N5 91.54(12) . . ? N1 Fe1 N6 177.77(13) . . ? N1 Fe1 N10 89.82(12) . . ? N3 Fe1 N5 88.02(12) . . ? N3 Fe1 N10 89.14(13) . . ? N5 Fe1 N10 176.79(12) . . ? N6 Fe1 N3 94.69(13) . . ? N6 Fe1 N5 89.56(12) . . ? N6 Fe1 N10 89.18(13) . . ? N8 Fe1 N1 92.30(13) . . ? N8 Fe1 N3 179.56(13) . . ? N8 Fe1 N5 91.85(12) . . ? N8 Fe1 N6 85.72(13) . . ? N8 Fe1 N10 91.00(13) . . ? N2 N1 Fe1 119.3(2) . . ? C1 N1 Fe1 133.6(3) . . ? C1 N1 N2 107.1(3) . . ? N1 N2 B1 121.0(3) . . ? C3 N2 N1 109.4(3) . . ? C3 N2 B1 129.5(3) . . ? N4 N3 Fe1 120.6(2) . . ? C4 N3 Fe1 132.5(3) . . ? C4 N3 N4 106.6(3) . . ? N3 N4 B1 118.2(3) . . ? C6 N4 N3 109.0(3) . . ? C6 N4 B1 132.4(3) . . ? C14 N5 Fe1 119.0(2) . . ? C14 N5 C18 121.6(3) . . ? C18 N5 Fe1 118.8(2) . . ? N7 N6 Fe1 121.6(2) . . ? C26 N6 Fe1 131.9(3) . . ? C26 N6 N7 106.4(3) . . ? N6 N7 B2 116.8(3) . . ? C28 N7 N6 109.4(3) . . ? C28 N7 B2 133.8(3) . . ? N9 N8 Fe1 119.0(2) . . ? C29 N8 Fe1 133.9(3) . . ? C29 N8 N9 107.0(3) . . ? N8 N9 B2 120.8(3) . . ? C31 N9 N8 108.8(3) . . ? C31 N9 B2 129.9(3) . . ? N1 C1 C2 110.1(3) . . ? C1 C2 C3 104.9(3) . . ? N2 C3 C2 108.5(3) . . ? N3 C4 C5 110.7(4) . . ? C6 C5 C4 105.0(4) . . ? N4 C6 C5 108.7(4) . . ? C8 C7 C12 116.3(4) . . ? C8 C7 B1 125.0(4) . . ? C12 C7 B1 117.6(4) . . ? C9 C8 C7 121.6(4) . . ? C10 C9 C8 121.5(4) . . ? C9 C10 C11 117.8(4) . . ? C9 C10 C13 121.0(5) . . ? C11 C10 C13 121.2(5) . . ? C12 C11 C10 120.8(5) . . ? C11 C12 C7 122.0(4) . . ? N5 C14 C15 118.8(3) . . ? N5 C14 B1 118.9(3) . . ? C15 C14 B1 121.8(3) . . ? C16 C15 C14 120.8(4) . . ? C15 C16 C17 118.7(4) . . ? C16 C17 C18 120.6(4) . . ? N5 C18 C17 119.0(3) . . ? N5 C18 B2 118.2(3) . . ? C17 C18 B2 122.6(3) . . ? C20 C19 B2 119.0(3) . . ? C24 C19 C20 115.0(3) . . ? C24 C19 B2 125.8(3) . . ? C21 C20 C19 122.5(4) . . ? C20 C21 C22 121.1(4) . . ? C21 C22 C23 117.6(4) . . ? C21 C22 C25 120.6(4) . . ? C23 C22 C25 121.8(4) . . ? C24 C23 C22 121.0(4) . . ? C23 C24 C19 122.8(4) . . ? N6 C26 C27 110.3(3) . . ? C26 C27 C28 105.5(3) . . ? N7 C28 C27 108.2(3) . . ? N8 C29 C30 109.8(4) . . ? C31 C30 C29 105.4(4) . . ? N9 C31 C30 108.9(4) . . ? C2S C1S C6S 120.4(7) . . ? C1S C2S C3S 119.4(7) . . ? C4S C3S C2S 118.0(7) . . ? C5S C4S C3S 121.1(7) . . ? C6S C5S C4S 120.0(7) . . ? C5S C6S C1S 121.0(7) . . ? N2 B1 C7 105.3(3) . . ? N2 B1 C14 109.9(3) . . ? N4 B1 N2 104.8(3) . . ? N4 B1 C7 117.6(3) . . ? N4 B1 C14 101.7(3) . . ? C7 B1 C14 116.9(3) . . ? N7 B2 N9 105.4(3) . . ? N7 B2 C18 102.5(3) . . ? N7 B2 C19 116.7(3) . . ? N9 B2 C18 109.5(3) . . ? N9 B2 C19 106.7(3) . . ? C19 B2 C18 115.6(3) . . ? _shelx_res_file ; TITL ln582red_a.res in P2(1)/n ln582red.res created by SHELXL-2018/3 at 09:18:55 on 24-Apr-2019 REM Old TITL LN582red in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.309, Rweak 0.018, Alpha 0.036 REM 0.454 for 201 systematic absences, Orientation as input REM Formula found by SHELXT: C37 B2 N10 F7 Sb CELL 1.54178 11.98 25.1657 14.4893 90 114.204 90 ZERR 4 0.0002 0.0005 0.0003 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H B F Fe N Sb UNIT 148 152 8 24 4 40 4 L.S. 20 PLAN 20 SIZE 0.043 0.059 0.074 TEMP -100.15 BOND list 4 fmap 2 53 ACTA REM REM REM WGHT 0.061700 4.007200 FVAR 0.27601 SB1 7 0.784071 0.495682 0.632540 11.00000 0.05538 0.03814 = 0.05467 -0.01426 0.02633 -0.00335 FE1 5 0.462180 0.662191 0.693396 11.00000 0.02298 0.02239 = 0.02793 -0.00128 0.00802 -0.00120 F1 4 0.787286 0.524676 0.752775 11.00000 0.15250 0.08392 = 0.07234 -0.02984 0.06312 0.01657 F2 4 0.640682 0.533987 0.564989 11.00000 0.05521 0.09701 = 0.10676 -0.01859 0.02247 0.02495 F3 4 0.870516 0.553248 0.619411 11.00000 0.08869 0.06156 = 0.13418 -0.03336 0.06025 -0.04219 F4 4 0.695383 0.438559 0.646992 11.00000 0.20807 0.05644 = 0.21032 -0.03440 0.17010 -0.05085 F5 4 0.927239 0.458238 0.702064 11.00000 0.12226 0.13585 = 0.06443 0.00216 0.02307 0.07666 F6 4 0.774060 0.466700 0.510489 11.00000 0.07705 0.04947 = 0.04918 -0.01768 0.02820 -0.00323 N1 6 0.573766 0.637948 0.827499 11.00000 0.02611 0.02503 = 0.03124 -0.00065 0.00904 -0.00078 N2 6 0.550699 0.650977 0.908875 11.00000 0.02777 0.02613 = 0.02972 -0.00156 0.00825 -0.00075 N3 6 0.325098 0.638101 0.728130 11.00000 0.02991 0.02756 = 0.03370 -0.00247 0.01279 -0.00228 N4 6 0.323591 0.650910 0.819013 11.00000 0.02697 0.03110 = 0.03121 -0.00113 0.01213 -0.00186 N5 6 0.447917 0.734193 0.747451 11.00000 0.02316 0.02347 = 0.03006 -0.00316 0.00700 -0.00098 N6 6 0.353391 0.686420 0.554654 11.00000 0.03041 0.02678 = 0.02709 -0.00248 0.00842 -0.00121 N7 6 0.365108 0.735718 0.520258 11.00000 0.02999 0.02704 = 0.02943 0.00253 0.00802 -0.00087 N8 6 0.596173 0.685604 0.660753 11.00000 0.02593 0.02579 = 0.03644 0.00142 0.01181 -0.00023 N9 6 0.591466 0.735025 0.621087 11.00000 0.02932 0.02765 = 0.03331 -0.00067 0.01193 -0.00296 N10 6 0.466457 0.589514 0.637429 11.00000 0.03164 0.02756 = 0.03607 -0.00264 0.01050 0.00128 AFIX 137 H10A 2 0.390937 0.581259 0.589571 11.00000 -1.20000 H10B 2 0.488740 0.565175 0.688285 11.00000 -1.20000 H10C 2 0.521630 0.589200 0.609089 11.00000 -1.20000 AFIX 0 C1 1 0.674175 0.607482 0.861285 11.00000 0.03046 0.02818 = 0.03917 0.00116 0.01093 0.00369 AFIX 43 H1 2 0.710117 0.592212 0.819983 11.00000 -1.20000 AFIX 0 C2 1 0.717994 0.601468 0.965100 11.00000 0.03231 0.03221 = 0.03924 0.00285 0.00575 0.00645 AFIX 43 H2 2 0.788551 0.582388 1.008241 11.00000 -1.20000 AFIX 0 C3 1 0.636463 0.629359 0.992401 11.00000 0.03414 0.03248 = 0.03140 0.00139 0.00786 0.00090 AFIX 43 H3 2 0.640643 0.632611 1.059063 11.00000 -1.20000 AFIX 0 C4 1 0.218990 0.613750 0.674366 11.00000 0.03234 0.04149 = 0.03617 -0.00557 0.00997 -0.01090 AFIX 43 H4 2 0.196468 0.599566 0.608392 11.00000 -1.20000 AFIX 0 C5 1 0.146710 0.612043 0.727791 11.00000 0.03316 0.04989 = 0.04558 -0.00229 0.01483 -0.01033 AFIX 43 H5 2 0.066984 0.597346 0.706462 11.00000 -1.20000 AFIX 0 C6 1 0.215025 0.636211 0.818577 11.00000 0.02974 0.03884 = 0.04212 0.00075 0.01621 -0.00294 AFIX 43 H6 2 0.190001 0.641674 0.872164 11.00000 -1.20000 AFIX 0 C7 1 0.441122 0.691019 1.008535 11.00000 0.03284 0.03423 = 0.03334 0.00052 0.01200 0.00784 C8 1 0.393206 0.655532 1.056712 11.00000 0.04022 0.04014 = 0.04014 0.00166 0.01531 0.00515 AFIX 43 H8 2 0.340560 0.627892 1.018421 11.00000 -1.20000 AFIX 0 C9 1 0.420636 0.659605 1.159667 11.00000 0.05689 0.05143 = 0.04309 0.01331 0.02624 0.01555 AFIX 43 H9 2 0.384009 0.635470 1.189426 11.00000 -1.20000 AFIX 0 C10 1 0.499827 0.697918 1.219379 11.00000 0.05862 0.05991 = 0.03504 0.00009 0.01519 0.02703 C11 1 0.550299 0.733335 1.172884 11.00000 0.05470 0.04401 = 0.04157 -0.01015 0.00822 0.01073 AFIX 43 H11 2 0.605567 0.759949 1.212232 11.00000 -1.20000 AFIX 0 C12 1 0.520806 0.730160 1.070094 11.00000 0.04187 0.03777 = 0.03681 -0.00037 0.01004 0.00543 AFIX 43 H12 2 0.555438 0.755174 1.040249 11.00000 -1.20000 AFIX 0 C13 1 0.532749 0.700759 1.332559 11.00000 0.10037 0.09147 = 0.03596 -0.00574 0.02552 0.02657 AFIX 137 H13A 2 0.458698 0.695929 1.344681 11.00000 -1.50000 H13B 2 0.569011 0.735497 1.358508 11.00000 -1.50000 H13C 2 0.591722 0.672678 1.367314 11.00000 -1.50000 AFIX 0 C14 1 0.426841 0.737396 0.832594 11.00000 0.02272 0.02972 = 0.03002 -0.00472 0.00717 -0.00119 C15 1 0.385451 0.785423 0.855421 11.00000 0.03378 0.03591 = 0.04055 -0.00209 0.01566 0.00489 AFIX 43 H15 2 0.368696 0.787921 0.913931 11.00000 -1.20000 AFIX 0 C16 1 0.368674 0.829108 0.794260 11.00000 0.04075 0.03108 = 0.04581 0.00025 0.01503 0.01005 AFIX 43 H16 2 0.335729 0.861075 0.807564 11.00000 -1.20000 AFIX 0 C17 1 0.400638 0.825637 0.713071 11.00000 0.03278 0.02826 = 0.03618 0.00377 0.00571 0.00361 AFIX 43 H17 2 0.393845 0.856065 0.672302 11.00000 -1.20000 AFIX 0 C18 1 0.442745 0.777913 0.690445 11.00000 0.02216 0.02570 = 0.02993 -0.00147 0.00224 -0.00286 C19 1 0.500713 0.824909 0.545498 11.00000 0.03070 0.02779 = 0.03629 0.00315 0.01283 0.00065 C20 1 0.571990 0.864705 0.611545 11.00000 0.04143 0.03555 = 0.04056 0.00234 0.01363 -0.00262 AFIX 43 H20 2 0.598839 0.859595 0.682372 11.00000 -1.20000 AFIX 0 C21 1 0.604380 0.910833 0.577453 11.00000 0.04521 0.03238 = 0.05316 -0.00682 0.01991 -0.00755 AFIX 43 H21 2 0.653167 0.936461 0.625036 11.00000 -1.20000 AFIX 0 C22 1 0.566993 0.920457 0.474965 11.00000 0.04236 0.02829 = 0.05626 0.00884 0.03052 0.00720 C23 1 0.498485 0.881490 0.408223 11.00000 0.03583 0.04472 = 0.04151 0.00618 0.02168 0.00769 AFIX 43 H23 2 0.472062 0.886856 0.337501 11.00000 -1.20000 AFIX 0 C24 1 0.468041 0.835000 0.442901 11.00000 0.03467 0.03212 = 0.03877 -0.00253 0.01618 0.00000 AFIX 43 H24 2 0.422967 0.808758 0.394969 11.00000 -1.20000 AFIX 0 C25 1 0.602399 0.971147 0.438625 11.00000 0.06786 0.03804 = 0.07648 0.00895 0.04556 0.00213 AFIX 137 H25A 2 0.597101 0.966009 0.369904 11.00000 -1.50000 H25B 2 0.686442 0.980710 0.483901 11.00000 -1.50000 H25C 2 0.546696 0.999710 0.438421 11.00000 -1.50000 AFIX 0 C26 1 0.258019 0.663425 0.480659 11.00000 0.03321 0.03067 = 0.03384 -0.00447 0.00692 -0.00252 AFIX 43 H26 2 0.230652 0.628199 0.482768 11.00000 -1.20000 AFIX 0 C27 1 0.205206 0.697952 0.401149 11.00000 0.03299 0.04163 = 0.03412 -0.00495 0.00349 -0.00191 AFIX 43 H27 2 0.135481 0.691689 0.339888 11.00000 -1.20000 AFIX 0 C28 1 0.274594 0.743593 0.428891 11.00000 0.03197 0.03559 = 0.03338 0.00267 0.00822 0.00381 AFIX 43 H28 2 0.260600 0.775201 0.389889 11.00000 -1.20000 AFIX 0 C29 1 0.699388 0.662530 0.665168 11.00000 0.03458 0.03524 = 0.04281 0.00161 0.01712 0.00381 AFIX 43 H29 2 0.725374 0.627580 0.689138 11.00000 -1.20000 AFIX 0 C30 1 0.761945 0.697161 0.629710 11.00000 0.03152 0.04954 = 0.05451 0.00134 0.02309 0.00147 AFIX 43 H30 2 0.837667 0.691060 0.624954 11.00000 -1.20000 AFIX 0 C31 1 0.691591 0.742347 0.602723 11.00000 0.03050 0.04065 = 0.04415 0.00405 0.01404 -0.00602 AFIX 43 H31 2 0.710616 0.773671 0.575510 11.00000 -1.20000 AFIX 0 C1S 1 0.355740 0.496343 0.837654 11.00000 0.09078 0.07231 = 0.11220 -0.00519 0.06162 -0.00245 AFIX 43 H1S 2 0.329227 0.509957 0.886459 11.00000 -1.20000 AFIX 0 C2S 1 0.273141 0.475060 0.750544 11.00000 0.06722 0.07214 = 0.13464 0.02332 0.04140 -0.00067 AFIX 43 H2S 2 0.188784 0.474115 0.737730 11.00000 -1.20000 AFIX 0 C3S 1 0.313204 0.454426 0.679419 11.00000 0.11455 0.05041 = 0.08713 0.01396 0.01212 -0.02417 AFIX 43 H3S 2 0.257046 0.439190 0.617897 11.00000 -1.20000 AFIX 0 C4S 1 0.437550 0.456934 0.701627 11.00000 0.11485 0.05146 = 0.09292 0.01030 0.06015 0.00100 AFIX 43 H4S 2 0.466622 0.443403 0.654335 11.00000 -1.20000 AFIX 0 C5S 1 0.517694 0.478284 0.789308 11.00000 0.07544 0.06052 = 0.10144 0.02079 0.04873 0.00684 AFIX 43 H5S 2 0.602544 0.479077 0.803841 11.00000 -1.20000 AFIX 0 C6S 1 0.477424 0.498369 0.855858 11.00000 0.08984 0.06193 = 0.08448 0.00315 0.03975 -0.01228 AFIX 43 H6S 2 0.534013 0.514230 0.916498 11.00000 -1.20000 AFIX 0 B1 3 0.433672 0.683808 0.896115 11.00000 0.02866 0.02953 = 0.03440 -0.00272 0.01169 0.00093 B2 3 0.474264 0.770758 0.592363 11.00000 0.02719 0.02955 = 0.03229 0.00065 0.00731 -0.00155 HKLF 4 REM ln582red_a.res in P2(1)/n REM wR2 = 0.1195, GooF = S = 1.040, Restrained GooF = 1.040 for all data REM R1 = 0.0447 for 6088 Fo > 4sig(Fo) and 0.0593 for all 7559 data REM 517 parameters refined using 0 restraints END WGHT 0.0617 4.0069 REM Highest difference peak 1.416, deepest hole -0.975, 1-sigma level 0.086 Q1 1 0.8622 0.4872 0.6269 11.00000 0.05 1.42 Q2 1 0.4513 0.5242 0.6674 11.00000 0.05 0.62 Q3 1 0.8041 0.4955 0.6956 11.00000 0.05 0.57 Q4 1 0.4868 0.8020 0.5639 11.00000 0.05 0.38 Q5 1 0.4571 0.7040 0.7209 11.00000 0.05 0.36 Q6 1 0.7643 0.4259 0.6549 11.00000 0.05 0.34 Q7 1 0.4697 0.7787 0.6430 11.00000 0.05 0.33 Q8 1 0.9425 0.5168 0.6412 11.00000 0.05 0.33 Q9 1 0.6360 0.4525 0.5743 11.00000 0.05 0.33 Q10 1 0.8531 0.4214 0.6722 11.00000 0.05 0.32 Q11 1 0.5101 0.6475 0.7050 11.00000 0.05 0.32 Q12 1 0.5166 0.8199 0.5021 11.00000 0.05 0.32 Q13 1 0.4957 0.5842 0.4889 11.00000 0.05 0.31 Q14 1 0.8479 0.4378 0.7042 11.00000 0.05 0.31 Q15 1 0.4025 0.7558 0.5482 11.00000 0.05 0.30 Q16 1 0.3173 0.6615 0.7023 11.00000 0.05 0.30 Q17 1 0.4645 0.6409 0.6552 11.00000 0.05 0.29 Q18 1 0.4622 0.5842 0.5713 11.00000 0.05 0.29 Q19 1 0.6196 0.9976 0.4920 11.00000 0.05 0.29 Q20 1 0.4284 0.7168 0.8548 11.00000 0.05 0.29 ; _shelx_res_checksum 71805 _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_ln512_0m_a _database_code_depnum_ccdc_archive 'CCDC 2044412' loop_ _audit_author_name _audit_author_address 'Benjamin S. Gelfand' ;University of Calgary Canada ; _audit_update_record ; 2020-11-14 deposited with the CCDC. 2020-12-22 downloaded from the CCDC. ; _audit_creation_date 2020-04-20 _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 'C31 H29 B2 Br Fe N9, 2(C6 H6)' _chemical_formula_sum 'C43 H41 B2 Br Fe N9' _chemical_formula_weight 841.23 _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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' _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 triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.252(5) _cell_length_b 12.025(5) _cell_length_c 18.400(8) _cell_angle_alpha 104.192(5) _cell_angle_beta 92.618(5) _cell_angle_gamma 112.901(5) _cell_volume 2000.3(15) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1687 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 19.741 _cell_measurement_theta_min 2.304 _shelx_estimated_absorpt_T_max 0.945 _shelx_estimated_absorpt_T_min 0.848 _exptl_absorpt_coefficient_mu 1.420 _exptl_absorpt_correction_T_max 0.9143 _exptl_absorpt_correction_T_min 0.8450 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0580 before and 0.0529 after correction. The Ratio of minimum to maximum transmission is 0.9242. 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 1.397 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 866 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1088 _diffrn_reflns_av_unetI/netI 0.1247 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 26732 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.998 _diffrn_reflns_theta_min 1.918 _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 4570 _reflns_number_total 7875 _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 v8.37A (Bruker, 2015)' _computing_data_collection ? _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _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 'olex2.solve (Bourhis et al., 2015)' _refine_diff_density_max 0.433 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.087 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 506 _refine_ls_number_reflns 7875 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1238 _refine_ls_R_factor_gt 0.0521 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0189P)^2^+1.2216P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.0964 _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 2.a Riding coordinates: C31(H31a,H31b,H31c) 2.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C29(H29), C30(H30), C1S(H1S), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S), C7S(H7S), C8S(H8S), C9S(H9S), C10S(H10S), C11S(H11S), C12S(H12S) 2.c Idealised Me refined as rotating group: C18(H18a,H18b,H18c) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _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 Br1 Br 0.23770(5) 0.50064(5) 0.51342(2) 0.02873(14) Uani 1 1 d . . . . . Fe1 Fe 0.30581(6) 0.56253(6) 0.65179(3) 0.01886(16) Uani 1 1 d . . . . . N1 N 0.3585(3) 0.6230(3) 0.77718(17) 0.0179(8) Uani 1 1 d . . . . . N2 N 0.3372(3) 0.3601(3) 0.70797(17) 0.0194(8) Uani 1 1 d . . . . . N3 N 0.3782(3) 0.4248(3) 0.65538(18) 0.0218(8) Uani 1 1 d . . . . . N4 N 0.0960(3) 0.3687(3) 0.71867(17) 0.0196(8) Uani 1 1 d . . . . . N5 N 0.1084(3) 0.4312(3) 0.66463(18) 0.0216(8) Uani 1 1 d . . . . . N6 N 0.5621(3) 0.8090(3) 0.70497(17) 0.0191(8) Uani 1 1 d . . . . . N7 N 0.5109(3) 0.6928(3) 0.65401(18) 0.0209(8) Uani 1 1 d . . . . . N8 N 0.3255(3) 0.8284(3) 0.71930(17) 0.0193(8) Uani 1 1 d . . . . . N9 N 0.2462(3) 0.7149(3) 0.66602(17) 0.0198(8) Uani 1 1 d . . . . . C1 C 0.3061(4) 0.5344(4) 0.8151(2) 0.0187(9) Uani 1 1 d . . . . . C2 C 0.3027(4) 0.5733(4) 0.8921(2) 0.0235(10) Uani 1 1 d . . . . . H2 H 0.263794 0.512187 0.918629 0.028 Uiso 1 1 calc R . . . . C3 C 0.3554(4) 0.7000(4) 0.9309(2) 0.0248(10) Uani 1 1 d . . . . . H3 H 0.351335 0.726504 0.983471 0.030 Uiso 1 1 calc R . . . . C4 C 0.4137(4) 0.7870(4) 0.8916(2) 0.0223(10) Uani 1 1 d . . . . . H4 H 0.452278 0.874357 0.917733 0.027 Uiso 1 1 calc R . . . . C5 C 0.4169(4) 0.7485(4) 0.8143(2) 0.0170(9) Uani 1 1 d . . . . . C6 C 0.4535(4) 0.3736(4) 0.6128(2) 0.0255(10) Uani 1 1 d . . . . . H6 H 0.494975 0.400491 0.571593 0.031 Uiso 1 1 calc R . . . . C7 C 0.4633(4) 0.2765(4) 0.6363(2) 0.0284(11) Uani 1 1 d . . . . . H7 H 0.510941 0.225046 0.615594 0.034 Uiso 1 1 calc R . . . . C8 C 0.3888(4) 0.2706(4) 0.6964(2) 0.0250(10) Uani 1 1 d . . . . . H8 H 0.375687 0.212724 0.725395 0.030 Uiso 1 1 calc R . . . . C9 C -0.0263(4) 0.4021(4) 0.6333(2) 0.0279(11) Uani 1 1 d . . . . . H9 H -0.050071 0.430957 0.593094 0.033 Uiso 1 1 calc R . . . . C10 C -0.1245(5) 0.3251(4) 0.6675(2) 0.0322(11) Uani 1 1 d . . . . . H10 H -0.226105 0.291900 0.656309 0.039 Uiso 1 1 calc R . . . . C11 C -0.0440(4) 0.3062(4) 0.7218(2) 0.0273(11) Uani 1 1 d . . . . . H11 H -0.081072 0.257323 0.755575 0.033 Uiso 1 1 calc R . . . . C12 C 0.2161(4) 0.2877(4) 0.8157(2) 0.0215(10) Uani 1 1 d . . . . . C13 C 0.1052(5) 0.1670(4) 0.7982(2) 0.0306(11) Uani 1 1 d . . . . . H13 H 0.031229 0.141184 0.756676 0.037 Uiso 1 1 calc R . . . . C14 C 0.1001(5) 0.0838(4) 0.8400(3) 0.0369(12) Uani 1 1 d . . . . . H14 H 0.021165 0.003665 0.827202 0.044 Uiso 1 1 calc R . . . . C15 C 0.2065(6) 0.1143(5) 0.8994(3) 0.0360(12) Uani 1 1 d . . . . . C16 C 0.3202(5) 0.2313(4) 0.9151(2) 0.0367(12) Uani 1 1 d . . . . . H16 H 0.397206 0.254136 0.954350 0.044 Uiso 1 1 calc R . . . . C17 C 0.3246(5) 0.3156(4) 0.8751(2) 0.0294(11) Uani 1 1 d . . . . . H17 H 0.404072 0.395408 0.888406 0.035 Uiso 1 1 calc R . . . . C18 C 0.2015(6) 0.0224(5) 0.9437(3) 0.0601(17) Uani 1 1 d . . . . . H18A H 0.174093 0.048452 0.993273 0.090 Uiso 1 1 calc GR . . . . H18B H 0.296317 0.021419 0.951060 0.090 Uiso 1 1 calc GR . . . . H18C H 0.130967 -0.062130 0.915552 0.090 Uiso 1 1 calc GR . . . . C19 C 0.6116(4) 0.6927(4) 0.6104(2) 0.0277(11) Uani 1 1 d . . . . . H19 H 0.603798 0.622911 0.569821 0.033 Uiso 1 1 calc R . . . . C20 C 0.7279(4) 0.8073(4) 0.6321(2) 0.0303(11) Uani 1 1 d . . . . . H20 H 0.813532 0.831891 0.610576 0.036 Uiso 1 1 calc R . . . . C21 C 0.6925(4) 0.8786(4) 0.6923(2) 0.0277(11) Uani 1 1 d . . . . . H21 H 0.751195 0.963352 0.720226 0.033 Uiso 1 1 calc R . . . . C22 C 0.1224(4) 0.7183(4) 0.6434(2) 0.0283(11) Uani 1 1 d . . . . . H22 H 0.047657 0.652869 0.605697 0.034 Uiso 1 1 calc R . . . . C23 C 0.1186(5) 0.8308(4) 0.6826(2) 0.0298(11) Uani 1 1 d . . . . . H23 H 0.042991 0.856796 0.677624 0.036 Uiso 1 1 calc R . . . . C24 C 0.2477(4) 0.8968(4) 0.7304(2) 0.0250(10) Uani 1 1 d . . . . . H24 H 0.277101 0.977714 0.765590 0.030 Uiso 1 1 calc R . . . . C25 C 0.5696(4) 0.9925(4) 0.8110(2) 0.0216(10) Uani 1 1 d . . . . . C26 C 0.5711(5) 1.0956(4) 0.7888(2) 0.0286(11) Uani 1 1 d . . . . . H26 H 0.501507 1.082076 0.747915 0.034 Uiso 1 1 calc R . . . . C27 C 0.6710(5) 1.2178(4) 0.8246(3) 0.0306(11) Uani 1 1 d . . . . . H27 H 0.666059 1.285704 0.808708 0.037 Uiso 1 1 calc R . . . . C28 C 0.7776(5) 1.2423(4) 0.8829(2) 0.0299(11) Uani 1 1 d . . . . . C29 C 0.7794(5) 1.1399(4) 0.9040(2) 0.0328(12) Uani 1 1 d . . . . . H29 H 0.851919 1.153175 0.943286 0.039 Uiso 1 1 calc R . . . . C30 C 0.6782(4) 1.0188(4) 0.8694(2) 0.0278(11) Uani 1 1 d . . . . . H30 H 0.682730 0.951315 0.885900 0.033 Uiso 1 1 calc R . . . . C31 C 0.8889(5) 1.3736(4) 0.9206(3) 0.0520(15) Uani 1 1 d . . . . . H31A H 0.899946 1.424020 0.886169 0.078 Uiso 1 1 d R . . . . H31B H 0.978716 1.370500 0.933990 0.078 Uiso 1 1 d R . . . . H31C H 0.858906 1.410160 0.965520 0.078 Uiso 1 1 d R . . . . B1 B 0.2382(5) 0.3862(4) 0.7671(2) 0.0190(11) Uani 1 1 d . . . . . B2 B 0.4701(5) 0.8479(4) 0.7651(2) 0.0177(11) Uani 1 1 d . . . . . C1S C 0.9539(5) 0.6379(5) 0.8071(3) 0.0428(13) Uani 1 1 d . . . . . H1S H 1.031540 0.629476 0.783666 0.051 Uiso 1 1 calc R . . . . C2S C 0.9681(5) 0.6782(4) 0.8849(3) 0.0407(13) Uani 1 1 d . . . . . H2S H 1.056051 0.698530 0.915451 0.049 Uiso 1 1 calc R . . . . C3S C 0.8553(6) 0.6889(5) 0.9183(3) 0.0481(14) Uani 1 1 d . . . . . H3S H 0.864928 0.716089 0.972027 0.058 Uiso 1 1 calc R . . . . C4S C 0.7280(6) 0.6605(5) 0.8745(3) 0.0571(16) Uani 1 1 d . . . . . H4S H 0.649972 0.668297 0.897804 0.068 Uiso 1 1 calc R . . . . C5S C 0.7147(6) 0.6208(5) 0.7968(3) 0.0627(17) Uani 1 1 d . . . . . H5S H 0.627065 0.600764 0.766049 0.075 Uiso 1 1 calc R . . . . C6S C 0.8276(6) 0.6101(6) 0.7636(3) 0.0571(17) Uani 1 1 d . . . . . H6S H 0.818100 0.583127 0.709888 0.069 Uiso 1 1 calc R . . . . C7S C 0.3709(5) 0.9102(5) 0.5055(3) 0.0405(13) Uani 1 1 d . . . . . H7S H 0.281534 0.847623 0.508981 0.049 Uiso 1 1 calc R . . . . C8S C 0.4949(5) 0.9248(5) 0.5467(3) 0.0393(13) Uani 1 1 d . . . . . H8S H 0.491229 0.873615 0.579204 0.047 Uiso 1 1 calc R . . . . C9S C 0.6246(5) 1.0147(5) 0.5404(3) 0.0456(14) Uani 1 1 d . . . . . H9S H 0.710872 1.024472 0.568016 0.055 Uiso 1 1 calc R . . . . C10S C 0.0917(5) 1.0138(5) 0.5614(3) 0.0416(13) Uani 1 1 d . . . . . H10S H 0.155057 1.023160 0.603944 0.050 Uiso 1 1 calc R . . . . C11S C 0.0148(5) 0.8967(4) 0.5119(3) 0.0347(12) Uani 1 1 d . . . . . H11S H 0.025397 0.825558 0.520313 0.042 Uiso 1 1 calc R . . . . C12S C -0.0783(5) 0.8815(5) 0.4498(3) 0.0370(12) Uani 1 1 d . . . . . H12S H -0.132161 0.800460 0.415403 0.044 Uiso 1 1 calc R . . . . 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 Br1 0.0305(3) 0.0387(3) 0.0170(2) 0.0041(2) 0.0010(2) 0.0170(2) Fe1 0.0187(3) 0.0217(4) 0.0163(3) 0.0044(3) 0.0022(3) 0.0091(3) N1 0.0145(18) 0.021(2) 0.0180(19) 0.0047(16) 0.0002(15) 0.0085(16) N2 0.0180(19) 0.020(2) 0.0179(19) 0.0025(16) 0.0000(15) 0.0068(16) N3 0.0206(19) 0.025(2) 0.0178(19) 0.0039(16) 0.0039(15) 0.0091(17) N4 0.0161(19) 0.022(2) 0.0196(19) 0.0054(16) 0.0013(15) 0.0071(16) N5 0.019(2) 0.025(2) 0.0203(19) 0.0077(17) 0.0004(15) 0.0090(17) N6 0.0155(18) 0.021(2) 0.0197(19) 0.0062(16) -0.0008(15) 0.0071(16) N7 0.0212(19) 0.023(2) 0.0202(19) 0.0037(17) 0.0041(15) 0.0119(17) N8 0.0185(19) 0.022(2) 0.0183(19) 0.0058(16) 0.0003(15) 0.0096(17) N9 0.0189(19) 0.022(2) 0.0174(18) 0.0045(16) -0.0022(15) 0.0084(17) C1 0.017(2) 0.022(2) 0.017(2) 0.0062(19) 0.0036(17) 0.0070(19) C2 0.021(2) 0.029(3) 0.020(2) 0.009(2) 0.0054(19) 0.008(2) C3 0.026(3) 0.032(3) 0.015(2) 0.004(2) 0.0042(19) 0.012(2) C4 0.023(2) 0.020(2) 0.019(2) 0.000(2) -0.0017(19) 0.008(2) C5 0.015(2) 0.018(2) 0.018(2) 0.0025(19) 0.0014(17) 0.0083(19) C6 0.024(2) 0.031(3) 0.024(2) 0.008(2) 0.008(2) 0.014(2) C7 0.028(3) 0.035(3) 0.027(3) 0.002(2) 0.005(2) 0.022(2) C8 0.026(3) 0.020(3) 0.030(3) 0.006(2) -0.001(2) 0.012(2) C9 0.024(3) 0.032(3) 0.029(3) 0.006(2) -0.001(2) 0.015(2) C10 0.015(2) 0.036(3) 0.044(3) 0.013(2) 0.002(2) 0.008(2) C11 0.021(2) 0.028(3) 0.029(3) 0.008(2) 0.006(2) 0.007(2) C12 0.022(2) 0.024(3) 0.020(2) 0.008(2) 0.0066(19) 0.010(2) C13 0.029(3) 0.028(3) 0.035(3) 0.008(2) 0.005(2) 0.012(2) C14 0.046(3) 0.022(3) 0.046(3) 0.014(2) 0.018(3) 0.013(3) C15 0.061(4) 0.035(3) 0.026(3) 0.014(2) 0.013(3) 0.031(3) C16 0.053(3) 0.037(3) 0.028(3) 0.011(2) -0.003(2) 0.026(3) C17 0.033(3) 0.025(3) 0.029(3) 0.006(2) 0.000(2) 0.011(2) C18 0.101(5) 0.048(4) 0.052(4) 0.032(3) 0.017(3) 0.039(4) C19 0.027(3) 0.037(3) 0.024(3) 0.010(2) 0.009(2) 0.017(2) C20 0.018(2) 0.041(3) 0.033(3) 0.015(2) 0.009(2) 0.010(2) C21 0.021(3) 0.028(3) 0.032(3) 0.012(2) 0.000(2) 0.007(2) C22 0.023(3) 0.038(3) 0.028(3) 0.011(2) -0.002(2) 0.016(2) C23 0.025(3) 0.031(3) 0.039(3) 0.011(2) 0.003(2) 0.018(2) C24 0.027(3) 0.022(3) 0.031(3) 0.009(2) 0.006(2) 0.014(2) C25 0.020(2) 0.020(3) 0.024(2) 0.006(2) 0.0074(19) 0.007(2) C26 0.027(3) 0.025(3) 0.029(3) 0.007(2) 0.005(2) 0.008(2) C27 0.034(3) 0.015(3) 0.041(3) 0.009(2) 0.015(2) 0.006(2) C28 0.035(3) 0.024(3) 0.020(3) 0.001(2) 0.010(2) 0.003(2) C29 0.029(3) 0.033(3) 0.022(3) 0.004(2) -0.001(2) 0.002(2) C30 0.031(3) 0.023(3) 0.026(3) 0.008(2) 0.003(2) 0.008(2) C31 0.055(4) 0.030(3) 0.043(3) 0.005(3) 0.013(3) -0.009(3) B1 0.020(3) 0.021(3) 0.017(3) 0.007(2) 0.003(2) 0.009(2) B2 0.015(2) 0.019(3) 0.019(3) 0.004(2) 0.004(2) 0.008(2) C1S 0.032(3) 0.057(4) 0.050(3) 0.025(3) 0.017(3) 0.022(3) C2S 0.037(3) 0.038(3) 0.046(3) 0.012(3) -0.002(3) 0.016(3) C3S 0.056(4) 0.052(4) 0.037(3) 0.005(3) 0.008(3) 0.028(3) C4S 0.038(3) 0.084(5) 0.055(4) 0.011(3) 0.015(3) 0.036(3) C5S 0.045(4) 0.080(5) 0.057(4) 0.005(4) -0.008(3) 0.029(3) C6S 0.056(4) 0.093(5) 0.031(3) 0.010(3) 0.005(3) 0.045(4) C7S 0.030(3) 0.040(3) 0.049(3) 0.021(3) 0.010(2) 0.007(3) C8S 0.047(3) 0.048(3) 0.032(3) 0.021(3) 0.009(3) 0.022(3) C9S 0.040(3) 0.054(4) 0.046(3) 0.021(3) 0.001(3) 0.020(3) C10S 0.037(3) 0.041(3) 0.034(3) 0.003(3) -0.012(2) 0.009(3) C11S 0.032(3) 0.030(3) 0.041(3) 0.008(3) 0.006(2) 0.012(2) C12S 0.032(3) 0.029(3) 0.036(3) 0.003(2) 0.003(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 Br1 Fe1 2.4552(13) . ? Fe1 N1 2.214(3) . ? Fe1 N3 2.074(3) . ? Fe1 N5 2.094(3) . ? Fe1 N7 2.067(3) . ? Fe1 N9 2.109(3) . ? N1 C1 1.366(5) . ? N1 C5 1.362(5) . ? N2 N3 1.368(4) . ? N2 C8 1.351(5) . ? N2 B1 1.579(5) . ? N3 C6 1.334(5) . ? N4 N5 1.369(4) . ? N4 C11 1.348(5) . ? N4 B1 1.585(5) . ? N5 C9 1.347(5) . ? N6 N7 1.359(4) . ? N6 C21 1.340(5) . ? N6 B2 1.586(5) . ? N7 C19 1.337(5) . ? N8 N9 1.376(4) . ? N8 C24 1.340(5) . ? N8 B2 1.576(5) . ? N9 C22 1.336(5) . ? C1 C2 1.386(5) . ? C1 B1 1.627(6) . ? C2 H2 0.9500 . ? C2 C3 1.384(5) . ? C3 H3 0.9500 . ? C3 C4 1.377(5) . ? C4 H4 0.9500 . ? C4 C5 1.390(5) . ? C5 B2 1.616(6) . ? C6 H6 0.9500 . ? C6 C7 1.377(6) . ? C7 H7 0.9500 . ? C7 C8 1.373(5) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C9 C10 1.374(6) . ? C10 H10 0.9500 . ? C10 C11 1.383(6) . ? C11 H11 0.9500 . ? C12 C13 1.398(6) . ? C12 C17 1.403(5) . ? C12 B1 1.606(6) . ? C13 H13 0.9500 . ? C13 C14 1.391(6) . ? C14 H14 0.9500 . ? C14 C15 1.379(6) . ? C15 C16 1.384(6) . ? C15 C18 1.515(6) . ? C16 H16 0.9500 . ? C16 C17 1.379(6) . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19 0.9500 . ? C19 C20 1.374(6) . ? C20 H20 0.9500 . ? C20 C21 1.381(5) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C22 C23 1.385(6) . ? C23 H23 0.9500 . ? C23 C24 1.374(6) . ? C24 H24 0.9500 . ? C25 C26 1.392(6) . ? C25 C30 1.394(5) . ? C25 B2 1.612(6) . ? C26 H26 0.9500 . ? C26 C27 1.390(6) . ? C27 H27 0.9500 . ? C27 C28 1.386(6) . ? C28 C29 1.385(6) . ? C28 C31 1.505(6) . ? C29 H29 0.9500 . ? C29 C30 1.383(6) . ? C30 H30 0.9500 . ? C31 H31A 0.9601 . ? C31 H31B 0.9600 . ? C31 H31C 0.9599 . ? C1S H1S 0.9500 . ? C1S C2S 1.376(6) . ? C1S C6S 1.365(6) . ? C2S H2S 0.9500 . ? C2S C3S 1.369(6) . ? C3S H3S 0.9500 . ? C3S C4S 1.374(7) . ? C4S H4S 0.9500 . ? C4S C5S 1.375(7) . ? C5S H5S 0.9500 . ? C5S C6S 1.367(7) . ? C6S H6S 0.9500 . ? C7S H7S 0.9500 . ? C7S C8S 1.376(6) . ? C7S C9S 1.371(6) 2_676 ? C8S H8S 0.9500 . ? C8S C9S 1.381(6) . ? C9S H9S 0.9500 . ? C10S H10S 0.9500 . ? C10S C11S 1.370(6) . ? C10S C12S 1.379(6) 2_576 ? C11S H11S 0.9500 . ? C11S C12S 1.384(6) . ? C12S H12S 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 N1 Fe1 Br1 176.82(9) . . ? N3 Fe1 Br1 97.02(9) . . ? N3 Fe1 N1 85.86(12) . . ? N3 Fe1 N5 84.71(13) . . ? N3 Fe1 N9 171.15(12) . . ? N5 Fe1 Br1 92.22(9) . . ? N5 Fe1 N1 86.70(12) . . ? N5 Fe1 N9 96.53(13) . . ? N7 Fe1 Br1 95.34(9) . . ? N7 Fe1 N1 85.89(12) . . ? N7 Fe1 N3 91.94(13) . . ? N7 Fe1 N5 172.07(13) . . ? N7 Fe1 N9 85.69(13) . . ? N9 Fe1 Br1 91.70(9) . . ? N9 Fe1 N1 85.46(12) . . ? C1 N1 Fe1 118.4(3) . . ? C5 N1 Fe1 118.8(3) . . ? C5 N1 C1 121.5(3) . . ? N3 N2 B1 123.1(3) . . ? C8 N2 N3 108.3(3) . . ? C8 N2 B1 128.5(3) . . ? N2 N3 Fe1 118.8(2) . . ? C6 N3 Fe1 134.3(3) . . ? C6 N3 N2 106.6(3) . . ? N5 N4 B1 118.4(3) . . ? C11 N4 N5 109.2(3) . . ? C11 N4 B1 132.3(3) . . ? N4 N5 Fe1 122.3(2) . . ? C9 N5 Fe1 130.9(3) . . ? C9 N5 N4 106.3(3) . . ? N7 N6 B2 121.9(3) . . ? C21 N6 N7 108.9(3) . . ? C21 N6 B2 129.1(3) . . ? N6 N7 Fe1 119.9(2) . . ? C19 N7 Fe1 133.2(3) . . ? C19 N7 N6 106.8(3) . . ? N9 N8 B2 119.1(3) . . ? C24 N8 N9 109.0(3) . . ? C24 N8 B2 131.0(3) . . ? N8 N9 Fe1 121.0(2) . . ? C22 N9 Fe1 130.9(3) . . ? C22 N9 N8 106.5(3) . . ? N1 C1 C2 119.0(4) . . ? N1 C1 B1 118.8(3) . . ? C2 C1 B1 122.0(4) . . ? C1 C2 H2 119.6 . . ? C3 C2 C1 120.8(4) . . ? C3 C2 H2 119.6 . . ? C2 C3 H3 120.7 . . ? C4 C3 C2 118.6(4) . . ? C4 C3 H3 120.7 . . ? C3 C4 H4 119.6 . . ? C3 C4 C5 120.8(4) . . ? C5 C4 H4 119.6 . . ? N1 C5 C4 119.1(4) . . ? N1 C5 B2 118.6(3) . . ? C4 C5 B2 121.9(4) . . ? N3 C6 H6 124.4 . . ? N3 C6 C7 111.1(4) . . ? C7 C6 H6 124.4 . . ? C6 C7 H7 127.7 . . ? C8 C7 C6 104.5(4) . . ? C8 C7 H7 127.7 . . ? N2 C8 C7 109.4(4) . . ? N2 C8 H8 125.3 . . ? C7 C8 H8 125.3 . . ? N5 C9 H9 124.7 . . ? N5 C9 C10 110.7(4) . . ? C10 C9 H9 124.7 . . ? C9 C10 H10 127.4 . . ? C9 C10 C11 105.3(4) . . ? C11 C10 H10 127.4 . . ? N4 C11 C10 108.5(4) . . ? N4 C11 H11 125.8 . . ? C10 C11 H11 125.8 . . ? C13 C12 C17 115.3(4) . . ? C13 C12 B1 125.5(4) . . ? C17 C12 B1 118.7(4) . . ? C12 C13 H13 119.1 . . ? C14 C13 C12 121.9(4) . . ? C14 C13 H13 119.1 . . ? C13 C14 H14 119.1 . . ? C15 C14 C13 121.8(5) . . ? C15 C14 H14 119.1 . . ? C14 C15 C16 117.0(4) . . ? C14 C15 C18 121.5(5) . . ? C16 C15 C18 121.5(5) . . ? C15 C16 H16 119.2 . . ? C17 C16 C15 121.6(4) . . ? C17 C16 H16 119.2 . . ? C12 C17 H17 118.8 . . ? C16 C17 C12 122.4(4) . . ? C16 C17 H17 118.8 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N7 C19 H19 124.6 . . ? N7 C19 C20 110.8(4) . . ? C20 C19 H19 124.6 . . ? C19 C20 H20 127.7 . . ? C19 C20 C21 104.6(4) . . ? C21 C20 H20 127.7 . . ? N6 C21 C20 109.0(4) . . ? N6 C21 H21 125.5 . . ? C20 C21 H21 125.5 . . ? N9 C22 H22 124.8 . . ? N9 C22 C23 110.4(4) . . ? C23 C22 H22 124.8 . . ? C22 C23 H23 127.4 . . ? C24 C23 C22 105.1(4) . . ? C24 C23 H23 127.4 . . ? N8 C24 C23 109.0(4) . . ? N8 C24 H24 125.5 . . ? C23 C24 H24 125.5 . . ? C26 C25 C30 115.8(4) . . ? C26 C25 B2 124.2(4) . . ? C30 C25 B2 119.2(4) . . ? C25 C26 H26 118.9 . . ? C27 C26 C25 122.2(4) . . ? C27 C26 H26 118.9 . . ? C26 C27 H27 119.4 . . ? C28 C27 C26 121.2(4) . . ? C28 C27 H27 119.4 . . ? C27 C28 C31 121.7(4) . . ? C29 C28 C27 117.0(4) . . ? C29 C28 C31 121.3(4) . . ? C28 C29 H29 119.2 . . ? C30 C29 C28 121.6(4) . . ? C30 C29 H29 119.2 . . ? C25 C30 H30 118.9 . . ? C29 C30 C25 122.1(4) . . ? C29 C30 H30 118.9 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N2 B1 N4 106.1(3) . . ? N2 B1 C1 110.4(3) . . ? N2 B1 C12 105.8(3) . . ? N4 B1 C1 103.2(3) . . ? N4 B1 C12 114.8(3) . . ? C12 B1 C1 116.2(3) . . ? N6 B2 C5 110.7(3) . . ? N6 B2 C25 104.8(3) . . ? N8 B2 N6 107.2(3) . . ? N8 B2 C5 102.9(3) . . ? N8 B2 C25 113.9(3) . . ? C25 B2 C5 117.1(3) . . ? C2S C1S H1S 120.2 . . ? C6S C1S H1S 120.2 . . ? C6S C1S C2S 119.7(5) . . ? C1S C2S H2S 120.1 . . ? C3S C2S C1S 119.8(5) . . ? C3S C2S H2S 120.1 . . ? C2S C3S H3S 119.8 . . ? C2S C3S C4S 120.5(5) . . ? C4S C3S H3S 119.8 . . ? C3S C4S H4S 120.3 . . ? C3S C4S C5S 119.4(5) . . ? C5S C4S H4S 120.3 . . ? C4S C5S H5S 120.0 . . ? C6S C5S C4S 120.0(5) . . ? C6S C5S H5S 120.0 . . ? C1S C6S C5S 120.7(5) . . ? C1S C6S H6S 119.7 . . ? C5S C6S H6S 119.7 . . ? C8S C7S H7S 119.7 . . ? C9S C7S H7S 119.7 2_676 . ? C9S C7S C8S 120.5(5) 2_676 . ? C7S C8S H8S 120.3 . . ? C7S C8S C9S 119.4(5) . . ? C9S C8S H8S 120.3 . . ? C7S C9S C8S 120.1(5) 2_676 . ? C7S C9S H9S 119.9 2_676 . ? C8S C9S H9S 119.9 . . ? C11S C10S H10S 119.5 . . ? C11S C10S C12S 120.9(4) . 2_576 ? C12S C10S H10S 119.5 2_576 . ? C10S C11S H11S 119.9 . . ? C10S C11S C12S 120.2(5) . . ? C12S C11S H11S 119.9 . . ? C10S C12S C11S 118.9(4) 2_576 . ? C10S C12S H12S 120.6 2_576 . ? C11S C12S H12S 120.6 . . ? _shelx_res_file ; TITL mo_LN512_0m_a.res in P-1 mo_ln512_0m_a.res created by SHELXL-2018/3 at 16:12:41 on 20-Apr-2020 REM Old TITL mo_LN512_0m in P-1 REM SHELXT solution in P-1 REM R1 0.164, Rweak 0.021, Alpha 0.078, Orientation as input REM Formula found by SHELXT: C43 B2 Br Fe N9 CELL 0.71073 10.2515 12.0247 18.4005 104.192 92.618 112.901 ZERR 2 0.0046 0.0053 0.0082 0.005 0.005 0.005 LATT 1 SFAC C H B Br Fe N UNIT 86 82 4 2 2 18 L.S. 500 PLAN 1 SIZE 0.12 0.07 0.04 TEMP -100(2) BOND $H LIST 6 fmap 2 acta OMIT -3 52 REM REM REM WGHT 0.018900 1.221600 FVAR 0.43280 BR1 4 0.237696 0.500638 0.513423 11.00000 0.03051 0.03871 = 0.01701 0.00406 0.00101 0.01697 FE1 5 0.305808 0.562533 0.651790 11.00000 0.01866 0.02170 = 0.01633 0.00438 0.00219 0.00915 N1 6 0.358469 0.623035 0.777183 11.00000 0.01450 0.02144 = 0.01804 0.00468 0.00017 0.00848 N2 6 0.337167 0.360079 0.707973 11.00000 0.01801 0.01952 = 0.01794 0.00245 0.00004 0.00683 N3 6 0.378222 0.424848 0.655378 11.00000 0.02065 0.02523 = 0.01782 0.00393 0.00387 0.00913 N4 6 0.096044 0.368711 0.718668 11.00000 0.01614 0.02192 = 0.01961 0.00541 0.00130 0.00711 N5 6 0.108406 0.431182 0.664628 11.00000 0.01925 0.02545 = 0.02025 0.00769 0.00043 0.00895 N6 6 0.562097 0.809000 0.704970 11.00000 0.01547 0.02150 = 0.01968 0.00619 -0.00078 0.00712 N7 6 0.510899 0.692839 0.654005 11.00000 0.02123 0.02264 = 0.02020 0.00366 0.00412 0.01185 N8 6 0.325498 0.828426 0.719304 11.00000 0.01850 0.02207 = 0.01834 0.00577 0.00029 0.00960 N9 6 0.246221 0.714920 0.666017 11.00000 0.01888 0.02203 = 0.01737 0.00446 -0.00224 0.00840 C1 1 0.306143 0.534365 0.815106 11.00000 0.01713 0.02178 = 0.01665 0.00617 0.00361 0.00702 C2 1 0.302745 0.573288 0.892115 11.00000 0.02100 0.02945 = 0.01956 0.00935 0.00542 0.00824 AFIX 43 H2 2 0.263794 0.512187 0.918629 11.00000 -1.20000 AFIX 0 C3 1 0.355377 0.700039 0.930876 11.00000 0.02609 0.03220 = 0.01491 0.00424 0.00423 0.01226 AFIX 43 H3 2 0.351335 0.726504 0.983471 11.00000 -1.20000 AFIX 0 C4 1 0.413714 0.786992 0.891646 11.00000 0.02334 0.01952 = 0.01921 -0.00025 -0.00173 0.00792 AFIX 43 H4 2 0.452278 0.874357 0.917733 11.00000 -1.20000 AFIX 0 C5 1 0.416892 0.748531 0.814313 11.00000 0.01511 0.01783 = 0.01779 0.00252 0.00137 0.00835 C6 1 0.453525 0.373553 0.612781 11.00000 0.02447 0.03115 = 0.02385 0.00773 0.00769 0.01428 AFIX 43 H6 2 0.494975 0.400491 0.571593 11.00000 -1.20000 AFIX 0 C7 1 0.463318 0.276475 0.636312 11.00000 0.02795 0.03543 = 0.02654 0.00192 0.00485 0.02191 AFIX 43 H7 2 0.510941 0.225046 0.615594 11.00000 -1.20000 AFIX 0 C8 1 0.388829 0.270636 0.696436 11.00000 0.02610 0.02042 = 0.03007 0.00648 -0.00074 0.01222 AFIX 43 H8 2 0.375687 0.212724 0.725395 11.00000 -1.20000 AFIX 0 C9 1 -0.026285 0.402127 0.633316 11.00000 0.02364 0.03219 = 0.02936 0.00606 -0.00055 0.01521 AFIX 43 H9 2 -0.050071 0.430957 0.593094 11.00000 -1.20000 AFIX 0 C10 1 -0.124542 0.325087 0.667524 11.00000 0.01539 0.03604 = 0.04356 0.01287 0.00151 0.00836 AFIX 43 H10 2 -0.226105 0.291900 0.656309 11.00000 -1.20000 AFIX 0 C11 1 -0.043991 0.306157 0.721796 11.00000 0.02126 0.02819 = 0.02933 0.00799 0.00610 0.00698 AFIX 43 H11 2 -0.081072 0.257323 0.755575 11.00000 -1.20000 AFIX 0 C12 1 0.216084 0.287714 0.815653 11.00000 0.02182 0.02358 = 0.02049 0.00801 0.00661 0.00957 C13 1 0.105177 0.167033 0.798206 11.00000 0.02873 0.02814 = 0.03478 0.00828 0.00470 0.01214 AFIX 43 H13 2 0.031229 0.141184 0.756676 11.00000 -1.20000 AFIX 0 C14 1 0.100082 0.083755 0.839958 11.00000 0.04553 0.02230 = 0.04604 0.01408 0.01844 0.01337 AFIX 43 H14 2 0.021165 0.003665 0.827202 11.00000 -1.20000 AFIX 0 C15 1 0.206490 0.114338 0.899352 11.00000 0.06082 0.03539 = 0.02626 0.01415 0.01342 0.03104 C16 1 0.320237 0.231325 0.915069 11.00000 0.05295 0.03663 = 0.02766 0.01109 -0.00309 0.02565 AFIX 43 H16 2 0.397206 0.254136 0.954350 11.00000 -1.20000 AFIX 0 C17 1 0.324649 0.315589 0.875147 11.00000 0.03291 0.02454 = 0.02852 0.00554 0.00009 0.01124 AFIX 43 H17 2 0.404072 0.395408 0.888406 11.00000 -1.20000 AFIX 0 C18 1 0.201529 0.022409 0.943724 11.00000 0.10056 0.04752 = 0.05158 0.03223 0.01701 0.03907 AFIX 137 H18A 2 0.174093 0.048452 0.993273 11.00000 -1.50000 H18B 2 0.296317 0.021419 0.951060 11.00000 -1.50000 H18C 2 0.130967 -0.062130 0.915552 11.00000 -1.50000 AFIX 0 C19 1 0.611603 0.692708 0.610359 11.00000 0.02688 0.03703 = 0.02443 0.00977 0.00910 0.01739 AFIX 43 H19 2 0.603798 0.622911 0.569821 11.00000 -1.20000 AFIX 0 C20 1 0.727898 0.807254 0.632118 11.00000 0.01762 0.04061 = 0.03333 0.01461 0.00852 0.00986 AFIX 43 H20 2 0.813532 0.831891 0.610576 11.00000 -1.20000 AFIX 0 C21 1 0.692521 0.878590 0.692300 11.00000 0.02112 0.02803 = 0.03217 0.01167 -0.00009 0.00699 AFIX 43 H21 2 0.751195 0.963352 0.720226 11.00000 -1.20000 AFIX 0 C22 1 0.122439 0.718348 0.643386 11.00000 0.02315 0.03757 = 0.02775 0.01117 -0.00222 0.01588 AFIX 43 H22 2 0.047657 0.652869 0.605697 11.00000 -1.20000 AFIX 0 C23 1 0.118583 0.830822 0.682633 11.00000 0.02531 0.03107 = 0.03910 0.01069 0.00330 0.01780 AFIX 43 H23 2 0.042991 0.856796 0.677624 11.00000 -1.20000 AFIX 0 C24 1 0.247727 0.896764 0.730398 11.00000 0.02680 0.02223 = 0.03100 0.00927 0.00567 0.01432 AFIX 43 H24 2 0.277101 0.977714 0.765590 11.00000 -1.20000 AFIX 0 C25 1 0.569628 0.992536 0.810993 11.00000 0.01983 0.01994 = 0.02373 0.00612 0.00735 0.00661 C26 1 0.571089 1.095634 0.788832 11.00000 0.02731 0.02521 = 0.02943 0.00660 0.00487 0.00763 AFIX 43 H26 2 0.501507 1.082076 0.747915 11.00000 -1.20000 AFIX 0 C27 1 0.670960 1.217772 0.824571 11.00000 0.03368 0.01479 = 0.04118 0.00904 0.01488 0.00608 AFIX 43 H27 2 0.666059 1.285704 0.808708 11.00000 -1.20000 AFIX 0 C28 1 0.777587 1.242272 0.882940 11.00000 0.03472 0.02408 = 0.01950 0.00087 0.00966 0.00313 C29 1 0.779355 1.139885 0.904028 11.00000 0.02867 0.03349 = 0.02208 0.00356 -0.00119 0.00156 AFIX 43 H29 2 0.851919 1.153175 0.943286 11.00000 -1.20000 AFIX 0 C30 1 0.678150 1.018802 0.869377 11.00000 0.03125 0.02307 = 0.02618 0.00809 0.00269 0.00786 AFIX 43 H30 2 0.682730 0.951315 0.885900 11.00000 -1.20000 AFIX 0 C31 1 0.888866 1.373630 0.920570 11.00000 0.05530 0.02952 = 0.04305 0.00499 0.01304 -0.00881 AFIX 3 H31A 2 0.899946 1.424020 0.886169 11.00000 -1.50000 H31B 2 0.978716 1.370500 0.933990 11.00000 -1.50000 H31C 2 0.858906 1.410160 0.965520 11.00000 -1.50000 AFIX 0 B1 3 0.238168 0.386160 0.767065 11.00000 0.02023 0.02097 = 0.01707 0.00701 0.00334 0.00877 B2 3 0.470120 0.847855 0.765109 11.00000 0.01549 0.01893 = 0.01854 0.00373 0.00394 0.00778 C1S 1 0.953881 0.637914 0.807080 11.00000 0.03169 0.05701 = 0.05008 0.02469 0.01734 0.02226 AFIX 43 H1S 2 1.031540 0.629476 0.783666 11.00000 -1.20000 AFIX 0 C2S 1 0.968128 0.678195 0.884930 11.00000 0.03697 0.03800 = 0.04611 0.01154 -0.00151 0.01558 AFIX 43 H2S 2 1.056051 0.698530 0.915451 11.00000 -1.20000 AFIX 0 C3S 1 0.855252 0.688878 0.918267 11.00000 0.05613 0.05208 = 0.03673 0.00451 0.00792 0.02788 AFIX 43 H3S 2 0.864928 0.716089 0.972027 11.00000 -1.20000 AFIX 0 C4S 1 0.728024 0.660519 0.874517 11.00000 0.03785 0.08350 = 0.05541 0.01054 0.01460 0.03563 AFIX 43 H4S 2 0.649972 0.668297 0.897804 11.00000 -1.20000 AFIX 0 C5S 1 0.714681 0.620791 0.796751 11.00000 0.04464 0.07952 = 0.05727 0.00483 -0.00823 0.02944 AFIX 43 H5S 2 0.627065 0.600764 0.766049 11.00000 -1.20000 AFIX 0 C6S 1 0.827596 0.610132 0.763646 11.00000 0.05557 0.09332 = 0.03116 0.00991 0.00523 0.04464 AFIX 43 H6S 2 0.818100 0.583127 0.709888 11.00000 -1.20000 AFIX 0 C7S 1 0.370929 0.910241 0.505535 11.00000 0.03040 0.04020 = 0.04890 0.02056 0.00953 0.00741 AFIX 43 H7S 2 0.281534 0.847623 0.508981 11.00000 -1.20000 AFIX 0 C8S 1 0.494872 0.924849 0.546735 11.00000 0.04659 0.04817 = 0.03169 0.02123 0.00903 0.02233 AFIX 43 H8S 2 0.491229 0.873615 0.579204 11.00000 -1.20000 AFIX 0 C9S 1 0.624583 1.014680 0.540438 11.00000 0.04046 0.05423 = 0.04578 0.02064 0.00068 0.02023 AFIX 43 H9S 2 0.710872 1.024472 0.568016 11.00000 -1.20000 AFIX 0 C10S 1 0.091657 1.013834 0.561365 11.00000 0.03685 0.04070 = 0.03434 0.00349 -0.01176 0.00903 AFIX 43 H10S 2 0.155057 1.023160 0.603944 11.00000 -1.20000 AFIX 0 C11S 1 0.014773 0.896667 0.511924 11.00000 0.03166 0.02989 = 0.04074 0.00798 0.00644 0.01215 AFIX 43 H11S 2 0.025397 0.825558 0.520313 11.00000 -1.20000 AFIX 0 C12S 1 -0.078328 0.881550 0.449793 11.00000 0.03222 0.02879 = 0.03634 0.00258 0.00274 0.00286 AFIX 43 H12S 2 -0.132161 0.800460 0.415403 11.00000 -1.20000 AFIX 0 HKLF 4 REM mo_LN512_0m_a.res in P-1 REM wR2 = 0.0964, GooF = S = 0.997, Restrained GooF = 0.997 for all data REM R1 = 0.0521 for 4570 Fo > 4sig(Fo) and 0.1238 for all 7875 data REM 506 parameters refined using 0 restraints END WGHT 0.0189 1.2216 REM Highest difference peak 0.433, deepest hole -0.399, 1-sigma level 0.087 Q1 1 0.6422 0.9967 0.8287 11.00000 0.05 0.43 ; _shelx_res_checksum 67552 _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_ln582yellow _database_code_depnum_ccdc_archive 'CCDC 2044413' loop_ _audit_author_name _audit_author_address 'Benjamin S. Gelfand' ;University of Calgary Canada ; _audit_update_record ; 2020-11-14 deposited with the CCDC. 2020-12-22 downloaded from the CCDC. ; _audit_creation_date 2019-04-23 _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 'C31 H29 B2 F Fe N9' _chemical_formula_sum 'C31 H29 B2 F Fe N9' _chemical_formula_weight 624.10 _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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _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 8.2450(4) _cell_length_b 19.3287(10) _cell_length_c 18.0484(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2876.3(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7772 _cell_measurement_temperature 173 _cell_measurement_theta_max 28.277 _cell_measurement_theta_min 2.913 _shelx_estimated_absorpt_T_max 0.889 _shelx_estimated_absorpt_T_min 0.858 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_T_max 0.8364 _exptl_absorpt_correction_T_min 0.7159 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0594 before and 0.0468 after correction. The Ratio of minimum to maximum transmission is 0.8559. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1292 _exptl_crystal_size_max 0.276 _exptl_crystal_size_mid 0.238 _exptl_crystal_size_min 0.211 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_unetI/netI 0.0347 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 19799 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.295 _diffrn_reflns_theta_min 3.439 _diffrn_ambient_temperature 173 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _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_special_details ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2721 _reflns_number_total 3656 _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 v8.37A (Bruker, 2015)' _computing_data_collection ? _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _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 0.429 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.086 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 206 _refine_ls_number_reflns 3656 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0432 _refine_ls_restrained_S_all 1.073 _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^)+(0.0717P)^2^+0.6681P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1125 _refine_ls_wR_factor_ref 0.1285 _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 2.a Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C15(H15), C16(H16) 2.b Idealised Me refined as rotating group: C13(H13A,H13B,H13C) ; _atom_sites_solution_hydrogens geom _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 Fe1 Fe 0.50682(5) 0.250000 0.49905(2) 0.02174(14) Uani 1 2 d S T P . . F1 F 0.4154(2) 0.250000 0.59173(9) 0.0356(4) Uani 1 2 d S T P . . N1 N 0.3574(2) 0.33065(8) 0.45993(9) 0.0253(4) Uani 1 1 d . . . . . N2 N 0.4181(2) 0.38202(8) 0.41586(8) 0.0233(4) Uani 1 1 d . . . . . N3 N 0.6720(2) 0.32741(9) 0.52428(9) 0.0256(4) Uani 1 1 d . . . . . N4 N 0.69430(19) 0.38069(8) 0.47601(9) 0.0227(3) Uani 1 1 d . . . . . N5 N 0.6181(3) 0.250000 0.38867(12) 0.0194(4) Uani 1 2 d S T P . . C1 C 0.1968(3) 0.33946(11) 0.46149(12) 0.0319(5) Uani 1 1 d . . . . . H1 H 0.123652 0.311599 0.489098 0.038 Uiso 1 1 calc R . . . . C2 C 0.1519(3) 0.39451(12) 0.41755(12) 0.0325(5) Uani 1 1 d . . . . . H2 H 0.045392 0.411321 0.408617 0.039 Uiso 1 1 calc R . . . . C3 C 0.2952(3) 0.41976(11) 0.38948(11) 0.0279(4) Uani 1 1 d . . . . . H3 H 0.305249 0.457904 0.356603 0.034 Uiso 1 1 calc R . . . . C4 C 0.7561(3) 0.34242(12) 0.58520(11) 0.0331(5) Uani 1 1 d . . . . . H4 H 0.761171 0.314007 0.628089 0.040 Uiso 1 1 calc R . . . . C5 C 0.8349(3) 0.40486(12) 0.57736(12) 0.0332(5) Uani 1 1 d . . . . . H5 H 0.903593 0.427152 0.612235 0.040 Uiso 1 1 calc R . . . . C6 C 0.7921(2) 0.42785(11) 0.50778(11) 0.0272(4) Uani 1 1 d . . . . . H6 H 0.826046 0.470110 0.485831 0.033 Uiso 1 1 calc R . . . . C7 C 0.6624(2) 0.45508(10) 0.36164(10) 0.0232(4) Uani 1 1 d . . . . . C8 C 0.5985(2) 0.51832(11) 0.38648(11) 0.0263(4) Uani 1 1 d . . . . . H8 H 0.510863 0.517594 0.420616 0.032 Uiso 1 1 calc R . . . . C9 C 0.6583(3) 0.58180(10) 0.36322(11) 0.0277(4) Uani 1 1 d . . . . . H9 H 0.610734 0.623246 0.381368 0.033 Uiso 1 1 calc R . . . . C10 C 0.7870(3) 0.58538(10) 0.31361(11) 0.0272(4) Uani 1 1 d . . . . . C11 C 0.8543(3) 0.52353(11) 0.28929(11) 0.0278(4) Uani 1 1 d . . . . . H11 H 0.943360 0.524415 0.255930 0.033 Uiso 1 1 calc R . . . . C12 C 0.7930(2) 0.46043(10) 0.31313(10) 0.0249(4) Uani 1 1 d . . . . . H12 H 0.842342 0.419145 0.295587 0.030 Uiso 1 1 calc R . . . . C13 C 0.8532(3) 0.65433(11) 0.28998(14) 0.0402(6) Uani 1 1 d . . . . . H13A H 0.907233 0.676521 0.332106 0.060 Uiso 1 1 calc GR . . . . H13B H 0.764186 0.683777 0.272680 0.060 Uiso 1 1 calc GR . . . . H13C H 0.931477 0.647670 0.249735 0.060 Uiso 1 1 calc GR . . . . C14 C 0.6328(2) 0.31165(9) 0.35246(10) 0.0214(4) Uani 1 1 d . . . . . C15 C 0.6497(3) 0.31145(10) 0.27524(11) 0.0258(4) Uani 1 1 d . . . . . H15 H 0.656844 0.354035 0.249163 0.031 Uiso 1 1 calc R . . . . C16 C 0.6562(4) 0.250000 0.23692(15) 0.0312(7) Uani 1 2 d S T P . . H16 H 0.664940 0.250000 0.184435 0.037 Uiso 1 2 calc RS T P . . B1 B 0.6057(3) 0.38323(11) 0.39846(12) 0.0221(4) 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 Fe1 0.0236(2) 0.0244(2) 0.0171(2) 0.000 0.00241(14) 0.000 F1 0.0486(12) 0.0316(9) 0.0266(9) 0.000 0.0136(8) 0.000 N1 0.0232(9) 0.0269(8) 0.0258(9) 0.0018(7) 0.0034(6) 0.0007(7) N2 0.0244(9) 0.0241(8) 0.0215(8) -0.0016(7) 0.0008(6) 0.0010(7) N3 0.0288(9) 0.0274(9) 0.0207(8) 0.0010(7) -0.0010(7) -0.0005(7) N4 0.0228(9) 0.0238(8) 0.0216(7) -0.0019(7) 0.0021(6) 0.0008(6) N5 0.0184(11) 0.0199(10) 0.0199(10) 0.000 -0.0004(8) 0.000 C1 0.0244(11) 0.0348(12) 0.0367(12) -0.0025(10) 0.0067(9) 0.0008(8) C2 0.0232(11) 0.0376(12) 0.0368(12) -0.0015(10) -0.0019(8) 0.0076(9) C3 0.0287(11) 0.0285(11) 0.0267(10) -0.0004(8) -0.0027(8) 0.0054(8) C4 0.0377(13) 0.0374(12) 0.0240(10) -0.0014(9) -0.0070(8) -0.0003(9) C5 0.0314(12) 0.0366(12) 0.0317(11) -0.0066(9) -0.0089(9) -0.0014(9) C6 0.0230(10) 0.0281(10) 0.0305(10) -0.0053(8) -0.0006(8) -0.0014(8) C7 0.0241(10) 0.0248(9) 0.0207(9) -0.0012(8) -0.0020(7) 0.0009(7) C8 0.0254(11) 0.0296(10) 0.0239(9) -0.0025(8) 0.0019(8) 0.0017(8) C9 0.0324(12) 0.0223(10) 0.0283(10) -0.0054(8) -0.0036(8) 0.0046(8) C10 0.0331(11) 0.0243(10) 0.0242(9) 0.0008(8) -0.0070(8) -0.0043(8) C11 0.0280(11) 0.0319(10) 0.0235(9) -0.0031(9) 0.0032(8) -0.0055(8) C12 0.0271(11) 0.0247(10) 0.0229(9) -0.0043(8) 0.0008(7) 0.0013(8) C13 0.0523(16) 0.0277(11) 0.0406(13) 0.0050(10) -0.0035(11) -0.0070(10) C14 0.0193(9) 0.0243(9) 0.0205(9) 0.0009(7) 0.0012(7) 0.0001(7) C15 0.0350(12) 0.0225(9) 0.0201(9) 0.0034(8) 0.0012(8) -0.0014(8) C16 0.0451(19) 0.0315(15) 0.0170(13) 0.000 0.0016(12) 0.000 B1 0.0221(11) 0.0229(10) 0.0211(10) 0.0000(8) 0.0021(8) 0.0020(8) _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 Fe1 F1 1.8349(16) . ? Fe1 N1 2.1086(17) 7_565 ? Fe1 N1 2.1086(17) . ? Fe1 N3 2.0737(18) . ? Fe1 N3 2.0737(17) 7_565 ? Fe1 N5 2.193(2) . ? N1 N2 1.367(2) . ? N1 C1 1.335(3) . ? N2 C3 1.336(3) . ? N2 B1 1.579(3) . ? N3 N4 1.361(2) . ? N3 C4 1.332(3) . ? N4 C6 1.345(3) . ? N4 B1 1.580(3) . ? N5 C14 1.365(2) 7_565 ? N5 C14 1.365(2) . ? C1 C2 1.378(3) . ? C2 C3 1.375(3) . ? C4 C5 1.378(3) . ? C5 C6 1.378(3) . ? C7 C8 1.404(3) . ? C7 C12 1.392(3) . ? C7 B1 1.609(3) . ? C8 C9 1.387(3) . ? C9 C10 1.390(3) . ? C10 C11 1.389(3) . ? C10 C13 1.502(3) . ? C11 C12 1.388(3) . ? C14 C15 1.401(3) . ? C14 B1 1.629(3) . ? C15 C16 1.375(2) . ? 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 F1 Fe1 N1 93.74(6) . . ? F1 Fe1 N1 93.74(6) . 7_565 ? F1 Fe1 N3 93.99(6) . 7_565 ? F1 Fe1 N3 93.99(6) . . ? F1 Fe1 N5 179.54(8) . . ? N1 Fe1 N1 95.34(9) . 7_565 ? N1 Fe1 N5 86.57(6) . . ? N1 Fe1 N5 86.57(6) 7_565 . ? N3 Fe1 N1 172.13(7) . 7_565 ? N3 Fe1 N1 85.63(7) . . ? N3 Fe1 N1 85.63(7) 7_565 7_565 ? N3 Fe1 N1 172.13(7) 7_565 . ? N3 Fe1 N3 92.36(10) 7_565 . ? N3 Fe1 N5 85.69(6) 7_565 . ? N3 Fe1 N5 85.69(6) . . ? N2 N1 Fe1 121.20(12) . . ? C1 N1 Fe1 131.80(14) . . ? C1 N1 N2 106.41(16) . . ? N1 N2 B1 119.02(15) . . ? C3 N2 N1 109.05(16) . . ? C3 N2 B1 131.61(17) . . ? N4 N3 Fe1 119.61(12) . . ? C4 N3 Fe1 132.88(15) . . ? C4 N3 N4 107.04(17) . . ? N3 N4 B1 121.87(16) . . ? C6 N4 N3 108.72(16) . . ? C6 N4 B1 129.32(16) . . ? C14 N5 Fe1 118.18(11) . . ? C14 N5 Fe1 118.18(11) 7_565 . ? C14 N5 C14 121.7(2) 7_565 . ? N1 C1 C2 110.68(19) . . ? C3 C2 C1 104.77(19) . . ? N2 C3 C2 109.06(19) . . ? N3 C4 C5 110.58(19) . . ? C4 C5 C6 104.79(19) . . ? N4 C6 C5 108.87(19) . . ? C8 C7 B1 120.71(17) . . ? C12 C7 C8 115.22(18) . . ? C12 C7 B1 123.27(17) . . ? C9 C8 C7 122.71(19) . . ? C8 C9 C10 120.65(18) . . ? C9 C10 C13 120.30(19) . . ? C11 C10 C9 117.75(18) . . ? C11 C10 C13 121.9(2) . . ? C12 C11 C10 120.85(19) . . ? C11 C12 C7 122.80(19) . . ? N5 C14 C15 118.88(17) . . ? N5 C14 B1 119.04(16) . . ? C15 C14 B1 121.55(16) . . ? C16 C15 C14 120.44(18) . . ? C15 C16 C15 119.4(3) 7_565 . ? N2 B1 N4 106.05(14) . . ? N2 B1 C7 112.30(15) . . ? N2 B1 C14 102.91(15) . . ? N4 B1 C7 104.99(15) . . ? N4 B1 C14 111.21(15) . . ? C7 B1 C14 118.86(16) . . ? _shelx_res_file ; TITL ln582yellow_a.res in Pnma ln582yellow.res created by SHELXL-2018/3 at 09:37:16 on 23-Apr-2019 REM Old TITL LN582yellow in Pnma REM SHELXT solution in Pnma: R1 0.109, Rweak 0.002, Alpha 0.016 REM 0.699 for 322 systematic absences, Orientation as input REM Formula found by SHELXT: C33 B2 N7 F Fe CELL 0.71073 8.245 19.3287 18.0484 90 90 90 ZERR 4 0.0004 0.001 0.0009 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 B F Fe N UNIT 124 116 8 4 4 36 L.S. 10 PLAN 20 SIZE 0.211 0.238 0.276 TEMP -100.15 BOND list 4 fmap 2 53 ACTA OMIT 0 1 1 OMIT 1 0 1 OMIT 0 2 0 REM REM REM WGHT 0.071700 0.668100 FVAR 0.28681 FE1 5 0.506821 0.250000 0.499047 10.50000 0.02365 0.02445 = 0.01712 0.00000 0.00241 0.00000 F1 4 0.415371 0.250000 0.591732 10.50000 0.04859 0.03162 = 0.02664 0.00000 0.01361 0.00000 N1 6 0.357402 0.330651 0.459926 11.00000 0.02317 0.02691 = 0.02584 0.00176 0.00344 0.00074 N2 6 0.418076 0.382025 0.415860 11.00000 0.02444 0.02407 = 0.02152 -0.00160 0.00084 0.00101 N3 6 0.671978 0.327408 0.524280 11.00000 0.02876 0.02741 = 0.02075 0.00100 -0.00098 -0.00045 N4 6 0.694301 0.380691 0.476015 11.00000 0.02281 0.02383 = 0.02156 -0.00191 0.00214 0.00080 N5 6 0.618087 0.250000 0.388668 10.50000 0.01841 0.01992 = 0.01994 0.00000 -0.00043 0.00000 C1 1 0.196848 0.339459 0.461488 11.00000 0.02437 0.03480 = 0.03667 -0.00246 0.00674 0.00085 AFIX 43 H1 2 0.123652 0.311599 0.489098 11.00000 -1.20000 AFIX 0 C2 1 0.151888 0.394513 0.417548 11.00000 0.02316 0.03764 = 0.03684 -0.00152 -0.00186 0.00763 AFIX 43 H2 2 0.045392 0.411321 0.408617 11.00000 -1.20000 AFIX 0 C3 1 0.295216 0.419758 0.389477 11.00000 0.02865 0.02848 = 0.02666 -0.00035 -0.00269 0.00537 AFIX 43 H3 2 0.305249 0.457904 0.356603 11.00000 -1.20000 AFIX 0 C4 1 0.756147 0.342416 0.585198 11.00000 0.03773 0.03745 = 0.02403 -0.00135 -0.00697 -0.00030 AFIX 43 H4 2 0.761171 0.314007 0.628089 11.00000 -1.20000 AFIX 0 C5 1 0.834907 0.404861 0.577362 11.00000 0.03136 0.03659 = 0.03169 -0.00662 -0.00885 -0.00136 AFIX 43 H5 2 0.903593 0.427152 0.612235 11.00000 -1.20000 AFIX 0 C6 1 0.792071 0.427853 0.507779 11.00000 0.02303 0.02808 = 0.03050 -0.00532 -0.00060 -0.00142 AFIX 43 H6 2 0.826046 0.470110 0.485831 11.00000 -1.20000 AFIX 0 C7 1 0.662351 0.455078 0.361639 11.00000 0.02413 0.02477 = 0.02075 -0.00120 -0.00201 0.00087 C8 1 0.598544 0.518317 0.386476 11.00000 0.02539 0.02959 = 0.02392 -0.00252 0.00189 0.00169 AFIX 43 H8 2 0.510863 0.517594 0.420616 11.00000 -1.20000 AFIX 0 C9 1 0.658261 0.581804 0.363216 11.00000 0.03241 0.02234 = 0.02829 -0.00536 -0.00361 0.00460 AFIX 43 H9 2 0.610734 0.623246 0.381368 11.00000 -1.20000 AFIX 0 C10 1 0.786968 0.585379 0.313607 11.00000 0.03306 0.02433 = 0.02418 0.00080 -0.00698 -0.00426 C11 1 0.854268 0.523529 0.289294 11.00000 0.02804 0.03185 = 0.02353 -0.00306 0.00323 -0.00546 AFIX 43 H11 2 0.943360 0.524415 0.255930 11.00000 -1.20000 AFIX 0 C12 1 0.792995 0.460427 0.313132 11.00000 0.02707 0.02470 = 0.02287 -0.00429 0.00081 0.00129 AFIX 43 H12 2 0.842342 0.419145 0.295587 11.00000 -1.20000 AFIX 0 C13 1 0.853224 0.654328 0.289979 11.00000 0.05225 0.02766 = 0.04056 0.00498 -0.00349 -0.00696 AFIX 137 H13A 2 0.907233 0.676521 0.332106 11.00000 -1.50000 H13B 2 0.764186 0.683777 0.272680 11.00000 -1.50000 H13C 2 0.931477 0.647670 0.249735 11.00000 -1.50000 AFIX 0 C14 1 0.632827 0.311655 0.352459 11.00000 0.01931 0.02428 = 0.02050 0.00088 0.00117 0.00013 C15 1 0.649748 0.311450 0.275242 11.00000 0.03500 0.02247 = 0.02008 0.00340 0.00118 -0.00143 AFIX 43 H15 2 0.656844 0.354035 0.249163 11.00000 -1.20000 AFIX 0 C16 1 0.656160 0.250000 0.236918 10.50000 0.04506 0.03153 = 0.01697 0.00000 0.00163 0.00000 AFIX 43 H16 2 0.664940 0.250000 0.184435 10.50000 -1.20000 AFIX 0 B1 3 0.605700 0.383234 0.398462 11.00000 0.02215 0.02288 = 0.02114 0.00004 0.00208 0.00200 HKLF 4 REM ln582yellow_a.res in Pnma REM wR2 = 0.1285, GooF = S = 1.073, Restrained GooF = 1.073 for all data REM R1 = 0.0432 for 2721 Fo > 4sig(Fo) and 0.0657 for all 3656 data REM 206 parameters refined using 0 restraints END WGHT 0.0716 0.6677 REM Highest difference peak 0.429, deepest hole -0.580, 1-sigma level 0.086 Q1 1 0.6327 0.4218 0.3786 11.00000 0.05 0.43 Q2 1 0.6503 0.4831 0.3792 11.00000 0.05 0.41 Q3 1 0.6293 0.5445 0.3638 11.00000 0.05 0.40 Q4 1 0.6927 0.4581 0.3215 11.00000 0.05 0.34 Q5 1 0.8177 0.6189 0.3032 11.00000 0.05 0.34 Q6 1 0.5451 0.5207 0.3842 11.00000 0.05 0.34 Q7 1 0.7550 0.4587 0.3593 11.00000 0.05 0.32 Q8 1 0.6395 0.2801 0.2568 11.00000 0.05 0.30 Q9 1 0.7123 0.4163 0.5005 11.00000 0.05 0.30 Q10 1 0.7926 0.4964 0.2943 11.00000 0.05 0.29 Q11 1 0.1724 0.3590 0.4209 11.00000 0.05 0.29 Q12 1 0.6862 0.3579 0.4998 11.00000 0.05 0.29 Q13 1 0.8064 0.5574 0.3026 11.00000 0.05 0.28 Q14 1 0.7413 0.5817 0.3504 11.00000 0.05 0.28 Q15 1 0.6169 0.5924 0.3602 11.00000 0.05 0.27 Q16 1 0.1389 0.2837 0.4810 11.00000 0.05 0.26 Q17 1 0.5850 0.5605 0.3986 11.00000 0.05 0.25 Q18 1 0.6266 0.2500 0.5018 10.50000 0.05 0.25 Q19 1 0.8056 0.4465 0.3040 11.00000 0.05 0.24 Q20 1 0.4213 0.2961 0.4806 11.00000 0.05 0.24 ; _shelx_res_checksum 29552 _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_ln620_nh_sq _database_code_depnum_ccdc_archive 'CCDC 2044410' loop_ _audit_author_name _audit_author_address 'Benjamin S. Gelfand' ;University of Calgary Canada ; _audit_update_record ; 2020-11-14 deposited with the CCDC. 2020-12-22 downloaded from the CCDC. ; _audit_creation_date 2020-03-19 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2017/1 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C45 H50 B2 Fe N10 O' _chemical_formula_sum 'C45 H50 B2 Fe N10 O' _chemical_formula_weight 824.42 _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 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 13 _space_group_name_H-M_alt 'P 1 2/c 1' _space_group_name_Hall '-P 2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 18.7182(7) _cell_length_b 24.1607(11) _cell_length_c 23.6620(9) _cell_angle_alpha 90 _cell_angle_beta 98.957(3) _cell_angle_gamma 90 _cell_volume 10570.5(7) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9900 _cell_measurement_temperature 173 _cell_measurement_theta_max 68.204 _cell_measurement_theta_min 2.389 _shelx_estimated_absorpt_T_max 0.725 _shelx_estimated_absorpt_T_min 0.656 _exptl_absorpt_coefficient_mu 2.588 _exptl_absorpt_correction_T_max 0.7531 _exptl_absorpt_correction_T_min 0.5557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0798 before and 0.0659 after correction. The Ratio of minimum to maximum transmission is 0.7379. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.036 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 3472 _exptl_crystal_size_max 0.178 _exptl_crystal_size_mid 0.135 _exptl_crystal_size_min 0.133 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0704 _diffrn_reflns_av_unetI/netI 0.0660 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 19096 _diffrn_reflns_point_group_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.348 _diffrn_reflns_theta_min 1.828 _diffrn_ambient_temperature 173.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 13918 _reflns_number_total 19096 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _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 ? _computing_data_collection ? _computing_data_reduction ? _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 1.145 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.073 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 1194 _refine_ls_number_reflns 19096 _refine_ls_number_restraints 542 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0677 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1188P)^2^+1.7449P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1758 _refine_ls_wR_factor_ref 0.1953 _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 2. Restrained distances C66A-C70A \\sim C70A-C68A \\sim C66-C70 \\sim C68-C70 with sigma of 0.02 C11-C13 \\sim C9-C13 \\sim C13A-C11A \\sim C9A-C13A with sigma of 0.02 C7-B1 \\sim C7A-B1 with sigma of 0.02 C13A-C10A \\sim C13-C10 with sigma of 0.01 C64-B4 \\sim C64A-B4 with sigma of 0.02 C70A-C67A \\sim C70-C67 with sigma of 0.01 Fe1-H10 \\sim H20-Fe2 with sigma of 0.02 C90A-C81 \\sim C90-C81 \\sim C88A-C81 \\sim C88-C81 \\sim C89A-C81 \\sim C89-C81 with sigma of 0.02 C89A-C90A \\sim C89-C90 \\sim C90A-C88A \\sim C90-C88 \\sim C88A-C89A \\sim C88-C89 with sigma of 0.02 C90A-C87 \\sim C90-C87 \\sim C88A-C87 \\sim C88-C87 \\sim C89A-C87 \\sim C89-C87 with sigma of 0.01 3. Restrained planarity C10, C11, C12, C7, C8, C9, C13 with sigma of 0.1 C13A, C11A, C12A, C8A, C7A with sigma of 0.1 4. Uiso/Uaniso restraints and constraints C10 \\sim C11 \\sim C12 \\sim C7 \\sim C8 \\sim C9 \\sim C13 \\sim C11A \\sim C12A \\sim C7A \\sim C8A \\sim C9A \\sim C10A \\sim C13A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C64A \\sim C65A \\sim C66A \\sim C67A \\sim C68A \\sim C69A \\sim C70A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C87) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C89A) \\sim Ueq, Uanis(C88A) \\sim Ueq, Uanis(C90A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 5. Others Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)= Sof(H9A)=Sof(C10A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=1-FVAR(1) Sof(C10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C7)=Sof(C8)=Sof(H8)=Sof(C9)= Sof(H9)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=FVAR(1) Sof(C64A)=Sof(C69A)=Sof(H69A)=Sof(C68A)=Sof(H68A)=Sof(C67A)=Sof(C66A)= Sof(H66A)=Sof(C65A)=Sof(H65A)=Sof(C70A)=Sof(H70D)=Sof(H70E)=Sof(H70F)=1-FVAR(2) Sof(C64)=Sof(C69)=Sof(H69)=Sof(C68)=Sof(H68)=Sof(C67)=Sof(C66)=Sof(H66)= Sof(C65)=Sof(H65)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=FVAR(2) Sof(C89A)=Sof(H89D)=Sof(H89E)=Sof(H89F)=Sof(C88A)=Sof(H88D)=Sof(H88E)= Sof(H88F)=Sof(C90A)=Sof(H90D)=Sof(H90E)=Sof(H90F)=1-FVAR(3) Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(H88C)=Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(H89C)= Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(H90C)=FVAR(3) 6.a Me refined with riding coordinates: C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C89A(H89D,H89E, H89F), C88A(H88D,H88E,H88F), C90A(H90D,H90E,H90F) 6.b Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C8(H8), C9(H9), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20A), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C29(H29), C30(H30), C35(H35), C37(H37), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C53(H53), C54(H54), C56(H56), C57(H57), C60(H60), C61(H61), C62(H62), C69(H69), C68(H68), C66(H66), C65(H65), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C80(H80), C82(H82), C11A(H11A), C12A(H12A), C8A(H8A), C9A(H9A), C69A(H69A), C68A(H68A), C66A(H66A), C65A(H65A) 6.c Fitted hexagon refined as free rotating group: C10(C11,C12,C7,C8,C9), C64(C69,C68,C67,C66,C65), C11A(C12A,C7A,C8A,C9A,C10A), C64A(C69A,C68A,C67A,C66A,C65A) 6.d Idealised Me refined as rotating group: C13(H13A,H13B,H13C), C31(H31A,H31B,H31C), C39(H39A,H39B,H39C), C40(H40A,H40B, H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A, H45B,H45C), C58(H58A,H58B,H58C), C70(H70A,H70B,H70C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C13A(H13D,H13E,H13F), C70A(H70D,H70E, H70F) ; _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 Fe1 Fe 0.57738(2) 0.12409(2) 0.62012(2) 0.03117(12) Uani 1 1 d D . . . . O1 O 0.69965(15) 0.28430(10) 0.65347(12) 0.0595(7) Uani 1 1 d . . . . . N1 N 0.55469(13) 0.15776(10) 0.54177(10) 0.0339(5) Uani 1 1 d . . . . . N2 N 0.48522(14) 0.15857(11) 0.51302(10) 0.0364(5) Uani 1 1 d . . . . . N3 N 0.49636(13) 0.16986(10) 0.63714(10) 0.0338(5) Uani 1 1 d . . . . . N4 N 0.43166(13) 0.16900(11) 0.60176(10) 0.0360(5) Uani 1 1 d . . . . . N5 N 0.50962(13) 0.06034(10) 0.59282(9) 0.0331(5) Uani 1 1 d . . . . . N6 N 0.59171(13) 0.08950(10) 0.69619(10) 0.0349(5) Uani 1 1 d . . . . . N7 N 0.60442(14) 0.03446(11) 0.70123(10) 0.0371(5) Uani 1 1 d . . . . . N8 N 0.65925(13) 0.07936(10) 0.60061(10) 0.0347(5) Uani 1 1 d . . . . . N9 N 0.66564(14) 0.02450(11) 0.61399(10) 0.0370(5) Uani 1 1 d . . . . . N10 N 0.63947(14) 0.18254(11) 0.64275(10) 0.0367(5) Uani 1 1 d . . . . . C1 C 0.59637(18) 0.18078(14) 0.50834(14) 0.0435(7) Uani 1 1 d . . . . . H1 H 0.646921 0.186666 0.518525 0.052 Uiso 1 1 calc R . . . . C2 C 0.5559(2) 0.19529(16) 0.45593(14) 0.0520(8) Uani 1 1 d . . . . . H2 H 0.572669 0.211739 0.423973 0.062 Uiso 1 1 calc R . . . . C3 C 0.4864(2) 0.18052(16) 0.46081(14) 0.0498(8) Uani 1 1 d . . . . . H3 H 0.445478 0.185047 0.431925 0.060 Uiso 1 1 calc R . . . . C4 C 0.49136(17) 0.20870(12) 0.67650(12) 0.0359(6) Uani 1 1 d . . . . . H4 H 0.529328 0.218580 0.706276 0.043 Uiso 1 1 calc R . . . . C5 C 0.42308(19) 0.23267(13) 0.66798(13) 0.0421(7) Uani 1 1 d . . . . . H5 H 0.405202 0.260840 0.690054 0.050 Uiso 1 1 calc R . . . . C6 C 0.38712(17) 0.20622(13) 0.62012(12) 0.0397(6) Uani 1 1 d . . . . . H6 H 0.338646 0.213220 0.602931 0.048 Uiso 1 1 calc R . . . . C10 C 0.19724(17) 0.1641(3) 0.4604(2) 0.0719(17) Uani 0.613(6) 1 d D U P A 1 C11 C 0.2138(2) 0.1222(2) 0.5005(2) 0.0589(16) Uani 0.613(6) 1 d DG U P A 1 H11 H 0.176468 0.099237 0.510488 0.071 Uiso 0.613(6) 1 calc R . P A 1 C12 C 0.2850(3) 0.11376(19) 0.5260(2) 0.0476(13) Uani 0.613(6) 1 d G U P A 1 H12 H 0.296357 0.085111 0.553449 0.057 Uiso 0.613(6) 1 calc R . P A 1 C7 C 0.33967(19) 0.1473(2) 0.51142(19) 0.0427(14) Uani 0.613(6) 1 d DG U P A 1 C8 C 0.3231(2) 0.1892(2) 0.47129(19) 0.0531(14) Uani 0.613(6) 1 d G U P A 1 H8 H 0.360443 0.212140 0.461303 0.064 Uiso 0.613(6) 1 calc R . P A 1 C9 C 0.2519(2) 0.1976(2) 0.44577(18) 0.0669(16) Uani 0.613(6) 1 d DG U P A 1 H9 H 0.240554 0.226267 0.418342 0.080 Uiso 0.613(6) 1 calc R . P A 1 C13 C 0.1180(4) 0.1736(5) 0.4308(5) 0.110(3) Uani 0.613(6) 1 d D U P A 1 H13A H 0.085485 0.149741 0.448641 0.165 Uiso 0.613(6) 1 calc GR . P A 1 H13B H 0.113911 0.164551 0.390077 0.165 Uiso 0.613(6) 1 calc GR . P A 1 H13C H 0.104800 0.212412 0.435163 0.165 Uiso 0.613(6) 1 calc GR . P A 1 C14 C 0.44590(16) 0.07138(13) 0.55776(11) 0.0349(6) Uani 1 1 d . . . . . C15 C 0.40620(17) 0.02761(14) 0.53039(13) 0.0412(7) Uani 1 1 d . . . . . H15 H 0.362141 0.035161 0.505803 0.049 Uiso 1 1 calc R . . . . C16 C 0.42935(18) -0.02639(14) 0.53816(13) 0.0428(7) Uani 1 1 d . . . . . H16 H 0.402589 -0.055901 0.518533 0.051 Uiso 1 1 calc R . . . . C17 C 0.49264(18) -0.03638(13) 0.57532(13) 0.0405(6) Uani 1 1 d . . . . . H17 H 0.509776 -0.073252 0.581350 0.049 Uiso 1 1 calc R . . . . C18 C 0.53141(16) 0.00696(12) 0.60392(11) 0.0343(6) Uani 1 1 d . . . . . C19 C 0.58976(17) 0.10889(14) 0.74860(13) 0.0403(7) Uani 1 1 d . . . . . H19 H 0.582244 0.146525 0.757694 0.048 Uiso 1 1 calc R . . . . C20 C 0.60037(19) 0.06583(15) 0.78809(13) 0.0454(7) Uani 1 1 d . . . . . H20A H 0.601279 0.068074 0.828284 0.054 Uiso 1 1 calc R . . . . C21 C 0.60921(18) 0.01947(14) 0.75649(13) 0.0425(7) Uani 1 1 d . . . . . H21 H 0.617339 -0.016997 0.771095 0.051 Uiso 1 1 calc R . . . . C22 C 0.71280(16) 0.09205(14) 0.57298(13) 0.0416(7) Uani 1 1 d . . . . . H22 H 0.721999 0.128042 0.559636 0.050 Uiso 1 1 calc R . . . . C23 C 0.75396(18) 0.04553(15) 0.56605(15) 0.0479(8) Uani 1 1 d . . . . . H23 H 0.795421 0.043244 0.547557 0.057 Uiso 1 1 calc R . . . . C24 C 0.72157(18) 0.00350(15) 0.59181(14) 0.0441(7) Uani 1 1 d . . . . . H24 H 0.736310 -0.034168 0.593617 0.053 Uiso 1 1 calc R . . . . C25 C 0.63103(19) -0.06414(13) 0.66961(13) 0.0410(7) Uani 1 1 d . . . . . C26 C 0.7034(2) -0.07629(15) 0.68865(16) 0.0519(8) Uani 1 1 d . . . . . H26 H 0.738271 -0.047588 0.689466 0.062 Uiso 1 1 calc R . . . . C27 C 0.7263(2) -0.12861(18) 0.7064(2) 0.0661(11) Uani 1 1 d . . . . . H27 H 0.776284 -0.135160 0.718779 0.079 Uiso 1 1 calc R . . . . C28 C 0.6773(3) -0.17208(16) 0.70640(19) 0.0646(11) Uani 1 1 d . . . . . C29 C 0.6053(3) -0.15957(16) 0.69321(17) 0.0606(10) Uani 1 1 d . . . . . H29 H 0.570331 -0.187381 0.696469 0.073 Uiso 1 1 calc R . . . . C30 C 0.5827(2) -0.10693(14) 0.67516(14) 0.0487(8) Uani 1 1 d . . . . . H30 H 0.532293 -0.099772 0.666223 0.058 Uiso 1 1 calc R . . . . C31 C 0.7043(4) -0.2305(2) 0.7215(3) 0.108(2) Uani 1 1 d . . . . . H31A H 0.710828 -0.235461 0.763123 0.162 Uiso 1 1 calc GR . . . . H31B H 0.750644 -0.236302 0.707981 0.162 Uiso 1 1 calc GR . . . . H31C H 0.668888 -0.257418 0.703208 0.162 Uiso 1 1 calc GR . . . . C32 C 0.70192(16) 0.18971(13) 0.67722(12) 0.0376(6) Uani 1 1 d . . . . . C33 C 0.73062(19) 0.24695(14) 0.68380(14) 0.0444(7) Uani 1 1 d . . . . . C34 C 0.7949(2) 0.25615(15) 0.72737(15) 0.0509(8) Uani 1 1 d . . . . . C35 C 0.82383(19) 0.21159(16) 0.75696(14) 0.0508(8) Uani 1 1 d . . . . . H35 H 0.863540 0.217929 0.786492 0.061 Uiso 1 1 calc R . . . . C36 C 0.79964(17) 0.15536(15) 0.74755(14) 0.0438(7) Uani 1 1 d . . . . . C37 C 0.74009(16) 0.14524(14) 0.70832(13) 0.0401(6) Uani 1 1 d . . . . . H37 H 0.723640 0.108287 0.701469 0.048 Uiso 1 1 calc R . . . . C38 C 0.8259(3) 0.31499(18) 0.73594(18) 0.0676(12) Uani 1 1 d . . . . . C39 C 0.7691(3) 0.35552(19) 0.7507(2) 0.0876(17) Uani 1 1 d . . . . . H39A H 0.726600 0.354453 0.720767 0.131 Uiso 1 1 calc GR . . . . H39B H 0.789280 0.393023 0.753472 0.131 Uiso 1 1 calc GR . . . . H39C H 0.754912 0.345116 0.787451 0.131 Uiso 1 1 calc GR . . . . C40 C 0.8529(3) 0.33347(19) 0.6808(2) 0.0739(13) Uani 1 1 d . . . . . H40A H 0.892762 0.309476 0.673680 0.111 Uiso 1 1 calc GR . . . . H40B H 0.869853 0.371843 0.684945 0.111 Uiso 1 1 calc GR . . . . H40C H 0.813241 0.330870 0.648529 0.111 Uiso 1 1 calc GR . . . . C41 C 0.8914(3) 0.3161(2) 0.7844(2) 0.106(2) Uani 1 1 d . . . . . H41A H 0.875194 0.307776 0.820940 0.158 Uiso 1 1 calc GR . . . . H41B H 0.913589 0.352957 0.786352 0.158 Uiso 1 1 calc GR . . . . H41C H 0.926870 0.288433 0.776771 0.158 Uiso 1 1 calc GR . . . . C42 C 0.84032(19) 0.10943(16) 0.78339(16) 0.0512(8) Uani 1 1 d . . . . . C43 C 0.9210(2) 0.1123(2) 0.7782(2) 0.0682(11) Uani 1 1 d . . . . . H43A H 0.927166 0.105889 0.738354 0.102 Uiso 1 1 calc GR . . . . H43B H 0.947414 0.083806 0.802617 0.102 Uiso 1 1 calc GR . . . . H43C H 0.940063 0.148868 0.790408 0.102 Uiso 1 1 calc GR . . . . C44 C 0.8306(2) 0.11814(18) 0.84639(17) 0.0648(11) Uani 1 1 d . . . . . H44A H 0.848178 0.155030 0.858976 0.097 Uiso 1 1 calc GR . . . . H44B H 0.858300 0.090000 0.870355 0.097 Uiso 1 1 calc GR . . . . H44C H 0.779306 0.114919 0.849829 0.097 Uiso 1 1 calc GR . . . . C45 C 0.8125(2) 0.05226(17) 0.7639(2) 0.0653(11) Uani 1 1 d . . . . . H45A H 0.761779 0.048715 0.769098 0.098 Uiso 1 1 calc GR . . . . H45B H 0.841437 0.023934 0.786615 0.098 Uiso 1 1 calc GR . . . . H45C H 0.816367 0.047314 0.723356 0.098 Uiso 1 1 calc GR . . . . B1 B 0.42317(19) 0.13529(16) 0.54408(14) 0.0387(7) Uani 1 1 d D . . . . B2 B 0.6075(2) -0.00222(15) 0.64692(14) 0.0381(7) Uani 1 1 d . . . . . Fe2 Fe 0.64905(2) 0.38160(2) 0.46216(2) 0.03540(13) Uani 1 1 d D . . . . O2 O 0.76192(12) 0.22259(10) 0.52313(12) 0.0541(6) Uani 1 1 d . . . . . N11 N 0.71880(14) 0.41687(11) 0.41937(11) 0.0409(6) Uani 1 1 d . . . . . N12 N 0.73161(14) 0.47171(11) 0.42515(11) 0.0413(6) Uani 1 1 d . . . . . N13 N 0.68948(14) 0.42700(11) 0.52987(11) 0.0395(6) Uani 1 1 d . . . . . N14 N 0.70533(14) 0.48164(11) 0.52531(11) 0.0399(6) Uani 1 1 d . . . . . N15 N 0.57983(14) 0.44442(11) 0.43746(10) 0.0377(5) Uani 1 1 d . . . . . N16 N 0.57282(13) 0.34686(11) 0.50130(11) 0.0379(5) Uani 1 1 d . . . . . N17 N 0.50262(14) 0.34327(12) 0.47566(12) 0.0419(6) Uani 1 1 d . . . . . N18 N 0.60635(15) 0.33658(12) 0.39520(11) 0.0416(6) Uani 1 1 d . . . . . N19 N 0.53331(15) 0.33639(12) 0.37815(12) 0.0456(6) Uani 1 1 d . . . . . N20 N 0.71095(14) 0.32344(11) 0.48786(11) 0.0397(5) Uani 1 1 d . . . . . C46 C 0.7621(2) 0.39741(16) 0.38479(16) 0.0518(8) Uani 1 1 d . . . . . H46 H 0.764651 0.359777 0.373667 0.062 Uiso 1 1 calc R . . . . C47 C 0.8029(2) 0.43989(18) 0.36726(18) 0.0605(10) Uani 1 1 d . . . . . H47 H 0.837708 0.437439 0.342123 0.073 Uiso 1 1 calc R . . . . C48 C 0.7824(2) 0.48632(16) 0.39390(16) 0.0537(8) Uani 1 1 d . . . . . H48 H 0.801045 0.522580 0.390756 0.064 Uiso 1 1 calc R . . . . C49 C 0.70510(18) 0.41404(15) 0.58535(14) 0.0457(7) Uani 1 1 d . . . . . H49 H 0.700999 0.378072 0.600745 0.055 Uiso 1 1 calc R . . . . C50 C 0.72820(19) 0.46080(16) 0.61725(15) 0.0501(8) Uani 1 1 d . . . . . H50 H 0.741595 0.463271 0.657583 0.060 Uiso 1 1 calc R . . . . C51 C 0.72750(18) 0.50271(15) 0.57786(14) 0.0458(7) Uani 1 1 d . . . . . H51 H 0.740443 0.540169 0.586255 0.055 Uiso 1 1 calc R . . . . C52 C 0.71850(18) 0.57063(14) 0.45956(15) 0.0449(7) Uani 1 1 d . . . . . C53 C 0.78115(19) 0.59125(16) 0.49360(17) 0.0530(8) Uani 1 1 d . . . . . H53 H 0.805606 0.568858 0.523513 0.064 Uiso 1 1 calc R . . . . C54 C 0.8080(2) 0.64312(17) 0.48467(19) 0.0595(9) Uani 1 1 d . . . . . H54 H 0.849611 0.655784 0.509455 0.071 Uiso 1 1 calc R . . . . C55 C 0.7762(2) 0.67776(16) 0.4405(2) 0.0586(10) Uani 1 1 d . . . . . C56 C 0.7165(2) 0.65722(16) 0.40579(19) 0.0603(10) Uani 1 1 d . . . . . H56 H 0.693877 0.679073 0.374686 0.072 Uiso 1 1 calc R . . . . C57 C 0.6884(2) 0.60571(15) 0.41478(16) 0.0515(8) Uani 1 1 d . . . . . H57 H 0.646823 0.593464 0.389607 0.062 Uiso 1 1 calc R . . . . C58 C 0.8070(3) 0.73442(18) 0.4303(3) 0.0862(16) Uani 1 1 d . . . . . H58A H 0.788422 0.761755 0.454912 0.129 Uiso 1 1 calc GR . . . . H58B H 0.792606 0.744895 0.390104 0.129 Uiso 1 1 calc GR . . . . H58C H 0.859909 0.733161 0.439195 0.129 Uiso 1 1 calc GR . . . . C59 C 0.60308(17) 0.49781(13) 0.44492(12) 0.0390(6) Uani 1 1 d . . . . . C60 C 0.55341(18) 0.54054(14) 0.44002(14) 0.0445(7) Uani 1 1 d . . . . . H60 H 0.569483 0.577507 0.447462 0.053 Uiso 1 1 calc R . . . . C61 C 0.48008(19) 0.52974(15) 0.42428(16) 0.0504(8) Uani 1 1 d . . . . . H61 H 0.445487 0.558789 0.421285 0.060 Uiso 1 1 calc R . . . . C62 C 0.45916(18) 0.47609(15) 0.41322(15) 0.0485(8) Uani 1 1 d . . . . . H62 H 0.409630 0.468130 0.400189 0.058 Uiso 1 1 calc R . . . . C63 C 0.50884(17) 0.43298(14) 0.42064(13) 0.0406(7) Uani 1 1 d . . . . . C64 C 0.39856(11) 0.36495(14) 0.37961(12) 0.0475(10) Uani 0.824(5) 1 d D U P B 1 C69 C 0.38888(14) 0.37846(15) 0.32182(12) 0.0572(11) Uani 0.824(5) 1 d G U P B 1 H69 H 0.429489 0.387271 0.303933 0.069 Uiso 0.824(5) 1 calc R . P B 1 C68 C 0.31977(16) 0.37908(15) 0.29020(10) 0.0617(12) Uani 0.824(5) 1 d DG U P B 1 H68 H 0.313145 0.388313 0.250702 0.074 Uiso 0.824(5) 1 calc R . P B 1 C67 C 0.26034(12) 0.36619(15) 0.31637(13) 0.0576(11) Uani 0.824(5) 1 d DG U P B 1 C66 C 0.27003(12) 0.35268(15) 0.37416(13) 0.0575(11) Uani 0.824(5) 1 d DG U P B 1 H66 H 0.229419 0.343868 0.392045 0.069 Uiso 0.824(5) 1 calc R . P B 1 C65 C 0.33914(15) 0.35206(15) 0.40578(9) 0.0515(10) Uani 0.824(5) 1 d G U P B 1 H65 H 0.345762 0.342825 0.445277 0.062 Uiso 0.824(5) 1 calc R . P B 1 C70 C 0.1845(3) 0.3653(3) 0.2812(3) 0.0810(18) Uani 0.824(5) 1 d D U P B 1 H70A H 0.151373 0.345951 0.302702 0.122 Uiso 0.824(5) 1 calc GR . P B 1 H70B H 0.185960 0.345994 0.244964 0.122 Uiso 0.824(5) 1 calc GR . P B 1 H70C H 0.167667 0.403330 0.273410 0.122 Uiso 0.824(5) 1 calc GR . P B 1 C71 C 0.57767(19) 0.32031(14) 0.55084(14) 0.0453(7) Uani 1 1 d . . . . . H71 H 0.620974 0.316008 0.577320 0.054 Uiso 1 1 calc R . . . . C72 C 0.5110(2) 0.29981(17) 0.55853(16) 0.0561(9) Uani 1 1 d . . . . . H72 H 0.499237 0.279784 0.590382 0.067 Uiso 1 1 calc R . . . . C73 C 0.46566(19) 0.31496(16) 0.50962(17) 0.0556(9) Uani 1 1 d . . . . . H73 H 0.415553 0.306489 0.501365 0.067 Uiso 1 1 calc R . . . . C74 C 0.6338(2) 0.29937(15) 0.36302(14) 0.0482(8) Uani 1 1 d . . . . . H74 H 0.683817 0.291158 0.365708 0.058 Uiso 1 1 calc R . . . . C75 C 0.5795(2) 0.27415(18) 0.32500(15) 0.0587(9) Uani 1 1 d . . . . . H75 H 0.584500 0.246353 0.297503 0.070 Uiso 1 1 calc R . . . . C76 C 0.5172(2) 0.29830(16) 0.33606(14) 0.0531(8) Uani 1 1 d . . . . . H76 H 0.469962 0.289742 0.317178 0.064 Uiso 1 1 calc R . . . . C77 C 0.78080(17) 0.31793(14) 0.50885(13) 0.0405(7) Uani 1 1 d . . . . . C78 C 0.80586(17) 0.26091(14) 0.52558(14) 0.0431(7) Uani 1 1 d . . . . . C79 C 0.88431(18) 0.25359(16) 0.54439(15) 0.0484(8) Uani 1 1 d . . . . . C80 C 0.92621(18) 0.29946(17) 0.54705(18) 0.0588(10) Uani 1 1 d . . . . . H80 H 0.976829 0.294482 0.557923 0.071 Uiso 1 1 calc R . . . . C81 C 0.9008(2) 0.35538(17) 0.53483(18) 0.0579(10) Uani 1 1 d D . . . . C82 C 0.83025(18) 0.36348(15) 0.51599(15) 0.0470(8) Uani 1 1 d . . . . . H82 H 0.812870 0.399922 0.507276 0.056 Uiso 1 1 calc R . . . . C83 C 0.91407(18) 0.19595(16) 0.56077(17) 0.0514(8) Uani 1 1 d . . . . . C84 C 0.9970(2) 0.1957(2) 0.5748(2) 0.0715(13) Uani 1 1 d . . . . . H84A H 1.017511 0.207764 0.541192 0.107 Uiso 1 1 calc GR . . . . H84B H 1.013878 0.158193 0.585514 0.107 Uiso 1 1 calc GR . . . . H84C H 1.012560 0.221025 0.606733 0.107 Uiso 1 1 calc GR . . . . C85 C 0.8932(2) 0.15516(19) 0.51181(19) 0.0656(10) Uani 1 1 d . . . . . H85A H 0.911462 0.118269 0.523674 0.098 Uiso 1 1 calc GR . . . . H85B H 0.914281 0.167154 0.478437 0.098 Uiso 1 1 calc GR . . . . H85C H 0.840400 0.153847 0.501844 0.098 Uiso 1 1 calc GR . . . . C86 C 0.8845(2) 0.17589(16) 0.61438(16) 0.0564(9) Uani 1 1 d . . . . . H86A H 0.901621 0.200515 0.646563 0.085 Uiso 1 1 calc GR . . . . H86B H 0.901576 0.138152 0.623766 0.085 Uiso 1 1 calc GR . . . . H86C H 0.831527 0.176224 0.606962 0.085 Uiso 1 1 calc GR . . . . C87 C 0.9557(2) 0.40254(18) 0.5421(2) 0.0762(13) Uani 1 1 d D U . . . C88 C 0.9980(4) 0.3995(3) 0.4904(4) 0.114(3) Uani 0.869(16) 1 d D U P C 1 H88A H 0.964328 0.404527 0.454730 0.172 Uiso 0.869(16) 1 calc R . P C 1 H88B H 1.034695 0.428793 0.494006 0.172 Uiso 0.869(16) 1 calc R . P C 1 H88C H 1.021640 0.363353 0.490091 0.172 Uiso 0.869(16) 1 calc R . P C 1 C89 C 0.9195(3) 0.4591(2) 0.5419(4) 0.084(2) Uani 0.869(16) 1 d D U P C 1 H89A H 0.884157 0.463135 0.506959 0.126 Uiso 0.869(16) 1 calc R . P C 1 H89B H 0.894806 0.462286 0.575384 0.126 Uiso 0.869(16) 1 calc R . P C 1 H89C H 0.956179 0.488188 0.543261 0.126 Uiso 0.869(16) 1 calc R . P C 1 C90 C 1.0112(4) 0.3945(3) 0.5959(4) 0.106(3) Uani 0.869(16) 1 d D U P C 1 H90A H 1.033601 0.357887 0.594873 0.159 Uiso 0.869(16) 1 calc R . P C 1 H90B H 1.048566 0.423120 0.597607 0.159 Uiso 0.869(16) 1 calc R . P C 1 H90C H 0.987192 0.397218 0.629731 0.159 Uiso 0.869(16) 1 calc R . P C 1 B3 B 0.6892(2) 0.50852(16) 0.46387(16) 0.0421(8) Uani 1 1 d . . . . . B4 B 0.4826(2) 0.36894(16) 0.41399(16) 0.0432(8) Uani 1 1 d D . . . . H10 H 0.6279(18) 0.2156(13) 0.6287(14) 0.035(8) Uiso 1 1 d D . . . . H20 H 0.690(2) 0.2894(13) 0.4876(17) 0.058(12) Uiso 1 1 d D . . . . C11A C 0.2165(4) 0.1155(4) 0.5222(3) 0.058(2) Uani 0.387(6) 1 d D U P A 2 H11A H 0.182576 0.101367 0.544444 0.070 Uiso 0.387(6) 1 calc R . P A 2 C12A C 0.2896(4) 0.1175(4) 0.5448(3) 0.054(2) Uani 0.387(6) 1 d G U P A 2 H12A H 0.305577 0.104587 0.582634 0.065 Uiso 0.387(6) 1 calc R . P A 2 C7A C 0.3392(3) 0.1382(4) 0.5123(3) 0.044(2) Uani 0.387(6) 1 d DG U P A 2 C8A C 0.3157(3) 0.1570(4) 0.4570(3) 0.0604(19) Uani 0.387(6) 1 d G U P A 2 H8A H 0.349651 0.171225 0.434689 0.072 Uiso 0.387(6) 1 calc R . P A 2 C9A C 0.2427(3) 0.1551(4) 0.4343(2) 0.0659(19) Uani 0.387(6) 1 d DG U P A 2 H9A H 0.226651 0.168006 0.396498 0.079 Uiso 0.387(6) 1 calc R . P A 2 C10A C 0.1930(3) 0.1344(4) 0.4669(3) 0.0561(19) Uani 0.387(6) 1 d DG U P A 2 C13A C 0.1121(4) 0.1308(6) 0.4393(5) 0.076(3) Uani 0.387(6) 1 d D U P A 2 H13D H 0.092399 0.094781 0.448028 0.115 Uiso 0.387(6) 1 calc GR . P A 2 H13E H 0.108022 0.135088 0.397690 0.115 Uiso 0.387(6) 1 calc GR . P A 2 H13F H 0.084771 0.160343 0.454653 0.115 Uiso 0.387(6) 1 calc GR . P A 2 C64A C 0.3984(5) 0.3571(7) 0.3900(7) 0.046(3) Uani 0.176(5) 1 d D U P B 2 C69A C 0.3724(7) 0.3906(6) 0.3436(7) 0.056(2) Uani 0.176(5) 1 d G U P B 2 H69A H 0.402996 0.417632 0.330659 0.067 Uiso 0.176(5) 1 calc R . P B 2 C68A C 0.3016(8) 0.3846(6) 0.3161(7) 0.060(2) Uani 0.176(5) 1 d DG U P B 2 H68A H 0.283788 0.407560 0.284407 0.072 Uiso 0.176(5) 1 calc R . P B 2 C67A C 0.2568(6) 0.3451(7) 0.3350(7) 0.063(3) Uani 0.176(5) 1 d DG U P B 2 C66A C 0.2828(7) 0.3116(7) 0.3814(6) 0.061(3) Uani 0.176(5) 1 d DG U P B 2 H66A H 0.252143 0.284598 0.394369 0.073 Uiso 0.176(5) 1 calc R . P B 2 C65A C 0.3536(7) 0.3176(7) 0.4089(6) 0.054(3) Uani 0.176(5) 1 d G U P B 2 H65A H 0.371352 0.294669 0.440622 0.065 Uiso 0.176(5) 1 calc R . P B 2 C70A C 0.1795(10) 0.3368(13) 0.3035(13) 0.088(6) Uani 0.176(5) 1 d D U P B 2 H70D H 0.151777 0.315005 0.327469 0.132 Uiso 0.176(5) 1 calc GR . P B 2 H70E H 0.181131 0.317063 0.267495 0.132 Uiso 0.176(5) 1 calc GR . P B 2 H70F H 0.156368 0.372868 0.295314 0.132 Uiso 0.176(5) 1 calc GR . P B 2 C89A C 0.9209(14) 0.4558(7) 0.5152(16) 0.081(15) Uani 0.131(16) 1 d D U P C 2 H89D H 0.876476 0.463598 0.530901 0.121 Uiso 0.131(16) 1 calc R . P C 2 H89E H 0.954695 0.486741 0.523806 0.121 Uiso 0.131(16) 1 calc R . P C 2 H89F H 0.909188 0.451128 0.473621 0.121 Uiso 0.131(16) 1 calc R . P C 2 C88A C 1.0246(11) 0.3906(11) 0.5176(17) 0.096(16) Uani 0.131(16) 1 d D U P C 2 H88D H 1.057006 0.422586 0.523916 0.144 Uiso 0.131(16) 1 calc R . P C 2 H88E H 1.048690 0.358063 0.536729 0.144 Uiso 0.131(16) 1 calc R . P C 2 H88F H 1.012498 0.383324 0.476512 0.144 Uiso 0.131(16) 1 calc R . P C 2 C90A C 0.9767(19) 0.4139(13) 0.6073(5) 0.072(11) Uani 0.131(16) 1 d D U P C 2 H90D H 0.932991 0.421716 0.623873 0.108 Uiso 0.131(16) 1 calc R . P C 2 H90E H 1.001081 0.381297 0.625941 0.108 Uiso 0.131(16) 1 calc R . P C 2 H90F H 1.009350 0.445811 0.613065 0.108 Uiso 0.131(16) 1 calc R . P C 2 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 Fe1 0.0270(2) 0.0366(2) 0.0288(2) -0.00134(15) 0.00087(17) -0.00274(18) O1 0.0604(15) 0.0448(14) 0.0633(15) 0.0081(11) -0.0215(13) -0.0111(12) N1 0.0279(11) 0.0423(13) 0.0307(11) -0.0006(9) 0.0017(10) -0.0040(10) N2 0.0313(12) 0.0449(14) 0.0318(11) 0.0011(9) 0.0011(10) -0.0035(10) N3 0.0311(12) 0.0391(13) 0.0301(11) 0.0007(9) 0.0011(10) -0.0005(10) N4 0.0262(11) 0.0444(14) 0.0358(12) 0.0009(10) -0.0005(10) -0.0003(10) N5 0.0307(12) 0.0402(13) 0.0289(11) -0.0010(8) 0.0060(10) -0.0043(10) N6 0.0307(12) 0.0378(13) 0.0352(12) -0.0031(9) 0.0017(10) 0.0000(10) N7 0.0346(12) 0.0398(14) 0.0359(12) 0.0014(10) 0.0019(10) -0.0004(10) N8 0.0284(11) 0.0399(13) 0.0346(12) -0.0024(9) 0.0012(10) -0.0018(10) N9 0.0347(12) 0.0386(13) 0.0371(12) -0.0048(9) 0.0042(10) -0.0011(10) N10 0.0350(13) 0.0389(14) 0.0348(12) 0.0019(9) 0.0009(10) -0.0001(10) C1 0.0362(15) 0.0482(18) 0.0461(17) 0.0056(13) 0.0067(14) -0.0030(13) C2 0.0491(19) 0.068(2) 0.0389(16) 0.0181(14) 0.0072(15) -0.0052(17) C3 0.0460(18) 0.065(2) 0.0365(16) 0.0116(14) -0.0002(14) -0.0035(16) C4 0.0376(15) 0.0395(15) 0.0302(13) 0.0026(10) 0.0041(12) 0.0023(12) C5 0.0476(18) 0.0434(17) 0.0364(14) -0.0001(11) 0.0106(14) 0.0079(14) C6 0.0344(14) 0.0490(18) 0.0356(14) 0.0018(12) 0.0051(12) 0.0043(13) C10 0.039(3) 0.111(4) 0.060(3) -0.004(3) -0.008(3) 0.012(3) C11 0.034(3) 0.092(4) 0.049(4) -0.010(3) 0.001(3) -0.007(3) C12 0.036(2) 0.069(3) 0.036(3) -0.007(2) 0.002(2) -0.005(2) C7 0.034(3) 0.052(3) 0.040(3) -0.007(2) 0.000(2) -0.010(2) C8 0.040(2) 0.074(4) 0.042(2) 0.003(2) -0.003(2) 0.005(3) C9 0.044(3) 0.103(4) 0.050(3) 0.007(3) -0.003(2) 0.021(3) C13 0.052(4) 0.164(9) 0.102(6) -0.015(7) -0.024(4) 0.015(6) C14 0.0294(13) 0.0478(17) 0.0279(13) -0.0010(11) 0.0056(11) -0.0071(12) C15 0.0359(15) 0.0489(18) 0.0375(15) -0.0026(12) 0.0017(13) -0.0087(13) C16 0.0442(17) 0.0471(18) 0.0371(15) -0.0067(12) 0.0060(13) -0.0135(14) C17 0.0437(16) 0.0376(16) 0.0400(15) -0.0018(11) 0.0063(13) -0.0042(13) C18 0.0348(14) 0.0389(15) 0.0301(13) -0.0031(10) 0.0074(12) -0.0049(12) C19 0.0386(16) 0.0466(17) 0.0346(14) -0.0052(12) 0.0019(12) 0.0057(13) C20 0.0474(18) 0.056(2) 0.0321(14) 0.0008(12) 0.0042(13) 0.0090(15) C21 0.0441(17) 0.0447(18) 0.0377(15) 0.0042(12) 0.0033(13) 0.0021(14) C22 0.0312(14) 0.0523(19) 0.0404(15) 0.0020(12) 0.0031(13) -0.0005(13) C23 0.0348(15) 0.063(2) 0.0474(17) -0.0004(14) 0.0121(14) 0.0020(15) C24 0.0370(16) 0.0504(19) 0.0439(16) -0.0044(13) 0.0029(13) 0.0057(14) C25 0.0466(17) 0.0407(17) 0.0350(14) -0.0018(11) 0.0044(13) 0.0002(13) C26 0.0467(19) 0.0471(19) 0.061(2) 0.0068(15) 0.0054(16) -0.0020(15) C27 0.059(2) 0.063(3) 0.077(3) 0.0170(19) 0.012(2) 0.013(2) C28 0.084(3) 0.042(2) 0.073(3) 0.0083(17) 0.028(2) 0.012(2) C29 0.079(3) 0.048(2) 0.057(2) 0.0015(15) 0.016(2) -0.0100(19) C30 0.054(2) 0.0463(18) 0.0441(17) 0.0039(13) 0.0038(15) -0.0012(15) C31 0.124(5) 0.060(3) 0.151(6) 0.038(3) 0.056(5) 0.025(3) C32 0.0307(14) 0.0471(17) 0.0335(14) -0.0009(11) 0.0004(12) -0.0075(13) C33 0.0436(17) 0.0448(18) 0.0407(16) 0.0020(12) -0.0063(14) -0.0072(14) C34 0.0476(19) 0.055(2) 0.0447(17) 0.0029(14) -0.0099(15) -0.0199(16) C35 0.0417(17) 0.064(2) 0.0411(16) 0.0063(14) -0.0104(14) -0.0143(16) C36 0.0328(15) 0.056(2) 0.0400(15) 0.0033(13) -0.0026(13) -0.0052(14) C37 0.0299(14) 0.0455(17) 0.0431(16) 0.0009(12) -0.0005(13) -0.0034(13) C38 0.077(3) 0.059(2) 0.055(2) 0.0037(17) -0.025(2) -0.026(2) C39 0.133(5) 0.056(3) 0.067(3) -0.011(2) -0.006(3) -0.020(3) C40 0.067(3) 0.070(3) 0.076(3) 0.019(2) -0.016(2) -0.029(2) C41 0.117(5) 0.083(4) 0.093(4) 0.019(3) -0.059(3) -0.056(3) C42 0.0343(17) 0.058(2) 0.057(2) 0.0091(15) -0.0069(15) -0.0039(15) C43 0.040(2) 0.080(3) 0.080(3) 0.013(2) -0.0072(19) 0.0011(19) C44 0.060(2) 0.076(3) 0.054(2) 0.0205(18) -0.0050(19) 0.001(2) C45 0.050(2) 0.055(2) 0.082(3) 0.0124(19) -0.018(2) 0.0056(18) B1 0.0334(16) 0.051(2) 0.0309(15) -0.0018(13) 0.0024(13) -0.0072(15) B2 0.0387(17) 0.0397(18) 0.0353(16) -0.0029(12) 0.0040(14) -0.0026(14) Fe2 0.0278(2) 0.0405(3) 0.0364(2) 0.00547(17) 0.00040(18) -0.00031(19) O2 0.0322(11) 0.0469(14) 0.0797(17) 0.0095(11) -0.0024(11) -0.0022(10) N11 0.0335(12) 0.0446(15) 0.0446(14) 0.0077(10) 0.0061(11) 0.0011(11) N12 0.0348(13) 0.0448(15) 0.0441(14) 0.0084(10) 0.0061(11) -0.0014(11) N13 0.0317(12) 0.0452(15) 0.0396(13) 0.0082(10) -0.0004(11) -0.0007(11) N14 0.0343(12) 0.0415(14) 0.0429(13) 0.0036(10) 0.0023(11) -0.0018(11) N15 0.0357(13) 0.0434(14) 0.0328(12) 0.0061(9) 0.0020(10) 0.0007(11) N16 0.0294(12) 0.0427(14) 0.0415(13) 0.0059(10) 0.0045(10) -0.0030(10) N17 0.0297(12) 0.0465(15) 0.0481(15) 0.0063(11) 0.0018(11) -0.0019(11) N18 0.0365(13) 0.0479(15) 0.0399(13) 0.0065(10) 0.0046(11) -0.0015(11) N19 0.0389(14) 0.0500(16) 0.0445(14) 0.0022(11) -0.0040(12) -0.0003(12) N20 0.0305(12) 0.0434(15) 0.0437(13) 0.0045(10) 0.0012(11) -0.0030(11) C46 0.0450(18) 0.057(2) 0.056(2) 0.0027(15) 0.0141(16) 0.0031(16) C47 0.057(2) 0.068(3) 0.062(2) 0.0046(18) 0.029(2) -0.0062(19) C48 0.050(2) 0.055(2) 0.058(2) 0.0085(15) 0.0149(17) -0.0044(16) C49 0.0383(16) 0.056(2) 0.0416(16) 0.0077(13) 0.0008(14) -0.0029(14) C50 0.0438(17) 0.061(2) 0.0421(16) 0.0030(14) -0.0037(14) -0.0064(16) C51 0.0379(16) 0.0493(19) 0.0483(17) -0.0034(13) 0.0010(14) -0.0034(14) C52 0.0372(16) 0.0452(18) 0.0522(18) 0.0030(13) 0.0072(14) -0.0014(14) C53 0.0397(17) 0.057(2) 0.062(2) 0.0051(16) 0.0050(16) -0.0057(16) C54 0.0360(17) 0.064(2) 0.078(3) -0.0100(19) 0.0085(18) -0.0120(17) C55 0.0417(18) 0.044(2) 0.093(3) 0.0052(18) 0.021(2) -0.0007(15) C56 0.050(2) 0.049(2) 0.083(3) 0.0144(18) 0.013(2) 0.0016(17) C57 0.0459(18) 0.051(2) 0.057(2) 0.0089(15) 0.0046(16) -0.0036(15) C58 0.058(3) 0.048(2) 0.155(5) 0.008(3) 0.027(3) -0.008(2) C59 0.0350(15) 0.0453(17) 0.0351(14) 0.0060(11) 0.0000(12) 0.0002(13) C60 0.0406(17) 0.0435(17) 0.0481(17) 0.0045(13) 0.0026(14) 0.0016(14) C61 0.0389(17) 0.0499(19) 0.062(2) 0.0122(15) 0.0051(15) 0.0073(15) C62 0.0315(15) 0.054(2) 0.0579(19) 0.0088(15) -0.0013(14) 0.0020(14) C63 0.0327(15) 0.0502(18) 0.0374(15) 0.0067(12) 0.0010(12) 0.0016(13) C64 0.0388(19) 0.049(2) 0.052(2) 0.0027(18) -0.0017(18) -0.0030(17) C69 0.046(2) 0.068(3) 0.053(2) 0.0081(19) -0.006(2) -0.004(2) C68 0.050(2) 0.075(3) 0.054(2) 0.008(2) -0.012(2) 0.003(2) C67 0.040(2) 0.060(3) 0.067(3) 0.005(2) -0.010(2) 0.000(2) C66 0.041(2) 0.063(3) 0.066(2) 0.000(2) 0.0011(19) 0.0053(19) C65 0.0381(19) 0.061(2) 0.053(2) 0.0007(18) -0.0017(17) 0.0015(18) C70 0.044(3) 0.101(5) 0.089(4) 0.011(3) -0.020(3) 0.002(3) C71 0.0461(18) 0.0459(18) 0.0419(16) 0.0083(12) 0.0011(14) -0.0024(14) C72 0.052(2) 0.064(2) 0.053(2) 0.0209(16) 0.0109(17) -0.0013(18) C73 0.0331(16) 0.060(2) 0.073(2) 0.0222(18) 0.0068(17) -0.0002(15) C74 0.0467(18) 0.057(2) 0.0422(16) -0.0009(14) 0.0120(15) -0.0023(16) C75 0.066(2) 0.069(2) 0.0427(18) -0.0078(15) 0.0130(18) -0.011(2) C76 0.052(2) 0.062(2) 0.0418(17) 0.0004(14) -0.0035(15) -0.0096(17) C77 0.0298(14) 0.0494(18) 0.0420(15) 0.0067(12) 0.0041(12) 0.0007(13) C78 0.0320(15) 0.0501(19) 0.0469(17) 0.0082(13) 0.0053(13) -0.0011(13) C79 0.0327(16) 0.060(2) 0.0520(18) 0.0155(15) 0.0055(14) 0.0013(15) C80 0.0299(15) 0.069(2) 0.074(2) 0.0315(19) -0.0047(16) -0.0030(16) C81 0.0358(17) 0.063(2) 0.071(2) 0.0274(18) -0.0029(17) -0.0056(16) C82 0.0349(16) 0.0478(19) 0.0563(19) 0.0145(14) 0.0006(15) -0.0023(14) C83 0.0337(16) 0.056(2) 0.062(2) 0.0137(16) 0.0017(15) 0.0038(15) C84 0.0384(19) 0.074(3) 0.098(3) 0.029(2) 0.000(2) 0.0109(19) C85 0.056(2) 0.069(3) 0.070(3) 0.0051(19) 0.005(2) 0.015(2) C86 0.055(2) 0.054(2) 0.059(2) 0.0156(16) 0.0014(17) -0.0009(17) C87 0.0448(19) 0.070(2) 0.105(3) 0.039(2) -0.015(2) -0.0128(18) C88 0.055(3) 0.116(5) 0.177(7) 0.074(5) 0.033(4) -0.009(3) C89 0.057(3) 0.061(3) 0.124(6) 0.021(3) -0.017(3) -0.022(2) C90 0.075(4) 0.078(4) 0.142(6) 0.045(4) -0.052(4) -0.031(3) B3 0.0361(18) 0.044(2) 0.0456(18) 0.0042(14) 0.0035(15) 0.0004(15) B4 0.0370(18) 0.048(2) 0.0426(18) 0.0056(14) -0.0002(15) 0.0003(15) C11A 0.040(3) 0.089(4) 0.042(4) 0.002(4) -0.006(3) -0.004(3) C12A 0.040(3) 0.076(4) 0.042(4) -0.007(4) -0.006(4) -0.008(3) C7A 0.034(4) 0.057(4) 0.039(4) 0.000(3) -0.001(3) 0.016(3) C8A 0.042(3) 0.086(4) 0.050(4) 0.012(4) 0.000(3) 0.006(4) C9A 0.043(3) 0.099(4) 0.051(3) 0.015(4) -0.004(3) 0.006(4) C10A 0.031(3) 0.086(4) 0.049(4) -0.002(4) -0.002(3) 0.003(4) C13A 0.030(4) 0.116(9) 0.077(6) -0.008(7) -0.009(5) 0.010(6) C64A 0.038(4) 0.049(5) 0.045(4) 0.012(4) -0.016(4) 0.010(4) C69A 0.044(4) 0.062(4) 0.056(4) 0.009(4) -0.008(4) 0.001(4) C68A 0.041(4) 0.069(4) 0.064(4) 0.004(4) -0.007(4) -0.002(4) C67A 0.041(4) 0.073(5) 0.072(5) 0.002(5) -0.003(4) 0.001(4) C66A 0.044(5) 0.067(5) 0.068(5) -0.003(5) -0.002(5) 0.001(5) C65A 0.040(4) 0.059(5) 0.060(5) -0.001(4) -0.004(4) 0.002(4) C70A 0.052(9) 0.102(11) 0.099(11) -0.002(10) -0.024(10) 0.007(10) C89A 0.080(17) 0.083(17) 0.081(17) 0.006(9) 0.016(10) -0.010(9) C88A 0.095(18) 0.097(18) 0.095(18) 0.008(10) 0.010(10) -0.004(10) C90A 0.069(14) 0.071(14) 0.074(14) -0.007(9) 0.006(9) -0.002(9) _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 Fe1 N1 2.008(2) . ? Fe1 N3 1.968(2) . ? Fe1 N5 2.036(2) . ? Fe1 N6 1.965(2) . ? Fe1 N8 1.988(2) . ? Fe1 N10 1.854(3) . ? O1 C33 1.239(4) . ? N1 N2 1.370(3) . ? N1 C1 1.318(4) . ? N2 C3 1.348(4) . ? N2 B1 1.572(4) . ? N3 N4 1.361(3) . ? N3 C4 1.336(4) . ? N4 C6 1.344(4) . ? N4 B1 1.576(4) . ? N5 C14 1.369(4) . ? N5 C18 1.366(4) . ? N6 N7 1.353(4) . ? N6 C19 1.331(4) . ? N7 C21 1.346(4) . ? N7 B2 1.569(4) . ? N8 N9 1.364(4) . ? N8 C22 1.315(4) . ? N9 C24 1.342(4) . ? N9 B2 1.572(4) . ? N10 C32 1.329(4) . ? C1 C2 1.394(5) . ? C2 C3 1.371(5) . ? C4 C5 1.389(4) . ? C5 C6 1.381(4) . ? C10 C11 1.3900 . ? C10 C9 1.3900 . ? C10 C13 1.554(7) . ? C11 C12 1.3900 . ? C12 C7 1.3900 . ? C7 C8 1.3900 . ? C7 B1 1.658(5) . ? C8 C9 1.3900 . ? C14 C15 1.393(4) . ? C14 B1 1.621(5) . ? C15 C16 1.378(5) . ? C16 C17 1.382(5) . ? C17 C18 1.389(4) . ? C18 B2 1.631(4) . ? C19 C20 1.392(4) . ? C20 C21 1.371(5) . ? C22 C23 1.387(5) . ? C23 C24 1.373(5) . ? C25 C26 1.391(5) . ? C25 C30 1.393(5) . ? C25 B2 1.627(5) . ? C26 C27 1.379(5) . ? C27 C28 1.394(6) . ? C28 C29 1.368(6) . ? C28 C31 1.524(6) . ? C29 C30 1.387(5) . ? C32 C33 1.483(4) . ? C32 C37 1.429(4) . ? C33 C34 1.474(4) . ? C34 C35 1.351(5) . ? C34 C38 1.537(5) . ? C35 C36 1.438(5) . ? C36 C37 1.357(4) . ? C36 C42 1.526(5) . ? C38 C39 1.526(7) . ? C38 C40 1.538(6) . ? C38 C41 1.543(6) . ? C42 C43 1.536(5) . ? C42 C44 1.544(6) . ? C42 C45 1.522(5) . ? B1 C7A 1.636(6) . ? Fe2 N11 1.967(3) . ? Fe2 N13 1.991(3) . ? Fe2 N15 2.022(3) . ? Fe2 N16 2.002(2) . ? Fe2 N18 1.984(3) . ? Fe2 N20 1.862(3) . ? O2 C78 1.234(4) . ? N11 N12 1.350(4) . ? N11 C46 1.324(4) . ? N12 C48 1.340(4) . ? N12 B3 1.578(4) . ? N13 N14 1.361(4) . ? N13 C49 1.337(4) . ? N14 C51 1.348(4) . ? N14 B3 1.578(4) . ? N15 C59 1.364(4) . ? N15 C63 1.355(4) . ? N16 N17 1.362(4) . ? N16 C71 1.327(4) . ? N17 C73 1.329(4) . ? N17 B4 1.576(4) . ? N18 N19 1.364(4) . ? N18 C74 1.332(4) . ? N19 C76 1.355(4) . ? N19 B4 1.578(5) . ? N20 C77 1.331(4) . ? C46 C47 1.381(5) . ? C47 C48 1.370(5) . ? C49 C50 1.390(5) . ? C50 C51 1.375(5) . ? C52 C53 1.406(5) . ? C52 C57 1.405(5) . ? C52 B3 1.607(5) . ? C53 C54 1.379(5) . ? C54 C55 1.397(6) . ? C55 C56 1.373(6) . ? C55 C58 1.520(5) . ? C56 C57 1.381(5) . ? C59 C60 1.382(5) . ? C59 B3 1.625(5) . ? C60 C61 1.390(5) . ? C61 C62 1.368(5) . ? C62 C63 1.389(5) . ? C63 B4 1.623(5) . ? C64 C69 1.3900 . ? C64 C65 1.3900 . ? C64 B4 1.658(4) . ? C69 C68 1.3900 . ? C68 C67 1.3900 . ? C67 C66 1.3900 . ? C67 C70 1.529(5) . ? C66 C65 1.3900 . ? C71 C72 1.380(5) . ? C72 C73 1.374(5) . ? C74 C75 1.389(5) . ? C75 C76 1.364(6) . ? C77 C78 1.489(4) . ? C77 C82 1.431(5) . ? C78 C79 1.477(4) . ? C79 C80 1.354(5) . ? C79 C83 1.527(5) . ? C80 C81 1.446(5) . ? C81 C82 1.341(5) . ? C81 C87 1.526(5) . ? C83 C84 1.536(5) . ? C83 C85 1.525(6) . ? C83 C86 1.539(5) . ? C87 C88 1.559(6) . ? C87 C89 1.525(6) . ? C87 C90 1.525(5) . ? C87 C89A 1.536(8) . ? C87 C88A 1.521(8) . ? C87 C90A 1.555(8) . ? B4 C64A 1.616(10) . ? C11A C12A 1.3900 . ? C11A C10A 1.3900 . ? C12A C7A 1.3900 . ? C7A C8A 1.3900 . ? C8A C9A 1.3900 . ? C9A C10A 1.3900 . ? C10A C13A 1.557(8) . ? C64A C69A 1.3900 . ? C64A C65A 1.3900 . ? C69A C68A 1.3900 . ? C68A C67A 1.3900 . ? C67A C66A 1.3900 . ? C67A C70A 1.533(9) . ? C66A C65A 1.3900 . ? 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 N1 Fe1 N5 88.96(10) . . ? N3 Fe1 N1 84.40(10) . . ? N3 Fe1 N5 91.62(10) . . ? N3 Fe1 N8 178.10(10) . . ? N6 Fe1 N1 175.59(10) . . ? N6 Fe1 N3 92.93(10) . . ? N6 Fe1 N5 87.61(10) . . ? N6 Fe1 N8 88.93(10) . . ? N8 Fe1 N1 93.77(10) . . ? N8 Fe1 N5 88.83(10) . . ? N10 Fe1 N1 89.49(10) . . ? N10 Fe1 N3 88.93(11) . . ? N10 Fe1 N5 178.29(10) . . ? N10 Fe1 N6 93.98(10) . . ? N10 Fe1 N8 90.57(11) . . ? N2 N1 Fe1 120.79(18) . . ? C1 N1 Fe1 131.7(2) . . ? C1 N1 N2 107.5(2) . . ? N1 N2 B1 118.4(2) . . ? C3 N2 N1 108.1(3) . . ? C3 N2 B1 133.5(3) . . ? N4 N3 Fe1 120.37(18) . . ? C4 N3 Fe1 132.6(2) . . ? C4 N3 N4 106.7(2) . . ? N3 N4 B1 120.0(2) . . ? C6 N4 N3 109.2(2) . . ? C6 N4 B1 129.9(3) . . ? C14 N5 Fe1 119.1(2) . . ? C18 N5 Fe1 120.1(2) . . ? C18 N5 C14 120.4(3) . . ? N7 N6 Fe1 119.73(18) . . ? C19 N6 Fe1 133.2(2) . . ? C19 N6 N7 107.1(2) . . ? N6 N7 B2 120.8(2) . . ? C21 N7 N6 109.5(2) . . ? C21 N7 B2 129.6(3) . . ? N9 N8 Fe1 121.16(18) . . ? C22 N8 Fe1 131.6(2) . . ? C22 N8 N9 107.2(2) . . ? N8 N9 B2 118.1(2) . . ? C24 N9 N8 108.8(3) . . ? C24 N9 B2 132.9(3) . . ? C32 N10 Fe1 136.8(2) . . ? N1 C1 C2 110.4(3) . . ? C3 C2 C1 104.6(3) . . ? N2 C3 C2 109.3(3) . . ? N3 C4 C5 110.8(3) . . ? C6 C5 C4 104.3(3) . . ? N4 C6 C5 109.1(3) . . ? C11 C10 C9 120.0 . . ? C11 C10 C13 120.7(5) . . ? C9 C10 C13 119.3(5) . . ? C10 C11 C12 120.0 . . ? C7 C12 C11 120.0 . . ? C12 C7 C8 120.0 . . ? C12 C7 B1 117.3(3) . . ? C8 C7 B1 122.7(3) . . ? C7 C8 C9 120.0 . . ? C8 C9 C10 120.0 . . ? N5 C14 C15 119.0(3) . . ? N5 C14 B1 118.9(3) . . ? C15 C14 B1 121.7(3) . . ? C16 C15 C14 121.5(3) . . ? C15 C16 C17 118.1(3) . . ? C16 C17 C18 120.6(3) . . ? N5 C18 C17 120.0(3) . . ? N5 C18 B2 117.0(2) . . ? C17 C18 B2 122.7(3) . . ? N6 C19 C20 109.9(3) . . ? C21 C20 C19 105.1(3) . . ? N7 C21 C20 108.3(3) . . ? N8 C22 C23 110.5(3) . . ? C24 C23 C22 104.8(3) . . ? N9 C24 C23 108.6(3) . . ? C26 C25 C30 115.3(3) . . ? C26 C25 B2 120.1(3) . . ? C30 C25 B2 124.5(3) . . ? C27 C26 C25 122.1(4) . . ? C26 C27 C28 121.2(4) . . ? C27 C28 C31 120.3(5) . . ? C29 C28 C27 117.2(4) . . ? C29 C28 C31 122.5(5) . . ? C28 C29 C30 121.0(4) . . ? C29 C30 C25 122.5(4) . . ? N10 C32 C33 117.1(3) . . ? N10 C32 C37 122.7(3) . . ? C37 C32 C33 120.2(3) . . ? O1 C33 C32 119.3(3) . . ? O1 C33 C34 123.5(3) . . ? C34 C33 C32 117.2(3) . . ? C33 C34 C38 118.8(3) . . ? C35 C34 C33 117.4(3) . . ? C35 C34 C38 123.8(3) . . ? C34 C35 C36 125.5(3) . . ? C35 C36 C42 118.9(3) . . ? C37 C36 C35 118.8(3) . . ? C37 C36 C42 122.3(3) . . ? C36 C37 C32 120.5(3) . . ? C34 C38 C40 108.9(4) . . ? C34 C38 C41 110.8(4) . . ? C39 C38 C34 111.2(4) . . ? C39 C38 C40 109.9(4) . . ? C39 C38 C41 108.6(4) . . ? C40 C38 C41 107.3(4) . . ? C36 C42 C43 109.6(3) . . ? C36 C42 C44 108.3(3) . . ? C43 C42 C44 109.6(3) . . ? C45 C42 C36 112.0(3) . . ? C45 C42 C43 108.1(4) . . ? C45 C42 C44 109.3(3) . . ? N2 B1 N4 103.7(2) . . ? N2 B1 C7 115.5(3) . . ? N2 B1 C14 104.1(3) . . ? N2 B1 C7A 119.8(4) . . ? N4 B1 C7 105.9(3) . . ? N4 B1 C14 109.4(2) . . ? N4 B1 C7A 109.7(4) . . ? C14 B1 C7 117.3(3) . . ? C14 B1 C7A 109.7(4) . . ? N7 B2 N9 106.9(2) . . ? N7 B2 C18 107.1(2) . . ? N7 B2 C25 107.0(2) . . ? N9 B2 C18 103.9(2) . . ? N9 B2 C25 111.6(3) . . ? C25 B2 C18 119.7(3) . . ? N11 Fe2 N13 88.62(11) . . ? N11 Fe2 N15 88.44(10) . . ? N11 Fe2 N16 176.15(11) . . ? N11 Fe2 N18 92.50(11) . . ? N13 Fe2 N15 88.01(11) . . ? N13 Fe2 N16 93.88(11) . . ? N16 Fe2 N15 88.72(10) . . ? N18 Fe2 N13 178.59(11) . . ? N18 Fe2 N15 91.16(11) . . ? N18 Fe2 N16 84.96(11) . . ? N20 Fe2 N11 93.78(11) . . ? N20 Fe2 N13 90.78(11) . . ? N20 Fe2 N15 177.45(11) . . ? N20 Fe2 N16 89.12(11) . . ? N20 Fe2 N18 90.00(12) . . ? N12 N11 Fe2 119.7(2) . . ? C46 N11 Fe2 133.1(3) . . ? C46 N11 N12 107.2(3) . . ? N11 N12 B3 121.0(2) . . ? C48 N12 N11 109.5(3) . . ? C48 N12 B3 129.6(3) . . ? N14 N13 Fe2 122.05(19) . . ? C49 N13 Fe2 131.2(2) . . ? C49 N13 N14 106.7(3) . . ? N13 N14 B3 117.4(3) . . ? C51 N14 N13 109.4(3) . . ? C51 N14 B3 133.0(3) . . ? C59 N15 Fe2 119.7(2) . . ? C63 N15 Fe2 119.1(2) . . ? C63 N15 C59 120.6(3) . . ? N17 N16 Fe2 121.88(19) . . ? C71 N16 Fe2 131.0(2) . . ? C71 N16 N17 106.9(3) . . ? N16 N17 B4 117.5(2) . . ? C73 N17 N16 108.7(3) . . ? C73 N17 B4 133.8(3) . . ? N19 N18 Fe2 119.9(2) . . ? C74 N18 Fe2 133.1(2) . . ? C74 N18 N19 106.6(3) . . ? N18 N19 B4 119.9(3) . . ? C76 N19 N18 108.5(3) . . ? C76 N19 B4 130.6(3) . . ? C77 N20 Fe2 136.3(2) . . ? N11 C46 C47 110.0(3) . . ? C48 C47 C46 105.2(3) . . ? N12 C48 C47 108.2(3) . . ? N13 C49 C50 110.2(3) . . ? C51 C50 C49 105.1(3) . . ? N14 C51 C50 108.5(3) . . ? C53 C52 B3 123.9(3) . . ? C57 C52 C53 114.8(3) . . ? C57 C52 B3 120.7(3) . . ? C54 C53 C52 121.7(4) . . ? C53 C54 C55 122.4(4) . . ? C54 C55 C58 122.1(4) . . ? C56 C55 C54 116.3(4) . . ? C56 C55 C58 121.6(4) . . ? C55 C56 C57 121.9(4) . . ? C56 C57 C52 122.8(4) . . ? N15 C59 C60 119.9(3) . . ? N15 C59 B3 118.0(3) . . ? C60 C59 B3 122.0(3) . . ? C59 C60 C61 120.4(3) . . ? C62 C61 C60 118.1(3) . . ? C61 C62 C63 121.4(3) . . ? N15 C63 C62 119.4(3) . . ? N15 C63 B4 119.4(3) . . ? C62 C63 B4 121.1(3) . . ? C69 C64 C65 120.0 . . ? C69 C64 B4 115.9(2) . . ? C65 C64 B4 124.0(2) . . ? C68 C69 C64 120.0 . . ? C69 C68 C67 120.0 . . ? C68 C67 C66 120.0 . . ? C68 C67 C70 120.0(3) . . ? C66 C67 C70 120.0(3) . . ? C67 C66 C65 120.0 . . ? C66 C65 C64 120.0 . . ? N16 C71 C72 110.6(3) . . ? C73 C72 C71 104.2(3) . . ? N17 C73 C72 109.6(3) . . ? N18 C74 C75 111.0(3) . . ? C76 C75 C74 104.4(3) . . ? N19 C76 C75 109.5(3) . . ? N20 C77 C78 116.3(3) . . ? N20 C77 C82 123.2(3) . . ? C82 C77 C78 120.6(3) . . ? O2 C78 C77 120.1(3) . . ? O2 C78 C79 123.3(3) . . ? C79 C78 C77 116.6(3) . . ? C78 C79 C83 119.5(3) . . ? C80 C79 C78 117.2(3) . . ? C80 C79 C83 123.3(3) . . ? C79 C80 C81 125.9(3) . . ? C80 C81 C87 118.7(3) . . ? C82 C81 C80 118.6(4) . . ? C82 C81 C87 122.6(3) . . ? C81 C82 C77 120.8(3) . . ? C79 C83 C84 112.0(3) . . ? C79 C83 C86 109.4(3) . . ? C84 C83 C86 107.5(3) . . ? C85 C83 C79 110.9(3) . . ? C85 C83 C84 107.0(4) . . ? C85 C83 C86 109.9(3) . . ? C81 C87 C88 107.0(4) . . ? C81 C87 C89A 110.1(9) . . ? C81 C87 C90A 107.8(8) . . ? C89 C87 C81 112.2(3) . . ? C89 C87 C88 108.6(4) . . ? C90 C87 C81 111.0(3) . . ? C90 C87 C88 106.6(5) . . ? C90 C87 C89 111.2(5) . . ? C89A C87 C90A 106.8(9) . . ? C88A C87 C81 114.2(9) . . ? C88A C87 C89A 109.4(9) . . ? C88A C87 C90A 108.2(9) . . ? N12 B3 N14 105.2(3) . . ? N12 B3 C52 106.4(3) . . ? N12 B3 C59 108.5(3) . . ? N14 B3 C52 115.1(3) . . ? N14 B3 C59 103.2(2) . . ? C52 B3 C59 117.7(3) . . ? N17 B4 N19 103.0(3) . . ? N17 B4 C63 105.1(3) . . ? N17 B4 C64 120.1(3) . . ? N17 B4 C64A 109.5(7) . . ? N19 B4 C63 109.2(3) . . ? N19 B4 C64 108.2(3) . . ? N19 B4 C64A 111.0(7) . . ? C63 B4 C64 110.6(3) . . ? C64A B4 C63 117.8(7) . . ? C12A C11A C10A 120.0 . . ? C11A C12A C7A 120.0 . . ? C12A C7A B1 114.0(5) . . ? C8A C7A B1 126.0(5) . . ? C8A C7A C12A 120.0 . . ? C7A C8A C9A 120.0 . . ? C8A C9A C10A 120.0 . . ? C11A C10A C13A 121.4(5) . . ? C9A C10A C11A 120.0 . . ? C9A C10A C13A 118.6(5) . . ? C69A C64A B4 112.1(9) . . ? C69A C64A C65A 120.0 . . ? C65A C64A B4 127.8(9) . . ? C68A C69A C64A 120.0 . . ? C67A C68A C69A 120.0 . . ? C68A C67A C66A 120.0 . . ? C68A C67A C70A 120.3(7) . . ? C66A C67A C70A 119.7(7) . . ? C65A C66A C67A 120.0 . . ? C66A C65A C64A 120.0 . . ? _shelx_res_file ; TITL ln620_o1+o2_a.res in P2/c ln620_nh_sq.res created by SHELXL-2017/1 at 12:57:51 on 19-Mar-2020 REM Old TITL LN620_O1+O2 in P2/c REM SHELXT solution in P2/c: R1 0.199, Rweak 0.008, Alpha 0.061 REM 0.614 for 460 systematic absences, Orientation as input REM Formula found by SHELXT: C92 B7 N14 O8 Fe2 CELL 1.54178 18.7182 24.1607 23.662 90 98.957 90 ZERR 2 0.0007 0.0011 0.0009 0 0.003 0 LATT 1 SYMM -X,+Y,0.5-Z SFAC C H B Fe N O UNIT 360 400 16 8 80 8 SADI C66A C70A C70A C68A C66 C70 C68 C70 SADI C11 C13 C9 C13 C13A C11A C9A C13A SADI C7 B1 C7A B1 SADI 0.01 C13A C10A C13 C10 SADI C64 B4 C64A B4 SADI 0.01 C70A C67A C70 C67 SADI Fe1 H10 H20 Fe2 SADI C90A C81 C90 C81 C88A C81 C88 C81 C89A C81 C89 C81 SADI C89A C90A C89 C90 C90A C88A C90 C88 C88A C89A C88 C89 SADI 0.01 C90A C87 C90 C87 C88A C87 C88 C87 C89A C87 C89 C87 FLAT C10 C11 C12 C7 C8 C9 C13 FLAT C13A C11A C12A C8A C7A SIMU 0.01 0.02 2 C10 C11 C12 C7 C8 C9 C13 C11A C12A C7A C8A C9A C10A C13A SIMU 0.01 0.02 2 C64 C65 C66 C67 C68 C69 C70 C64A C65A C66A C67A C68A C69A = C70A ISOR 0.005 0.01 C87 C88 C89 C90 C89A C88A C90A L.S. 15 0 128 PLAN 40 SIZE 0.133 0.135 0.178 TEMP -100.15 BOND ABIN fmap 2 53 acta OMIT -8 2 26 REM REM REM WGHT 0.118800 1.744900 FVAR 0.13688 0.61252 0.82433 0.86852 FE1 4 0.577379 0.124093 0.620118 11.00000 0.02696 0.03661 = 0.02884 -0.00134 0.00087 -0.00274 O1 6 0.699651 0.284305 0.653466 11.00000 0.06040 0.04476 = 0.06329 0.00814 -0.02148 -0.01115 N1 5 0.554685 0.157762 0.541767 11.00000 0.02793 0.04226 = 0.03067 -0.00055 0.00172 -0.00401 N2 5 0.485225 0.158573 0.513024 11.00000 0.03135 0.04492 = 0.03180 0.00106 0.00108 -0.00348 N3 5 0.496363 0.169859 0.637140 11.00000 0.03112 0.03907 = 0.03012 0.00074 0.00106 -0.00054 N4 5 0.431665 0.169001 0.601756 11.00000 0.02622 0.04444 = 0.03575 0.00091 -0.00050 -0.00031 N5 5 0.509621 0.060339 0.592817 11.00000 0.03067 0.04022 = 0.02887 -0.00097 0.00605 -0.00428 N6 5 0.591713 0.089504 0.696190 11.00000 0.03067 0.03783 = 0.03518 -0.00309 0.00165 -0.00003 N7 5 0.604421 0.034463 0.701226 11.00000 0.03463 0.03979 = 0.03586 0.00140 0.00194 -0.00043 N8 5 0.659252 0.079360 0.600606 11.00000 0.02837 0.03994 = 0.03465 -0.00245 0.00116 -0.00177 N9 5 0.665636 0.024497 0.613993 11.00000 0.03473 0.03864 = 0.03706 -0.00483 0.00421 -0.00115 N10 5 0.639468 0.182542 0.642747 11.00000 0.03503 0.03891 = 0.03476 0.00189 0.00090 -0.00013 C1 1 0.596373 0.180784 0.508339 11.00000 0.03621 0.04825 = 0.04614 0.00558 0.00671 -0.00296 AFIX 43 H1 2 0.646921 0.186666 0.518525 11.00000 -1.20000 AFIX 0 C2 1 0.555874 0.195292 0.455929 11.00000 0.04914 0.06795 = 0.03892 0.01813 0.00717 -0.00518 AFIX 43 H2 2 0.572669 0.211739 0.423973 11.00000 -1.20000 AFIX 0 C3 1 0.486388 0.180522 0.460809 11.00000 0.04597 0.06467 = 0.03655 0.01164 -0.00017 -0.00351 AFIX 43 H3 2 0.445478 0.185047 0.431925 11.00000 -1.20000 AFIX 0 C4 1 0.491359 0.208697 0.676504 11.00000 0.03763 0.03948 = 0.03017 0.00264 0.00409 0.00226 AFIX 43 H4 2 0.529328 0.218580 0.706276 11.00000 -1.20000 AFIX 0 C5 1 0.423084 0.232668 0.667983 11.00000 0.04764 0.04344 = 0.03642 -0.00012 0.01056 0.00793 AFIX 43 H5 2 0.405202 0.260840 0.690054 11.00000 -1.20000 AFIX 0 C6 1 0.387122 0.206222 0.620123 11.00000 0.03441 0.04901 = 0.03556 0.00179 0.00512 0.00426 AFIX 43 H6 2 0.338646 0.213220 0.602931 11.00000 -1.20000 AFIX 66 PART 1 C10 1 0.197238 0.164079 0.460376 21.00000 0.03901 0.11121 = 0.06045 -0.00431 -0.00812 0.01185 C11 1 0.213813 0.122156 0.500504 21.00000 0.03406 0.09219 = 0.04853 -0.01017 0.00060 -0.00723 AFIX 43 H11 2 0.176468 0.099237 0.510488 21.00000 -1.20000 AFIX 65 C12 1 0.285029 0.113765 0.526023 21.00000 0.03618 0.06937 = 0.03620 -0.00722 0.00193 -0.00464 AFIX 43 H12 2 0.296357 0.085111 0.553449 21.00000 -1.20000 AFIX 65 C7 1 0.339671 0.147298 0.511415 21.00000 0.03390 0.05249 = 0.04000 -0.00708 -0.00003 -0.01035 C8 1 0.323097 0.189222 0.471287 21.00000 0.03986 0.07437 = 0.04205 0.00338 -0.00315 0.00547 AFIX 43 H8 2 0.360443 0.212140 0.461303 21.00000 -1.20000 AFIX 65 C9 1 0.251881 0.197613 0.445767 21.00000 0.04390 0.10346 = 0.05001 0.00696 -0.00322 0.02076 AFIX 43 H9 2 0.240554 0.226267 0.418342 21.00000 -1.20000 AFIX 0 C13 1 0.118043 0.173573 0.430835 21.00000 0.05222 0.16417 = 0.10232 -0.01526 -0.02382 0.01452 AFIX 137 H13A 2 0.085485 0.149741 0.448641 21.00000 -1.50000 H13B 2 0.113911 0.164551 0.390077 21.00000 -1.50000 H13C 2 0.104800 0.212412 0.435163 21.00000 -1.50000 AFIX 0 PART 0 C14 1 0.445896 0.071381 0.557762 11.00000 0.02944 0.04778 = 0.02792 -0.00100 0.00560 -0.00709 C15 1 0.406199 0.027612 0.530393 11.00000 0.03592 0.04890 = 0.03746 -0.00261 0.00173 -0.00872 AFIX 43 H15 2 0.362141 0.035161 0.505803 11.00000 -1.20000 AFIX 0 C16 1 0.429354 -0.026392 0.538158 11.00000 0.04415 0.04707 = 0.03711 -0.00669 0.00598 -0.01349 AFIX 43 H16 2 0.402589 -0.055901 0.518533 11.00000 -1.20000 AFIX 0 C17 1 0.492639 -0.036383 0.575319 11.00000 0.04371 0.03762 = 0.03998 -0.00181 0.00630 -0.00421 AFIX 43 H17 2 0.509776 -0.073252 0.581350 11.00000 -1.20000 AFIX 0 C18 1 0.531412 0.006960 0.603925 11.00000 0.03476 0.03895 = 0.03008 -0.00311 0.00737 -0.00491 C19 1 0.589761 0.108886 0.748602 11.00000 0.03858 0.04658 = 0.03459 -0.00516 0.00190 0.00565 AFIX 43 H19 2 0.582244 0.146525 0.757694 11.00000 -1.20000 AFIX 0 C20 1 0.600367 0.065827 0.788095 11.00000 0.04740 0.05602 = 0.03210 0.00075 0.00423 0.00899 AFIX 43 H20A 2 0.601279 0.068074 0.828284 11.00000 -1.20000 AFIX 0 C21 1 0.609214 0.019472 0.756494 11.00000 0.04410 0.04470 = 0.03773 0.00422 0.00326 0.00208 AFIX 43 H21 2 0.617339 -0.016997 0.771095 11.00000 -1.20000 AFIX 0 C22 1 0.712805 0.092047 0.572977 11.00000 0.03123 0.05226 = 0.04042 0.00196 0.00311 -0.00050 AFIX 43 H22 2 0.721999 0.128042 0.559636 11.00000 -1.20000 AFIX 0 C23 1 0.753960 0.045529 0.566048 11.00000 0.03475 0.06326 = 0.04744 -0.00043 0.01207 0.00204 AFIX 43 H23 2 0.795421 0.043244 0.547557 11.00000 -1.20000 AFIX 0 C24 1 0.721573 0.003500 0.591806 11.00000 0.03700 0.05041 = 0.04394 -0.00443 0.00292 0.00570 AFIX 43 H24 2 0.736310 -0.034168 0.593617 11.00000 -1.20000 AFIX 0 C25 1 0.631029 -0.064142 0.669615 11.00000 0.04655 0.04075 = 0.03499 -0.00181 0.00438 0.00021 C26 1 0.703429 -0.076285 0.688649 11.00000 0.04671 0.04712 = 0.06097 0.00678 0.00536 -0.00198 AFIX 43 H26 2 0.738271 -0.047588 0.689466 11.00000 -1.20000 AFIX 0 C27 1 0.726259 -0.128608 0.706366 11.00000 0.05884 0.06297 = 0.07698 0.01700 0.01217 0.01344 AFIX 43 H27 2 0.776284 -0.135160 0.718779 11.00000 -1.20000 AFIX 0 C28 1 0.677297 -0.172076 0.706402 11.00000 0.08389 0.04200 = 0.07310 0.00834 0.02837 0.01192 C29 1 0.605333 -0.159568 0.693209 11.00000 0.07862 0.04799 = 0.05710 0.00145 0.01609 -0.01003 AFIX 43 H29 2 0.570331 -0.187381 0.696469 11.00000 -1.20000 AFIX 0 C30 1 0.582692 -0.106932 0.675156 11.00000 0.05438 0.04626 = 0.04408 0.00385 0.00377 -0.00115 AFIX 43 H30 2 0.532293 -0.099772 0.666223 11.00000 -1.20000 AFIX 0 C31 1 0.704326 -0.230530 0.721528 11.00000 0.12424 0.05991 = 0.15054 0.03759 0.05615 0.02544 AFIX 137 H31A 2 0.710828 -0.235461 0.763123 11.00000 -1.50000 H31B 2 0.750644 -0.236302 0.707981 11.00000 -1.50000 H31C 2 0.668888 -0.257418 0.703208 11.00000 -1.50000 AFIX 0 C32 1 0.701921 0.189710 0.677224 11.00000 0.03068 0.04708 = 0.03350 -0.00088 0.00040 -0.00746 C33 1 0.730616 0.246949 0.683796 11.00000 0.04357 0.04475 = 0.04074 0.00195 -0.00629 -0.00722 C34 1 0.794878 0.256154 0.727369 11.00000 0.04759 0.05496 = 0.04465 0.00288 -0.00988 -0.01988 C35 1 0.823831 0.211590 0.756960 11.00000 0.04170 0.06435 = 0.04109 0.00632 -0.01036 -0.01429 AFIX 43 H35 2 0.863540 0.217929 0.786492 11.00000 -1.20000 AFIX 0 C36 1 0.799643 0.155363 0.747551 11.00000 0.03283 0.05590 = 0.04004 0.00333 -0.00261 -0.00519 C37 1 0.740089 0.145237 0.708318 11.00000 0.02993 0.04547 = 0.04308 0.00087 -0.00046 -0.00345 AFIX 43 H37 2 0.723640 0.108287 0.701469 11.00000 -1.20000 AFIX 0 C38 1 0.825895 0.314991 0.735944 11.00000 0.07691 0.05925 = 0.05534 0.00372 -0.02489 -0.02646 C39 1 0.769093 0.355519 0.750730 11.00000 0.13266 0.05596 = 0.06740 -0.01115 -0.00583 -0.02028 AFIX 137 H39A 2 0.726600 0.354453 0.720767 11.00000 -1.50000 H39B 2 0.789280 0.393023 0.753472 11.00000 -1.50000 H39C 2 0.754912 0.345116 0.787451 11.00000 -1.50000 AFIX 0 C40 1 0.852885 0.333470 0.680773 11.00000 0.06705 0.06958 = 0.07647 0.01870 -0.01570 -0.02920 AFIX 137 H40A 2 0.892762 0.309476 0.673680 11.00000 -1.50000 H40B 2 0.869853 0.371843 0.684945 11.00000 -1.50000 H40C 2 0.813241 0.330870 0.648529 11.00000 -1.50000 AFIX 0 C41 1 0.891358 0.316144 0.784423 11.00000 0.11651 0.08283 = 0.09350 0.01886 -0.05884 -0.05568 AFIX 137 H41A 2 0.875194 0.307776 0.820940 11.00000 -1.50000 H41B 2 0.913589 0.352957 0.786352 11.00000 -1.50000 H41C 2 0.926870 0.288433 0.776771 11.00000 -1.50000 AFIX 0 C42 1 0.840319 0.109429 0.783387 11.00000 0.03431 0.05801 = 0.05669 0.00908 -0.00686 -0.00393 C43 1 0.921050 0.112254 0.778224 11.00000 0.03968 0.07953 = 0.08022 0.01275 -0.00716 0.00109 AFIX 137 H43A 2 0.927166 0.105889 0.738354 11.00000 -1.50000 H43B 2 0.947414 0.083806 0.802617 11.00000 -1.50000 H43C 2 0.940063 0.148868 0.790408 11.00000 -1.50000 AFIX 0 C44 1 0.830642 0.118140 0.846389 11.00000 0.06038 0.07575 = 0.05384 0.02053 -0.00497 0.00106 AFIX 137 H44A 2 0.848178 0.155030 0.858976 11.00000 -1.50000 H44B 2 0.858300 0.090000 0.870355 11.00000 -1.50000 H44C 2 0.779306 0.114919 0.849829 11.00000 -1.50000 AFIX 0 C45 1 0.812497 0.052256 0.763876 11.00000 0.04993 0.05546 = 0.08163 0.01244 -0.01792 0.00556 AFIX 137 H45A 2 0.761779 0.048715 0.769098 11.00000 -1.50000 H45B 2 0.841437 0.023934 0.786615 11.00000 -1.50000 H45C 2 0.816367 0.047314 0.723356 11.00000 -1.50000 AFIX 0 B1 3 0.423174 0.135286 0.544083 11.00000 0.03337 0.05106 = 0.03091 -0.00176 0.00240 -0.00718 B2 3 0.607490 -0.002221 0.646921 11.00000 0.03873 0.03975 = 0.03532 -0.00294 0.00401 -0.00256 FE2 4 0.649049 0.381601 0.462161 11.00000 0.02780 0.04049 = 0.03643 0.00547 0.00040 -0.00031 O2 6 0.761918 0.222590 0.523131 11.00000 0.03223 0.04693 = 0.07974 0.00948 -0.00241 -0.00218 N11 5 0.718799 0.416873 0.419370 11.00000 0.03349 0.04459 = 0.04456 0.00765 0.00607 0.00109 N12 5 0.731609 0.471709 0.425146 11.00000 0.03481 0.04485 = 0.04409 0.00839 0.00606 -0.00143 N13 5 0.689483 0.426999 0.529871 11.00000 0.03174 0.04517 = 0.03959 0.00824 -0.00038 -0.00071 N14 5 0.705330 0.481640 0.525305 11.00000 0.03431 0.04151 = 0.04285 0.00360 0.00232 -0.00177 N15 5 0.579826 0.444422 0.437456 11.00000 0.03569 0.04342 = 0.03285 0.00606 0.00196 0.00074 N16 5 0.572823 0.346862 0.501305 11.00000 0.02936 0.04265 = 0.04147 0.00595 0.00453 -0.00299 N17 5 0.502617 0.343273 0.475656 11.00000 0.02971 0.04650 = 0.04806 0.00634 0.00182 -0.00189 N18 5 0.606352 0.336583 0.395200 11.00000 0.03651 0.04790 = 0.03988 0.00647 0.00458 -0.00146 N19 5 0.533311 0.336386 0.378146 11.00000 0.03891 0.05005 = 0.04449 0.00219 -0.00396 -0.00027 N20 5 0.710952 0.323443 0.487863 11.00000 0.03050 0.04339 = 0.04375 0.00454 0.00115 -0.00303 C46 1 0.762066 0.397415 0.384789 11.00000 0.04499 0.05655 = 0.05589 0.00267 0.01406 0.00306 AFIX 43 H46 2 0.764651 0.359777 0.373667 11.00000 -1.20000 AFIX 0 C47 1 0.802898 0.439891 0.367259 11.00000 0.05688 0.06837 = 0.06245 0.00461 0.02891 -0.00621 AFIX 43 H47 2 0.837708 0.437439 0.342123 11.00000 -1.20000 AFIX 0 C48 1 0.782430 0.486320 0.393898 11.00000 0.05024 0.05489 = 0.05796 0.00852 0.01491 -0.00444 AFIX 43 H48 2 0.801045 0.522580 0.390756 11.00000 -1.20000 AFIX 0 C49 1 0.705101 0.414041 0.585354 11.00000 0.03827 0.05562 = 0.04156 0.00767 0.00078 -0.00295 AFIX 43 H49 2 0.700999 0.378072 0.600745 11.00000 -1.20000 AFIX 0 C50 1 0.728203 0.460797 0.617255 11.00000 0.04381 0.06102 = 0.04212 0.00296 -0.00372 -0.00636 AFIX 43 H50 2 0.741595 0.463271 0.657583 11.00000 -1.20000 AFIX 0 C51 1 0.727497 0.502705 0.577857 11.00000 0.03792 0.04930 = 0.04830 -0.00336 0.00098 -0.00335 AFIX 43 H51 2 0.740443 0.540169 0.586255 11.00000 -1.20000 AFIX 0 C52 1 0.718497 0.570635 0.459559 11.00000 0.03721 0.04525 = 0.05224 0.00298 0.00720 -0.00139 C53 1 0.781147 0.591252 0.493598 11.00000 0.03969 0.05701 = 0.06152 0.00508 0.00499 -0.00572 AFIX 43 H53 2 0.805606 0.568858 0.523513 11.00000 -1.20000 AFIX 0 C54 1 0.807979 0.643124 0.484669 11.00000 0.03601 0.06414 = 0.07813 -0.01003 0.00848 -0.01195 AFIX 43 H54 2 0.849611 0.655784 0.509455 11.00000 -1.20000 AFIX 0 C55 1 0.776213 0.677760 0.440522 11.00000 0.04174 0.04396 = 0.09348 0.00523 0.02082 -0.00067 C56 1 0.716485 0.657220 0.405789 11.00000 0.05002 0.04919 = 0.08254 0.01442 0.01326 0.00158 AFIX 43 H56 2 0.693877 0.679073 0.374686 11.00000 -1.20000 AFIX 0 C57 1 0.688353 0.605709 0.414784 11.00000 0.04592 0.05069 = 0.05679 0.00892 0.00455 -0.00359 AFIX 43 H57 2 0.646823 0.593464 0.389607 11.00000 -1.20000 AFIX 0 C58 1 0.807022 0.734423 0.430274 11.00000 0.05844 0.04793 = 0.15545 0.00751 0.02671 -0.00789 AFIX 137 H58A 2 0.788422 0.761755 0.454912 11.00000 -1.50000 H58B 2 0.792606 0.744895 0.390104 11.00000 -1.50000 H58C 2 0.859909 0.733161 0.439195 11.00000 -1.50000 AFIX 0 C59 1 0.603079 0.497806 0.444924 11.00000 0.03503 0.04530 = 0.03507 0.00600 -0.00001 0.00020 C60 1 0.553410 0.540545 0.440025 11.00000 0.04058 0.04346 = 0.04811 0.00449 0.00257 0.00159 AFIX 43 H60 2 0.569483 0.577507 0.447462 11.00000 -1.20000 AFIX 0 C61 1 0.480078 0.529742 0.424278 11.00000 0.03886 0.04994 = 0.06153 0.01221 0.00507 0.00728 AFIX 43 H61 2 0.445487 0.558789 0.421285 11.00000 -1.20000 AFIX 0 C62 1 0.459159 0.476085 0.413217 11.00000 0.03151 0.05355 = 0.05788 0.00882 -0.00127 0.00204 AFIX 43 H62 2 0.409630 0.468130 0.400189 11.00000 -1.20000 AFIX 0 C63 1 0.508845 0.432982 0.420639 11.00000 0.03272 0.05022 = 0.03740 0.00674 0.00099 0.00156 PART 1 AFIX 66 C64 1 0.398565 0.364950 0.379610 31.00000 0.03878 0.04860 = 0.05218 0.00265 -0.00174 -0.00295 C69 1 0.388877 0.378460 0.321819 31.00000 0.04607 0.06809 = 0.05329 0.00812 -0.00551 -0.00450 AFIX 43 H69 2 0.429489 0.387271 0.303933 31.00000 -1.20000 AFIX 65 C68 1 0.319767 0.379079 0.290199 31.00000 0.04984 0.07494 = 0.05388 0.00800 -0.01230 0.00278 AFIX 43 H68 2 0.313145 0.388313 0.250702 31.00000 -1.20000 AFIX 65 C67 1 0.260344 0.366188 0.316369 31.00000 0.04030 0.05958 = 0.06729 0.00546 -0.00963 -0.00046 C66 1 0.270031 0.352678 0.374159 31.00000 0.04065 0.06345 = 0.06602 -0.00025 0.00108 0.00529 AFIX 43 H66 2 0.229419 0.343868 0.392045 31.00000 -1.20000 AFIX 65 C65 1 0.339141 0.352059 0.405780 31.00000 0.03811 0.06088 = 0.05273 0.00071 -0.00169 0.00155 AFIX 43 H65 2 0.345762 0.342825 0.445277 31.00000 -1.20000 AFIX 0 C70 1 0.184527 0.365285 0.281203 31.00000 0.04419 0.10067 = 0.08857 0.01143 -0.01989 0.00160 AFIX 137 H70A 2 0.151373 0.345951 0.302702 31.00000 -1.50000 H70B 2 0.185960 0.345994 0.244964 31.00000 -1.50000 H70C 2 0.167667 0.403330 0.273410 31.00000 -1.50000 AFIX 0 PART 0 C71 1 0.577665 0.320309 0.550836 11.00000 0.04614 0.04593 = 0.04186 0.00828 0.00108 -0.00245 AFIX 43 H71 2 0.620974 0.316008 0.577320 11.00000 -1.20000 AFIX 0 C72 1 0.511039 0.299806 0.558535 11.00000 0.05215 0.06439 = 0.05276 0.02089 0.01092 -0.00134 AFIX 43 H72 2 0.499237 0.279784 0.590382 11.00000 -1.20000 AFIX 0 C73 1 0.465655 0.314958 0.509623 11.00000 0.03313 0.06029 = 0.07304 0.02220 0.00678 -0.00024 AFIX 43 H73 2 0.415553 0.306489 0.501365 11.00000 -1.20000 AFIX 0 C74 1 0.633768 0.299368 0.363020 11.00000 0.04673 0.05736 = 0.04218 -0.00094 0.01196 -0.00229 AFIX 43 H74 2 0.683817 0.291158 0.365708 11.00000 -1.20000 AFIX 0 C75 1 0.579451 0.274150 0.325002 11.00000 0.06626 0.06867 = 0.04271 -0.00784 0.01302 -0.01108 AFIX 43 H75 2 0.584500 0.246353 0.297503 11.00000 -1.20000 AFIX 0 C76 1 0.517243 0.298299 0.336060 11.00000 0.05241 0.06172 = 0.04181 0.00041 -0.00351 -0.00964 AFIX 43 H76 2 0.469962 0.289742 0.317178 11.00000 -1.20000 AFIX 0 C77 1 0.780797 0.317931 0.508849 11.00000 0.02975 0.04940 = 0.04198 0.00666 0.00412 0.00071 C78 1 0.805857 0.260912 0.525582 11.00000 0.03197 0.05008 = 0.04689 0.00819 0.00527 -0.00106 C79 1 0.884308 0.253591 0.544394 11.00000 0.03270 0.06010 = 0.05201 0.01554 0.00551 0.00133 C80 1 0.926210 0.299464 0.547054 11.00000 0.02994 0.06876 = 0.07359 0.03148 -0.00473 -0.00301 AFIX 43 H80 2 0.976829 0.294482 0.557923 11.00000 -1.20000 AFIX 0 C81 1 0.900837 0.355381 0.534834 11.00000 0.03576 0.06304 = 0.07138 0.02743 -0.00294 -0.00562 C82 1 0.830250 0.363484 0.515990 11.00000 0.03489 0.04775 = 0.05633 0.01447 0.00057 -0.00229 AFIX 43 H82 2 0.812870 0.399922 0.507276 11.00000 -1.20000 AFIX 0 C83 1 0.914073 0.195945 0.560770 11.00000 0.03371 0.05642 = 0.06221 0.01372 0.00166 0.00375 C84 1 0.997013 0.195711 0.574825 11.00000 0.03838 0.07450 = 0.09836 0.02908 0.00044 0.01094 AFIX 137 H84A 2 1.017511 0.207764 0.541192 11.00000 -1.50000 H84B 2 1.013878 0.158193 0.585514 11.00000 -1.50000 H84C 2 1.012560 0.221025 0.606733 11.00000 -1.50000 AFIX 0 C85 1 0.893189 0.155161 0.511808 11.00000 0.05573 0.06950 = 0.06989 0.00509 0.00482 0.01545 AFIX 137 H85A 2 0.911462 0.118269 0.523674 11.00000 -1.50000 H85B 2 0.914281 0.167154 0.478437 11.00000 -1.50000 H85C 2 0.840400 0.153847 0.501844 11.00000 -1.50000 AFIX 0 C86 1 0.884515 0.175887 0.614385 11.00000 0.05453 0.05378 = 0.05855 0.01565 0.00135 -0.00090 AFIX 137 H86A 2 0.901621 0.200515 0.646563 11.00000 -1.50000 H86B 2 0.901576 0.138152 0.623766 11.00000 -1.50000 H86C 2 0.831527 0.176224 0.606962 11.00000 -1.50000 AFIX 0 C87 1 0.955718 0.402543 0.542119 11.00000 0.04477 0.06981 = 0.10550 0.03862 -0.01488 -0.01276 PART 1 C88 1 0.998021 0.399524 0.490440 41.00000 0.05481 0.11621 = 0.17715 0.07355 0.03311 -0.00945 AFIX 33 H88A 2 0.964328 0.404527 0.454730 41.00000 -1.50000 H88B 2 1.034695 0.428793 0.494006 41.00000 -1.50000 H88C 2 1.021640 0.363353 0.490091 41.00000 -1.50000 AFIX 0 C89 1 0.919477 0.459090 0.541912 41.00000 0.05705 0.06124 = 0.12401 0.02137 -0.01718 -0.02199 AFIX 33 H89A 2 0.884157 0.463135 0.506959 41.00000 -1.50000 H89B 2 0.894806 0.462286 0.575384 41.00000 -1.50000 H89C 2 0.956179 0.488188 0.543261 41.00000 -1.50000 AFIX 0 C90 1 1.011226 0.394471 0.595884 41.00000 0.07504 0.07802 = 0.14218 0.04479 -0.05172 -0.03145 AFIX 33 H90A 2 1.033601 0.357887 0.594873 41.00000 -1.50000 H90B 2 1.048566 0.423120 0.597607 41.00000 -1.50000 H90C 2 0.987192 0.397218 0.629731 41.00000 -1.50000 AFIX 0 PART 0 B3 3 0.689163 0.508519 0.463872 11.00000 0.03611 0.04377 = 0.04558 0.00423 0.00350 0.00044 B4 3 0.482615 0.368943 0.413986 11.00000 0.03695 0.04810 = 0.04262 0.00563 -0.00015 0.00033 H10 2 0.627947 0.215603 0.628743 11.00000 0.03521 H20 2 0.690461 0.289425 0.487568 11.00000 0.05792 PART 2 AFIX 66 C11A 1 0.216491 0.115548 0.522164 -21.00000 0.03955 0.08924 = 0.04178 0.00191 -0.00587 -0.00410 AFIX 43 H11A 2 0.182576 0.101367 0.544444 -21.00000 -1.20000 AFIX 65 C12A 1 0.289555 0.117461 0.544850 -21.00000 0.03980 0.07567 = 0.04219 -0.00684 -0.00590 -0.00756 AFIX 43 H12A 2 0.305577 0.104587 0.582634 -21.00000 -1.20000 AFIX 65 C7A 1 0.339177 0.138209 0.512252 -21.00000 0.03400 0.05705 = 0.03927 0.00022 -0.00056 0.01649 C8A 1 0.315736 0.157045 0.456968 -21.00000 0.04248 0.08590 = 0.05046 0.01228 0.00021 0.00587 AFIX 43 H8A 2 0.349651 0.171225 0.434689 -21.00000 -1.20000 AFIX 65 C9A 1 0.242672 0.155133 0.434282 -21.00000 0.04336 0.09949 = 0.05150 0.01457 -0.00359 0.00588 AFIX 43 H9A 2 0.226651 0.168006 0.396498 -21.00000 -1.20000 AFIX 65 C10A 1 0.193049 0.134384 0.466879 -21.00000 0.03053 0.08557 = 0.04939 -0.00156 -0.00232 0.00266 AFIX 0 C13A 1 0.112056 0.130819 0.439253 -21.00000 0.03046 0.11599 = 0.07712 -0.00813 -0.00920 0.00955 AFIX 137 H13D 2 0.092399 0.094781 0.448028 -21.00000 -1.50000 H13E 2 0.108022 0.135088 0.397690 -21.00000 -1.50000 H13F 2 0.084771 0.160343 0.454653 -21.00000 -1.50000 AFIX 66 C64A 1 0.398383 0.357098 0.389989 -31.00000 0.03773 0.04911 = 0.04531 0.01218 -0.01603 0.01044 C69A 1 0.372375 0.390628 0.343592 -31.00000 0.04379 0.06213 = 0.05602 0.00935 -0.00815 0.00054 AFIX 43 H69A 2 0.402996 0.417632 0.330659 -31.00000 -1.20000 AFIX 65 C68A 1 0.301563 0.384645 0.316118 -31.00000 0.04091 0.06899 = 0.06420 0.00404 -0.00688 -0.00197 AFIX 43 H68A 2 0.283788 0.407560 0.284407 -31.00000 -1.20000 AFIX 65 C67A 1 0.256758 0.345133 0.335040 -31.00000 0.04106 0.07330 = 0.07162 0.00236 -0.00323 0.00056 C66A 1 0.282765 0.311603 0.381437 -31.00000 0.04427 0.06690 = 0.06781 -0.00318 -0.00167 0.00088 AFIX 43 H66A 2 0.252143 0.284598 0.394369 -31.00000 -1.20000 AFIX 65 C65A 1 0.353577 0.317585 0.408912 -31.00000 0.03990 0.05868 = 0.05973 -0.00051 -0.00414 0.00240 AFIX 43 H65A 2 0.371352 0.294669 0.440622 -31.00000 -1.20000 AFIX 0 C70A 1 0.179541 0.336762 0.303482 -31.00000 0.05203 0.10171 = 0.09913 -0.00246 -0.02376 0.00657 AFIX 137 H70D 2 0.151777 0.315005 0.327469 -31.00000 -1.50000 H70E 2 0.181131 0.317063 0.267495 -31.00000 -1.50000 H70F 2 0.156368 0.372868 0.295314 -31.00000 -1.50000 AFIX 0 C89A 1 0.920864 0.455825 0.515172 -41.00000 0.07952 0.08331 = 0.08117 0.00557 0.01579 -0.01008 AFIX 33 H89D 2 0.876476 0.463598 0.530901 -41.00000 -1.50000 H89E 2 0.954695 0.486741 0.523806 -41.00000 -1.50000 H89F 2 0.909188 0.451128 0.473621 -41.00000 -1.50000 AFIX 0 C88A 1 1.024606 0.390563 0.517641 -41.00000 0.09469 0.09734 = 0.09485 0.00752 0.01013 -0.00441 AFIX 33 H88D 2 1.057006 0.422586 0.523916 -41.00000 -1.50000 H88E 2 1.048690 0.358063 0.536729 -41.00000 -1.50000 H88F 2 1.012498 0.383324 0.476512 -41.00000 -1.50000 AFIX 0 C90A 1 0.976727 0.413891 0.607272 -41.00000 0.06902 0.07116 = 0.07398 -0.00656 0.00554 -0.00169 AFIX 33 H90D 2 0.932991 0.421716 0.623873 -41.00000 -1.50000 H90E 2 1.001081 0.381297 0.625941 -41.00000 -1.50000 H90F 2 1.009350 0.445811 0.613065 -41.00000 -1.50000 AFIX 0 HKLF 4 REM ln620_o1+o2_a.res in P2/c REM R1 = 0.0677 for 13886 Fo > 4sig(Fo) and 0.0915 for all 19096 data REM 1194 parameters refined using 542 restraints END WGHT 0.1191 1.7354 REM Highest difference peak 1.145, deepest hole -0.566, 1-sigma level 0.073 Q1 1 0.6154 0.1211 0.6011 11.00000 0.05 1.14 Q2 1 0.6859 0.3828 0.4387 11.00000 0.05 1.12 Q3 1 0.5411 0.1232 0.6406 11.00000 0.05 1.00 Q4 1 0.6057 0.3780 0.4797 11.00000 0.05 0.98 Q5 1 0.5863 0.0825 0.6198 11.00000 0.05 0.60 Q6 1 0.5765 0.1597 0.6199 11.00000 0.05 0.56 Q7 1 0.6569 0.4189 0.4568 11.00000 0.05 0.54 Q8 1 0.6564 0.3422 0.4678 11.00000 0.05 0.47 Q9 1 0.4548 0.1414 0.5239 11.00000 0.05 0.45 Q10 1 0.7069 0.4832 0.4415 11.00000 0.05 0.42 Q11 1 0.3595 0.1395 0.5106 11.00000 0.05 0.41 Q12 1 0.6033 0.1802 0.6575 11.00000 0.05 0.41 Q13 1 0.6140 0.4399 0.4247 11.00000 0.05 0.39 Q14 1 0.6420 0.0086 0.6246 11.00000 0.05 0.38 Q15 1 0.4192 0.3610 0.3869 11.00000 0.05 0.37 Q16 1 0.9613 0.3845 0.5197 11.00000 0.05 0.36 Q17 1 0.6751 0.3257 0.5079 11.00000 0.05 0.36 Q18 1 0.5528 0.0614 0.5810 11.00000 0.05 0.35 Q19 1 0.7158 0.5403 0.4612 11.00000 0.05 0.35 Q20 1 0.4740 0.3526 0.5022 11.00000 0.05 0.34 Q21 1 0.5611 0.1992 0.5410 11.00000 0.05 0.33 Q22 1 0.5071 0.3476 0.4032 11.00000 0.05 0.33 Q23 1 0.7615 0.2557 0.5400 11.00000 0.05 0.33 Q24 1 0.9955 0.4017 0.5240 11.00000 0.05 0.32 Q25 1 0.4834 0.0598 0.6202 11.00000 0.05 0.32 Q26 1 0.7518 0.4789 0.4105 11.00000 0.05 0.31 Q27 1 0.6281 0.0231 0.6780 11.00000 0.05 0.31 Q28 1 0.3632 0.3638 0.3994 11.00000 0.05 0.31 Q29 1 0.6836 0.0174 0.6059 11.00000 0.05 0.30 Q30 1 0.5377 0.2205 0.4783 11.00000 0.05 0.29 Q31 1 0.8960 0.1940 0.5849 11.00000 0.05 0.29 Q32 1 0.7049 0.4422 0.5148 11.00000 0.05 0.29 Q33 1 0.7788 0.0397 0.5435 11.00000 0.05 0.29 Q34 1 0.7746 0.4637 0.4003 11.00000 0.05 0.28 Q35 1 0.5994 -0.0671 0.6845 11.00000 0.05 0.28 Q36 1 0.7149 0.0396 0.5857 11.00000 0.05 0.28 Q37 1 0.5966 0.1316 0.5333 11.00000 0.05 0.27 Q38 1 0.4617 0.3348 0.5394 11.00000 0.05 0.27 Q39 1 0.4712 0.1967 0.4955 11.00000 0.05 0.27 Q40 1 0.3974 0.1754 0.6185 11.00000 0.05 0.27 ; _shelx_res_checksum 78959 _shelx_fab_file ; 1 0 0 198.61 0.00 2 0 0 167.84 0.00 3 0 0 120.82 0.00 4 0 0 120.53 0.00 5 0 0 66.29 0.00 6 0 0 37.48 0.00 7 0 0 33.41 0.00 8 0 0 18.35 0.00 9 0 0 11.05 0.00 10 0 0 19.65 0.00 11 0 0 12.90 0.00 12 0 0 10.80 0.00 13 0 0 7.05 0.00 14 0 0 7.27 0.00 15 0 0 4.21 0.00 16 0 0 0.90 0.00 17 0 0 1.33 0.00 18 0 0 1.52 0.00 19 0 0 1.84 0.00 20 0 0 1.98 0.00 21 0 0 0.49 0.00 22 0 0 0.73 0.00 0 1 0 54.63 0.00 1 1 0 92.55 0.00 2 1 0 -90.42 0.00 3 1 0 25.08 0.00 4 1 0 25.36 0.00 5 1 0 -8.12 0.00 6 1 0 -1.33 0.00 7 1 0 -5.00 0.00 8 1 0 -12.01 0.00 9 1 0 -8.73 0.00 10 1 0 -7.43 0.00 11 1 0 -3.46 0.00 12 1 0 -7.30 0.00 13 1 0 -2.14 0.00 14 1 0 -1.24 0.00 15 1 0 -1.43 0.00 16 1 0 -3.14 0.00 17 1 0 -3.01 0.00 18 1 0 -1.06 0.00 19 1 0 -1.28 0.00 20 1 0 -1.03 0.00 21 1 0 -0.78 0.00 22 1 0 -1.34 0.00 0 2 0 112.45 0.00 1 2 0 -4.58 0.00 2 2 0 43.68 0.00 3 2 0 31.05 0.00 4 2 0 29.74 0.00 5 2 0 15.60 0.00 6 2 0 -6.25 0.00 7 2 0 -5.03 0.00 8 2 0 -2.81 0.00 9 2 0 -6.34 0.00 10 2 0 0.78 0.00 11 2 0 2.69 0.00 12 2 0 5.28 0.00 13 2 0 5.65 0.00 14 2 0 6.54 0.00 15 2 0 5.35 0.00 16 2 0 2.96 0.00 17 2 0 1.80 0.00 18 2 0 1.58 0.00 19 2 0 -0.16 0.00 20 2 0 -1.35 0.00 21 2 0 -0.66 0.00 22 2 0 0.03 0.00 0 3 0 14.53 0.00 1 3 0 86.99 0.00 2 3 0 60.36 0.00 3 3 0 31.80 0.00 4 3 0 35.73 0.00 5 3 0 16.29 0.00 6 3 0 16.80 0.00 7 3 0 18.23 0.00 8 3 0 12.20 0.00 9 3 0 11.76 0.00 10 3 0 4.57 0.00 11 3 0 5.60 0.00 12 3 0 5.03 0.00 13 3 0 0.86 0.00 14 3 0 -0.27 0.00 15 3 0 -0.51 0.00 16 3 0 -1.61 0.00 17 3 0 -0.28 0.00 18 3 0 0.16 0.00 19 3 0 -0.12 0.00 20 3 0 -0.76 0.00 21 3 0 -0.59 0.00 22 3 0 -0.30 0.00 0 4 0 72.23 0.00 1 4 0 86.48 0.00 2 4 0 81.28 0.00 3 4 0 20.94 0.00 4 4 0 -5.66 0.00 5 4 0 11.38 0.00 6 4 0 -3.77 0.00 7 4 0 -7.88 0.00 8 4 0 0.13 0.00 9 4 0 -10.65 0.00 10 4 0 -7.39 0.00 11 4 0 -2.10 0.00 12 4 0 0.10 0.00 13 4 0 -2.09 0.00 14 4 0 -3.46 0.00 15 4 0 -2.85 0.00 16 4 0 -0.42 0.00 17 4 0 -1.62 0.00 18 4 0 -1.23 0.00 19 4 0 -0.30 0.00 20 4 0 -1.99 0.00 21 4 0 -0.74 0.00 22 4 0 -1.25 0.00 0 5 0 -43.82 0.00 1 5 0 2.16 0.00 3 5 0 -22.09 0.00 4 5 0 8.74 0.00 5 5 0 13.14 0.00 6 5 0 9.13 0.00 7 5 0 12.33 0.00 8 5 0 1.01 0.00 9 5 0 2.65 0.00 10 5 0 -4.53 0.00 11 5 0 -0.07 0.00 12 5 0 2.61 0.00 13 5 0 0.16 0.00 14 5 0 -0.91 0.00 15 5 0 -0.55 0.00 16 5 0 0.28 0.00 17 5 0 -0.19 0.00 18 5 0 -0.71 0.00 19 5 0 -0.64 0.00 20 5 0 0.55 0.00 21 5 0 -0.51 0.00 0 6 0 6.13 0.00 1 6 0 4.55 0.00 2 6 0 17.69 0.00 3 6 0 4.24 0.00 4 6 0 -3.41 0.00 5 6 0 3.27 0.00 6 6 0 -6.30 0.00 7 6 0 -12.50 0.00 8 6 0 0.63 0.00 9 6 0 -5.49 0.00 10 6 0 -1.36 0.00 11 6 0 -1.25 0.00 12 6 0 1.82 0.00 13 6 0 1.05 0.00 14 6 0 -0.08 0.00 15 6 0 -0.30 0.00 16 6 0 0.66 0.00 17 6 0 0.68 0.00 18 6 0 -0.42 0.00 19 6 0 1.27 0.00 20 6 0 0.22 0.00 21 6 0 1.15 0.00 0 7 0 -6.32 0.00 1 7 0 9.83 0.00 2 7 0 9.75 0.00 3 7 0 9.80 0.00 4 7 0 5.40 0.00 5 7 0 6.06 0.00 6 7 0 5.62 0.00 7 7 0 7.79 0.00 8 7 0 3.30 0.00 9 7 0 8.55 0.00 10 7 0 0.70 0.00 11 7 0 1.25 0.00 12 7 0 -0.14 0.00 13 7 0 -0.73 0.00 14 7 0 -1.62 0.00 15 7 0 -2.69 0.00 16 7 0 -0.99 0.00 17 7 0 -0.54 0.00 18 7 0 0.00 0.00 19 7 0 -0.06 0.00 20 7 0 1.34 0.00 21 7 0 0.36 0.00 0 8 0 7.13 0.00 1 8 0 -3.29 0.00 2 8 0 12.29 0.00 3 8 0 12.22 0.00 4 8 0 -5.80 0.00 5 8 0 2.73 0.00 6 8 0 6.58 0.00 7 8 0 -3.77 0.00 8 8 0 1.47 0.00 9 8 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0.00 -11 8 27 0.77 0.00 -10 8 27 1.18 0.00 -9 8 27 1.07 0.00 -8 8 27 -0.23 0.00 1 8 27 2.02 0.00 2 8 27 1.75 0.00 3 8 27 1.00 0.00 4 8 27 1.65 0.00 5 8 27 1.21 0.00 6 8 27 -0.63 0.00 -12 9 27 0.26 0.00 -11 9 27 0.54 0.00 -10 9 27 0.91 0.00 -9 9 27 0.66 0.00 -8 9 27 0.98 0.00 -7 9 27 -0.48 0.00 -6 9 27 1.53 0.00 -1 9 27 -0.67 0.00 0 9 27 -0.81 0.00 1 9 27 -0.66 0.00 2 9 27 -1.28 0.00 3 9 27 -1.60 0.00 4 9 27 -1.17 0.00 5 9 27 0.06 0.00 6 9 27 -0.53 0.00 -12 10 27 0.10 0.00 -11 10 27 0.96 0.00 -10 10 27 0.75 0.00 -9 10 27 0.62 0.00 -8 10 27 -0.14 0.00 -7 10 27 -0.94 0.00 -6 10 27 -0.72 0.00 -5 10 27 0.58 0.00 -4 10 27 -0.88 0.00 -3 10 27 -0.87 0.00 -2 10 27 -0.55 0.00 -1 10 27 -0.33 0.00 0 10 27 -0.03 0.00 1 10 27 -0.41 0.00 2 10 27 0.46 0.00 3 10 27 -0.20 0.00 4 10 27 -0.29 0.00 5 10 27 0.84 0.00 -11 11 27 0.05 0.00 -10 11 27 -0.24 0.00 -9 11 27 0.85 0.00 -8 11 27 0.42 0.00 -7 11 27 0.20 0.00 -6 11 27 1.42 0.00 -5 11 27 0.33 0.00 -4 11 27 -0.04 0.00 -3 11 27 0.25 0.00 -2 11 27 -0.71 0.00 -1 11 27 -0.74 0.00 0 11 27 -1.09 0.00 1 11 27 -0.69 0.00 2 11 27 -0.18 0.00 3 11 27 0.43 0.00 4 11 27 -0.13 0.00 -10 12 27 0.49 0.00 -9 12 27 0.29 0.00 -8 12 27 0.27 0.00 -7 12 27 1.05 0.00 -6 12 27 0.22 0.00 -5 12 27 0.03 0.00 -4 12 27 0.44 0.00 -3 12 27 -0.20 0.00 -2 12 27 0.62 0.00 -1 12 27 0.32 0.00 0 12 27 0.95 0.00 1 12 27 -0.75 0.00 2 12 27 0.60 0.00 3 12 27 0.35 0.00 4 12 27 -0.52 0.00 -9 13 27 0.41 0.00 -8 13 27 0.24 0.00 -7 13 27 0.58 0.00 -6 13 27 0.90 0.00 -5 13 27 0.66 0.00 -4 13 27 0.59 0.00 -3 13 27 0.85 0.00 -2 13 27 -0.28 0.00 -1 13 27 1.10 0.00 0 13 27 -0.67 0.00 1 13 27 0.00 0.00 2 13 27 -0.14 0.00 3 13 27 0.22 0.00 -8 14 27 0.42 0.00 -7 14 27 0.50 0.00 -6 14 27 0.22 0.00 -5 14 27 0.30 0.00 -4 14 27 0.62 0.00 -3 14 27 -0.30 0.00 -2 14 27 0.32 0.00 -1 14 27 0.08 0.00 0 14 27 0.03 0.00 1 14 27 -0.44 0.00 -6 15 27 0.00 0.00 -5 15 27 0.83 0.00 -4 15 27 0.15 0.00 -3 15 27 0.38 0.00 -2 15 27 0.14 0.00 -1 15 27 -0.14 0.00 -13 0 28 4.21 0.00 -12 0 28 0.74 0.00 -11 0 28 2.90 0.00 -10 0 28 4.52 0.00 -9 0 28 -2.08 0.00 -8 0 28 3.02 0.00 1 0 28 -0.57 0.00 2 0 28 -0.33 0.00 3 0 28 -0.39 0.00 4 0 28 0.60 0.00 5 0 28 0.22 0.00 6 0 28 -0.52 0.00 -13 1 28 0.72 0.00 -12 1 28 0.00 0.00 -11 1 28 2.25 0.00 -10 1 28 -0.55 0.00 -9 1 28 -0.26 0.00 -8 1 28 0.41 0.00 1 1 28 -1.01 0.00 2 1 28 -0.25 0.00 3 1 28 -0.03 0.00 4 1 28 -0.07 0.00 5 1 28 0.09 0.00 6 1 28 -0.33 0.00 -13 2 28 3.88 0.00 -12 2 28 2.70 0.00 -11 2 28 4.21 0.00 -10 2 28 2.99 0.00 -9 2 28 -0.18 0.00 -8 2 28 1.01 0.00 1 2 28 0.03 0.00 2 2 28 -0.39 0.00 3 2 28 -0.95 0.00 4 2 28 -0.86 0.00 5 2 28 -0.45 0.00 6 2 28 -0.55 0.00 -13 3 28 -2.13 0.00 -12 3 28 1.60 0.00 -11 3 28 -1.34 0.00 -10 3 28 -2.40 0.00 -9 3 28 -2.90 0.00 -8 3 28 -3.00 0.00 1 3 28 0.37 0.00 2 3 28 1.63 0.00 3 3 28 0.28 0.00 4 3 28 -0.27 0.00 5 3 28 -0.24 0.00 6 3 28 -0.53 0.00 -13 4 28 1.57 0.00 -12 4 28 2.65 0.00 -11 4 28 2.53 0.00 -10 4 28 2.06 0.00 -9 4 28 2.41 0.00 -8 4 28 -1.49 0.00 -7 4 28 0.98 0.00 0 4 28 -1.15 0.00 1 4 28 0.27 0.00 2 4 28 -0.39 0.00 3 4 28 -0.79 0.00 4 4 28 -0.50 0.00 5 4 28 -0.79 0.00 6 4 28 -0.58 0.00 -12 5 28 0.30 0.00 -11 5 28 -1.84 0.00 -10 5 28 0.21 0.00 -9 5 28 -0.72 0.00 -8 5 28 -2.77 0.00 -7 5 28 -3.46 0.00 -6 5 28 -0.03 0.00 -1 5 28 -0.53 0.00 0 5 28 -0.09 0.00 1 5 28 -0.71 0.00 2 5 28 -1.43 0.00 3 5 28 -1.28 0.00 4 5 28 -0.43 0.00 5 5 28 0.24 0.00 6 5 28 0.20 0.00 -12 6 28 0.54 0.00 -11 6 28 0.76 0.00 -10 6 28 1.35 0.00 -9 6 28 1.33 0.00 -8 6 28 -1.60 0.00 -7 6 28 -0.70 0.00 -6 6 28 -1.34 0.00 -5 6 28 -0.66 0.00 -4 6 28 -0.42 0.00 -3 6 28 -0.69 0.00 -2 6 28 -0.56 0.00 -1 6 28 0.04 0.00 0 6 28 0.06 0.00 1 6 28 -0.63 0.00 2 6 28 -1.93 0.00 3 6 28 -1.18 0.00 4 6 28 -0.27 0.00 5 6 28 0.54 0.00 -12 7 28 0.20 0.00 -11 7 28 -0.32 0.00 -10 7 28 0.24 0.00 -9 7 28 -0.59 0.00 -8 7 28 0.21 0.00 -7 7 28 -0.36 0.00 -6 7 28 0.58 0.00 -5 7 28 0.91 0.00 -4 7 28 0.32 0.00 -3 7 28 0.10 0.00 -2 7 28 0.24 0.00 -1 7 28 1.26 0.00 0 7 28 2.11 0.00 1 7 28 1.02 0.00 2 7 28 0.91 0.00 3 7 28 0.29 0.00 4 7 28 0.87 0.00 5 7 28 1.00 0.00 -11 8 28 1.54 0.00 -10 8 28 0.15 0.00 -9 8 28 -0.45 0.00 -8 8 28 0.28 0.00 -7 8 28 -0.72 0.00 -6 8 28 -0.88 0.00 -5 8 28 0.12 0.00 -4 8 28 -0.22 0.00 -3 8 28 -1.37 0.00 -2 8 28 -1.22 0.00 -1 8 28 0.35 0.00 0 8 28 0.46 0.00 1 8 28 0.43 0.00 2 8 28 -0.11 0.00 3 8 28 0.05 0.00 4 8 28 -1.35 0.00 -11 9 28 0.75 0.00 -10 9 28 -0.24 0.00 -9 9 28 -0.31 0.00 -8 9 28 -0.06 0.00 -7 9 28 -0.80 0.00 -6 9 28 -0.74 0.00 -5 9 28 -0.03 0.00 -4 9 28 -1.15 0.00 -3 9 28 -1.21 0.00 -2 9 28 -0.87 0.00 -1 9 28 -1.28 0.00 0 9 28 -0.15 0.00 1 9 28 -0.81 0.00 2 9 28 -0.38 0.00 3 9 28 -0.12 0.00 4 9 28 -0.08 0.00 -10 10 28 -0.17 0.00 -9 10 28 -0.47 0.00 -8 10 28 -0.39 0.00 -7 10 28 0.33 0.00 -6 10 28 0.14 0.00 -5 10 28 -0.46 0.00 -4 10 28 0.22 0.00 -3 10 28 0.30 0.00 -2 10 28 0.47 0.00 -1 10 28 0.84 0.00 0 10 28 0.72 0.00 1 10 28 -0.34 0.00 2 10 28 -0.18 0.00 3 10 28 0.53 0.00 -9 11 28 -0.50 0.00 -8 11 28 -0.28 0.00 -7 11 28 0.95 0.00 -6 11 28 1.15 0.00 -5 11 28 0.20 0.00 -4 11 28 -0.20 0.00 -3 11 28 -0.13 0.00 -2 11 28 -0.64 0.00 -1 11 28 0.08 0.00 0 11 28 0.06 0.00 1 11 28 0.11 0.00 2 11 28 -0.40 0.00 -8 12 28 -0.27 0.00 -7 12 28 0.57 0.00 -6 12 28 0.06 0.00 -5 12 28 -0.52 0.00 -4 12 28 0.01 0.00 -3 12 28 -0.23 0.00 -2 12 28 0.14 0.00 -1 12 28 0.99 0.00 0 12 28 1.22 0.00 1 12 28 0.45 0.00 -5 13 28 0.28 0.00 -4 13 28 0.28 0.00 -3 13 28 -0.19 0.00 -2 13 28 -0.10 0.00 -1 13 28 -0.05 0.00 -11 1 29 0.17 0.00 -10 1 29 0.17 0.00 -9 1 29 0.18 0.00 -8 1 29 0.21 0.00 -7 1 29 -1.70 0.00 -6 1 29 -0.76 0.00 -5 1 29 0.82 0.00 -4 1 29 0.48 0.00 -3 1 29 -0.07 0.00 -2 1 29 0.07 0.00 -1 1 29 0.29 0.00 0 1 29 -0.08 0.00 1 1 29 0.22 0.00 2 1 29 0.55 0.00 3 1 29 -0.28 0.00 4 1 29 -0.47 0.00 -11 2 29 0.42 0.00 -10 2 29 -2.37 0.00 -9 2 29 0.98 0.00 -8 2 29 -2.19 0.00 -7 2 29 -2.19 0.00 -6 2 29 -1.05 0.00 -5 2 29 0.34 0.00 -4 2 29 -0.13 0.00 -3 2 29 -0.95 0.00 -2 2 29 0.55 0.00 -1 2 29 0.35 0.00 0 2 29 0.57 0.00 1 2 29 1.02 0.00 2 2 29 0.78 0.00 3 2 29 0.74 0.00 4 2 29 0.33 0.00 -11 3 29 -0.17 0.00 -10 3 29 0.25 0.00 -9 3 29 1.38 0.00 -8 3 29 0.80 0.00 -7 3 29 -1.39 0.00 -6 3 29 1.00 0.00 -5 3 29 0.90 0.00 -4 3 29 -0.23 0.00 -3 3 29 0.07 0.00 -2 3 29 1.11 0.00 -1 3 29 0.84 0.00 0 3 29 0.47 0.00 1 3 29 0.82 0.00 2 3 29 0.26 0.00 3 3 29 -0.09 0.00 4 3 29 -0.07 0.00 -11 4 29 -0.83 0.00 -10 4 29 -0.41 0.00 -9 4 29 1.83 0.00 -8 4 29 -0.07 0.00 -7 4 29 -0.14 0.00 -6 4 29 0.51 0.00 -5 4 29 0.07 0.00 -4 4 29 -0.69 0.00 -3 4 29 0.43 0.00 -2 4 29 0.63 0.00 -1 4 29 0.10 0.00 0 4 29 0.58 0.00 1 4 29 0.38 0.00 2 4 29 -0.56 0.00 3 4 29 -0.43 0.00 4 4 29 0.07 0.00 -11 5 29 0.13 0.00 -10 5 29 0.48 0.00 -9 5 29 0.51 0.00 -8 5 29 0.48 0.00 -7 5 29 -0.26 0.00 -6 5 29 -0.53 0.00 -5 5 29 -1.01 0.00 -4 5 29 -1.08 0.00 -3 5 29 -0.03 0.00 -2 5 29 0.63 0.00 -1 5 29 0.98 0.00 0 5 29 1.27 0.00 1 5 29 1.11 0.00 2 5 29 0.19 0.00 3 5 29 -0.13 0.00 -10 6 29 0.55 0.00 -9 6 29 -0.67 0.00 -8 6 29 1.50 0.00 -7 6 29 1.62 0.00 -6 6 29 1.57 0.00 -5 6 29 1.28 0.00 -4 6 29 0.73 0.00 -3 6 29 0.59 0.00 -2 6 29 0.23 0.00 -1 6 29 0.59 0.00 0 6 29 0.96 0.00 1 6 29 0.53 0.00 2 6 29 0.40 0.00 3 6 29 0.99 0.00 -10 7 29 0.09 0.00 -9 7 29 -0.24 0.00 -8 7 29 0.41 0.00 -7 7 29 1.27 0.00 -6 7 29 -0.06 0.00 -5 7 29 0.56 0.00 -4 7 29 0.30 0.00 -3 7 29 -0.46 0.00 -2 7 29 0.61 0.00 -1 7 29 0.23 0.00 0 7 29 0.62 0.00 1 7 29 0.60 0.00 2 7 29 1.23 0.00 -9 8 29 -0.10 0.00 -8 8 29 0.91 0.00 -7 8 29 0.52 0.00 -6 8 29 0.83 0.00 -5 8 29 0.15 0.00 -4 8 29 -0.73 0.00 -3 8 29 -0.06 0.00 -2 8 29 -0.58 0.00 -1 8 29 -0.23 0.00 0 8 29 -0.88 0.00 1 8 29 -0.41 0.00 2 8 29 -0.01 0.00 -8 9 29 -0.33 0.00 -7 9 29 0.60 0.00 -6 9 29 0.82 0.00 -5 9 29 -0.13 0.00 -4 9 29 0.26 0.00 -3 9 29 0.54 0.00 -2 9 29 2.07 0.00 -1 9 29 0.99 0.00 0 9 29 0.75 0.00 1 9 29 0.16 0.00 -7 10 29 0.96 0.00 -6 10 29 2.21 0.00 -5 10 29 0.89 0.00 -4 10 29 -0.15 0.00 -3 10 29 0.61 0.00 -2 10 29 -0.23 0.00 -1 10 29 0.21 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 130220) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 2847 456 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 2 5 0 10.370 1 6 1 11.523 -3 0 2 7.586 -3 1 3 8.646 -2 0 4 8.319 1 4 5 12.570 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL ln620_o1+o2_a.res in P2/c CELL 18.7182 24.1607 23.6620 90.00 98.96 90.00 SPGR P2/c # Solvent Accessible Volume = 2836 # Electrons Found in S.A.V. = 456 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others C101 0.989 0.689 0.796 ! 3.06 eA-3 C102 1.000 0.289 0.248 ! 3.04 eA-3 C103 0.975 0.281 0.350 ! 2.79 eA-3 C104 1.000 0.594 0.752 ! 2.73 eA-3 C105 0.991 0.368 0.299 ! 2.62 eA-3 C106 0.907 0.304 0.373 ! 2.30 eA-3 C107 0.035 0.783 0.654 ! 2.25 eA-3 C108 0.285 0.920 0.617 ! 2.22 eA-3 C109 1.000 0.531 0.750 ! 2.00 eA-3 C110 0.213 0.088 0.124 ! 1.87 eA-3 C111 0.039 0.298 0.397 ! 1.84 eA-3 C112 0.015 0.592 0.665 ! 1.78 eA-3 C113 0.789 0.167 0.361 ! 1.62 eA-3 C114 0.444 0.553 0.243 ! 1.58 eA-3 C115 0.500 0.523 0.252 ! 1.55 eA-3 C116 0.162 0.037 0.094 ! 1.50 eA-3 C117 0.777 0.125 0.366 ! 1.49 eA-3 C118 0.383 0.517 0.228 ! 1.38 eA-3 C119 0.283 0.851 0.622 ! 1.37 eA-3 C120 0.068 0.508 0.767 ! 1.35 eA-3 Q121 0.609 0.877 0.095 ! 1.30 eA-3 Q122 0.318 0.616 0.562 ! 1.27 eA-3 C123 0.164 0.229 0.133 ! 1.20 eA-3 C124 0.016 0.993 0.923 ! 1.19 eA-3 C125 1.000 0.086 0.249 ! 1.18 eA-3 Q126 0.546 0.873 0.148 ! 1.16 eA-3 C127 1.007 0.039 0.366 ! 1.14 eA-3 C128 0.124 0.254 0.135 ! 1.13 eA-3 C129 0.920 0.962 0.898 ! 1.13 eA-3 C130 0.996 0.045 0.163 ! 1.11 eA-3 Q131 0.612 0.383 0.483 ! 1.10 eA-3 C132 0.408 0.531 0.250 ! 1.10 eA-3 C133 0.051 0.070 0.289 ! 1.08 eA-3 C134 0.989 0.046 0.206 ! 1.06 eA-3 C135 0.975 0.993 0.456 ! 1.06 eA-3 C136 0.022 0.054 0.267 ! 1.01 eA-3 C137 1.000 0.484 0.180 ! 1.01 eA-3 C138 0.014 0.007 0.514 ! 0.99 eA-3 C139 0.058 0.040 0.320 ! 0.98 eA-3 C140 0.536 0.359 0.728 ! 0.95 eA-3 C141 0.500 0.609 0.250 ! 0.87 eA-3 C142 0.500 0.648 0.249 ! 0.86 eA-3 C143 0.023 0.250 0.203 ! 0.73 eA-3 Q144 0.584 0.916 0.119 ! 0.68 eA-3 Q145 0.427 0.833 0.386 ! 0.68 eA-3 Q146 0.653 0.344 0.469 ! 0.67 eA-3 C147 1.000 0.484 0.751 ! 0.65 eA-3 Q148 0.453 0.850 0.032 ! 0.61 eA-3 C149 0.430 0.375 0.744 ! 0.60 eA-3 Q150 0.344 0.422 0.034 ! 0.58 eA-3 C151 1.000 0.148 0.251 ! 0.55 eA-3 Q152 0.718 0.482 0.454 ! 0.55 eA-3 Q153 0.587 0.634 0.612 ! 0.54 eA-3 Q154 0.641 0.139 0.992 ! 0.52 eA-3 C155 0.037 0.078 0.202 ! 0.51 eA-3 ) ; _shelx_fab_checksum 75435 _olex2_submission_special_instructions 'No special instructions were received'