# Electronic Supplementary Material (ESI) for RSC Advances. # This journal is © The Royal Society of Chemistry 2019 ####################################################################### # # 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_xu017 _database_code_depnum_ccdc_archive 'CCDC 1908492' loop_ _audit_author_name _audit_author_address 'Toshikazu Ono' ;Kyushu University Japan ; _audit_update_record ; 2019-04-08 deposited with the CCDC. 2019-05-24 downloaded from the CCDC. ; _audit_creation_date 2018-05-20 _audit_creation_method ; Olex2 1.2-ac3 (compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C88 H56 Fe2 N8 O' _chemical_formula_sum 'C88 H56 Fe2 N8 O' _chemical_formula_weight 1353.10 _chemical_melting_point ? _chemical_oxdiff_formula 'C H N Fe Cl' _chemical_oxdiff_usercomment 'Fe-PhPc (Cl anion Ch2Cl2 hexane)' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 tetragonal _space_group_IT_number 88 _space_group_name_H-M_alt 'I 41/a' _space_group_name_Hall '-I 4ad' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 17.9013(3) _cell_length_b 17.9013(3) _cell_length_c 42.9649(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13768.4(5) _cell_formula_units_Z 8 _cell_measurement_reflns_used 7906 _cell_measurement_temperature 93 _cell_measurement_theta_max 28.9190 _cell_measurement_theta_min 2.5870 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.477 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.48847 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.34a (Rigaku Oxford Diffraction, 2017) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour violet _exptl_crystal_colour_primary violet _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 5600 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0762 _diffrn_reflns_av_unetI/netI 0.0590 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_number 35926 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 2.465 _diffrn_ambient_temperature 93 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -74.00 118.00 0.75 75.00 -- 30.00 54.00-150.00 256 2 \w -74.00 27.25 0.75 75.00 -- 30.00 54.00 30.00 135 ; _diffrn_measurement_device 'two-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Mini (JP)' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0153013000 _diffrn_orient_matrix_UB_12 0.0346561000 _diffrn_orient_matrix_UB_13 0.0048420000 _diffrn_orient_matrix_UB_21 -0.0306595000 _diffrn_orient_matrix_UB_22 -0.0190603000 _diffrn_orient_matrix_UB_23 0.0068172000 _diffrn_orient_matrix_UB_31 0.0198752000 _diffrn_orient_matrix_UB_32 -0.0026470000 _diffrn_orient_matrix_UB_33 0.0142310000 _diffrn_oxdiff_ac3_digest_frames ; 01b84de275002b8f4c809e416585e3f4e000391d57e ; _diffrn_oxdiff_ac3_digest_hkl 01cfdcc26aa6282d2ab95a47ba7c02172d9f11 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 5243 _reflns_number_total 7049 _reflns_odcompleteness_completeness 99.85 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)' _computing_data_collection 'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)' _computing_data_reduction 'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)' _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 0.979 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.077 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 447 _refine_ls_number_reflns 7049 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_gt 0.0546 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1466 _refine_ls_wR_factor_ref 0.1745 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C6(H6), C7(H7), C12(H12), C13(H13), C16(H16), C17(H17), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44) ; _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 0.52985(2) 0.15626(2) 0.56509(2) 0.01854(15) Uani 1 1 d . . . . . O1 O 0.500000 0.250000 0.56567(6) 0.0266(6) Uani 1 2 d S T P . . N1 N 0.55867(12) 0.12756(12) 0.52052(5) 0.0207(5) Uani 1 1 d . . . . . C1 C 0.52518(15) 0.11653(15) 0.49200(6) 0.0220(6) Uani 1 1 d . . . . . N2 N 0.64362(12) 0.15240(12) 0.57008(5) 0.0204(5) Uani 1 1 d . . . . . C2 C 0.58346(16) 0.11856(16) 0.46854(6) 0.0245(6) Uani 1 1 d . . . . . H2 H 0.576421 0.111955 0.446795 0.029 Uiso 1 1 calc R . . . . N3 N 0.52208(13) 0.11340(13) 0.60901(5) 0.0225(5) Uani 1 1 d . . . . . C3 C 0.64990(16) 0.13151(16) 0.48294(6) 0.0265(6) Uani 1 1 d . . . . . H3 H 0.697583 0.135430 0.473377 0.032 Uiso 1 1 calc R . . . . N4 N 0.43658(13) 0.09129(13) 0.55949(5) 0.0219(5) Uani 1 1 d . . . . . C4 C 0.63353(15) 0.13798(15) 0.51520(6) 0.0216(6) Uani 1 1 d . . . . . C5 C 0.67870(15) 0.15325(15) 0.54165(6) 0.0228(6) Uani 1 1 d . . . . . C6 C 0.75515(16) 0.17187(16) 0.54525(6) 0.0262(6) Uani 1 1 d . . . . . H6 H 0.791447 0.175423 0.529185 0.031 Uiso 1 1 calc R . . . . C7 C 0.76647(16) 0.18368(16) 0.57619(7) 0.0245(6) Uani 1 1 d . . . . . H7 H 0.812165 0.198286 0.585644 0.029 Uiso 1 1 calc R . . . . C8 C 0.69651(15) 0.17002(15) 0.59214(6) 0.0228(6) Uani 1 1 d . . . . . C9 C 0.68749(16) 0.17310(15) 0.62514(6) 0.0233(6) Uani 1 1 d . . . . . C10 C 0.62716(16) 0.15145(15) 0.64443(6) 0.0228(6) Uani 1 1 d . . . . . C11 C 0.55627(16) 0.12005(15) 0.63752(6) 0.0231(6) Uani 1 1 d . . . . . C12 C 0.50752(17) 0.08709(17) 0.66063(6) 0.0290(7) Uani 1 1 d . . . . . H12 H 0.517298 0.083987 0.682322 0.035 Uiso 1 1 calc R . . . . C13 C 0.44536(17) 0.06133(17) 0.64597(6) 0.0291(7) Uani 1 1 d . . . . . H13 H 0.403909 0.036858 0.655281 0.035 Uiso 1 1 calc R . . . . C14 C 0.45492(15) 0.07844(16) 0.61383(6) 0.0243(6) Uani 1 1 d . . . . . C15 C 0.40872(16) 0.06777(16) 0.58767(6) 0.0236(6) Uani 1 1 d . . . . . C16 C 0.33451(16) 0.04044(17) 0.58381(7) 0.0285(7) Uani 1 1 d . . . . . H16 H 0.303272 0.019859 0.599491 0.034 Uiso 1 1 calc R . . . . C17 C 0.31732(16) 0.04965(17) 0.55329(7) 0.0281(6) Uani 1 1 d . . . . . H17 H 0.270967 0.037551 0.543773 0.034 Uiso 1 1 calc R . . . . C18 C 0.38206(15) 0.08121(15) 0.53768(6) 0.0229(6) Uani 1 1 d . . . . . C19 C 0.38558(15) 0.09549(15) 0.50510(6) 0.0219(6) Uani 1 1 d . . . . . C20 C 0.44792(15) 0.10840(15) 0.48546(6) 0.0217(6) Uani 1 1 d . . . . . C21 C 0.42944(15) 0.11893(16) 0.45131(6) 0.0227(6) Uani 1 1 d . . . . . C22 C 0.40426(17) 0.18842(18) 0.44129(7) 0.0320(7) Uani 1 1 d . . . . . H22 H 0.401649 0.228774 0.455609 0.038 Uiso 1 1 calc R . . . . C23 C 0.38295(19) 0.19930(19) 0.41060(8) 0.0386(8) Uani 1 1 d . . . . . H23 H 0.365815 0.246952 0.403990 0.046 Uiso 1 1 calc R . . . . C24 C 0.38661(18) 0.1409(2) 0.38961(7) 0.0365(8) Uani 1 1 d . . . . . H24 H 0.370930 0.148148 0.368701 0.044 Uiso 1 1 calc R . . . . C25 C 0.41292(18) 0.07243(19) 0.39900(7) 0.0336(7) Uani 1 1 d . . . . . H25 H 0.416282 0.032720 0.384396 0.040 Uiso 1 1 calc R . . . . C26 C 0.43472(16) 0.06070(17) 0.42974(6) 0.0267(6) Uani 1 1 d . . . . . H26 H 0.453125 0.013263 0.436029 0.032 Uiso 1 1 calc R . . . . C27 C 0.30943(15) 0.09412(16) 0.48999(6) 0.0236(6) Uani 1 1 d . . . . . C28 C 0.25772(17) 0.14967(18) 0.49737(7) 0.0315(7) Uani 1 1 d . . . . . H28 H 0.271083 0.188290 0.511482 0.038 Uiso 1 1 calc R . . . . C29 C 0.18650(18) 0.1489(2) 0.48417(8) 0.0384(8) Uani 1 1 d . . . . . H29 H 0.151618 0.186944 0.489302 0.046 Uiso 1 1 calc R . . . . C30 C 0.16661(18) 0.0929(2) 0.46364(7) 0.0379(8) Uani 1 1 d . . . . . H30 H 0.118080 0.092332 0.454698 0.045 Uiso 1 1 calc R . . . . C31 C 0.21721(18) 0.03796(18) 0.45620(7) 0.0325(7) Uani 1 1 d . . . . . H31 H 0.203585 -0.000325 0.441976 0.039 Uiso 1 1 calc R . . . . C32 C 0.28843(17) 0.03803(16) 0.46937(6) 0.0266(6) Uani 1 1 d . . . . . H32 H 0.322798 -0.000473 0.464226 0.032 Uiso 1 1 calc R . . . . C33 C 0.75614(16) 0.20312(16) 0.64138(6) 0.0257(6) Uani 1 1 d . . . . . C34 C 0.81677(19) 0.1568(2) 0.64803(8) 0.0425(8) Uani 1 1 d . . . . . H34 H 0.814415 0.105330 0.642749 0.051 Uiso 1 1 calc R . . . . C35 C 0.8804(2) 0.1849(2) 0.66223(9) 0.0530(10) Uani 1 1 d . . . . . H35 H 0.921177 0.152659 0.666758 0.064 Uiso 1 1 calc R . . . . C36 C 0.8845(2) 0.2606(2) 0.66987(8) 0.0470(9) Uani 1 1 d . . . . . H36 H 0.928114 0.280278 0.679474 0.056 Uiso 1 1 calc R . . . . C37 C 0.82497(19) 0.3065(2) 0.66337(8) 0.0424(9) Uani 1 1 d . . . . . H37 H 0.827515 0.358014 0.668556 0.051 Uiso 1 1 calc R . . . . C38 C 0.76130(17) 0.27834(17) 0.64935(7) 0.0312(7) Uani 1 1 d . . . . . H38 H 0.720568 0.310794 0.645096 0.037 Uiso 1 1 calc R . . . . C39 C 0.63974(17) 0.15908(16) 0.67914(6) 0.0257(6) Uani 1 1 d . . . . . C40 C 0.6815(2) 0.1060(2) 0.69528(7) 0.0418(9) Uani 1 1 d . . . . . H40 H 0.703219 0.065459 0.684272 0.050 Uiso 1 1 calc R . . . . C41 C 0.6916(2) 0.1115(2) 0.72710(8) 0.0476(9) Uani 1 1 d . . . . . H41 H 0.720965 0.075317 0.737669 0.057 Uiso 1 1 calc R . . . . C42 C 0.6593(2) 0.16955(18) 0.74367(7) 0.0413(8) Uani 1 1 d . . . . . H42 H 0.666381 0.173577 0.765517 0.050 Uiso 1 1 calc R . . . . C43 C 0.6165(2) 0.22132(19) 0.72793(8) 0.0446(9) Uani 1 1 d . . . . . H43 H 0.593851 0.261067 0.739123 0.054 Uiso 1 1 calc R . . . . C44 C 0.60622(19) 0.21627(17) 0.69601(7) 0.0339(7) Uani 1 1 d . . . . . H44 H 0.576059 0.252093 0.685605 0.041 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 Fe1 0.0179(2) 0.0174(2) 0.0203(2) 0.00118(14) 0.00000(14) 0.00084(15) O1 0.0266(16) 0.0241(15) 0.0290(14) 0.000 0.000 0.0064(12) N1 0.0203(12) 0.0186(12) 0.0233(11) 0.0024(9) 0.0010(9) 0.0012(9) C1 0.0257(15) 0.0158(14) 0.0246(13) 0.0015(11) -0.0026(11) 0.0015(11) N2 0.0197(12) 0.0188(12) 0.0226(11) 0.0014(9) 0.0007(9) 0.0015(9) C2 0.0253(15) 0.0266(15) 0.0215(13) -0.0008(11) 0.0035(11) 0.0050(12) N3 0.0203(12) 0.0251(13) 0.0222(11) 0.0032(9) -0.0029(9) -0.0003(10) C3 0.0218(15) 0.0281(16) 0.0296(15) 0.0020(12) 0.0055(12) 0.0018(12) N4 0.0218(12) 0.0206(12) 0.0233(11) 0.0015(9) 0.0003(9) -0.0001(9) C4 0.0188(14) 0.0201(14) 0.0259(14) 0.0016(11) 0.0010(11) 0.0021(11) C5 0.0199(14) 0.0222(14) 0.0264(14) 0.0036(11) 0.0025(11) 0.0047(11) C6 0.0217(15) 0.0264(16) 0.0304(15) 0.0047(12) 0.0026(12) 0.0021(12) C7 0.0185(14) 0.0239(15) 0.0311(14) -0.0006(11) -0.0049(11) 0.0000(11) C8 0.0223(15) 0.0195(14) 0.0267(14) 0.0013(11) -0.0016(11) 0.0027(11) C9 0.0238(15) 0.0198(14) 0.0262(14) -0.0002(11) -0.0048(11) 0.0039(11) C10 0.0270(15) 0.0159(14) 0.0254(14) 0.0010(11) -0.0025(11) 0.0040(11) C11 0.0273(15) 0.0209(14) 0.0210(13) 0.0007(11) -0.0002(11) 0.0045(12) C12 0.0349(18) 0.0306(17) 0.0215(13) 0.0041(12) 0.0000(12) -0.0050(13) C13 0.0293(16) 0.0331(17) 0.0248(14) 0.0029(12) 0.0039(12) -0.0066(13) C14 0.0218(15) 0.0235(15) 0.0277(14) 0.0027(11) 0.0004(11) -0.0031(12) C15 0.0233(15) 0.0232(15) 0.0243(13) 0.0026(11) 0.0016(11) -0.0009(12) C16 0.0239(15) 0.0341(17) 0.0276(14) 0.0022(12) 0.0043(12) -0.0047(13) C17 0.0229(15) 0.0311(17) 0.0302(15) 0.0018(12) -0.0019(12) -0.0044(12) C18 0.0233(15) 0.0191(14) 0.0261(14) 0.0000(11) -0.0024(11) 0.0001(11) C19 0.0230(15) 0.0169(14) 0.0259(14) 0.0004(11) -0.0024(11) 0.0010(11) C20 0.0239(15) 0.0151(13) 0.0260(14) 0.0002(10) -0.0011(11) 0.0026(11) C21 0.0218(14) 0.0236(15) 0.0228(13) 0.0002(11) -0.0005(11) 0.0003(11) C22 0.0336(18) 0.0262(17) 0.0361(16) 0.0046(13) -0.0061(13) 0.0033(13) C23 0.0394(19) 0.0346(18) 0.0417(18) 0.0136(15) -0.0043(15) 0.0085(15) C24 0.0310(18) 0.053(2) 0.0258(15) 0.0102(14) -0.0023(13) 0.0030(15) C25 0.0327(18) 0.045(2) 0.0232(14) -0.0038(13) -0.0003(12) 0.0023(15) C26 0.0268(16) 0.0262(16) 0.0270(14) 0.0019(12) 0.0002(12) 0.0058(12) C27 0.0221(15) 0.0247(15) 0.0239(13) 0.0045(11) -0.0022(11) -0.0027(12) C28 0.0290(17) 0.0319(17) 0.0335(15) -0.0031(13) -0.0009(13) 0.0017(13) C29 0.0252(17) 0.046(2) 0.0437(19) 0.0062(15) -0.0010(14) 0.0060(15) C30 0.0256(17) 0.055(2) 0.0328(16) 0.0148(15) -0.0071(13) -0.0061(15) C31 0.0344(18) 0.0389(18) 0.0241(14) 0.0069(13) -0.0075(13) -0.0120(14) C32 0.0307(16) 0.0265(16) 0.0226(13) 0.0033(11) 0.0007(11) -0.0039(13) C33 0.0235(15) 0.0273(16) 0.0261(14) -0.0026(11) -0.0033(11) 0.0006(12) C34 0.0336(19) 0.036(2) 0.058(2) -0.0073(16) -0.0140(16) 0.0046(15) C35 0.033(2) 0.063(3) 0.064(2) -0.007(2) -0.0209(18) 0.0076(18) C36 0.0308(19) 0.064(3) 0.046(2) -0.0151(18) -0.0090(15) -0.0087(18) C37 0.0316(19) 0.045(2) 0.051(2) -0.0209(16) 0.0052(15) -0.0082(16) C38 0.0254(16) 0.0297(17) 0.0386(16) -0.0062(13) 0.0030(13) 0.0005(13) C39 0.0285(16) 0.0233(15) 0.0253(14) -0.0004(11) -0.0010(12) -0.0020(12) C40 0.056(2) 0.038(2) 0.0317(16) -0.0028(14) -0.0081(15) 0.0178(17) C41 0.062(3) 0.051(2) 0.0298(17) 0.0025(16) -0.0105(16) 0.0108(19) C42 0.065(2) 0.0364(19) 0.0222(15) -0.0010(13) -0.0044(15) -0.0101(17) C43 0.074(3) 0.0262(18) 0.0337(17) -0.0072(14) 0.0135(17) 0.0004(17) C44 0.048(2) 0.0262(16) 0.0278(15) 0.0019(12) 0.0047(14) 0.0054(14) _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 O1 1.7612(4) . ? Fe1 N1 2.049(2) . ? Fe1 N2 2.049(2) . ? Fe1 N3 2.042(2) . ? Fe1 N4 2.049(2) . ? N1 C1 1.378(3) . ? N1 C4 1.372(3) . ? C1 C2 1.451(4) . ? C1 C20 1.419(4) . ? N2 C5 1.374(3) . ? N2 C8 1.376(3) . ? C2 H2 0.9500 . ? C2 C3 1.361(4) . ? N3 C11 1.375(3) . ? N3 C14 1.371(3) . ? C3 H3 0.9500 . ? C3 C4 1.421(4) . ? N4 C15 1.375(3) . ? N4 C18 1.365(3) . ? C4 C5 1.421(4) . ? C5 C6 1.417(4) . ? C6 H6 0.9500 . ? C6 C7 1.361(4) . ? C7 H7 0.9500 . ? C7 C8 1.449(4) . ? C8 C9 1.428(4) . ? C9 C10 1.416(4) . ? C9 C33 1.512(4) . ? C10 C11 1.419(4) . ? C10 C39 1.514(4) . ? C11 C12 1.447(4) . ? C12 H12 0.9500 . ? C12 C13 1.359(4) . ? C13 H13 0.9500 . ? C13 C14 1.425(4) . ? C14 C15 1.409(4) . ? C15 C16 1.425(4) . ? C16 H16 0.9500 . ? C16 C17 1.357(4) . ? C17 H17 0.9500 . ? C17 C18 1.454(4) . ? C18 C19 1.424(4) . ? C19 C20 1.418(4) . ? C19 C27 1.510(4) . ? C20 C21 1.516(4) . ? C21 C22 1.391(4) . ? C21 C26 1.398(4) . ? C22 H22 0.9500 . ? C22 C23 1.387(4) . ? C23 H23 0.9500 . ? C23 C24 1.382(5) . ? C24 H24 0.9500 . ? C24 C25 1.374(4) . ? C25 H25 0.9500 . ? C25 C26 1.393(4) . ? C26 H26 0.9500 . ? C27 C28 1.395(4) . ? C27 C32 1.391(4) . ? C28 H28 0.9500 . ? C28 C29 1.396(4) . ? C29 H29 0.9500 . ? C29 C30 1.382(5) . ? C30 H30 0.9500 . ? C30 C31 1.375(5) . ? C31 H31 0.9500 . ? C31 C32 1.395(4) . ? C32 H32 0.9500 . ? C33 C34 1.395(4) . ? C33 C38 1.392(4) . ? C34 H34 0.9500 . ? C34 C35 1.387(5) . ? C35 H35 0.9500 . ? C35 C36 1.397(6) . ? C36 H36 0.9500 . ? C36 C37 1.374(5) . ? C37 H37 0.9500 . ? C37 C38 1.384(4) . ? C38 H38 0.9500 . ? C39 C40 1.393(4) . ? C39 C44 1.390(4) . ? C40 H40 0.9500 . ? C40 C41 1.383(4) . ? C41 H41 0.9500 . ? C41 C42 1.386(5) . ? C42 H42 0.9500 . ? C42 C43 1.379(5) . ? C43 H43 0.9500 . ? C43 C44 1.387(4) . ? C44 H44 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 O1 Fe1 N1 109.17(10) . . ? O1 Fe1 N2 109.40(7) . . ? O1 Fe1 N3 108.93(11) . . ? O1 Fe1 N4 107.17(7) . . ? N2 Fe1 N1 80.74(9) . . ? N2 Fe1 N4 143.43(9) . . ? N3 Fe1 N1 141.89(9) . . ? N3 Fe1 N2 87.61(9) . . ? N3 Fe1 N4 80.78(9) . . ? N4 Fe1 N1 87.31(9) . . ? Fe1 O1 Fe1 178.39(17) . 6_554 ? C1 N1 Fe1 139.23(19) . . ? C4 N1 Fe1 111.55(17) . . ? C4 N1 C1 107.2(2) . . ? N1 C1 C2 107.5(2) . . ? N1 C1 C20 127.9(2) . . ? C20 C1 C2 124.5(2) . . ? C5 N2 Fe1 111.16(17) . . ? C5 N2 C8 107.2(2) . . ? C8 N2 Fe1 138.42(18) . . ? C1 C2 H2 125.8 . . ? C3 C2 C1 108.5(2) . . ? C3 C2 H2 125.8 . . ? C11 N3 Fe1 139.54(19) . . ? C14 N3 Fe1 111.77(17) . . ? C14 N3 C11 107.2(2) . . ? C2 C3 H3 127.0 . . ? C2 C3 C4 106.1(2) . . ? C4 C3 H3 127.0 . . ? C15 N4 Fe1 111.47(18) . . ? C18 N4 Fe1 137.58(19) . . ? C18 N4 C15 107.7(2) . . ? N1 C4 C3 110.6(2) . . ? N1 C4 C5 116.7(2) . . ? C5 C4 C3 132.7(3) . . ? N2 C5 C4 116.7(2) . . ? N2 C5 C6 110.3(2) . . ? C6 C5 C4 133.0(3) . . ? C5 C6 H6 126.7 . . ? C7 C6 C5 106.7(2) . . ? C7 C6 H6 126.7 . . ? C6 C7 H7 126.1 . . ? C6 C7 C8 107.9(2) . . ? C8 C7 H7 126.1 . . ? N2 C8 C7 107.9(2) . . ? N2 C8 C9 127.9(3) . . ? C9 C8 C7 124.1(3) . . ? C8 C9 C33 112.3(2) . . ? C10 C9 C8 131.1(3) . . ? C10 C9 C33 116.6(2) . . ? C9 C10 C11 131.9(3) . . ? C9 C10 C39 116.0(2) . . ? C11 C10 C39 112.0(2) . . ? N3 C11 C10 128.2(2) . . ? N3 C11 C12 107.9(2) . . ? C10 C11 C12 123.9(2) . . ? C11 C12 H12 125.8 . . ? C13 C12 C11 108.3(2) . . ? C13 C12 H12 125.8 . . ? C12 C13 H13 126.9 . . ? C12 C13 C14 106.1(3) . . ? C14 C13 H13 126.9 . . ? N3 C14 C13 110.5(2) . . ? N3 C14 C15 117.1(2) . . ? C15 C14 C13 132.4(3) . . ? N4 C15 C14 116.6(2) . . ? N4 C15 C16 109.9(2) . . ? C14 C15 C16 133.4(3) . . ? C15 C16 H16 126.8 . . ? C17 C16 C15 106.4(2) . . ? C17 C16 H16 126.8 . . ? C16 C17 H17 125.9 . . ? C16 C17 C18 108.2(3) . . ? C18 C17 H17 125.9 . . ? N4 C18 C17 107.7(2) . . ? N4 C18 C19 128.3(3) . . ? C19 C18 C17 124.0(3) . . ? C18 C19 C27 112.3(2) . . ? C20 C19 C18 130.5(3) . . ? C20 C19 C27 117.2(2) . . ? C1 C20 C21 113.1(2) . . ? C19 C20 C1 131.8(2) . . ? C19 C20 C21 115.1(2) . . ? C22 C21 C20 118.8(2) . . ? C22 C21 C26 118.9(3) . . ? C26 C21 C20 122.3(2) . . ? C21 C22 H22 119.7 . . ? C23 C22 C21 120.6(3) . . ? C23 C22 H22 119.7 . . ? C22 C23 H23 120.0 . . ? C24 C23 C22 120.1(3) . . ? C24 C23 H23 120.0 . . ? C23 C24 H24 120.0 . . ? C25 C24 C23 120.0(3) . . ? C25 C24 H24 120.0 . . ? C24 C25 H25 119.7 . . ? C24 C25 C26 120.6(3) . . ? C26 C25 H25 119.7 . . ? C21 C26 H26 120.1 . . ? C25 C26 C21 119.8(3) . . ? C25 C26 H26 120.1 . . ? C28 C27 C19 119.3(2) . . ? C32 C27 C19 122.0(3) . . ? C32 C27 C28 118.7(3) . . ? C27 C28 H28 119.8 . . ? C27 C28 C29 120.4(3) . . ? C29 C28 H28 119.8 . . ? C28 C29 H29 119.9 . . ? C30 C29 C28 120.1(3) . . ? C30 C29 H29 119.9 . . ? C29 C30 H30 120.1 . . ? C31 C30 C29 119.8(3) . . ? C31 C30 H30 120.1 . . ? C30 C31 H31 119.8 . . ? C30 C31 C32 120.5(3) . . ? C32 C31 H31 119.8 . . ? C27 C32 C31 120.4(3) . . ? C27 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C9 121.0(3) . . ? C38 C33 C9 120.7(3) . . ? C38 C33 C34 118.2(3) . . ? C33 C34 H34 119.5 . . ? C35 C34 C33 120.9(3) . . ? C35 C34 H34 119.5 . . ? C34 C35 H35 120.1 . . ? C34 C35 C36 119.9(3) . . ? C36 C35 H35 120.1 . . ? C35 C36 H36 120.3 . . ? C37 C36 C35 119.4(3) . . ? C37 C36 H36 120.3 . . ? C36 C37 H37 119.7 . . ? C36 C37 C38 120.7(3) . . ? C38 C37 H37 119.7 . . ? C33 C38 H38 119.5 . . ? C37 C38 C33 120.9(3) . . ? C37 C38 H38 119.5 . . ? C40 C39 C10 120.6(3) . . ? C44 C39 C10 121.0(3) . . ? C44 C39 C40 118.3(3) . . ? C39 C40 H40 119.5 . . ? C41 C40 C39 120.9(3) . . ? C41 C40 H40 119.5 . . ? C40 C41 H41 119.8 . . ? C40 C41 C42 120.4(3) . . ? C42 C41 H41 119.8 . . ? C41 C42 H42 120.5 . . ? C43 C42 C41 118.9(3) . . ? C43 C42 H42 120.5 . . ? C42 C43 H43 119.5 . . ? C42 C43 C44 121.0(3) . . ? C44 C43 H43 119.5 . . ? C39 C44 H44 119.8 . . ? C43 C44 C39 120.4(3) . . ? C43 C44 H44 119.8 . . ? _iucr_refine_instructions_details ; TITL xu017_a.res in I4(1)/a xu017.res created by SHELXL-2018/3 at 12:18:38 on 20-May-2018 REM Old TITL xu017_a.res in I4(1)/a REM SHELXT solution in I4(1)/a REM R1 0.122, Rweak 0.002, Alpha 0.027, Orientation as input REM Formula found by SHELXT: C88 Fe2 N8 O CELL 0.71073 17.9013 17.9013 42.9649 90 90 90 ZERR 8 0.0003 0.0003 0.0008 0 0 0 LATT 2 SYMM 0.5-X,-Y,0.5+Z SYMM 0.75-Y,0.25+X,0.25+Z SYMM 0.75+Y,0.75-X,0.75+Z SFAC C H Fe N O UNIT 704 448 16 64 8 L.S. 4 PLAN 7 TEMP -180.15 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.100000 FVAR 0.10133 FE1 3 0.529845 0.156260 0.565095 11.00000 0.01786 0.01744 = 0.02033 0.00118 0.00000 0.00084 O1 5 0.500000 0.250000 0.565671 10.50000 0.02662 0.02406 = 0.02903 0.00000 0.00000 0.00639 N1 4 0.558668 0.127559 0.520516 11.00000 0.02026 0.01864 = 0.02327 0.00241 0.00096 0.00121 C1 1 0.525176 0.116532 0.491996 11.00000 0.02569 0.01584 = 0.02457 0.00152 -0.00261 0.00150 N2 4 0.643622 0.152400 0.570082 11.00000 0.01966 0.01883 = 0.02260 0.00143 0.00069 0.00151 C2 1 0.583461 0.118556 0.468538 11.00000 0.02532 0.02664 = 0.02146 -0.00081 0.00350 0.00498 AFIX 43 H2 2 0.576421 0.111955 0.446795 11.00000 -1.20000 AFIX 0 N3 4 0.522081 0.113401 0.609011 11.00000 0.02026 0.02507 = 0.02224 0.00320 -0.00290 -0.00032 C3 1 0.649901 0.131508 0.482944 11.00000 0.02184 0.02810 = 0.02961 0.00197 0.00550 0.00181 AFIX 43 H3 2 0.697583 0.135430 0.473377 11.00000 -1.20000 AFIX 0 N4 4 0.436580 0.091294 0.559494 11.00000 0.02179 0.02062 = 0.02332 0.00146 0.00029 -0.00015 C4 1 0.633534 0.137984 0.515202 11.00000 0.01884 0.02008 = 0.02593 0.00164 0.00105 0.00205 C5 1 0.678701 0.153248 0.541651 11.00000 0.01991 0.02221 = 0.02637 0.00357 0.00247 0.00469 C6 1 0.755149 0.171869 0.545247 11.00000 0.02174 0.02639 = 0.03040 0.00469 0.00261 0.00212 AFIX 43 H6 2 0.791447 0.175423 0.529185 11.00000 -1.20000 AFIX 0 C7 1 0.766472 0.183676 0.576188 11.00000 0.01853 0.02393 = 0.03113 -0.00064 -0.00485 -0.00005 AFIX 43 H7 2 0.812165 0.198286 0.585644 11.00000 -1.20000 AFIX 0 C8 1 0.696506 0.170016 0.592142 11.00000 0.02228 0.01947 = 0.02669 0.00132 -0.00158 0.00268 C9 1 0.687490 0.173102 0.625138 11.00000 0.02380 0.01982 = 0.02620 -0.00020 -0.00478 0.00388 C10 1 0.627162 0.151450 0.644432 11.00000 0.02698 0.01593 = 0.02536 0.00095 -0.00246 0.00397 C11 1 0.556270 0.120050 0.637524 11.00000 0.02730 0.02089 = 0.02099 0.00070 -0.00023 0.00448 C12 1 0.507520 0.087087 0.660628 11.00000 0.03492 0.03058 = 0.02148 0.00414 0.00002 -0.00503 AFIX 43 H12 2 0.517298 0.083987 0.682322 11.00000 -1.20000 AFIX 0 C13 1 0.445362 0.061329 0.645973 11.00000 0.02933 0.03312 = 0.02482 0.00292 0.00393 -0.00658 AFIX 43 H13 2 0.403909 0.036858 0.655281 11.00000 -1.20000 AFIX 0 C14 1 0.454920 0.078437 0.613830 11.00000 0.02181 0.02354 = 0.02767 0.00271 0.00040 -0.00315 C15 1 0.408715 0.067768 0.587669 11.00000 0.02327 0.02316 = 0.02429 0.00258 0.00160 -0.00087 C16 1 0.334507 0.040440 0.583807 11.00000 0.02386 0.03411 = 0.02763 0.00223 0.00427 -0.00465 AFIX 43 H16 2 0.303272 0.019859 0.599491 11.00000 -1.20000 AFIX 0 C17 1 0.317317 0.049646 0.553290 11.00000 0.02295 0.03110 = 0.03017 0.00184 -0.00190 -0.00444 AFIX 43 H17 2 0.270967 0.037551 0.543773 11.00000 -1.20000 AFIX 0 C18 1 0.382062 0.081207 0.537675 11.00000 0.02333 0.01912 = 0.02610 -0.00002 -0.00243 0.00014 C19 1 0.385581 0.095494 0.505096 11.00000 0.02298 0.01693 = 0.02591 0.00043 -0.00240 0.00098 C20 1 0.447922 0.108398 0.485459 11.00000 0.02386 0.01511 = 0.02602 0.00021 -0.00112 0.00260 C21 1 0.429443 0.118926 0.451313 11.00000 0.02176 0.02359 = 0.02277 0.00020 -0.00052 0.00025 C22 1 0.404263 0.188418 0.441292 11.00000 0.03361 0.02616 = 0.03610 0.00455 -0.00605 0.00330 AFIX 43 H22 2 0.401649 0.228774 0.455609 11.00000 -1.20000 AFIX 0 C23 1 0.382952 0.199297 0.410599 11.00000 0.03942 0.03461 = 0.04172 0.01363 -0.00433 0.00846 AFIX 43 H23 2 0.365815 0.246952 0.403990 11.00000 -1.20000 AFIX 0 C24 1 0.386605 0.140927 0.389610 11.00000 0.03100 0.05275 = 0.02578 0.01024 -0.00226 0.00300 AFIX 43 H24 2 0.370930 0.148148 0.368701 11.00000 -1.20000 AFIX 0 C25 1 0.412923 0.072428 0.398997 11.00000 0.03273 0.04480 = 0.02316 -0.00376 -0.00027 0.00226 AFIX 43 H25 2 0.416282 0.032720 0.384396 11.00000 -1.20000 AFIX 0 C26 1 0.434724 0.060697 0.429742 11.00000 0.02681 0.02620 = 0.02702 0.00191 0.00024 0.00577 AFIX 43 H26 2 0.453125 0.013263 0.436029 11.00000 -1.20000 AFIX 0 C27 1 0.309428 0.094118 0.489991 11.00000 0.02205 0.02471 = 0.02393 0.00453 -0.00221 -0.00266 C28 1 0.257720 0.149675 0.497374 11.00000 0.02902 0.03188 = 0.03353 -0.00306 -0.00090 0.00167 AFIX 43 H28 2 0.271083 0.188290 0.511482 11.00000 -1.20000 AFIX 0 C29 1 0.186501 0.148894 0.484170 11.00000 0.02524 0.04617 = 0.04373 0.00623 -0.00096 0.00603 AFIX 43 H29 2 0.151618 0.186944 0.489302 11.00000 -1.20000 AFIX 0 C30 1 0.166610 0.092877 0.463641 11.00000 0.02561 0.05514 = 0.03281 0.01480 -0.00714 -0.00613 AFIX 43 H30 2 0.118080 0.092332 0.454698 11.00000 -1.20000 AFIX 0 C31 1 0.217214 0.037958 0.456197 11.00000 0.03439 0.03887 = 0.02412 0.00692 -0.00750 -0.01202 AFIX 43 H31 2 0.203585 -0.000325 0.441976 11.00000 -1.20000 AFIX 0 C32 1 0.288426 0.038029 0.469370 11.00000 0.03071 0.02649 = 0.02262 0.00329 0.00069 -0.00386 AFIX 43 H32 2 0.322798 -0.000473 0.464226 11.00000 -1.20000 AFIX 0 C33 1 0.756141 0.203122 0.641384 11.00000 0.02352 0.02733 = 0.02611 -0.00259 -0.00329 0.00059 C34 1 0.816771 0.156811 0.648028 11.00000 0.03359 0.03645 = 0.05758 -0.00730 -0.01401 0.00456 AFIX 43 H34 2 0.814415 0.105330 0.642749 11.00000 -1.20000 AFIX 0 C35 1 0.880434 0.184881 0.662232 11.00000 0.03282 0.06255 = 0.06374 -0.00745 -0.02087 0.00757 AFIX 43 H35 2 0.921177 0.152659 0.666758 11.00000 -1.20000 AFIX 0 C36 1 0.884533 0.260637 0.669871 11.00000 0.03084 0.06428 = 0.04603 -0.01508 -0.00897 -0.00874 AFIX 43 H36 2 0.928114 0.280278 0.679474 11.00000 -1.20000 AFIX 0 C37 1 0.824967 0.306488 0.663372 11.00000 0.03164 0.04462 = 0.05104 -0.02091 0.00517 -0.00823 AFIX 43 H37 2 0.827515 0.358014 0.668556 11.00000 -1.20000 AFIX 0 C38 1 0.761302 0.278345 0.649347 11.00000 0.02540 0.02967 = 0.03857 -0.00616 0.00299 0.00051 AFIX 43 H38 2 0.720568 0.310794 0.645096 11.00000 -1.20000 AFIX 0 C39 1 0.639737 0.159083 0.679136 11.00000 0.02850 0.02335 = 0.02533 -0.00043 -0.00098 -0.00195 C40 1 0.681453 0.106009 0.695282 11.00000 0.05598 0.03787 = 0.03168 -0.00283 -0.00806 0.01784 AFIX 43 H40 2 0.703219 0.065459 0.684272 11.00000 -1.20000 AFIX 0 C41 1 0.691615 0.111524 0.727097 11.00000 0.06197 0.05103 = 0.02977 0.00247 -0.01049 0.01075 AFIX 43 H41 2 0.720965 0.075317 0.737669 11.00000 -1.20000 AFIX 0 C42 1 0.659250 0.169553 0.743670 11.00000 0.06538 0.03644 = 0.02220 -0.00097 -0.00444 -0.01011 AFIX 43 H42 2 0.666381 0.173577 0.765517 11.00000 -1.20000 AFIX 0 C43 1 0.616548 0.221322 0.727932 11.00000 0.07399 0.02617 = 0.03374 -0.00724 0.01349 0.00037 AFIX 43 H43 2 0.593851 0.261067 0.739123 11.00000 -1.20000 AFIX 0 C44 1 0.606218 0.216268 0.696007 11.00000 0.04754 0.02620 = 0.02782 0.00194 0.00472 0.00545 AFIX 43 H44 2 0.576059 0.252093 0.685605 11.00000 -1.20000 AFIX 0 HKLF 4 REM xu017_a.res in I4(1)/a REM wR2 = 0.1745, GooF = S = 1.082, Restrained GooF = 1.082 for all data REM R1 = 0.0546 for 5243 Fo > 4sig(Fo) and 0.0798 for all 7049 data REM 447 parameters refined using 0 restraints END WGHT 0.0721 18.7389 REM Highest difference peak 0.979, deepest hole -0.698, 1-sigma level 0.077 Q1 1 0.6225 0.1364 0.5671 11.00000 0.05 0.44 Q2 1 0.5125 0.2137 0.5670 11.00000 0.05 0.42 Q3 1 0.9712 0.3464 0.6948 11.00000 0.05 0.40 Q4 1 0.5536 0.0987 0.5652 11.00000 0.05 0.40 Q5 1 0.4412 0.1773 0.5639 11.00000 0.05 0.38 Q6 1 0.6009 0.1848 0.5666 11.00000 0.05 0.36 Q7 1 0.6018 0.2763 0.6828 11.00000 0.05 0.36 REM The information below was added by Olex2. REM REM R1 = 0.0546 for 5243 Fo > 4sig(Fo) and 0.0798 for all 36170 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.98, deepest hole -0.70 REM Mean Shift 0, Max Shift 0.007. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0798 REM R1_gt = 0.0546 REM wR_ref = 0.1745 REM GOOF = 1.082 REM Shift_max = 0.007 REM Shift_mean = 0 REM Reflections_all = 36170 REM Reflections_gt = 5243 REM Parameters = n/a REM Hole = -0.70 REM Peak = 0.98 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.476 _oxdiff_exptl_absorpt_empirical_full_min 0.724