# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_K1 _audit_creation_date 2013-10-16 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:59:47, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C46 H55 Fe K N4 O6' _chemical_formula_sum 'C46 H55 Fe K N4 O6' _chemical_formula_weight 854.89 _chemical_melting_point ? _chemical_oxdiff_formula 'C46 H55 Fe N4 K O6' 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' N N 0.0311 0.0180 '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' K K 0.3868 1.0657 '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' _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_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.8231(2) _cell_length_b 21.9105(2) _cell_length_c 20.3007(1) _cell_angle_alpha 90.00 _cell_angle_beta 98.027(1) _cell_angle_gamma 90.00 _cell_volume 4766.9(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 56124 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 76.5880 _cell_measurement_theta_min 4.0040 _exptl_absorpt_coefficient_mu 3.699 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.22395 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dull dark violet' _exptl_crystal_colour_lustre dull _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary violet _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1808 _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.3553 _exptl_crystal_size_min 0.3271 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_unetI/netI 0.0145 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 96550 _diffrn_reflns_theta_full 76.72 _diffrn_reflns_theta_max 76.72 _diffrn_reflns_theta_min 2.98 _diffrn_ambient_temperature 123(2) _diffrn_detector_area_resol_mean 10.3546 _diffrn_measured_fraction_theta_full 0.9873 _diffrn_measured_fraction_theta_max 0.9873 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -86.00 -15.00 0.5000 3.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 -37.0000 60.0000 142 #__ type_ start__ end____ width___ exp.time_ 2 omega -70.00 25.00 0.5000 3.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 57.0000 30.0000 190 #__ type_ start__ end____ width___ exp.time_ 3 omega -68.00 -8.00 0.5000 3.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 -77.0000 0.0000 120 #__ type_ start__ end____ width___ exp.time_ 4 omega -69.00 -8.00 0.5000 3.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 -77.0000 -180.0000 122 #__ type_ start__ end____ width___ exp.time_ 5 omega -51.00 -8.00 0.5000 3.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 -77.0000 90.0000 86 #__ type_ start__ end____ width___ exp.time_ 6 omega -120.00 -8.00 0.5000 3.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 -77.0000 -90.0000 224 #__ type_ start__ end____ width___ exp.time_ 7 omega -71.00 32.00 0.5000 3.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 57.0000 -150.0000 206 #__ type_ start__ end____ width___ exp.time_ 8 omega -116.00 -86.00 0.5000 3.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 -77.0000 90.0000 60 #__ type_ start__ end____ width___ exp.time_ 9 omega -120.00 -49.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -77.0000 -30.0000 142 #__ type_ start__ end____ width___ exp.time_ 10 omega -137.00 -100.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -77.0000 168.8182 74 #__ type_ start__ end____ width___ exp.time_ 11 omega -75.00 -49.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -77.0000 60.0000 52 #__ type_ start__ end____ width___ exp.time_ 12 omega -76.00 -49.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -77.0000 120.0000 54 #__ type_ start__ end____ width___ exp.time_ 13 omega -75.00 -49.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -77.0000 -120.0000 52 #__ type_ start__ end____ width___ exp.time_ 14 omega -81.00 -51.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -71.0000 -57.8777 60 #__ type_ start__ end____ width___ exp.time_ 15 omega -85.00 -49.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -77.0000 -5.7675 72 #__ type_ start__ end____ width___ exp.time_ 16 omega -76.00 -50.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -74.0000 13.4472 52 #__ type_ start__ end____ width___ exp.time_ 17 omega -76.00 -50.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -72.0000 65.7967 52 #__ type_ start__ end____ width___ exp.time_ 18 omega -74.00 -49.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -77.0000 -90.0000 50 #__ type_ start__ end____ width___ exp.time_ 19 omega -88.00 -4.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 79.0000 -75.6547 168 #__ type_ start__ end____ width___ exp.time_ 20 omega -75.00 -49.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -77.0000 30.0000 52 #__ type_ start__ end____ width___ exp.time_ 21 omega -122.00 -49.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -77.0000 -60.0000 146 #__ type_ start__ end____ width___ exp.time_ 22 omega -76.00 -50.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -73.0000 40.0107 52 #__ type_ start__ end____ width___ exp.time_ 23 omega -83.00 -50.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -73.0000 134.9790 66 #__ type_ start__ end____ width___ exp.time_ 24 omega -76.00 -50.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -73.0000 -177.3206 52 #__ type_ start__ end____ width___ exp.time_ 25 omega -94.00 -49.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -77.0000 168.8182 90 #__ type_ start__ end____ width___ exp.time_ 26 omega -75.00 -49.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -77.0000 -150.0000 52 #__ type_ start__ end____ width___ exp.time_ 27 omega -75.00 -49.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -77.0000 90.0000 52 #__ type_ start__ end____ width___ exp.time_ 28 omega -86.00 -4.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 80.0000 101.9935 164 #__ type_ start__ end____ width___ exp.time_ 29 omega 79.00 115.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -90.0000 72 #__ type_ start__ end____ width___ exp.time_ 30 omega 132.00 158.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -60.0000 52 #__ type_ start__ end____ width___ exp.time_ 31 omega 77.00 124.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -80.0000 -142.7873 94 #__ type_ start__ end____ width___ exp.time_ 32 omega 83.00 139.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 60.0000 112 #__ type_ start__ end____ width___ exp.time_ 33 omega 45.00 75.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -45.0000 0.0000 60 #__ type_ start__ end____ width___ exp.time_ 34 omega 83.00 149.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 -60.0000 132 #__ type_ start__ end____ width___ exp.time_ 35 omega 33.00 61.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -80.0000 -142.7873 56 #__ type_ start__ end____ width___ exp.time_ 36 omega 127.00 154.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -180.0000 54 #__ type_ start__ end____ width___ exp.time_ 37 omega 79.00 105.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 30.0000 52 #__ type_ start__ end____ width___ exp.time_ 38 omega 79.00 105.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -180.0000 52 #__ type_ start__ end____ width___ exp.time_ 39 omega 36.00 62.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -30.0000 -150.0000 52 #__ type_ start__ end____ width___ exp.time_ 40 omega 132.00 158.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 120.0000 52 #__ type_ start__ end____ width___ exp.time_ 41 omega 79.00 105.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 120.0000 52 #__ type_ start__ end____ width___ exp.time_ 42 omega 83.00 122.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -80.0000 16.1050 78 #__ type_ start__ end____ width___ exp.time_ 43 omega 39.00 67.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -30.0000 90.0000 56 #__ type_ start__ end____ width___ exp.time_ 44 omega 132.00 158.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -150.0000 52 #__ type_ start__ end____ width___ exp.time_ 45 omega 34.00 112.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -80.0000 85.2036 156 #__ type_ start__ end____ width___ exp.time_ 46 omega 79.00 104.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -150.0000 50 #__ type_ start__ end____ width___ exp.time_ 47 omega 119.00 146.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -30.0000 54 #__ type_ start__ end____ width___ exp.time_ 48 omega 116.00 142.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -80.0000 172.5740 52 #__ type_ start__ end____ width___ exp.time_ 49 omega 43.00 79.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -80.0000 16.1050 72 #__ type_ start__ end____ width___ exp.time_ 50 omega 79.00 105.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -30.0000 52 #__ type_ start__ end____ width___ exp.time_ 51 omega 131.00 157.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 90.0000 52 #__ type_ start__ end____ width___ exp.time_ 52 omega 111.00 137.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 30.0000 52 #__ type_ start__ end____ width___ exp.time_ 53 omega 79.00 104.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 60.0000 50 #__ type_ start__ end____ width___ exp.time_ 54 omega 125.00 155.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 60.0000 60 #__ type_ start__ end____ width___ exp.time_ 55 omega 33.00 112.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -80.0000 172.5740 158 #__ type_ start__ end____ width___ exp.time_ 56 omega 79.00 105.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -120.0000 52 #__ type_ start__ end____ width___ exp.time_ 57 omega 122.00 158.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -120.0000 72 #__ type_ start__ end____ width___ exp.time_ 58 omega 79.00 105.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 -60.0000 52 #__ type_ start__ end____ width___ exp.time_ 59 omega 79.00 105.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 90.0000 52 #__ type_ start__ end____ width___ exp.time_ 60 omega 43.00 69.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -30.0000 -60.0000 52 #__ type_ start__ end____ width___ exp.time_ 61 omega 40.00 72.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -45.0000 60.0000 64 #__ type_ start__ end____ width___ exp.time_ 62 omega 120.00 150.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 0.0000 60 #__ type_ start__ end____ width___ exp.time_ 63 omega 121.00 147.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -79.0000 -47.8692 52 #__ type_ start__ end____ width___ exp.time_ 64 omega 84.00 113.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -80.0000 126.7107 58 #__ type_ start__ end____ width___ exp.time_ 65 omega 79.00 105.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 66 omega 119.00 155.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 -90.0000 72 #__ type_ start__ end____ width___ exp.time_ 67 omega 36.00 103.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -79.0000 -47.8692 134 #__ type_ start__ end____ width___ exp.time_ 68 omega 83.00 113.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 -90.0000 60 #__ type_ start__ end____ width___ exp.time_ 69 omega 36.00 62.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -30.0000 -30.0000 52 #__ type_ start__ end____ width___ exp.time_ 70 omega 83.00 109.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -80.0000 -15.3845 52 #__ type_ start__ end____ width___ exp.time_ 71 omega 33.00 72.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -80.0000 126.7107 78 #__ type_ start__ end____ width___ exp.time_ 72 omega 84.00 148.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 120.0000 128 #__ type_ start__ end____ width___ exp.time_ 73 omega 84.00 153.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 90.0000 138 #__ type_ start__ end____ width___ exp.time_ 74 omega 83.00 153.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 -120.0000 140 #__ type_ start__ end____ width___ exp.time_ 75 omega 38.00 70.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -45.0000 150.0000 64 #__ type_ start__ end____ width___ exp.time_ 76 omega 85.00 136.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 -30.0000 102 #__ type_ start__ end____ width___ exp.time_ 77 omega 83.00 134.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 0.0000 102 #__ type_ start__ end____ width___ exp.time_ 78 omega 83.00 138.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 30.0000 110 #__ type_ start__ end____ width___ exp.time_ 79 omega 36.00 62.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -30.0000 -90.0000 52 #__ type_ start__ end____ width___ exp.time_ 80 omega 83.00 156.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 150.0000 146 #__ type_ start__ end____ width___ exp.time_ 81 omega 121.00 148.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 150.0000 54 #__ type_ start__ end____ width___ exp.time_ 82 omega 34.00 73.50 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -80.0000 -15.3845 79 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0422617000 _diffrn_orient_matrix_UB_12 0.0314287000 _diffrn_orient_matrix_UB_13 -0.0610035000 _diffrn_orient_matrix_UB_21 -0.0347639000 _diffrn_orient_matrix_UB_22 0.0625894000 _diffrn_orient_matrix_UB_23 0.0267764000 _diffrn_orient_matrix_UB_31 0.1329712000 _diffrn_orient_matrix_UB_32 0.0063974000 _diffrn_orient_matrix_UB_33 0.0379332000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 9482 _reflns_number_total 9864 _reflns_odcompleteness_completeness 98.73 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 76.71 _reflns_threshold_expression >2\s(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 1.049 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.077 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 569 _refine_ls_number_reflns 9864 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0756 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1270P)^2^+5.7472P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2153 _refine_ls_wR_factor_ref 0.2174 _refine_special_details ; The structure contained badly disordered solvent molecules that could not be identified and refined successfully. The electron density associated with these solvate molecules (182 electrons in a solvent accessible void of 252 cubic Ang. was removed with SQUEEZE implemented in PLATON. One pyridyl substituent coordinated to K1 was disordered and was refined over split positions. Furthermore, two disordered carbon atoms of 18-crown-6 were also refined over split positions with DFIX and SIMU restraints. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; 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 -0.010 0.500 0.000 374 91 ' ' 2 -0.008 0.000 0.500 374 91 ' ' _platon_squeeze_details ; ; _olex2_refinement_description ; 1. Shared sites {H10R, H10Y} 2. Others Fixed Sof: H10X(0.78) H10Y(0.78) H10Q(0.22) H10R(0.22) C110(0.78) H11A(0.78) H11B(0.78) C210(0.22) H21X(0.22) H21Y(0.22) C111(0.78) H11C(0.78) H11D(0.78) C211(0.22) H21C(0.22) H21D(0.22) H11E(0.78) H11F(0.78) H11X(0.22) H11Y(0.22) Fixed Uiso: H12(0.053) H13(0.07) H14(0.069) H15(0.068) H22(0.068) H23(0.079) H24(0.073) H25(0.074) H32(0.055) H33(0.066) H34(0.059) H35(0.052) H32A(0.065) H33A(0.076) H34A(0.069) H35A(0.069) H42(0.05) H43(0.068) H44(0.076) H45(0.081) H10A(0.08) H10B(0.08) H10C(0.078) H10D(0.078) H10E(0.076) H10F(0.076) H10G(0.082) H10H(0.082) H10I(0.093) H10J(0.093) H10K(0.104) H10L(0.104) H10M(0.108) H10N(0.108) H10O(0.108) H10P(0.108) H10X(0.108) H10Y(0.108) H10Q(0.108) H10R(0.108) H11A(0.087) H11B(0.087) H21X(0.127) H21Y(0.127) H11C(0.087) H11D(0.087) H21C(0.117) H21D(0.117) H11E(0.094) H11F(0.094) H11X(0.094) H11Y(0.094) H51A(0.243) H51B(0.243) H51C(0.243) H61A(0.247) H61B(0.247) H61C(0.247) H71A(0.21) H71B(0.21) H71C(0.21) H81A(0.181) H81B(0.181) H81C(0.181) H91A(0.199) H91B(0.199) H91C(0.199) Fixed X: H12(0.1254) H13(0.2089) H14(0.4154) H15(0.5367) H22(-0.1009) H23(- 0.3002) H24(-0.3444) H25(-0.1811) H32(0.2011) H33(0.1011) H34(-0.0539) H35(- 0.1089) H32A(-0.0297) H33A(-0.1252) H34A(-0.0754) H35A(0.07) H42(0.3161) H43(0.4973) H44(0.6873) H45(0.6956) H10A(-0.0463) H10B(0.0154) H10C(0.1656) H10D(0.1093) H10E(0.3051) H10F(0.3556) H10G(0.4052) H10H(0.4689) H10I(0.446) H10J(0.4517) H10K(0.2748) H10L(0.3628) H10M(0.1962) H10N(0.1245) H10O(-0.0063) H10P(0.0613) H10X(-0.1154) H10Y(-0.1858) H10Q(-0.1305) H10R(-0.1837) H11A(- 0.2766) H11B(-0.3004) H21X(-0.1518) H21Y(-0.2839) H11C(-0.2771) H11D(-0.3265) H21C(-0.3183) H21D(-0.2078) H11E(-0.1594) H11F(-0.227) H11X(-0.1689) H11Y(- 0.2441) H51A(0.5076) H51B(0.4434) H51C(0.4164) H61A(0.5178) H61B(0.4298) H61C(0.4583) H71A(0.0881) H71B(0.2213) H71C(0.1952) H81A(-0.035) H81B(-0.0518) H81C(-0.0205) H91A(0.0708) H91B(0.1763) H91C(0.2023) Fixed Y: H12(0.3309) H13(0.3896) H14(0.4204) H15(0.3873) H22(0.2341) H23(0.2279) H24(0.2631) H25(0.2992) H32(0.1595) H33(0.1426) H34(0.2089) H35(0.2921) H32A(0.1657) H33A(0.148) H34A(0.2081) H35A(0.286) H42(0.2264) H43(0.2095) H44(0.2322) H45(0.2734) H10A(0.4652) H10B(0.4052) H10C(0.4803) H10D(0.5225) H10E(0.5179) H10F(0.4802) H10G(0.3994) H10H(0.4581) H10I(0.429) H10J(0.3707) H10K(0.3321) H10L(0.3515) H10M(0.3843) H10N(0.3421) H10O(0.418) H10P(0.4672) H10X(0.4906) H10Y(0.4502) H10Q(0.4864) H10R(0.4584) H11A(0.3933) H11B(0.4624) H21X(0.3623) H21Y(0.394) H11C(0.4776) H11D(0.4101) H21C(0.3973) H21D(0.3501) H11E(0.3768) H11F(0.4296) H11X(0.3878) H11Y(0.4467) H51A(0.1296) H51B(0.0689) H51C(0.1301) H61A(0.1779) H61B(0.2264) H61C(0.1649) H71A(0.1765) H71B(0.1619) H71C(0.2249) H81A(0.1303) H81B(0.1308) H81C(0.0696) H91A(0.0626) H91B(0.0918) H91C(0.0315) Fixed Z: H12(0.1684) H13(0.0919) H14(0.1111) H15(0.2066) H22(0.3355) H23(0.2797) H24(0.1715) H25(0.1198) H32(0.4568) H33(0.549) H34(0.5727) H35(0.5042) H32A(0.3764) H33A(0.47) H34A(0.564) H35A(0.5644) H42(0.4712) H43(0.5401) H44(0.5093) H45(0.4047) H10A(0.2075) H10B(0.2392) H10C(0.2233) H10D(0.2744) H10E(0.3496) H10F(0.293) H10G(0.364) H10H(0.3975) H10I(0.5197) H10J(0.4754) H10K(0.5087) H10L(0.5736) H10M(0.6401) H10N(0.5845) H10O(0.6305) H10P(0.5916) H10X(0.5161) H10Y(0.5626) H10Q(0.4987) H10R(0.5623) H11A(0.4744) H11B(0.4558) H21X(0.4825) H21Y(0.4743) H11C(0.3447) H11D(0.3439) H21C(0.3477) H21D(0.3569) H11E(0.2934) H11F(0.25) H11X(0.261) H11Y(0.2718) H51A(0.3415) H51B(0.3597) H51C(0.3951) H61A(0.2483) H61B(0.2091) H61C(0.1748) H71A(0.1218) H71B(0.104) H71C(0.1359) H81A(0.1803) H81B(0.2558) H81C(0.2216) H91A(0.3459) H91B(0.397) H91C(0.3598) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2301(3) 0.29148(13) 0.28513(13) 0.0341(6) Uani 1 1 d . . . C2 C 0.1022(3) 0.27343(13) 0.29555(15) 0.0388(6) Uani 1 1 d . A . C3 C 0.1510(3) 0.25012(13) 0.36239(15) 0.0388(6) Uani 1 1 d . . . C4 C 0.2788(3) 0.26854(13) 0.35323(14) 0.0385(6) Uani 1 1 d . A . C5 C 0.3259(5) 0.1246(2) 0.3009(2) 0.0705(13) Uani 1 1 d . . . C6 C 0.3336(4) 0.1543(2) 0.2409(3) 0.0762(15) Uani 1 1 d . A . C7 C 0.2128(5) 0.15543(16) 0.20341(18) 0.0679(13) Uani 1 1 d . . . C8 C 0.1318(4) 0.12556(17) 0.2418(2) 0.0617(10) Uani 1 1 d . A . C9 C 0.2020(5) 0.10673(16) 0.3007(2) 0.0632(11) Uani 1 1 d . A . C11 C 0.2835(3) 0.32549(13) 0.23449(15) 0.0388(6) Uani 1 1 d . . . C12 C 0.2086(3) 0.34284(15) 0.17635(16) 0.0441(7) Uani 1 1 d . . . H12 H 0.1254 0.3309 0.1684 0.053 Uiso 1 1 calc R . . C13 C 0.2589(4) 0.37786(18) 0.13084(18) 0.0587(9) Uani 1 1 d . . . H13 H 0.2089 0.3896 0.0919 0.070 Uiso 1 1 calc R . . C14 C 0.3817(4) 0.39594(16) 0.14159(19) 0.0578(10) Uani 1 1 d . . . H14 H 0.4154 0.4204 0.1111 0.069 Uiso 1 1 calc R . . C15 C 0.4528(4) 0.37646(18) 0.1992(2) 0.0569(9) Uani 1 1 d . . . H15 H 0.5367 0.3873 0.2066 0.068 Uiso 1 1 calc R . . C21 C -0.0219(3) 0.27150(14) 0.25985(16) 0.0428(7) Uani 1 1 d . . . C22 C -0.1178(3) 0.2476(2) 0.29178(17) 0.0568(9) Uani 1 1 d . A . H22 H -0.1009 0.2341 0.3355 0.068 Uiso 1 1 calc R . . C23 C -0.2368(4) 0.2441(2) 0.2584(2) 0.0662(11) Uani 1 1 d . . . H23 H -0.3002 0.2279 0.2797 0.079 Uiso 1 1 calc R A . C24 C -0.2635(4) 0.2642(2) 0.1941(2) 0.0606(9) Uani 1 1 d . A . H24 H -0.3444 0.2631 0.1715 0.073 Uiso 1 1 calc R . . C25 C -0.1650(4) 0.2864(2) 0.1639(2) 0.0619(10) Uani 1 1 d . . . H25 H -0.1811 0.2992 0.1198 0.074 Uiso 1 1 calc R A . C31 C 0.1060(3) 0.23597(14) 0.42522(15) 0.0420(14) Uani 0.680(5) 1 d PG A 1 C32 C 0.1390(3) 0.18612(13) 0.46627(17) 0.0456(11) Uani 0.680(5) 1 d PG A 1 H32 H 0.2011 0.1595 0.4568 0.055 Uiso 0.680(5) 1 calc PR A 1 C33 C 0.0791(4) 0.17597(14) 0.52154(16) 0.0548(13) Uani 0.680(5) 1 d PG A 1 H33 H 0.1011 0.1426 0.5490 0.066 Uiso 0.680(5) 1 calc PR A 1 C34 C -0.0138(4) 0.21569(17) 0.53576(16) 0.0489(19) Uani 0.680(5) 1 d PG A 1 H34 H -0.0539 0.2089 0.5727 0.059 Uiso 0.680(5) 1 calc PR A 1 C35 C -0.0468(3) 0.26554(13) 0.49470(16) 0.0430(11) Uani 0.680(5) 1 d PG A 1 H35 H -0.1089 0.2921 0.5042 0.052 Uiso 0.680(5) 1 calc PR A 1 N3 N 0.0131(3) 0.27568(11) 0.43943(13) 0.0391(9) Uani 0.680(5) 1 d PG A 1 C31A C 0.0774(2) 0.2364(2) 0.4143(2) 0.025(2) Uani 0.320(5) 1 d PG A 2 C32A C -0.0097(3) 0.1898(3) 0.4141(3) 0.054(3) Uani 0.320(5) 1 d PG A 2 H32A H -0.0297 0.1657 0.3764 0.065 Uiso 0.320(5) 1 calc PR A 2 C33A C -0.0670(3) 0.1792(3) 0.4702(3) 0.063(3) Uani 0.320(5) 1 d PG A 2 H33A H -0.1252 0.1480 0.4700 0.076 Uiso 0.320(5) 1 calc PR A 2 C34A C -0.0371(4) 0.2152(3) 0.5265(3) 0.058(5) Uani 0.320(5) 1 d PG A 2 H34A H -0.0754 0.2081 0.5640 0.069 Uiso 0.320(5) 1 calc PR A 2 C35A C 0.0500(4) 0.2619(3) 0.5267(2) 0.058(3) Uani 0.320(5) 1 d PG A 2 H35A H 0.0700 0.2860 0.5644 0.069 Uiso 0.320(5) 1 calc PR A 2 N3A N 0.1072(3) 0.27249(17) 0.4706(2) 0.049(2) Uani 0.320(5) 1 d PG A 2 C41 C 0.3963(2) 0.26084(13) 0.39573(11) 0.0443(7) Uani 1 1 d G . . C42 C 0.3922(2) 0.23618(13) 0.45748(11) 0.0419(7) Uani 1 1 d G A . H42 H 0.3161 0.2264 0.4712 0.050 Uiso 1 1 calc R . . C43 C 0.5006(4) 0.2262(2) 0.49824(18) 0.0571(9) Uani 1 1 d . . . H43 H 0.4973 0.2095 0.5401 0.068 Uiso 1 1 calc R A . C44 C 0.6144(4) 0.2397(2) 0.48036(19) 0.0630(10) Uani 1 1 d . A . H44 H 0.6873 0.2322 0.5093 0.076 Uiso 1 1 calc R . . C45 C 0.6189(4) 0.2646(2) 0.41819(19) 0.0671(11) Uani 1 1 d . . . H45 H 0.6956 0.2734 0.4047 0.081 Uiso 1 1 calc R A . C101 C 0.0010(5) 0.4481(2) 0.2473(2) 0.0669(11) Uani 1 1 d . . . H10A H -0.0463 0.4652 0.2075 0.080 Uiso 1 1 calc R A . H10B H 0.0154 0.4052 0.2392 0.080 Uiso 1 1 calc R . . C102 C 0.1229(5) 0.48041(18) 0.2623(2) 0.0653(11) Uani 1 1 d . A . H10C H 0.1656 0.4803 0.2233 0.078 Uiso 1 1 calc R . . H10D H 0.1093 0.5225 0.2744 0.078 Uiso 1 1 calc R . . C103 C 0.3142(4) 0.47712(19) 0.3322(2) 0.0636(11) Uani 1 1 d . A . H10E H 0.3051 0.5179 0.3496 0.076 Uiso 1 1 calc R . . H10F H 0.3556 0.4802 0.2930 0.076 Uiso 1 1 calc R . . C104 C 0.3892(4) 0.4386(2) 0.3833(2) 0.0681(11) Uani 1 1 d . A . H10G H 0.4052 0.3994 0.3640 0.082 Uiso 1 1 calc R . . H10H H 0.4689 0.4581 0.3975 0.082 Uiso 1 1 calc R . . C105 C 0.3958(5) 0.3995(3) 0.4922(3) 0.0775(13) Uani 1 1 d . A . H10I H 0.4460 0.4290 0.5197 0.093 Uiso 1 1 calc R . . H10J H 0.4517 0.3707 0.4754 0.093 Uiso 1 1 calc R . . C106 C 0.3139(5) 0.3666(3) 0.5332(3) 0.0866(15) Uani 1 1 d . . . H10K H 0.2748 0.3321 0.5087 0.104 Uiso 1 1 calc R A . H10L H 0.3628 0.3515 0.5736 0.104 Uiso 1 1 calc R . . C107 C 0.1494(6) 0.3838(3) 0.5958(3) 0.0900(16) Uani 1 1 d . . . H10M H 0.1962 0.3843 0.6401 0.108 Uiso 1 1 calc R A . H10N H 0.1245 0.3421 0.5845 0.108 Uiso 1 1 calc R . . C108 C 0.0365(6) 0.4247(3) 0.5922(2) 0.0904(17) Uani 1 1 d . A . H10O H -0.0063 0.4180 0.6305 0.108 Uiso 1 1 calc R . . H10P H 0.0613 0.4672 0.5916 0.108 Uiso 1 1 calc R . . C109 C -0.1445(5) 0.4495(3) 0.5232(3) 0.0902(16) Uani 1 1 d D . . H10X H -0.1154 0.4906 0.5161 0.108 Uiso 0.78 1 calc PR B 1 H10Y H -0.1858 0.4502 0.5626 0.108 Uiso 0.78 1 calc PR B 1 H10Q H -0.1305 0.4864 0.4987 0.108 Uiso 0.22 1 d PR B 2 H10R H -0.1837 0.4584 0.5623 0.108 Uiso 0.22 1 d PR B 2 C110 C -0.2365(5) 0.4312(3) 0.4648(3) 0.0725(16) Uani 0.78 1 d PDU A 1 H11A H -0.2766 0.3933 0.4744 0.087 Uiso 0.78 1 calc PR A 1 H11B H -0.3004 0.4624 0.4558 0.087 Uiso 0.78 1 calc PR A 1 C210 C -0.196(2) 0.4006(7) 0.4730(5) 0.106(7) Uani 0.22 1 d PDU A 2 H21X H -0.1518 0.3623 0.4825 0.127 Uiso 0.22 1 calc PR A 2 H21Y H -0.2839 0.3940 0.4743 0.127 Uiso 0.22 1 calc PR A 2 C111 C -0.2520(5) 0.4351(3) 0.3476(3) 0.0722(15) Uani 0.78 1 d PDU A 1 H11C H -0.2771 0.4776 0.3447 0.087 Uiso 0.78 1 calc PR A 1 H11D H -0.3265 0.4101 0.3439 0.087 Uiso 0.78 1 calc PR A 1 C211 C -0.228(3) 0.3932(12) 0.3530(5) 0.097(7) Uani 0.22 1 d PDU A 2 H21C H -0.3183 0.3973 0.3477 0.117 Uiso 0.22 1 calc PR A 2 H21D H -0.2078 0.3501 0.3569 0.117 Uiso 0.22 1 calc PR A 2 C112 C -0.1784(4) 0.4201(3) 0.2926(3) 0.0787(13) Uani 1 1 d D . . H11E H -0.1594 0.3768 0.2934 0.094 Uiso 0.78 1 calc PR A 1 H11F H -0.2270 0.4296 0.2500 0.094 Uiso 0.78 1 calc PR A 1 H11X H -0.1689 0.3878 0.2610 0.094 Uiso 0.22 1 d PR A 2 H11Y H -0.2441 0.4467 0.2718 0.094 Uiso 0.22 1 d PR A 2 N1 N 0.4061(3) 0.34204(14) 0.24583(15) 0.0535(7) Uani 1 1 d . . . N2 N -0.0465(3) 0.29015(16) 0.19570(19) 0.0610(8) Uani 1 1 d . A . N42 N 0.5100(4) 0.27648(19) 0.37606(17) 0.0675(9) Uani 1 1 d . A . Fe1 Fe 0.21362(4) 0.200384(19) 0.29104(2) 0.03347(15) Uani 1 1 d . A . K1 K 0.07813(8) 0.39197(4) 0.40814(4) 0.0574(2) Uani 1 1 d . A . O1 O -0.0670(3) 0.45395(16) 0.30062(16) 0.0747(9) Uani 1 1 d . A . O2 O 0.1970(3) 0.44995(11) 0.31590(14) 0.0591(7) Uani 1 1 d . . . O3 O 0.3263(3) 0.42949(17) 0.43902(16) 0.0748(8) Uani 1 1 d . . . O4 O 0.2217(4) 0.40747(16) 0.54927(17) 0.0845(10) Uani 1 1 d . A . O5 O -0.0409(4) 0.41008(14) 0.53421(17) 0.0763(9) Uani 1 1 d . A . O6 O -0.1753(3) 0.42378(18) 0.40966(19) 0.0798(9) Uani 1 1 d D . . C51 C 0.4328(8) 0.1122(3) 0.3540(4) 0.162(5) Uani 1 1 d . A . H51A H 0.5076 0.1296 0.3415 0.243 Uiso 1 1 calc R . . H51B H 0.4434 0.0689 0.3597 0.243 Uiso 1 1 calc R . . H51C H 0.4164 0.1301 0.3951 0.243 Uiso 1 1 calc R . . C61 C 0.4451(7) 0.1836(3) 0.2160(5) 0.165(5) Uani 1 1 d . . . H61A H 0.5178 0.1779 0.2483 0.247 Uiso 1 1 calc R A . H61B H 0.4298 0.2264 0.2091 0.247 Uiso 1 1 calc R . . H61C H 0.4583 0.1649 0.1748 0.247 Uiso 1 1 calc R . . C71 C 0.1760(10) 0.1821(3) 0.1351(2) 0.140(4) Uani 1 1 d . A . H71A H 0.0881 0.1765 0.1218 0.210 Uiso 1 1 calc R . . H71B H 0.2213 0.1619 0.1040 0.210 Uiso 1 1 calc R . . H71C H 0.1952 0.2249 0.1359 0.210 Uiso 1 1 calc R . . C81 C -0.0066(6) 0.1129(3) 0.2232(4) 0.121(3) Uani 1 1 d . . . H81A H -0.0350 0.1303 0.1803 0.181 Uiso 1 1 calc R A . H81B H -0.0518 0.1308 0.2558 0.181 Uiso 1 1 calc R . . H81C H -0.0205 0.0696 0.2216 0.181 Uiso 1 1 calc R . . C91 C 0.1590(10) 0.0698(2) 0.3559(3) 0.133(3) Uani 1 1 d . . . H91A H 0.0708 0.0626 0.3459 0.199 Uiso 1 1 calc R A . H91B H 0.1763 0.0918 0.3970 0.199 Uiso 1 1 calc R . . H91C H 0.2023 0.0315 0.3598 0.199 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 C1 0.0427(15) 0.0317(13) 0.0284(13) -0.0021(10) 0.0068(11) -0.0044(11) C2 0.0494(17) 0.0294(13) 0.0408(15) 0.0002(11) 0.0170(13) 0.0017(11) C3 0.0507(17) 0.0312(13) 0.0364(14) -0.0023(11) 0.0132(12) -0.0002(11) C4 0.0509(17) 0.0355(14) 0.0304(13) -0.0061(11) 0.0102(12) -0.0034(12) C5 0.076(3) 0.051(2) 0.077(3) -0.028(2) -0.015(2) 0.030(2) C6 0.073(3) 0.051(2) 0.115(4) -0.043(2) 0.051(3) -0.0122(19) C7 0.132(4) 0.0342(17) 0.0381(17) -0.0092(13) 0.014(2) 0.006(2) C8 0.055(2) 0.0390(17) 0.087(3) -0.0293(18) -0.0022(19) -0.0008(15) C9 0.114(4) 0.0288(16) 0.052(2) -0.0039(14) 0.033(2) 0.0064(17) C11 0.0528(17) 0.0296(13) 0.0369(14) -0.0053(11) 0.0165(12) 0.0001(12) C12 0.0538(18) 0.0419(16) 0.0383(15) 0.0046(12) 0.0126(13) 0.0001(13) C13 0.085(3) 0.053(2) 0.0413(17) 0.0080(15) 0.0189(17) 0.0098(19) C14 0.085(3) 0.0438(18) 0.053(2) -0.0018(15) 0.0396(19) -0.0055(17) C15 0.061(2) 0.055(2) 0.062(2) -0.0065(17) 0.0300(18) -0.0143(16) C21 0.0481(17) 0.0379(15) 0.0443(16) -0.0070(12) 0.0133(13) 0.0025(12) C22 0.0474(19) 0.088(3) 0.0351(16) -0.0080(16) 0.0070(14) -0.0160(18) C23 0.049(2) 0.101(3) 0.049(2) -0.010(2) 0.0071(16) -0.015(2) C24 0.051(2) 0.080(3) 0.050(2) -0.0096(18) 0.0038(16) -0.0018(18) C25 0.061(2) 0.063(2) 0.063(2) 0.0114(19) 0.0137(19) 0.0113(18) C31 0.053(3) 0.036(3) 0.035(2) -0.004(2) -0.002(2) -0.005(2) C32 0.056(3) 0.041(2) 0.041(2) 0.0061(19) 0.009(2) 0.002(2) C33 0.066(3) 0.051(3) 0.049(3) 0.012(2) 0.012(2) 0.001(2) C34 0.056(3) 0.057(5) 0.036(3) 0.004(3) 0.014(3) -0.008(3) C35 0.047(3) 0.042(2) 0.041(2) -0.0068(19) 0.013(2) -0.0057(19) N3 0.049(2) 0.0338(18) 0.0367(19) -0.0052(14) 0.0132(17) -0.0043(15) C31A 0.017(4) 0.030(5) 0.030(5) 0.004(4) 0.004(3) 0.005(3) C32A 0.061(7) 0.049(6) 0.054(6) -0.005(5) 0.014(5) -0.004(5) C33A 0.071(8) 0.053(7) 0.072(8) 0.007(6) 0.031(6) -0.002(6) C34A 0.074(10) 0.053(11) 0.054(8) 0.010(8) 0.033(8) 0.010(7) C35A 0.087(9) 0.049(6) 0.042(6) 0.009(5) 0.029(6) 0.018(6) N3A 0.078(7) 0.044(5) 0.025(4) -0.004(3) 0.013(4) -0.001(4) C41 0.0578(19) 0.0426(16) 0.0331(14) -0.0102(12) 0.0083(13) -0.0001(13) C42 0.0373(15) 0.0574(18) 0.0306(13) -0.0031(12) 0.0036(11) 0.0064(13) C43 0.057(2) 0.077(3) 0.0361(16) -0.0032(16) 0.0026(14) 0.0122(18) C44 0.054(2) 0.091(3) 0.0433(18) -0.0111(19) 0.0043(16) 0.004(2) C45 0.066(3) 0.092(3) 0.0428(19) -0.0115(19) 0.0049(17) -0.007(2) C101 0.086(3) 0.059(2) 0.056(2) -0.0001(18) 0.012(2) 0.006(2) C102 0.100(3) 0.0461(19) 0.054(2) 0.0054(16) 0.025(2) 0.002(2) C103 0.066(2) 0.056(2) 0.077(3) -0.0146(19) 0.039(2) -0.0157(18) C104 0.051(2) 0.075(3) 0.083(3) -0.020(2) 0.028(2) -0.0069(19) C105 0.069(3) 0.089(3) 0.071(3) -0.021(2) 0.000(2) 0.016(2) C106 0.088(4) 0.085(3) 0.084(3) -0.001(3) 0.002(3) 0.022(3) C107 0.114(4) 0.086(4) 0.072(3) 0.014(3) 0.022(3) 0.008(3) C108 0.150(5) 0.075(3) 0.054(2) -0.001(2) 0.044(3) 0.016(3) C109 0.106(4) 0.088(4) 0.083(3) -0.026(3) 0.039(3) 0.008(3) C110 0.054(3) 0.072(4) 0.098(4) 0.004(3) 0.033(3) 0.014(3) C210 0.099(14) 0.111(15) 0.113(15) 0.012(13) 0.033(12) 0.066(12) C111 0.059(3) 0.081(4) 0.075(4) -0.022(3) 0.004(3) -0.001(3) C211 0.087(13) 0.099(14) 0.115(14) -0.037(13) 0.042(11) -0.049(12) C112 0.062(3) 0.088(3) 0.084(3) -0.023(3) 0.001(2) -0.003(2) N1 0.0590(18) 0.0527(16) 0.0525(16) -0.0014(13) 0.0210(14) -0.0108(13) N2 0.0552(19) 0.0597(19) 0.070(2) 0.0201(16) 0.0163(16) 0.0072(14) N42 0.078(2) 0.077(2) 0.0474(17) -0.0106(16) 0.0083(16) -0.0117(19) Fe1 0.0423(3) 0.0283(2) 0.0305(2) -0.00320(15) 0.00733(18) 0.00046(16) K1 0.0605(5) 0.0491(4) 0.0669(5) 0.0151(3) 0.0236(4) -0.0057(3) O1 0.0717(19) 0.087(2) 0.0665(18) -0.0265(16) 0.0139(14) -0.0030(16) O2 0.0738(17) 0.0438(13) 0.0654(16) 0.0041(11) 0.0298(13) -0.0069(11) O3 0.0610(17) 0.098(2) 0.0689(18) -0.0010(17) 0.0203(14) 0.0105(16) O4 0.127(3) 0.0679(19) 0.0650(18) 0.0053(15) 0.0363(19) 0.0143(19) O5 0.103(2) 0.0555(16) 0.074(2) -0.0090(14) 0.0274(18) 0.0008(16) O6 0.0577(17) 0.096(2) 0.089(2) -0.0136(19) 0.0201(16) 0.0001(16) C51 0.175(8) 0.114(5) 0.164(7) -0.076(5) -0.096(6) 0.102(6) C61 0.131(6) 0.112(5) 0.286(12) -0.121(7) 0.152(7) -0.057(4) C71 0.314(12) 0.065(3) 0.040(2) -0.009(2) 0.024(4) 0.028(5) C81 0.074(3) 0.093(4) 0.188(8) -0.078(5) -0.011(4) -0.008(3) C91 0.274(10) 0.038(2) 0.108(5) 0.002(3) 0.102(6) -0.007(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C2 1.483(4) . ? C1 C4 1.496(4) . ? C1 C11 1.453(4) . ? C1 Fe1 2.009(3) . ? C2 C3 1.477(4) . ? C2 C21 1.434(5) . ? C2 Fe1 2.014(3) . ? C2 K1 3.493(3) . ? C3 C4 1.477(4) . ? C3 C31 1.460(4) . ? C3 C31A 1.438(4) . ? C3 Fe1 2.005(3) . ? C3 K1 3.369(3) . ? C4 C41 1.444(4) . ? C4 Fe1 2.018(3) . ? C5 C6 1.395(8) . ? C5 C9 1.396(7) . ? C5 Fe1 2.051(4) . ? C5 C51 1.493(7) . ? C6 C7 1.418(7) . ? C6 Fe1 2.028(4) . ? C6 C61 1.514(7) . ? C7 C8 1.413(7) . ? C7 Fe1 2.032(3) . ? C7 C71 1.506(6) . ? C8 C9 1.386(6) . ? C8 Fe1 2.055(3) . ? C8 C81 1.518(7) . ? C9 Fe1 2.067(4) . ? C9 C91 1.508(6) . ? C11 C12 1.388(5) . ? C11 N1 1.364(4) . ? C12 C13 1.371(5) . ? C13 C14 1.375(6) . ? C14 C15 1.374(6) . ? C15 N1 1.362(5) . ? C21 C22 1.401(5) . ? C21 N2 1.355(5) . ? C22 C23 1.371(5) . ? C23 C24 1.371(6) . ? C24 C25 1.390(6) . ? C25 N2 1.355(6) . ? C31 C32 1.3900 . ? C31 N3 1.3900 . ? C31 K1 3.445(3) . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 N3 1.3900 . ? N3 K1 2.741(3) . ? C31A C32A 1.3900 . ? C31A N3A 1.3900 . ? C31A K1 3.410(5) . ? C32A C33A 1.3900 . ? C33A C34A 1.3900 . ? C34A C35A 1.3900 . ? C35A N3A 1.3900 . ? N3A K1 2.907(4) . ? C41 C42 1.3717 . ? C41 N42 1.389(4) . ? C42 C43 1.356(4) . ? C43 C44 1.364(6) . ? C44 C45 1.382(6) . ? C45 N42 1.381(6) . ? C101 C102 1.491(7) . ? C101 K1 3.479(4) . ? C101 O1 1.397(5) . ? C102 O2 1.424(5) . ? C103 C104 1.487(7) . ? C103 O2 1.399(5) . ? C104 O3 1.413(5) . ? C105 C106 1.485(8) . ? C105 O3 1.391(6) . ? C106 K1 3.385(6) . ? C106 O4 1.411(6) . ? C107 C108 1.508(8) . ? C107 O4 1.407(7) . ? C108 O5 1.384(7) . ? C109 C110 1.493(7) . ? C109 C210 1.528(10) . ? C109 O5 1.408(7) . ? C110 O6 1.388(7) . ? C210 O6 1.428(10) . ? C111 C112 1.495(6) . ? C111 O6 1.431(7) . ? C211 C112 1.524(10) . ? C211 K1 3.35(3) . ? C211 O6 1.385(9) . ? C112 K1 3.430(5) . ? C112 O1 1.406(6) . ? K1 O1 2.849(4) . ? K1 O2 2.729(3) . ? K1 O3 2.795(3) . ? K1 O4 3.082(4) . ? K1 O5 3.048(3) . ? K1 O6 2.834(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C4 89.6(2) . . ? C2 C1 Fe1 68.54(15) . . ? C4 C1 Fe1 68.51(16) . . ? C11 C1 C2 135.1(3) . . ? C11 C1 C4 134.6(3) . . ? C11 C1 Fe1 126.8(2) . . ? C1 C2 Fe1 68.19(16) . . ? C1 C2 K1 92.94(17) . . ? C3 C2 C1 90.1(2) . . ? C3 C2 Fe1 68.12(16) . . ? C3 C2 K1 72.89(15) . . ? C21 C2 C1 139.7(3) . . ? C21 C2 C3 130.1(3) . . ? C21 C2 Fe1 118.6(2) . . ? C21 C2 K1 101.68(18) . . ? Fe1 C2 K1 136.09(14) . . ? C2 C3 C4 90.6(2) . . ? C2 C3 Fe1 68.76(16) . . ? C2 C3 K1 82.35(16) . . ? C4 C3 Fe1 68.93(16) . . ? C4 C3 K1 92.40(17) . . ? C31 C3 C2 139.1(3) . . ? C31 C3 C4 126.9(3) . . ? C31 C3 Fe1 134.7(2) . . ? C31 C3 K1 80.55(16) . . ? C31A C3 C2 125.5(3) . . ? C31A C3 C4 140.6(3) . . ? C31A C3 C31 14.06(19) . . ? C31A C3 Fe1 133.9(3) . . ? C31A C3 K1 79.4(2) . . ? Fe1 C3 K1 144.73(13) . . ? C1 C4 Fe1 67.87(15) . . ? C3 C4 C1 89.6(2) . . ? C3 C4 Fe1 67.99(16) . . ? C41 C4 C1 139.3(3) . . ? C41 C4 C3 130.9(3) . . ? C41 C4 Fe1 119.3(2) . . ? C6 C5 C9 107.6(4) . . ? C6 C5 Fe1 69.1(2) . . ? C6 C5 C51 125.6(7) . . ? C9 C5 Fe1 70.8(2) . . ? C9 C5 C51 126.8(7) . . ? C51 C5 Fe1 127.3(3) . . ? C5 C6 C7 108.3(4) . . ? C5 C6 Fe1 70.9(2) . . ? C5 C6 C61 129.5(7) . . ? C7 C6 Fe1 69.7(2) . . ? C7 C6 C61 122.1(7) . . ? C61 C6 Fe1 123.5(3) . . ? C6 C7 Fe1 69.4(2) . . ? C6 C7 C71 127.3(6) . . ? C8 C7 C6 107.0(4) . . ? C8 C7 Fe1 70.6(2) . . ? C8 C7 C71 125.7(6) . . ? C71 C7 Fe1 125.9(3) . . ? C7 C8 Fe1 68.9(2) . . ? C7 C8 C81 127.9(5) . . ? C9 C8 C7 107.8(4) . . ? C9 C8 Fe1 70.8(2) . . ? C9 C8 C81 124.3(5) . . ? C81 C8 Fe1 127.6(3) . . ? C5 C9 Fe1 69.6(2) . . ? C5 C9 C91 123.0(6) . . ? C8 C9 C5 109.3(4) . . ? C8 C9 Fe1 69.9(2) . . ? C8 C9 C91 127.7(6) . . ? C91 C9 Fe1 129.2(3) . . ? C12 C11 C1 120.0(3) . . ? N1 C11 C1 119.4(3) . . ? N1 C11 C12 120.6(3) . . ? C13 C12 C11 119.1(3) . . ? C12 C13 C14 121.4(4) . . ? C15 C14 C13 117.3(3) . . ? N1 C15 C14 123.1(4) . . ? C22 C21 C2 118.6(3) . . ? N2 C21 C2 121.4(3) . . ? N2 C21 C22 119.9(3) . . ? C23 C22 C21 119.9(4) . . ? C24 C23 C22 120.7(4) . . ? C23 C24 C25 117.4(4) . . ? N2 C25 C24 123.0(4) . . ? C3 C31 K1 74.73(16) . . ? C32 C31 C3 127.0(2) . . ? C32 C31 N3 120.0 . . ? C32 C31 K1 148.40(14) . . ? N3 C31 C3 112.8(2) . . ? N3 C31 K1 49.00(11) . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C33 C34 C35 120.0 . . ? N3 C35 C34 120.0 . . ? C31 N3 K1 108.50(14) . . ? C35 N3 C31 120.0 . . ? C35 N3 K1 119.96(15) . . ? C3 C31A K1 76.2(2) . . ? C32A C31A C3 126.6(2) . . ? C32A C31A N3A 120.0 . . ? C32A C31A K1 137.71(9) . . ? N3A C31A C3 113.3(2) . . ? N3A C31A K1 57.38(17) . . ? C31A C32A C33A 120.0 . . ? C34A C33A C32A 120.0 . . ? C35A C34A C33A 120.0 . . ? C34A C35A N3A 120.0 . . ? C31A N3A K1 98.9(2) . . ? C35A N3A C31A 120.0 . . ? C35A N3A K1 118.33(14) . . ? C42 C41 C4 116.99(16) . . ? C42 C41 N42 120.2(2) . . ? N42 C41 C4 122.8(3) . . ? C43 C42 C41 119.0(2) . . ? C42 C43 C44 122.7(4) . . ? C43 C44 C45 118.5(4) . . ? N42 C45 C44 120.3(4) . . ? C102 C101 K1 83.5(2) . . ? O1 C101 C102 110.2(4) . . ? O1 C101 K1 52.3(2) . . ? O2 C102 C101 108.7(3) . . ? O2 C103 C104 108.2(3) . . ? O3 C104 C103 111.2(3) . . ? O3 C105 C106 111.4(4) . . ? C105 C106 K1 86.9(3) . . ? O4 C106 C105 108.5(5) . . ? O4 C106 K1 65.6(3) . . ? O4 C107 C108 105.8(4) . . ? O5 C108 C107 107.1(4) . . ? C110 C109 C210 31.0(8) . . ? O5 C109 C110 112.9(4) . . ? O5 C109 C210 83.2(10) . . ? O6 C110 C109 109.3(4) . . ? O6 C210 C109 105.3(8) . . ? O6 C111 C112 108.4(4) . . ? C112 C211 K1 80.0(10) . . ? O6 C211 C112 109.2(8) . . ? O6 C211 K1 56.6(11) . . ? C111 C112 C211 36.9(12) . . ? C111 C112 K1 89.7(3) . . ? C211 C112 K1 74.0(11) . . ? O1 C112 C111 109.6(4) . . ? O1 C112 C211 120.4(7) . . ? O1 C112 K1 54.3(2) . . ? C15 N1 C11 118.5(3) . . ? C25 N2 C21 119.1(3) . . ? C45 N42 C41 119.3(3) . . ? C1 Fe1 C2 43.27(12) . . ? C1 Fe1 C4 43.62(11) . . ? C1 Fe1 C5 138.95(18) . . ? C1 Fe1 C6 113.36(16) . . ? C1 Fe1 C7 114.76(14) . . ? C1 Fe1 C8 143.06(16) . . ? C1 Fe1 C9 177.62(16) . . ? C2 Fe1 C4 62.78(13) . . ? C2 Fe1 C5 171.68(17) . . ? C2 Fe1 C6 148.0(2) . . ? C2 Fe1 C7 119.71(16) . . ? C2 Fe1 C8 115.83(15) . . ? C2 Fe1 C9 137.73(16) . . ? C3 Fe1 C1 62.93(12) . . ? C3 Fe1 C2 43.12(12) . . ? C3 Fe1 C4 43.08(12) . . ? C3 Fe1 C5 128.68(17) . . ? C3 Fe1 C6 159.79(19) . . ? C3 Fe1 C7 159.27(19) . . ? C3 Fe1 C8 128.21(16) . . ? C3 Fe1 C9 116.11(14) . . ? C4 Fe1 C5 112.81(15) . . ? C4 Fe1 C6 119.38(16) . . ? C4 Fe1 C7 149.85(17) . . ? C4 Fe1 C8 169.63(16) . . ? C4 Fe1 C9 134.11(15) . . ? C5 Fe1 C8 67.09(17) . . ? C5 Fe1 C9 39.6(2) . . ? C6 Fe1 C5 40.0(2) . . ? C6 Fe1 C7 40.9(2) . . ? C6 Fe1 C8 67.74(17) . . ? C6 Fe1 C9 66.71(18) . . ? C7 Fe1 C5 67.86(18) . . ? C7 Fe1 C8 40.44(19) . . ? C7 Fe1 C9 66.97(15) . . ? C8 Fe1 C9 39.31(18) . . ? C3 K1 C31A 24.49(8) . . ? C3 K1 C106 82.79(11) . . ? N3 K1 C3 44.26(8) . . ? N3 K1 C31A 20.07(8) . . ? N3 K1 N3A 22.71(9) . . ? N3 K1 C106 82.22(13) . . ? N3 K1 C211 79.1(4) . . ? N3 K1 O1 119.26(10) . . ? N3 K1 O3 119.41(10) . . ? N3 K1 O4 89.96(9) . . ? N3 K1 O5 76.95(8) . . ? N3 K1 O6 86.90(10) . . ? N3A K1 C3 43.45(9) . . ? N3A K1 C31A 23.8 . . ? N3A K1 C106 60.04(14) . . ? N3A K1 C211 101.2(4) . . ? N3A K1 O4 71.56(11) . . ? N3A K1 O5 77.51(9) . . ? C106 K1 C31A 79.29(12) . . ? C211 K1 C3 100.0(5) . . ? C211 K1 C31A 90.7(5) . . ? C211 K1 C106 149.3(2) . . ? O1 K1 C3 110.72(9) . . ? O1 K1 C31A 120.03(9) . . ? O1 K1 N3A 141.08(11) . . ? O1 K1 C106 158.44(13) . . ? O1 K1 C211 47.6(3) . . ? O1 K1 O4 144.32(9) . . ? O1 K1 O5 109.19(10) . . ? O2 K1 C3 95.13(8) . . ? O2 K1 N3 138.80(8) . . ? O2 K1 C31A 119.61(9) . . ? O2 K1 N3A 133.30(8) . . ? O2 K1 C106 102.29(13) . . ? O2 K1 C211 107.8(2) . . ? O2 K1 O1 60.97(9) . . ? O2 K1 O3 59.12(10) . . ? O2 K1 O4 111.21(10) . . ? O2 K1 O5 144.16(9) . . ? O2 K1 O6 116.27(11) . . ? O3 K1 C3 94.51(9) . . ? O3 K1 C31A 107.03(9) . . ? O3 K1 N3A 97.17(10) . . ? O3 K1 C106 43.93(13) . . ? O3 K1 C211 161.5(4) . . ? O3 K1 O1 116.19(10) . . ? O3 K1 O4 54.20(10) . . ? O3 K1 O5 106.20(10) . . ? O3 K1 O6 145.72(11) . . ? O4 K1 C3 104.53(9) . . ? O4 K1 C31A 94.56(9) . . ? O4 K1 C106 24.64(11) . . ? O4 K1 C211 131.1(2) . . ? O5 K1 C3 119.62(8) . . ? O5 K1 C31A 95.50(9) . . ? O5 K1 C106 75.77(12) . . ? O5 K1 C211 76.4(2) . . ? O5 K1 O4 54.72(10) . . ? O6 K1 C3 119.60(10) . . ? O6 K1 C31A 103.77(9) . . ? O6 K1 N3A 105.23(10) . . ? O6 K1 C106 131.41(13) . . ? O6 K1 C211 24.1(3) . . ? O6 K1 O1 57.34(10) . . ? O6 K1 O4 109.02(11) . . ? O6 K1 O5 55.64(11) . . ? C101 O1 C112 113.5(3) . . ? C101 O1 K1 104.8(3) . . ? C112 O1 K1 102.1(3) . . ? C102 O2 K1 118.3(2) . . ? C103 O2 C102 112.1(3) . . ? C103 O2 K1 122.3(2) . . ? C104 O3 K1 114.6(3) . . ? C105 O3 C104 114.8(4) . . ? C105 O3 K1 115.7(3) . . ? C106 O4 K1 89.8(3) . . ? C107 O4 C106 113.5(4) . . ? C107 O4 K1 109.1(4) . . ? C108 O5 C109 111.6(4) . . ? C108 O5 K1 117.9(3) . . ? C109 O5 K1 111.5(3) . . ? C110 O6 C210 33.3(9) . . ? C110 O6 C111 114.0(4) . . ? C110 O6 K1 127.6(3) . . ? C210 O6 C111 135.4(10) . . ? C210 O6 K1 101.2(11) . . ? C111 O6 K1 118.4(3) . . ? C211 O6 C110 122.6(9) . . ? C211 O6 C210 118.6(8) . . ? C211 O6 C111 39.7(13) . . ? C211 O6 K1 99.3(14) . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -4 -12 0 0.1557 -3.9994 -11.9984 0.0079 -0.5466 -0.6117 -0.6083 -6 1 7 0.1473 -5.9980 1.0059 7.0001 -0.6489 0.4589 -0.5256 1 3 12 0.1938 1.0022 3.0079 12.0002 -0.5952 0.4747 0.6077 -3 9 -8 0.1810 -3.0014 8.9944 -8.0079 0.6444 0.4529 -0.6453 6 0 5 0.1989 6.0004 0.0023 5.0014 -0.0514 -0.0745 0.9876 7 -1 -1 0.1503 6.9991 -1.0019 -0.9989 0.3252 -0.3328 0.8864 0 -14 0 0.1722 0.0002 -13.9991 0.0096 -0.4406 -0.8759 -0.0892 3 -8 9 0.1713 3.0016 -7.9938 9.0074 -0.6739 -0.3635 0.6897 -4 -8 -6 0.1764 -4.0006 -8.0028 -5.9959 -0.0548 -0.5224 -0.8106 -6 4 -2 0.1539 -5.9998 3.9995 -2.0036 -0.0056 0.4053 -0.8482 5 9 -5 0.2029 4.9984 8.9950 -5.0067 0.7994 0.2552 0.5323 -5 -9 6 0.1517 -4.9982 -8.9943 6.0069 -0.8604 -0.2284 -0.4943 3 -10 7 0.1600 3.0012 -9.9951 7.0084 -0.6148 -0.5423 0.6010 3 -4 -12 0.2017 2.9974 -4.0085 -11.9992 0.7327 -0.6764 -0.0822 -2 -1 -12 0.1948 -2.0021 -1.0078 -12.0017 0.6159 -0.3148 -0.7279 5 -10 0 0.1836 4.9996 -10.0003 0.0073 -0.1034 -0.7995 0.6011 -1 -13 -5 0.1504 -1.0007 -13.0024 -4.9921 -0.1464 -0.9127 -0.4056 5 6 6 0.1876 5.0006 6.0028 5.9974 0.0341 0.3625 0.9308 0 13 5 0.1856 0.0008 13.0026 4.9920 0.1042 0.9475 0.2726 _database_code_depnum_ccdc_archive 'CCDC 962751' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cpd_1 _audit_creation_date 2013-09-26 _audit_creation_method ; Olex2 1.2 (compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C34 H31 Fe N4' _chemical_formula_sum 'C34 H31 Fe N4' _chemical_formula_weight 551.49 _chemical_melting_point ? _chemical_oxdiff_formula C34H35FeN4Cu2 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0180 0.0090 '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' N N 0.0310 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1340 3.1970 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.6884(2) _cell_length_b 14.1246(2) _cell_length_c 15.0838(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.276(1) _cell_angle_gamma 90.00 _cell_volume 2679(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9578 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 73.6100 _cell_measurement_theta_min 3.6780 _exptl_absorpt_coefficient_mu 4.743 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.63391 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear reddish brown' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier reddish _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1156 _exptl_crystal_size_max 0.335 _exptl_crystal_size_mid 0.174 _exptl_crystal_size_min 0.102 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_unetI/netI 0.0215 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 14409 _diffrn_reflns_theta_full 73.68 _diffrn_reflns_theta_max 73.68 _diffrn_reflns_theta_min 3.70 _diffrn_ambient_temperature 123(2) _diffrn_detector_area_resol_mean 10.3546 _diffrn_measured_fraction_theta_full 0.9934 _diffrn_measured_fraction_theta_max 0.9602 _diffrn_measurement_device_type 'SuperNova, Single source at offset, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.1122087000 _diffrn_orient_matrix_UB_12 -0.0435972000 _diffrn_orient_matrix_UB_13 -0.0441714000 _diffrn_orient_matrix_UB_21 -0.0237251000 _diffrn_orient_matrix_UB_22 0.0570287000 _diffrn_orient_matrix_UB_23 -0.0933224000 _diffrn_orient_matrix_UB_31 0.0431200000 _diffrn_orient_matrix_UB_32 -0.0820420000 _diffrn_orient_matrix_UB_33 -0.0413798000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4952 _reflns_number_total 5200 _reflns_odcompleteness_completeness 99.34 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2\s(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.385 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.052 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 352 _refine_ls_number_reflns 5200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0341 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+1.2877P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0959 _refine_ls_wR_factor_ref 0.0976 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _olex2_refinement_description ; 1. Others Fixed Uiso: H6A(0.045) H6B(0.045) H6C(0.045) H7A(0.051) H7B(0.051) H7C(0.051) H8A(0.069) H8B(0.069) H8C(0.069) H9A(0.078) H9B(0.078) H9C(0.078) H10A(0.059) H10B(0.059) H10C(0.059) H115(0.034) H114(0.033) H113(0.031) H125(0.034) H124(0.039) H123(0.038) H135(0.039) H134(0.047) H133(0.045) H145(0.035) H144(0.04) H143(0.038) H112(0.027) H122(0.03) H132(0.033) H142(0.031) Fixed X: H6A(0.0611) H6B(0.1833) H6C(0.1289) H7A(-0.0565) H7B(-0.024) H7C(- 0.0718) H8A(0.1361) H8B(0.0687) H8C(0.0223) H9A(0.2848) H9B(0.3186) H9C(0.3783) H10A(0.3899) H10B(0.3139) H10C(0.3674) H115(0.5825) H114(0.715) H113(0.6883) H125(0.4481) H124(0.3815) H123(0.2725) H135(-0.0582) H134(- 0.1483) H133(-0.0749) H145(0.0747) H144(0.2132) H143(0.3858) H112(0.5262) H122(0.2335) H132(0.0871) H142(0.4124) Fixed Y: H6A(0.0622) H6B(0.0423) H6C(0.0423) H7A(0.3013) H7B(0.2043) H7C(0.2071) H8A(0.4811) H8B(0.4453) H8C(0.4388) H9A(0.4482) H9B(0.3746) H9C(0.3776) H10A(0.2038) H10B(0.1201) H10C(0.1229) H115(0.4561) H114(0.345) H113(0.1952) H125(-0.0713) H124(-0.1693) H123(-0.1053) H135(0.0564) H134(0.155) H133(0.3013) H145(0.5817) H144(0.6828) H143(0.6224) H112(0.1602) H122(0.0555) H132(0.3449) H142(0.4635) Fixed Z: H6A(0.3342) H6B(0.3863) H6C(0.2733) H7A(0.3307) H7B(0.3849) H7C(0.2718) H8A(0.319) H8B(0.3756) H8C(0.2626) H9A(0.3145) H9B(0.2542) H9C(0.3668) H10A(0.3204) H10B(0.2679) H10C(0.3809) H115(0.5225) H114(0.5558) H113(0.607) H125(0.5325) H124(0.6163) H123(0.6871) H135(0.5293) H134(0.5915) H133(0.6526) H145(0.5468) H144(0.627) H143(0.6921) H112(0.6155) H122(0.669) H132(0.6469) H142(0.6687) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.15134(13) 0.17468(12) 0.33003(11) 0.0196(3) Uani 1 1 d . . . C2 C 0.08213(14) 0.25000(12) 0.33104(13) 0.0220(4) Uani 1 1 d . . . C3 C 0.13336(16) 0.33733(13) 0.32740(12) 0.0277(4) Uani 1 1 d . . . C4 C 0.23328(15) 0.31523(14) 0.32328(12) 0.0289(4) Uani 1 1 d . . . C5 C 0.24449(14) 0.21522(14) 0.32550(12) 0.0239(4) Uani 1 1 d . . . C6 C 0.12917(16) 0.07108(13) 0.33106(14) 0.0302(4) Uani 1 1 d . . . H6A H 0.0611 0.0622 0.3342 0.045 Uiso 1 1 calc R . . H6B H 0.1833 0.0423 0.3863 0.045 Uiso 1 1 calc R . . H6C H 0.1289 0.0423 0.2733 0.045 Uiso 1 1 calc R . . C7 C -0.02735(15) 0.23976(16) 0.32943(15) 0.0342(5) Uani 1 1 d . . . H7A H -0.0565 0.3013 0.3307 0.051 Uiso 1 1 calc R . . H7B H -0.0240 0.2043 0.3849 0.051 Uiso 1 1 calc R . . H7C H -0.0718 0.2071 0.2718 0.051 Uiso 1 1 calc R . . C8 C 0.0858(2) 0.43443(16) 0.32052(15) 0.0462(6) Uani 1 1 d . . . H8A H 0.1361 0.4811 0.3190 0.069 Uiso 1 1 calc R . . H8B H 0.0687 0.4453 0.3756 0.069 Uiso 1 1 calc R . . H8C H 0.0223 0.4388 0.2626 0.069 Uiso 1 1 calc R . . C9 C 0.3107(2) 0.38518(19) 0.31383(16) 0.0519(7) Uani 1 1 d . . . H9A H 0.2848 0.4482 0.3145 0.078 Uiso 1 1 calc R . . H9B H 0.3186 0.3746 0.2542 0.078 Uiso 1 1 calc R . . H9C H 0.3783 0.3776 0.3668 0.078 Uiso 1 1 calc R . . C10 C 0.33723(15) 0.16061(18) 0.32351(14) 0.0391(5) Uani 1 1 d . . . H10A H 0.3899 0.2038 0.3204 0.059 Uiso 1 1 calc R . . H10B H 0.3139 0.1201 0.2679 0.059 Uiso 1 1 calc R . . H10C H 0.3674 0.1229 0.3809 0.059 Uiso 1 1 calc R . . C11 C 0.35631(13) 0.27123(12) 0.57456(12) 0.0181(3) Uani 1 1 d . . . C12 C 0.29489(12) 0.18545(12) 0.57469(11) 0.0177(3) Uani 1 1 d . . . C13 C 0.20861(14) 0.24514(11) 0.57820(12) 0.0181(3) Uani 1 1 d . . . C14 C 0.26975(12) 0.33082(12) 0.57813(11) 0.0183(3) Uani 1 1 d . . . C111 C 0.46093(12) 0.29024(12) 0.57328(11) 0.0187(3) Uani 1 1 d . . . C115 C 0.57107(14) 0.39578(14) 0.54126(14) 0.0285(4) Uani 1 1 d . . . H115 H 0.5825 0.4561 0.5225 0.034 Uiso 1 1 calc R . . C114 C 0.65163(13) 0.32989(14) 0.56167(13) 0.0276(4) Uani 1 1 d . . . H114 H 0.7150 0.3450 0.5558 0.033 Uiso 1 1 calc R . . C113 C 0.63511(14) 0.24085(13) 0.59102(14) 0.0258(4) Uani 1 1 d . . . H113 H 0.6883 0.1952 0.6070 0.031 Uiso 1 1 calc R . . C121 C 0.31735(12) 0.08374(12) 0.58690(11) 0.0190(3) Uani 1 1 d . . . C125 C 0.40337(14) -0.04570(13) 0.55931(13) 0.0282(4) Uani 1 1 d . . . H125 H 0.4481 -0.0713 0.5325 0.034 Uiso 1 1 calc R . . C124 C 0.36454(15) -0.10524(14) 0.61023(15) 0.0328(4) Uani 1 1 d . . . H124 H 0.3815 -0.1693 0.6163 0.039 Uiso 1 1 calc R . . C123 C 0.29976(15) -0.06717(14) 0.65202(15) 0.0320(4) Uani 1 1 d . . . H123 H 0.2725 -0.1053 0.6871 0.038 Uiso 1 1 calc R . . C131 C 0.10668(13) 0.22302(13) 0.58407(12) 0.0206(3) Uani 1 1 d . . . C135 C -0.02878(14) 0.11512(15) 0.55319(14) 0.0321(4) Uani 1 1 d . . . H135 H -0.0582 0.0564 0.5293 0.039 Uiso 1 1 calc R . . C134 C -0.08359(15) 0.17365(17) 0.59054(16) 0.0390(5) Uani 1 1 d . . . H134 H -0.1483 0.1550 0.5915 0.047 Uiso 1 1 calc R . . C133 C -0.04002(18) 0.26039(16) 0.62644(18) 0.0378(5) Uani 1 1 d . . . H133 H -0.0749 0.3013 0.6526 0.045 Uiso 1 1 calc R . . C141 C 0.25672(13) 0.43157(12) 0.59314(12) 0.0202(3) Uani 1 1 d . . . C145 C 0.14348(15) 0.55761(14) 0.57137(14) 0.0295(4) Uani 1 1 d . . . H145 H 0.0747 0.5817 0.5468 0.035 Uiso 1 1 calc R . . C144 C 0.22616(16) 0.61919(14) 0.62006(15) 0.0330(4) Uani 1 1 d . . . H144 H 0.2132 0.6828 0.6270 0.040 Uiso 1 1 calc R . . C143 C 0.32850(16) 0.58342(14) 0.65795(15) 0.0320(4) Uani 1 1 d . . . H143 H 0.3858 0.6224 0.6921 0.038 Uiso 1 1 calc R . . N1 N 0.47740(11) 0.37802(11) 0.54690(11) 0.0250(3) Uani 1 1 d . . . C112 C 0.53879(13) 0.22003(13) 0.59654(12) 0.0222(3) Uani 1 1 d . . . H112 H 0.5262 0.1602 0.6155 0.027 Uiso 1 1 calc R . . N2 N 0.38046(11) 0.04679(11) 0.54612(10) 0.0232(3) Uani 1 1 d . . . C122 C 0.27620(13) 0.02837(13) 0.64089(12) 0.0247(4) Uani 1 1 d . . . H122 H 0.2335 0.0555 0.6690 0.030 Uiso 1 1 calc R . . N3 N 0.06437(11) 0.13784(11) 0.54920(11) 0.0246(3) Uani 1 1 d . . . C132 C 0.05657(14) 0.28642(15) 0.62330(14) 0.0278(4) Uani 1 1 d . . . H132 H 0.0871 0.3449 0.6469 0.033 Uiso 1 1 calc R . . N4 N 0.15625(11) 0.46585(11) 0.55750(11) 0.0253(3) Uani 1 1 d . . . C142 C 0.34413(14) 0.48886(13) 0.64417(13) 0.0259(4) Uani 1 1 d . . . H142 H 0.4124 0.4635 0.6687 0.031 Uiso 1 1 calc R . . Fe1 Fe 0.225293(18) 0.260191(18) 0.452901(17) 0.01633(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 C1 0.0201(7) 0.0215(9) 0.0164(7) -0.0014(6) 0.0064(6) 0.0007(6) C2 0.0191(8) 0.0276(9) 0.0162(8) -0.0014(6) 0.0036(7) 0.0044(6) C3 0.0393(10) 0.0216(9) 0.0172(8) 0.0023(7) 0.0056(7) 0.0046(8) C4 0.0353(10) 0.0327(10) 0.0174(8) 0.0018(7) 0.0091(7) -0.0096(8) C5 0.0205(8) 0.0353(10) 0.0167(8) -0.0005(7) 0.0083(6) -0.0002(7) C6 0.0365(10) 0.0225(9) 0.0295(9) -0.0041(7) 0.0107(8) -0.0017(8) C7 0.0192(9) 0.0568(14) 0.0236(10) -0.0047(8) 0.0054(7) 0.0093(8) C8 0.0750(16) 0.0263(11) 0.0267(10) 0.0045(8) 0.0089(10) 0.0156(11) C9 0.0687(16) 0.0556(15) 0.0306(11) 0.0003(10) 0.0188(11) -0.0353(13) C10 0.0262(9) 0.0668(16) 0.0292(10) 0.0017(10) 0.0160(8) 0.0105(10) C11 0.0153(8) 0.0198(8) 0.0175(8) 0.0000(6) 0.0047(6) 0.0023(6) C12 0.0149(7) 0.0215(8) 0.0163(7) 0.0008(6) 0.0058(6) 0.0016(6) C13 0.0170(8) 0.0207(8) 0.0170(8) 0.0001(6) 0.0070(6) 0.0016(6) C14 0.0154(7) 0.0214(8) 0.0175(7) -0.0015(6) 0.0060(6) 0.0008(6) C111 0.0169(7) 0.0207(8) 0.0182(7) -0.0025(6) 0.0067(6) -0.0004(6) C115 0.0238(8) 0.0266(9) 0.0377(10) 0.0016(8) 0.0149(7) -0.0034(7) C114 0.0177(8) 0.0362(11) 0.0306(9) -0.0020(8) 0.0115(7) -0.0028(7) C113 0.0179(8) 0.0324(10) 0.0267(9) -0.0007(7) 0.0084(7) 0.0056(7) C121 0.0155(7) 0.0198(8) 0.0191(7) 0.0001(6) 0.0040(6) 0.0006(6) C125 0.0271(9) 0.0227(9) 0.0334(9) -0.0023(7) 0.0105(7) 0.0058(7) C124 0.0324(10) 0.0199(9) 0.0407(11) 0.0037(8) 0.0085(8) 0.0051(8) C123 0.0297(9) 0.0271(10) 0.0377(10) 0.0098(8) 0.0117(8) -0.0009(8) C131 0.0158(7) 0.0268(9) 0.0197(8) 0.0051(7) 0.0074(6) 0.0025(6) C135 0.0225(8) 0.0356(11) 0.0387(10) 0.0045(8) 0.0126(8) -0.0051(8) C134 0.0235(9) 0.0479(13) 0.0518(12) 0.0087(10) 0.0215(9) 0.0002(9) C133 0.0312(11) 0.0465(13) 0.0457(12) 0.0056(9) 0.0257(10) 0.0118(9) C141 0.0207(8) 0.0207(8) 0.0206(7) 0.0000(6) 0.0097(6) 0.0025(6) C145 0.0294(9) 0.0263(10) 0.0358(10) 0.0014(8) 0.0159(8) 0.0099(7) C144 0.0435(11) 0.0190(9) 0.0467(11) -0.0019(8) 0.0287(9) 0.0037(8) C143 0.0342(10) 0.0256(10) 0.0430(11) -0.0109(8) 0.0224(9) -0.0079(8) N1 0.0205(7) 0.0227(8) 0.0340(8) 0.0010(6) 0.0130(6) -0.0004(6) C112 0.0190(8) 0.0234(9) 0.0231(8) 0.0002(7) 0.0072(6) 0.0022(7) N2 0.0216(7) 0.0224(8) 0.0259(7) -0.0005(6) 0.0097(6) 0.0028(6) C122 0.0208(8) 0.0263(9) 0.0268(8) 0.0047(7) 0.0091(7) 0.0024(7) N3 0.0186(7) 0.0274(8) 0.0282(7) 0.0028(6) 0.0098(6) -0.0014(6) C132 0.0256(9) 0.0306(10) 0.0310(9) 0.0009(8) 0.0152(7) 0.0043(8) N4 0.0218(7) 0.0250(8) 0.0281(7) -0.0003(6) 0.0089(6) 0.0051(6) C142 0.0224(8) 0.0250(9) 0.0327(9) -0.0046(7) 0.0135(7) 0.0007(7) Fe1 0.01531(14) 0.01660(15) 0.01690(15) 0.00041(9) 0.00616(11) 0.00052(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C2 1.429(2) . ? C1 C5 1.424(2) . ? C1 C6 1.496(2) . ? C1 Fe1 2.1061(16) . ? C2 C3 1.431(3) . ? C2 C7 1.496(3) . ? C2 Fe1 2.0959(18) . ? C3 C4 1.428(3) . ? C3 C8 1.504(3) . ? C3 Fe1 2.1146(17) . ? C4 C5 1.420(3) . ? C4 C9 1.496(3) . ? C4 Fe1 2.1467(18) . ? C5 C10 1.496(3) . ? C5 Fe1 2.1365(17) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.475(2) . ? C11 C14 1.472(2) . ? C11 C111 1.465(2) . ? C11 Fe1 2.0018(16) . ? C12 C13 1.469(2) . ? C12 C121 1.465(2) . ? C12 Fe1 2.0034(16) . ? C13 C14 1.472(2) . ? C13 C131 1.466(2) . ? C13 Fe1 2.0027(17) . ? C14 C141 1.463(2) . ? C14 Fe1 2.0064(16) . ? C111 N1 1.348(2) . ? C111 C112 1.395(2) . ? C115 H115 0.9300 . ? C115 C114 1.382(3) . ? C115 N1 1.342(2) . ? C114 H114 0.9300 . ? C114 C113 1.381(3) . ? C113 H113 0.9300 . ? C113 C112 1.385(3) . ? C121 N2 1.348(2) . ? C121 C122 1.398(2) . ? C125 H125 0.9300 . ? C125 C124 1.379(3) . ? C125 N2 1.340(2) . ? C124 H124 0.9300 . ? C124 C123 1.384(3) . ? C123 H123 0.9300 . ? C123 C122 1.382(3) . ? C131 N3 1.349(2) . ? C131 C132 1.394(3) . ? C135 H135 0.9300 . ? C135 C134 1.378(3) . ? C135 N3 1.339(2) . ? C134 H134 0.9300 . ? C134 C133 1.377(3) . ? C133 H133 0.9300 . ? C133 C132 1.391(3) . ? C141 N4 1.353(2) . ? C141 C142 1.397(2) . ? C145 H145 0.9300 . ? C145 C144 1.386(3) . ? C145 N4 1.335(2) . ? C144 H144 0.9300 . ? C144 C143 1.383(3) . ? C143 H143 0.9300 . ? C143 C142 1.381(3) . ? C112 H112 0.9300 . ? C122 H122 0.9300 . ? C132 H132 0.9300 . ? C142 H142 0.9300 . ? 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 C2 C1 C6 126.18(16) . . ? C2 C1 Fe1 69.74(10) . . ? C5 C1 C2 108.13(16) . . ? C5 C1 C6 125.68(16) . . ? C5 C1 Fe1 71.55(10) . . ? C6 C1 Fe1 125.51(12) . . ? C1 C2 C3 107.73(16) . . ? C1 C2 C7 126.30(17) . . ? C1 C2 Fe1 70.51(10) . . ? C3 C2 C7 125.85(17) . . ? C3 C2 Fe1 70.84(10) . . ? C7 C2 Fe1 127.17(13) . . ? C2 C3 C8 125.72(19) . . ? C2 C3 Fe1 69.44(10) . . ? C4 C3 C2 107.80(16) . . ? C4 C3 C8 126.3(2) . . ? C4 C3 Fe1 71.64(10) . . ? C8 C3 Fe1 128.30(13) . . ? C3 C4 C9 125.9(2) . . ? C3 C4 Fe1 69.21(10) . . ? C5 C4 C3 108.23(15) . . ? C5 C4 C9 125.8(2) . . ? C5 C4 Fe1 70.25(9) . . ? C9 C4 Fe1 128.23(13) . . ? C1 C5 C10 125.22(19) . . ? C1 C5 Fe1 69.24(9) . . ? C4 C5 C1 108.11(15) . . ? C4 C5 C10 126.67(18) . . ? C4 C5 Fe1 71.03(10) . . ? C10 C5 Fe1 125.33(12) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 Fe1 68.44(9) . . ? C14 C11 C12 90.13(13) . . ? C14 C11 Fe1 68.62(9) . . ? C111 C11 C12 135.34(15) . . ? C111 C11 C14 134.52(16) . . ? C111 C11 Fe1 121.91(12) . . ? C11 C12 Fe1 68.33(9) . . ? C13 C12 C11 89.74(13) . . ? C13 C12 Fe1 68.46(9) . . ? C121 C12 C11 135.56(14) . . ? C121 C12 C13 133.61(15) . . ? C121 C12 Fe1 129.20(12) . . ? C12 C13 C14 90.36(13) . . ? C12 C13 Fe1 68.51(9) . . ? C14 C13 Fe1 68.59(9) . . ? C131 C13 C12 132.67(15) . . ? C131 C13 C14 136.91(15) . . ? C131 C13 Fe1 123.08(12) . . ? C11 C14 C13 89.77(13) . . ? C11 C14 Fe1 68.30(9) . . ? C13 C14 Fe1 68.33(9) . . ? C141 C14 C11 135.34(15) . . ? C141 C14 C13 134.08(15) . . ? C141 C14 Fe1 128.26(12) . . ? N1 C111 C11 116.80(14) . . ? N1 C111 C112 121.85(15) . . ? C112 C111 C11 121.34(16) . . ? C114 C115 H115 118.0 . . ? N1 C115 H115 118.0 . . ? N1 C115 C114 123.95(18) . . ? C115 C114 H114 121.1 . . ? C113 C114 C115 117.87(16) . . ? C113 C114 H114 121.1 . . ? C114 C113 H113 120.2 . . ? C114 C113 C112 119.53(17) . . ? C112 C113 H113 120.2 . . ? N2 C121 C12 117.55(15) . . ? N2 C121 C122 121.85(16) . . ? C122 C121 C12 120.58(15) . . ? C124 C125 H125 118.0 . . ? N2 C125 H125 118.0 . . ? N2 C125 C124 123.93(17) . . ? C125 C124 H124 120.9 . . ? C125 C124 C123 118.30(18) . . ? C123 C124 H124 120.9 . . ? C124 C123 H123 120.5 . . ? C122 C123 C124 119.00(18) . . ? C122 C123 H123 120.5 . . ? N3 C131 C13 116.03(15) . . ? N3 C131 C132 122.08(16) . . ? C132 C131 C13 121.89(17) . . ? C134 C135 H135 118.1 . . ? N3 C135 H135 118.1 . . ? N3 C135 C134 123.8(2) . . ? C135 C134 H134 120.9 . . ? C133 C134 C135 118.28(18) . . ? C133 C134 H134 120.9 . . ? C134 C133 H133 120.3 . . ? C134 C133 C132 119.45(19) . . ? C132 C133 H133 120.3 . . ? N4 C141 C14 116.98(15) . . ? N4 C141 C142 121.77(16) . . ? C142 C141 C14 121.23(15) . . ? C144 C145 H145 117.9 . . ? N4 C145 H145 117.9 . . ? N4 C145 C144 124.21(17) . . ? C145 C144 H144 120.9 . . ? C143 C144 C145 118.15(17) . . ? C143 C144 H144 120.9 . . ? C144 C143 H143 120.6 . . ? C142 C143 C144 118.88(18) . . ? C142 C143 H143 120.6 . . ? C115 N1 C111 117.78(15) . . ? C111 C112 H112 120.5 . . ? C113 C112 C111 118.99(17) . . ? C113 C112 H112 120.5 . . ? C125 N2 C121 117.66(15) . . ? C121 C122 H122 120.4 . . ? C123 C122 C121 119.24(17) . . ? C123 C122 H122 120.4 . . ? C135 N3 C131 117.78(16) . . ? C131 C132 H132 120.7 . . ? C133 C132 C131 118.59(19) . . ? C133 C132 H132 120.7 . . ? C145 N4 C141 117.43(16) . . ? C141 C142 H142 120.2 . . ? C143 C142 C141 119.55(17) . . ? C143 C142 H142 120.2 . . ? C1 Fe1 C3 66.34(7) . . ? C1 Fe1 C4 65.54(7) . . ? C1 Fe1 C5 39.21(7) . . ? C2 Fe1 C1 39.75(6) . . ? C2 Fe1 C3 39.72(7) . . ? C2 Fe1 C4 65.95(7) . . ? C2 Fe1 C5 66.13(7) . . ? C3 Fe1 C4 39.15(8) . . ? C3 Fe1 C5 65.74(7) . . ? C5 Fe1 C4 38.72(8) . . ? C11 Fe1 C1 142.78(7) . . ? C11 Fe1 C2 176.19(7) . . ? C11 Fe1 C3 141.37(7) . . ? C11 Fe1 C4 117.20(7) . . ? C11 Fe1 C5 117.62(7) . . ? C11 Fe1 C12 43.22(7) . . ? C11 Fe1 C13 62.49(7) . . ? C11 Fe1 C14 43.08(6) . . ? C12 Fe1 C1 113.19(7) . . ? C12 Fe1 C2 135.15(7) . . ? C12 Fe1 C3 172.53(7) . . ? C12 Fe1 C4 148.11(7) . . ? C12 Fe1 C5 119.02(7) . . ? C12 Fe1 C14 62.70(7) . . ? C13 Fe1 C1 125.11(7) . . ? C13 Fe1 C2 113.87(7) . . ? C13 Fe1 C3 130.55(7) . . ? C13 Fe1 C4 164.55(7) . . ? C13 Fe1 C5 156.60(7) . . ? C13 Fe1 C12 43.02(6) . . ? C13 Fe1 C14 43.07(7) . . ? C14 Fe1 C1 167.21(7) . . ? C14 Fe1 C2 133.67(7) . . ? C14 Fe1 C3 116.01(7) . . ? C14 Fe1 C4 124.88(7) . . ? C14 Fe1 C5 153.55(7) . . ? _database_code_depnum_ccdc_archive 'CCDC 962752' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cpd_2 _audit_creation_date 2013-10-15 _audit_creation_method ; Olex2 1.2 (compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601) ; _shelxl_version_number 2013-2 _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C46 H55 Cl2 Fe K N4 O6 Zn' _chemical_formula_sum 'C46 H55 Cl2 Fe K N4 O6 Zn' _chemical_formula_weight 991.16 _chemical_melting_point ? _chemical_oxdiff_formula 'C46 H55 N4 Fe K O6 Zn Cl2' 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' 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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 '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' Zn Zn -1.5491 0.6778 '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/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.4571(2) _cell_length_b 16.5968(2) _cell_length_c 17.0934(2) _cell_angle_alpha 90 _cell_angle_beta 94.918(1) _cell_angle_gamma 90 _cell_volume 4651.6(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 12674 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 73.4430 _cell_measurement_theta_min 3.6980 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 5.405 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.50246 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dark violet' _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary violet _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 2064 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.03 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_unetI/netI 0.0331 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.974 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 27914 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.974 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 73.795 _diffrn_reflns_theta_min 3.719 _diffrn_ambient_temperature 123(2) _diffrn_detector_area_resol_mean 10.3546 _diffrn_measured_fraction_theta_full 0.9972 _diffrn_measured_fraction_theta_max 0.9721 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -59.00 29.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 37.0000 -180.0000 88 #__ type_ start__ end____ width___ exp.time_ 2 omega -62.00 25.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 57.0000 -60.0000 87 #__ type_ start__ end____ width___ exp.time_ 3 omega 31.00 69.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -30.0000 -60.0000 38 #__ type_ start__ end____ width___ exp.time_ 4 omega 77.00 158.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 61.0000 -150.0000 81 #__ type_ start__ end____ width___ exp.time_ 5 omega 84.00 158.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 30.0000 -180.0000 74 #__ type_ start__ end____ width___ exp.time_ 6 omega 71.00 102.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -94.0000 150.0000 31 #__ type_ start__ end____ width___ exp.time_ 7 omega 79.00 154.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 45.0000 -60.0000 75 #__ type_ start__ end____ width___ exp.time_ 8 omega 25.00 106.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -94.0000 90.0000 81 #__ type_ start__ end____ width___ exp.time_ 9 omega 36.00 69.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -30.0000 -90.0000 33 #__ type_ start__ end____ width___ exp.time_ 10 omega -115.00 -12.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 -57.0000 30.0000 103 #__ type_ start__ end____ width___ exp.time_ 11 omega -120.00 -8.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 -77.0000 -180.0000 112 #__ type_ start__ end____ width___ exp.time_ 12 omega -162.00 -137.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -77.0000 -66.2458 25 #__ type_ start__ end____ width___ exp.time_ 13 omega 24.00 158.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -15.0000 120.0000 134 #__ type_ start__ end____ width___ exp.time_ 14 omega 23.00 109.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -94.0000 -60.0000 86 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0338806000 _diffrn_orient_matrix_UB_12 0.0708761000 _diffrn_orient_matrix_UB_13 0.0511379000 _diffrn_orient_matrix_UB_21 0.0875083000 _diffrn_orient_matrix_UB_22 -0.0242344000 _diffrn_orient_matrix_UB_23 -0.0156719000 _diffrn_orient_matrix_UB_31 -0.0049931000 _diffrn_orient_matrix_UB_32 0.0548501000 _diffrn_orient_matrix_UB_33 -0.0729119000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 8008 _reflns_number_total 9169 _reflns_odcompleteness_completeness 99.72 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.506 _refine_diff_density_min -0.393 _refine_diff_density_rms 0.057 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 550 _refine_ls_number_reflns 9169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0336 _refine_ls_restrained_S_all 1.017 _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^)+(0.0487P)^2^+1.6500P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0857 _refine_ls_wR_factor_ref 0.0911 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A, H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B) 2.b Me refined with riding coordinates: C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A, H10B,H10C) 2.c Aromatic/amide H refined with riding coordinates: C112(H112), C113(H113), C114(H114), C115(H115), C122(H122), C123(H123), C124(H124), C125(H125), C135(H135), C134(H134), C133(H133), C142(H142), C143(H143), C144(H144), C145(H145), C132(H132) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _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 C1 C -0.49413(12) -0.03119(14) 0.68883(14) 0.0320(5) Uani 1 1 d . . . . . C2 C -0.44979(13) -0.07773(14) 0.63624(14) 0.0326(5) Uani 1 1 d . . . . . C3 C -0.41506(13) -0.02289(14) 0.58348(13) 0.0298(5) Uani 1 1 d . . . . . C4 C -0.43793(12) 0.05630(13) 0.60344(13) 0.0275(4) Uani 1 1 d . . . . . C5 C -0.48642(12) 0.05227(14) 0.66883(14) 0.0293(5) Uani 1 1 d . . . . . C6 C -0.54542(14) -0.06461(17) 0.74931(18) 0.0460(7) Uani 1 1 d . . . . . H6A H -0.5693 -0.0202 0.7774 0.069 Uiso 1 1 calc R U . . . H6B H -0.5114 -0.0977 0.7866 0.069 Uiso 1 1 calc R U . . . H6C H -0.5891 -0.0978 0.7235 0.069 Uiso 1 1 calc R U . . . C7 C -0.44529(16) -0.16849(15) 0.63422(17) 0.0447(6) Uani 1 1 d . . . . . H7A H -0.4109 -0.1853 0.5931 0.067 Uiso 1 1 calc R U . . . H7B H -0.5003 -0.1907 0.6231 0.067 Uiso 1 1 calc R U . . . H7C H -0.4218 -0.1884 0.6852 0.067 Uiso 1 1 calc R U . . . C8 C -0.36411(16) -0.04381(16) 0.51734(15) 0.0412(6) Uani 1 1 d . . . . . H8A H -0.3565 -0.1023 0.5155 0.062 Uiso 1 1 calc R U . . . H8B H -0.3108 -0.0174 0.5259 0.062 Uiso 1 1 calc R U . . . H8C H -0.3918 -0.0254 0.4675 0.062 Uiso 1 1 calc R U . . . C9 C -0.41743(14) 0.13113(15) 0.56040(14) 0.0364(5) Uani 1 1 d . . . . . H9A H -0.4402 0.1781 0.5855 0.055 Uiso 1 1 calc R U . . . H9B H -0.4406 0.1276 0.5057 0.055 Uiso 1 1 calc R U . . . H9C H -0.3580 0.1367 0.5617 0.055 Uiso 1 1 calc R U . . . C10 C -0.52505(13) 0.12187(16) 0.70675(16) 0.0399(6) Uani 1 1 d . . . . . H10A H -0.5550 0.1024 0.7501 0.060 Uiso 1 1 calc R U . . . H10B H -0.5629 0.1492 0.6680 0.060 Uiso 1 1 calc R U . . . H10C H -0.4827 0.1598 0.7270 0.060 Uiso 1 1 calc R U . . . C11 C -0.25423(11) -0.02422(12) 0.72819(12) 0.0208(4) Uani 1 1 d . . . . . C12 C -0.27240(11) 0.06197(12) 0.74297(11) 0.0202(4) Uani 1 1 d . . . . . C13 C -0.32587(11) 0.03774(12) 0.80418(12) 0.0219(4) Uani 1 1 d . . . . . C14 C -0.30709(11) -0.04783(12) 0.78970(12) 0.0211(4) Uani 1 1 d . . . . . C15 C 0.05293(19) -0.22256(16) 0.68305(16) 0.0501(7) Uani 1 1 d . . . . . H15A H 0.0972 -0.2579 0.7061 0.060 Uiso 1 1 calc R U . . . H15B H 0.0331 -0.2444 0.6310 0.060 Uiso 1 1 calc R U . . . C16 C -0.01472(17) -0.22005(18) 0.73513(19) 0.0522(7) Uani 1 1 d . . . . . H16A H -0.0567 -0.1811 0.7144 0.063 Uiso 1 1 calc R U . . . H16B H -0.0405 -0.2738 0.7371 0.063 Uiso 1 1 calc R U . . . C17 C -0.04618(15) -0.18629(17) 0.8622(2) 0.0504(7) Uani 1 1 d . . . . . H17A H -0.0829 -0.2336 0.8586 0.060 Uiso 1 1 calc R U . . . H17B H -0.0787 -0.1378 0.8467 0.060 Uiso 1 1 calc R U . . . C18 C -0.00832(17) -0.17728(15) 0.94405(18) 0.0459(7) Uani 1 1 d . . . . . H18A H -0.0514 -0.1719 0.9808 0.055 Uiso 1 1 calc R U . . . H18B H 0.0247 -0.2256 0.9592 0.055 Uiso 1 1 calc R U . . . C19 C 0.09358(19) -0.10526(16) 1.01938(15) 0.0468(7) Uani 1 1 d . . . . . H19A H 0.1347 -0.1489 1.0197 0.056 Uiso 1 1 calc R U . . . H19B H 0.0608 -0.1134 1.0647 0.056 Uiso 1 1 calc R U . . . C20 C 0.13513(19) -0.02542(17) 1.02577(15) 0.0456(6) Uani 1 1 d . . . . . H20A H 0.0940 0.0182 1.0251 0.055 Uiso 1 1 calc R U . . . H20B H 0.1699 -0.0221 1.0759 0.055 Uiso 1 1 calc R U . . . C21 C 0.22494(19) 0.05927(19) 0.96499(19) 0.0557(8) Uani 1 1 d . . . . . H21A H 0.2605 0.0632 1.0146 0.067 Uiso 1 1 calc R U . . . H21B H 0.1847 0.1037 0.9639 0.067 Uiso 1 1 calc R U . . . C22 C 0.27530(17) 0.06667(18) 0.8966(2) 0.0538(8) Uani 1 1 d . . . . . H22A H 0.3073 0.1172 0.9009 0.065 Uiso 1 1 calc R U . . . H22B H 0.3139 0.0209 0.8963 0.065 Uiso 1 1 calc R U . . . C23 C 0.26689(19) 0.08394(19) 0.7593(2) 0.0585(8) Uani 1 1 d . . . . . H23A H 0.3183 0.0528 0.7623 0.070 Uiso 1 1 calc R U . . . H23B H 0.2807 0.1420 0.7583 0.070 Uiso 1 1 calc R U . . . C24 C 0.2155(2) 0.06201(18) 0.6861(2) 0.0571(8) Uani 1 1 d . . . . . H24A H 0.1626 0.0907 0.6843 0.069 Uiso 1 1 calc R U . . . H24B H 0.2434 0.0778 0.6394 0.069 Uiso 1 1 calc R U . . . C25 C 0.1645(2) -0.0507(2) 0.61279(17) 0.0587(8) Uani 1 1 d . . . . . H25A H 0.2021 -0.0440 0.5710 0.070 Uiso 1 1 calc R U . . . H25B H 0.1144 -0.0192 0.5981 0.070 Uiso 1 1 calc R U . . . C26 C 0.1437(2) -0.1373(2) 0.62128(16) 0.0577(8) Uani 1 1 d . . . . . H26A H 0.1233 -0.1599 0.5697 0.069 Uiso 1 1 calc R U . . . H26B H 0.1927 -0.1680 0.6413 0.069 Uiso 1 1 calc R U . . . C111 C -0.21350(11) -0.07166(12) 0.67296(11) 0.0210(4) Uani 1 1 d . . . . . C112 C -0.23216(13) -0.15424(13) 0.66102(13) 0.0267(4) Uani 1 1 d . . . . . H112 H -0.2700 -0.1799 0.6918 0.032 Uiso 1 1 calc R U . . . C113 C -0.19585(13) -0.19736(13) 0.60527(13) 0.0287(4) Uani 1 1 d . . . . . H113 H -0.2087 -0.2527 0.5973 0.034 Uiso 1 1 calc R U . . . C114 C -0.13994(13) -0.15988(13) 0.56002(13) 0.0300(5) Uani 1 1 d . . . . . H114 H -0.1158 -0.1883 0.5197 0.036 Uiso 1 1 calc R U . . . C115 C -0.12108(13) -0.08087(13) 0.57564(12) 0.0271(4) Uani 1 1 d . . . . . H115 H -0.0819 -0.0553 0.5463 0.032 Uiso 1 1 calc R U . . . C121 C -0.25842(11) 0.13958(12) 0.70915(11) 0.0203(4) Uani 1 1 d . . . . . C122 C -0.30910(12) 0.20580(13) 0.72344(13) 0.0257(4) Uani 1 1 d . . . . . H122 H -0.3523 0.1994 0.7564 0.031 Uiso 1 1 calc R U . . . C123 C -0.29607(13) 0.27942(12) 0.68978(13) 0.0281(4) Uani 1 1 d . . . . . H123 H -0.3295 0.3241 0.7004 0.034 Uiso 1 1 calc R U . . . C124 C -0.23408(13) 0.28835(13) 0.64027(13) 0.0284(4) Uani 1 1 d . . . . . H124 H -0.2255 0.3382 0.6149 0.034 Uiso 1 1 calc R U . . . C125 C -0.18545(12) 0.22268(12) 0.62909(12) 0.0253(4) Uani 1 1 d . . . . . H125 H -0.1426 0.2283 0.5956 0.030 Uiso 1 1 calc R U . . . C131 C -0.35468(12) 0.08076(12) 0.87077(12) 0.0242(4) Uani 1 1 d . . . . . N3 N -0.42117(12) 0.05284(12) 0.90350(13) 0.0360(4) Uani 1 1 d . . . . . C135 C -0.44459(16) 0.09246(16) 0.96629(16) 0.0426(6) Uani 1 1 d . . . . . H135 H -0.4906 0.0725 0.9902 0.051 Uiso 1 1 calc R U . . . C134 C -0.40656(15) 0.15995(15) 0.99828(15) 0.0382(5) Uani 1 1 d . . . . . H134 H -0.4257 0.1858 1.0428 0.046 Uiso 1 1 calc R U . . . C133 C -0.33962(15) 0.18903(14) 0.96373(14) 0.0349(5) Uani 1 1 d . . . . . H133 H -0.3123 0.2362 0.9834 0.042 Uiso 1 1 calc R U . . . C141 C -0.31433(12) -0.11986(12) 0.83763(12) 0.0219(4) Uani 1 1 d . . . . . C142 C -0.38142(13) -0.13117(13) 0.88108(13) 0.0280(4) Uani 1 1 d . . . . . H142 H -0.4250 -0.0934 0.8777 0.034 Uiso 1 1 calc R U . . . C143 C -0.38372(14) -0.19761(14) 0.92891(14) 0.0342(5) Uani 1 1 d . . . . . H143 H -0.4286 -0.2057 0.9594 0.041 Uiso 1 1 calc R U . . . C144 C -0.32042(15) -0.25269(14) 0.93238(15) 0.0357(5) Uani 1 1 d . . . . . H144 H -0.3210 -0.2991 0.9648 0.043 Uiso 1 1 calc R U . . . C145 C -0.25659(14) -0.23807(13) 0.88735(15) 0.0341(5) Uani 1 1 d . . . . . H145 H -0.2131 -0.2759 0.8896 0.041 Uiso 1 1 calc R U . . . N1 N -0.15580(10) -0.03745(10) 0.63111(10) 0.0221(3) Uani 1 1 d . . . . . N2 N -0.19569(9) 0.15027(10) 0.66360(10) 0.0210(3) Uani 1 1 d . . . . . C132 C -0.31312(13) 0.14870(13) 0.90050(13) 0.0271(4) Uani 1 1 d . . . . . H132 H -0.2663 0.1672 0.8770 0.032 Uiso 1 1 calc R U . . . N4 N -0.25199(11) -0.17332(11) 0.84023(11) 0.0282(4) Uani 1 1 d . . . . . O1 O 0.08271(13) -0.14294(11) 0.67482(10) 0.0471(4) Uani 1 1 d . . . . . O2 O 0.01698(9) -0.19660(10) 0.81150(10) 0.0366(4) Uani 1 1 d . . . . . O3 O 0.04212(11) -0.10764(10) 0.94829(10) 0.0378(4) Uani 1 1 d . . . . . O4 O 0.18379(11) -0.01607(10) 0.96144(10) 0.0385(4) Uani 1 1 d . . . . . O5 O 0.22371(10) 0.06697(11) 0.82643(12) 0.0449(4) Uani 1 1 d . . . . . O6 O 0.20245(12) -0.02258(12) 0.68616(11) 0.0484(5) Uani 1 1 d . . . . . Cl1 Cl -0.01890(3) 0.10582(3) 0.57431(3) 0.03443(13) Uani 1 1 d . . . . . Cl2 Cl -0.04305(3) 0.05890(3) 0.78562(3) 0.03329(12) Uani 1 1 d . . . . . K1 K 0.10304(3) -0.05211(3) 0.81092(3) 0.02904(11) Uani 1 1 d . . . . . Fe1 Fe -0.37414(2) 0.00119(2) 0.69991(2) 0.02047(8) Uani 1 1 d . . . . . Zn1 Zn -0.10434(2) 0.06900(2) 0.66343(2) 0.02132(8) 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 C1 0.0215(9) 0.0356(12) 0.0380(13) 0.0096(10) -0.0031(9) -0.0045(9) C2 0.0310(10) 0.0285(11) 0.0356(13) 0.0024(9) -0.0129(9) -0.0052(9) C3 0.0314(10) 0.0310(11) 0.0250(11) -0.0006(9) -0.0086(9) -0.0007(9) C4 0.0235(9) 0.0293(11) 0.0285(11) 0.0043(8) -0.0053(8) -0.0014(8) C5 0.0182(9) 0.0340(12) 0.0350(12) 0.0076(9) -0.0027(8) 0.0000(8) C6 0.0233(10) 0.0567(17) 0.0581(17) 0.0232(13) 0.0034(11) -0.0086(10) C7 0.0495(14) 0.0290(12) 0.0517(16) 0.0019(11) -0.0178(12) -0.0102(11) C8 0.0482(14) 0.0446(14) 0.0292(13) -0.0060(10) -0.0052(11) 0.0050(11) C9 0.0379(12) 0.0365(13) 0.0330(12) 0.0121(10) -0.0072(10) -0.0033(10) C10 0.0236(10) 0.0468(15) 0.0491(15) 0.0047(11) 0.0023(10) 0.0089(10) C11 0.0198(8) 0.0204(9) 0.0221(10) 0.0016(7) 0.0013(7) 0.0002(7) C12 0.0179(8) 0.0230(10) 0.0197(10) -0.0017(7) 0.0015(7) -0.0004(7) C13 0.0210(8) 0.0214(10) 0.0235(10) 0.0002(7) 0.0036(8) -0.0003(7) C14 0.0219(8) 0.0202(9) 0.0214(10) -0.0001(7) 0.0018(8) 0.0019(7) C15 0.0708(19) 0.0369(14) 0.0389(15) -0.0089(11) -0.0178(14) 0.0076(13) C16 0.0471(14) 0.0426(15) 0.0623(19) -0.0047(13) -0.0226(14) -0.0025(12) C17 0.0289(11) 0.0340(14) 0.089(2) -0.0013(13) 0.0127(13) -0.0003(10) C18 0.0481(14) 0.0293(12) 0.0652(19) 0.0050(12) 0.0335(14) 0.0022(11) C19 0.0749(19) 0.0409(14) 0.0266(12) 0.0047(10) 0.0157(13) 0.0123(13) C20 0.0663(17) 0.0421(14) 0.0286(13) -0.0069(10) 0.0059(12) 0.0142(13) C21 0.0567(17) 0.0542(18) 0.0550(18) -0.0211(14) -0.0026(14) -0.0137(14) C22 0.0370(13) 0.0489(17) 0.075(2) -0.0150(14) 0.0017(14) -0.0126(12) C23 0.0504(16) 0.0467(17) 0.083(2) 0.0101(15) 0.0327(16) -0.0045(13) C24 0.0670(19) 0.0489(17) 0.060(2) 0.0188(14) 0.0310(16) 0.0045(14) C25 0.080(2) 0.068(2) 0.0306(14) 0.0117(13) 0.0178(14) 0.0177(17) C26 0.084(2) 0.0606(19) 0.0287(14) -0.0025(12) 0.0082(14) 0.0248(17) C111 0.0212(8) 0.0224(10) 0.0189(9) -0.0003(7) -0.0016(7) 0.0017(7) C112 0.0300(10) 0.0239(10) 0.0261(11) -0.0022(8) 0.0015(8) -0.0009(8) C113 0.0336(10) 0.0223(10) 0.0295(11) -0.0064(8) -0.0017(9) 0.0018(8) C114 0.0342(10) 0.0313(11) 0.0244(11) -0.0086(8) 0.0029(9) 0.0055(9) C115 0.0288(10) 0.0311(11) 0.0216(10) -0.0026(8) 0.0038(8) 0.0038(8) C121 0.0205(8) 0.0208(9) 0.0190(9) -0.0015(7) -0.0011(7) -0.0005(7) C122 0.0253(9) 0.0257(10) 0.0262(11) -0.0005(8) 0.0036(8) 0.0027(8) C123 0.0299(10) 0.0196(10) 0.0342(12) -0.0004(8) -0.0002(9) 0.0036(8) C124 0.0308(10) 0.0203(10) 0.0334(12) 0.0050(8) -0.0018(9) -0.0025(8) C125 0.0254(9) 0.0252(10) 0.0254(10) 0.0030(8) 0.0022(8) -0.0024(8) C131 0.0250(9) 0.0225(10) 0.0253(11) 0.0004(8) 0.0030(8) 0.0030(8) N3 0.0372(10) 0.0315(10) 0.0416(12) -0.0089(8) 0.0176(9) -0.0027(8) C135 0.0425(13) 0.0413(14) 0.0474(15) -0.0084(11) 0.0235(12) 0.0004(11) C134 0.0443(13) 0.0392(13) 0.0327(13) -0.0109(10) 0.0122(10) 0.0072(10) C133 0.0417(12) 0.0297(12) 0.0330(12) -0.0079(9) 0.0018(10) 0.0012(9) C141 0.0255(9) 0.0190(9) 0.0209(10) 0.0002(7) 0.0004(8) -0.0012(7) C142 0.0266(9) 0.0274(11) 0.0305(11) 0.0036(8) 0.0058(8) -0.0007(8) C143 0.0339(11) 0.0341(12) 0.0353(13) 0.0081(10) 0.0062(10) -0.0054(9) C144 0.0403(12) 0.0294(12) 0.0367(13) 0.0128(9) -0.0005(10) -0.0041(9) C145 0.0348(11) 0.0251(11) 0.0420(13) 0.0064(9) 0.0008(10) 0.0042(9) N1 0.0233(8) 0.0227(8) 0.0205(8) -0.0015(6) 0.0028(7) 0.0013(6) N2 0.0214(7) 0.0204(8) 0.0211(8) 0.0010(6) 0.0013(6) -0.0004(6) C132 0.0287(10) 0.0278(11) 0.0248(11) -0.0021(8) 0.0030(8) 0.0002(8) N4 0.0296(8) 0.0242(9) 0.0308(10) 0.0029(7) 0.0033(7) 0.0028(7) O1 0.0712(12) 0.0386(10) 0.0307(9) -0.0022(7) 0.0002(9) 0.0117(9) O2 0.0280(7) 0.0352(9) 0.0455(10) 0.0000(7) -0.0038(7) 0.0012(6) O3 0.0479(9) 0.0281(8) 0.0395(10) 0.0049(7) 0.0155(8) 0.0018(7) O4 0.0469(9) 0.0366(9) 0.0314(9) -0.0073(7) 0.0004(7) 0.0038(7) O5 0.0323(8) 0.0447(10) 0.0594(12) 0.0030(8) 0.0134(8) -0.0037(7) O6 0.0601(11) 0.0454(11) 0.0420(11) 0.0120(8) 0.0175(9) 0.0075(9) Cl1 0.0398(3) 0.0299(3) 0.0366(3) 0.0003(2) 0.0211(2) -0.0013(2) Cl2 0.0348(3) 0.0394(3) 0.0245(3) -0.0029(2) -0.0040(2) 0.0092(2) K1 0.0298(2) 0.0295(2) 0.0281(2) 0.00159(17) 0.00369(18) 0.00178(17) Fe1 0.01937(14) 0.01938(16) 0.02238(17) 0.00183(11) 0.00011(12) -0.00090(11) Zn1 0.02167(13) 0.02233(14) 0.02042(14) -0.00038(10) 0.00448(10) 0.00097(10) _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 C1 C2 1.432(4) . ? C1 C5 1.435(3) . ? C1 C6 1.496(3) . ? C1 Fe1 2.040(2) . ? C2 C3 1.434(3) . ? C2 C7 1.509(3) . ? C2 Fe1 2.054(2) . ? C3 C4 1.417(3) . ? C3 C8 1.505(3) . ? C3 Fe1 2.084(2) . ? C4 C5 1.430(3) . ? C4 C9 1.497(3) . ? C4 Fe1 2.088(2) . ? C5 C10 1.493(3) . ? C5 Fe1 2.061(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.487(3) . ? C11 C14 1.474(3) . ? C11 C111 1.439(3) . ? C11 Fe1 2.0352(18) . ? C12 C13 1.479(3) . ? C12 C121 1.439(3) . ? C12 Fe1 2.0374(19) . ? C13 C14 1.479(3) . ? C13 C131 1.457(3) . ? C13 Fe1 1.983(2) . ? C14 C141 1.460(3) . ? C14 Fe1 1.986(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.485(4) . ? C15 O1 1.421(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 O2 1.418(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.489(5) . ? C17 O2 1.420(3) . ? C17 K1 3.482(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C18 O3 1.421(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.491(4) . ? C19 O3 1.421(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C20 O4 1.423(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 C22 1.496(5) . ? C21 O4 1.421(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C22 O5 1.408(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.493(5) . ? C23 O5 1.429(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 O6 1.420(4) . ? C24 K1 3.498(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 C26 1.487(5) . ? C25 O6 1.431(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26 O1 1.418(4) . ? C111 C112 1.416(3) . ? C111 N1 1.361(3) . ? C112 H112 0.9500 . ? C112 C113 1.369(3) . ? C113 H113 0.9500 . ? C113 C114 1.398(3) . ? C114 H114 0.9500 . ? C114 C115 1.369(3) . ? C115 H115 0.9500 . ? C115 N1 1.355(3) . ? C121 C122 1.414(3) . ? C121 N2 1.357(3) . ? C122 H122 0.9500 . ? C122 C123 1.375(3) . ? C123 H123 0.9500 . ? C123 C124 1.388(3) . ? C124 H124 0.9500 . ? C124 C125 1.375(3) . ? C124 K1 3.471(2) 2_556 ? C125 H125 0.9500 . ? C125 N2 1.356(3) . ? C131 N3 1.353(3) . ? C131 C132 1.392(3) . ? N3 C135 1.343(3) . ? C135 H135 0.9500 . ? C135 C134 1.374(4) . ? C134 H134 0.9500 . ? C134 C133 1.381(4) . ? C133 H133 0.9500 . ? C133 C132 1.374(3) . ? C141 C142 1.395(3) . ? C141 N4 1.354(3) . ? C142 H142 0.9500 . ? C142 C143 1.375(3) . ? C143 H143 0.9500 . ? C143 C144 1.383(3) . ? C144 H144 0.9500 . ? C144 C145 1.376(3) . ? C145 H145 0.9500 . ? C145 N4 1.349(3) . ? N1 Zn1 2.0159(17) . ? N2 Zn1 2.0201(16) . ? C132 H132 0.9500 . ? O1 K1 2.7681(18) . ? O2 K1 2.7854(17) . ? O3 K1 2.7878(17) . ? O4 K1 2.8561(17) . ? O5 K1 2.7981(18) . ? O6 K1 2.8395(19) . ? Cl1 Zn1 2.2446(6) . ? Cl2 K1 3.0306(7) . ? Cl2 Zn1 2.2465(6) . ? K1 C124 3.471(2) 2_546 ? 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 C2 C1 C5 108.1(2) . . ? C2 C1 C6 125.6(2) . . ? C2 C1 Fe1 70.06(12) . . ? C5 C1 C6 126.1(2) . . ? C5 C1 Fe1 70.32(12) . . ? C6 C1 Fe1 129.24(17) . . ? C1 C2 C3 107.7(2) . . ? C1 C2 C7 125.6(2) . . ? C1 C2 Fe1 69.00(12) . . ? C3 C2 C7 126.6(2) . . ? C3 C2 Fe1 70.87(12) . . ? C7 C2 Fe1 128.33(16) . . ? C2 C3 C8 127.2(2) . . ? C2 C3 Fe1 68.58(12) . . ? C4 C3 C2 108.0(2) . . ? C4 C3 C8 124.9(2) . . ? C4 C3 Fe1 70.30(12) . . ? C8 C3 Fe1 127.33(16) . . ? C3 C4 C5 108.82(19) . . ? C3 C4 C9 125.1(2) . . ? C3 C4 Fe1 70.00(12) . . ? C5 C4 C9 126.0(2) . . ? C5 C4 Fe1 68.82(12) . . ? C9 C4 Fe1 129.22(15) . . ? C1 C5 C10 126.4(2) . . ? C1 C5 Fe1 68.72(12) . . ? C4 C5 C1 107.3(2) . . ? C4 C5 C10 126.2(2) . . ? C4 C5 Fe1 70.88(12) . . ? C10 C5 Fe1 127.74(16) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 Fe1 68.66(10) . . ? C14 C11 C12 89.72(15) . . ? C14 C11 Fe1 66.74(10) . . ? C111 C11 C12 138.56(18) . . ? C111 C11 C14 131.25(18) . . ? C111 C11 Fe1 117.03(13) . . ? C11 C12 Fe1 68.50(10) . . ? C13 C12 C11 89.95(15) . . ? C13 C12 Fe1 66.47(10) . . ? C121 C12 C11 138.72(18) . . ? C121 C12 C13 130.77(18) . . ? C121 C12 Fe1 116.94(13) . . ? C12 C13 Fe1 70.38(11) . . ? C14 C13 C12 89.84(15) . . ? C14 C13 Fe1 68.23(11) . . ? C131 C13 C12 132.26(18) . . ? C131 C13 C14 133.47(18) . . ? C131 C13 Fe1 136.05(14) . . ? C11 C14 C13 90.49(15) . . ? C11 C14 Fe1 70.28(11) . . ? C13 C14 Fe1 68.02(11) . . ? C141 C14 C11 134.39(18) . . ? C141 C14 C13 131.63(18) . . ? C141 C14 Fe1 134.62(14) . . ? H15A C15 H15B 108.4 . . ? C16 C15 H15A 110.0 . . ? C16 C15 H15B 110.0 . . ? O1 C15 H15A 110.0 . . ? O1 C15 H15B 110.0 . . ? O1 C15 C16 108.4(2) . . ? C15 C16 H16A 109.9 . . ? C15 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? O2 C16 C15 108.9(2) . . ? O2 C16 H16A 109.9 . . ? O2 C16 H16B 109.9 . . ? H17A C17 H17B 108.4 . . ? C18 C17 H17A 110.0 . . ? C18 C17 H17B 110.0 . . ? C18 C17 K1 85.70(14) . . ? O2 C17 H17A 110.0 . . ? O2 C17 H17B 110.0 . . ? O2 C17 C18 108.4(2) . . ? O2 C17 K1 49.79(11) . . ? K1 C17 H17A 158.8 . . ? K1 C17 H17B 77.8 . . ? C17 C18 H18A 109.9 . . ? C17 C18 H18B 109.9 . . ? H18A C18 H18B 108.3 . . ? O3 C18 C17 109.0(2) . . ? O3 C18 H18A 109.9 . . ? O3 C18 H18B 109.9 . . ? H19A C19 H19B 108.3 . . ? C20 C19 H19A 109.9 . . ? C20 C19 H19B 109.9 . . ? O3 C19 H19A 109.9 . . ? O3 C19 H19B 109.9 . . ? O3 C19 C20 108.9(2) . . ? C19 C20 H20A 109.9 . . ? C19 C20 H20B 109.9 . . ? H20A C20 H20B 108.3 . . ? O4 C20 C19 109.0(2) . . ? O4 C20 H20A 109.9 . . ? O4 C20 H20B 109.9 . . ? H21A C21 H21B 108.2 . . ? C22 C21 H21A 109.8 . . ? C22 C21 H21B 109.8 . . ? O4 C21 H21A 109.8 . . ? O4 C21 H21B 109.8 . . ? O4 C21 C22 109.5(2) . . ? C21 C22 H22A 109.8 . . ? C21 C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? O5 C22 C21 109.4(2) . . ? O5 C22 H22A 109.8 . . ? O5 C22 H22B 109.8 . . ? H23A C23 H23B 108.2 . . ? C24 C23 H23A 109.7 . . ? C24 C23 H23B 109.7 . . ? O5 C23 H23A 109.7 . . ? O5 C23 H23B 109.7 . . ? O5 C23 C24 109.9(2) . . ? C23 C24 H24A 110.0 . . ? C23 C24 H24B 110.0 . . ? C23 C24 K1 84.99(16) . . ? H24A C24 H24B 108.4 . . ? O6 C24 C23 108.4(3) . . ? O6 C24 H24A 110.0 . . ? O6 C24 H24B 110.0 . . ? O6 C24 K1 51.44(12) . . ? K1 C24 H24A 76.7 . . ? K1 C24 H24B 160.3 . . ? H25A C25 H25B 108.4 . . ? C26 C25 H25A 110.0 . . ? C26 C25 H25B 110.0 . . ? O6 C25 H25A 110.0 . . ? O6 C25 H25B 110.0 . . ? O6 C25 C26 108.4(2) . . ? C25 C26 H26A 110.1 . . ? C25 C26 H26B 110.1 . . ? H26A C26 H26B 108.4 . . ? O1 C26 C25 108.0(2) . . ? O1 C26 H26A 110.1 . . ? O1 C26 H26B 110.1 . . ? C112 C111 C11 121.13(18) . . ? N1 C111 C11 120.14(18) . . ? N1 C111 C112 118.73(18) . . ? C111 C112 H112 119.9 . . ? C113 C112 C111 120.3(2) . . ? C113 C112 H112 119.9 . . ? C112 C113 H113 120.0 . . ? C112 C113 C114 120.0(2) . . ? C114 C113 H113 120.0 . . ? C113 C114 H114 121.1 . . ? C115 C114 C113 117.9(2) . . ? C115 C114 H114 121.1 . . ? C114 C115 H115 118.5 . . ? N1 C115 C114 122.9(2) . . ? N1 C115 H115 118.5 . . ? C122 C121 C12 120.64(18) . . ? N2 C121 C12 120.23(17) . . ? N2 C121 C122 119.12(18) . . ? C121 C122 H122 119.9 . . ? C123 C122 C121 120.20(19) . . ? C123 C122 H122 119.9 . . ? C122 C123 H123 120.0 . . ? C122 C123 C124 119.94(19) . . ? C124 C123 H123 120.0 . . ? C123 C124 H124 121.1 . . ? C123 C124 K1 114.14(14) . 2_556 ? C125 C124 C123 117.83(19) . . ? C125 C124 H124 121.1 . . ? C125 C124 K1 106.32(13) . 2_556 ? K1 C124 H124 48.1 2_556 . ? C124 C125 H125 118.4 . . ? N2 C125 C124 123.13(19) . . ? N2 C125 H125 118.4 . . ? N3 C131 C13 118.96(18) . . ? N3 C131 C132 121.06(19) . . ? C132 C131 C13 119.97(18) . . ? C135 N3 C131 117.4(2) . . ? N3 C135 H135 117.8 . . ? N3 C135 C134 124.4(2) . . ? C134 C135 H135 117.8 . . ? C135 C134 H134 121.1 . . ? C135 C134 C133 117.9(2) . . ? C133 C134 H134 121.1 . . ? C134 C133 H133 120.5 . . ? C132 C133 C134 119.0(2) . . ? C132 C133 H133 120.5 . . ? C142 C141 C14 121.02(18) . . ? N4 C141 C14 117.19(18) . . ? N4 C141 C142 121.74(18) . . ? C141 C142 H142 120.4 . . ? C143 C142 C141 119.2(2) . . ? C143 C142 H142 120.4 . . ? C142 C143 H143 120.1 . . ? C142 C143 C144 119.8(2) . . ? C144 C143 H143 120.1 . . ? C143 C144 H144 121.1 . . ? C145 C144 C143 117.9(2) . . ? C145 C144 H144 121.1 . . ? C144 C145 H145 118.0 . . ? N4 C145 C144 124.0(2) . . ? N4 C145 H145 118.0 . . ? C111 N1 Zn1 121.14(13) . . ? C115 N1 C111 120.06(18) . . ? C115 N1 Zn1 117.72(14) . . ? C121 N2 Zn1 121.09(13) . . ? C125 N2 C121 119.66(17) . . ? C125 N2 Zn1 118.10(13) . . ? C131 C132 H132 119.9 . . ? C133 C132 C131 120.2(2) . . ? C133 C132 H132 119.9 . . ? C145 N4 C141 117.42(19) . . ? C15 O1 K1 116.18(15) . . ? C26 O1 C15 113.3(2) . . ? C26 O1 K1 117.71(18) . . ? C16 O2 C17 111.4(2) . . ? C16 O2 K1 112.34(16) . . ? C17 O2 K1 107.31(14) . . ? C18 O3 K1 118.46(15) . . ? C19 O3 C18 111.7(2) . . ? C19 O3 K1 118.69(15) . . ? C20 O4 K1 115.09(15) . . ? C21 O4 C20 111.1(2) . . ? C21 O4 K1 113.96(16) . . ? C22 O5 C23 112.3(2) . . ? C22 O5 K1 116.71(16) . . ? C23 O5 K1 117.45(18) . . ? C24 O6 C25 112.1(2) . . ? C24 O6 K1 105.53(16) . . ? C25 O6 K1 111.44(17) . . ? Zn1 Cl2 K1 117.74(2) . . ? C17 K1 C24 157.07(8) . . ? C124 K1 C17 83.61(6) 2_546 . ? C124 K1 C24 102.08(7) 2_546 . ? O1 K1 C17 80.00(7) . . ? O1 K1 C24 79.31(7) . . ? O1 K1 C124 79.31(5) . 2_546 ? O1 K1 O2 60.61(6) . . ? O1 K1 O3 120.10(6) . . ? O1 K1 O4 152.19(5) . . ? O1 K1 O5 119.86(6) . . ? O1 K1 O6 59.92(6) . . ? O1 K1 Cl2 100.02(4) . . ? O2 K1 C17 22.91(6) . . ? O2 K1 C24 139.81(7) . . ? O2 K1 C124 69.40(5) . 2_546 ? O2 K1 O3 59.52(5) . . ? O2 K1 O4 112.00(5) . . ? O2 K1 O5 164.73(5) . . ? O2 K1 O6 118.50(6) . . ? O2 K1 Cl2 97.27(4) . . ? O3 K1 C17 42.63(7) . . ? O3 K1 C24 160.01(7) . . ? O3 K1 C124 78.83(5) . 2_546 ? O3 K1 O4 58.91(5) . . ? O3 K1 O5 117.21(6) . . ? O3 K1 O6 164.07(6) . . ? O3 K1 Cl2 89.02(4) . . ? O4 K1 C17 101.00(7) . . ? O4 K1 C24 101.90(7) . . ? O4 K1 C124 73.25(5) . 2_546 ? O4 K1 Cl2 107.66(4) . . ? O5 K1 C17 159.70(7) . . ? O5 K1 C24 42.87(7) . . ? O5 K1 C124 95.44(5) . 2_546 ? O5 K1 O4 59.68(6) . . ? O5 K1 O6 59.95(6) . . ? O5 K1 Cl2 97.59(4) . . ? O6 K1 C17 139.78(7) . . ? O6 K1 C24 23.03(7) . . ? O6 K1 C124 85.76(6) . 2_546 ? O6 K1 O4 112.76(6) . . ? O6 K1 Cl2 106.80(4) . . ? Cl2 K1 C17 81.76(5) . . ? Cl2 K1 C24 92.21(6) . . ? Cl2 K1 C124 165.24(4) . 2_546 ? C1 Fe1 C2 40.94(10) . . ? C1 Fe1 C3 68.28(9) . . ? C1 Fe1 C4 67.97(9) . . ? C1 Fe1 C5 40.96(9) . . ? C2 Fe1 C3 40.55(9) . . ? C2 Fe1 C4 67.66(9) . . ? C2 Fe1 C5 68.67(9) . . ? C3 Fe1 C4 39.70(9) . . ? C5 Fe1 C3 67.89(9) . . ? C5 Fe1 C4 40.30(9) . . ? C11 Fe1 C1 151.50(9) . . ? C11 Fe1 C2 121.68(9) . . ? C11 Fe1 C3 114.48(8) . . ? C11 Fe1 C4 133.62(8) . . ? C11 Fe1 C5 167.46(8) . . ? C11 Fe1 C12 42.84(8) . . ? C12 Fe1 C1 157.38(9) . . ? C12 Fe1 C2 161.67(9) . . ? C12 Fe1 C3 128.91(8) . . ? C12 Fe1 C4 114.22(8) . . ? C12 Fe1 C5 125.47(9) . . ? C13 Fe1 C1 118.30(9) . . ? C13 Fe1 C2 148.14(9) . . ? C13 Fe1 C3 171.31(9) . . ? C13 Fe1 C4 135.33(9) . . ? C13 Fe1 C5 112.77(9) . . ? C13 Fe1 C11 62.89(8) . . ? C13 Fe1 C12 43.15(8) . . ? C13 Fe1 C14 43.75(8) . . ? C14 Fe1 C1 115.67(9) . . ? C14 Fe1 C2 114.82(8) . . ? C14 Fe1 C3 140.53(9) . . ? C14 Fe1 C4 176.36(8) . . ? C14 Fe1 C5 142.58(9) . . ? C14 Fe1 C11 42.98(8) . . ? C14 Fe1 C12 62.53(8) . . ? N1 Zn1 N2 106.88(7) . . ? N1 Zn1 Cl1 109.00(5) . . ? N1 Zn1 Cl2 109.51(5) . . ? N2 Zn1 Cl1 109.19(5) . . ? N2 Zn1 Cl2 108.86(5) . . ? Cl1 Zn1 Cl2 113.20(2) . . ? _shelx_res_file ; TITL bab1 in P2(1)/c CELL 1.54178 16.4571 16.5968 17.0934 90 94.918 90 ZERR 4 0.0002 0.0002 0.0002 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O Cl K Fe Zn UNIT 184 220 16 24 8 4 4 4 L.S. 60 PLAN 25 TEMP -150.15 BOND $H fmap 2 acta MERG 2 REM Y:\Messdaten\X-ray\Babak\Bab330%20[K(18-crown-6)][(ZnCl2){(C5Me5)Fe(C REM 4py4)}]\tmp\fin\bab1.hkl WGHT 0.048700 1.650000 FVAR 0.07620 C1 1 -0.494127 -0.031187 0.688833 11.00000 0.02150 0.03564 = 0.03803 0.00962 -0.00314 -0.00453 C2 1 -0.449794 -0.077727 0.636239 11.00000 0.03104 0.02848 = 0.03559 0.00242 -0.01290 -0.00518 C3 1 -0.415056 -0.022895 0.583481 11.00000 0.03140 0.03100 = 0.02498 -0.00060 -0.00863 -0.00073 C4 1 -0.437930 0.056295 0.603443 11.00000 0.02346 0.02931 = 0.02845 0.00427 -0.00535 -0.00143 C5 1 -0.486421 0.052268 0.668832 11.00000 0.01818 0.03397 = 0.03496 0.00757 -0.00266 0.00000 C6 1 -0.545417 -0.064615 0.749311 11.00000 0.02329 0.05669 = 0.05812 0.02319 0.00345 -0.00862 AFIX 33 H6A 2 -0.569285 -0.020211 0.777407 11.00000 -1.50000 H6B 2 -0.511438 -0.097740 0.786614 11.00000 -1.50000 H6C 2 -0.589123 -0.097788 0.723524 11.00000 -1.50000 AFIX 0 C7 1 -0.445294 -0.168485 0.634218 11.00000 0.04954 0.02900 = 0.05170 0.00193 -0.01782 -0.01023 AFIX 33 H7A 2 -0.410929 -0.185306 0.593082 11.00000 -1.50000 H7B 2 -0.500253 -0.190674 0.623079 11.00000 -1.50000 H7C 2 -0.421777 -0.188431 0.685179 11.00000 -1.50000 AFIX 0 C8 1 -0.364107 -0.043805 0.517342 11.00000 0.04825 0.04458 = 0.02919 -0.00602 -0.00524 0.00499 AFIX 33 H8A 2 -0.356487 -0.102317 0.515531 11.00000 -1.50000 H8B 2 -0.310846 -0.017357 0.525905 11.00000 -1.50000 H8C 2 -0.391806 -0.025361 0.467513 11.00000 -1.50000 AFIX 0 C9 1 -0.417428 0.131128 0.560398 11.00000 0.03790 0.03651 = 0.03296 0.01209 -0.00723 -0.00327 AFIX 33 H9A 2 -0.440241 0.178080 0.585531 11.00000 -1.50000 H9B 2 -0.440576 0.127590 0.505742 11.00000 -1.50000 H9C 2 -0.358043 0.136710 0.561739 11.00000 -1.50000 AFIX 0 C10 1 -0.525050 0.121871 0.706747 11.00000 0.02357 0.04678 = 0.04909 0.00468 0.00230 0.00889 AFIX 33 H10A 2 -0.554978 0.102365 0.750148 11.00000 -1.50000 H10B 2 -0.562851 0.149159 0.667988 11.00000 -1.50000 H10C 2 -0.482675 0.159773 0.726991 11.00000 -1.50000 AFIX 0 C11 1 -0.254235 -0.024216 0.728195 11.00000 0.01983 0.02037 = 0.02207 0.00160 0.00133 0.00020 C12 1 -0.272404 0.061966 0.742968 11.00000 0.01787 0.02297 = 0.01973 -0.00169 0.00146 -0.00044 C13 1 -0.325867 0.037741 0.804178 11.00000 0.02096 0.02141 = 0.02355 0.00017 0.00356 -0.00034 C14 1 -0.307092 -0.047830 0.789704 11.00000 0.02189 0.02016 = 0.02135 -0.00010 0.00178 0.00194 C15 1 0.052933 -0.222562 0.683049 11.00000 0.07079 0.03686 = 0.03888 -0.00893 -0.01779 0.00756 AFIX 23 H15A 2 0.097184 -0.257900 0.706076 11.00000 -1.20000 H15B 2 0.033062 -0.244423 0.631005 11.00000 -1.20000 AFIX 0 C16 1 -0.014723 -0.220050 0.735127 11.00000 0.04713 0.04256 = 0.06227 -0.00475 -0.02259 -0.00254 AFIX 23 H16A 2 -0.056730 -0.181062 0.714407 11.00000 -1.20000 H16B 2 -0.040456 -0.273844 0.737129 11.00000 -1.20000 AFIX 0 C17 1 -0.046176 -0.186288 0.862208 11.00000 0.02895 0.03402 = 0.08948 -0.00134 0.01273 -0.00026 AFIX 23 H17A 2 -0.082942 -0.233601 0.858615 11.00000 -1.20000 H17B 2 -0.078681 -0.137774 0.846743 11.00000 -1.20000 AFIX 0 C18 1 -0.008322 -0.177280 0.944046 11.00000 0.04812 0.02932 = 0.06519 0.00499 0.03348 0.00224 AFIX 23 H18A 2 -0.051366 -0.171853 0.980765 11.00000 -1.20000 H18B 2 0.024667 -0.225573 0.959192 11.00000 -1.20000 AFIX 0 C19 1 0.093584 -0.105263 1.019376 11.00000 0.07486 0.04088 = 0.02661 0.00473 0.01567 0.01227 AFIX 23 H19A 2 0.134664 -0.148861 1.019657 11.00000 -1.20000 H19B 2 0.060826 -0.113375 1.064682 11.00000 -1.20000 AFIX 0 C20 1 0.135131 -0.025419 1.025771 11.00000 0.06635 0.04211 = 0.02859 -0.00692 0.00592 0.01419 AFIX 23 H20A 2 0.094022 0.018182 1.025075 11.00000 -1.20000 H20B 2 0.169927 -0.022122 1.075866 11.00000 -1.20000 AFIX 0 C21 1 0.224944 0.059267 0.964992 11.00000 0.05666 0.05417 = 0.05504 -0.02107 -0.00258 -0.01369 AFIX 23 H21A 2 0.260471 0.063167 1.014601 11.00000 -1.20000 H21B 2 0.184689 0.103667 0.963873 11.00000 -1.20000 AFIX 0 C22 1 0.275302 0.066674 0.896552 11.00000 0.03697 0.04892 = 0.07507 -0.01496 0.00168 -0.01261 AFIX 23 H22A 2 0.307332 0.117210 0.900859 11.00000 -1.20000 H22B 2 0.313852 0.020902 0.896295 11.00000 -1.20000 AFIX 0 C23 1 0.266887 0.083943 0.759287 11.00000 0.05038 0.04674 = 0.08303 0.01008 0.03271 -0.00452 AFIX 23 H23A 2 0.318348 0.052769 0.762321 11.00000 -1.20000 H23B 2 0.280731 0.141961 0.758269 11.00000 -1.20000 AFIX 0 C24 1 0.215492 0.062010 0.686129 11.00000 0.06705 0.04887 = 0.05982 0.01877 0.03105 0.00453 AFIX 23 H24A 2 0.162602 0.090661 0.684324 11.00000 -1.20000 H24B 2 0.243402 0.077787 0.639412 11.00000 -1.20000 AFIX 0 C25 1 0.164471 -0.050679 0.612791 11.00000 0.07959 0.06823 = 0.03056 0.01168 0.01784 0.01768 AFIX 23 H25A 2 0.202065 -0.043967 0.571044 11.00000 -1.20000 H25B 2 0.114410 -0.019165 0.598068 11.00000 -1.20000 AFIX 0 C26 1 0.143703 -0.137269 0.621280 11.00000 0.08428 0.06056 = 0.02870 -0.00247 0.00822 0.02478 AFIX 23 H26A 2 0.123266 -0.159941 0.569739 11.00000 -1.20000 H26B 2 0.192723 -0.167975 0.641278 11.00000 -1.20000 AFIX 0 C111 1 -0.213495 -0.071656 0.672961 11.00000 0.02121 0.02242 = 0.01892 -0.00031 -0.00158 0.00174 C112 1 -0.232162 -0.154242 0.661021 11.00000 0.03003 0.02388 = 0.02610 -0.00224 0.00150 -0.00090 AFIX 43 H112 2 -0.270034 -0.179856 0.691815 11.00000 -1.20000 AFIX 0 C113 1 -0.195855 -0.197356 0.605268 11.00000 0.03358 0.02232 = 0.02950 -0.00636 -0.00171 0.00183 AFIX 43 H113 2 -0.208665 -0.252729 0.597340 11.00000 -1.20000 AFIX 0 C114 1 -0.139936 -0.159879 0.560020 11.00000 0.03425 0.03131 = 0.02442 -0.00860 0.00287 0.00552 AFIX 43 H114 2 -0.115797 -0.188342 0.519716 11.00000 -1.20000 AFIX 0 C115 1 -0.121079 -0.080866 0.575645 11.00000 0.02877 0.03109 = 0.02163 -0.00263 0.00380 0.00384 AFIX 43 H115 2 -0.081903 -0.055304 0.546309 11.00000 -1.20000 AFIX 0 C121 1 -0.258419 0.139581 0.709147 11.00000 0.02053 0.02082 = 0.01897 -0.00155 -0.00105 -0.00051 C122 1 -0.309097 0.205805 0.723438 11.00000 0.02529 0.02574 = 0.02622 -0.00047 0.00362 0.00275 AFIX 43 H122 2 -0.352287 0.199435 0.756399 11.00000 -1.20000 AFIX 0 C123 1 -0.296068 0.279417 0.689776 11.00000 0.02988 0.01965 = 0.03416 -0.00044 -0.00021 0.00356 AFIX 43 H123 2 -0.329463 0.324119 0.700391 11.00000 -1.20000 AFIX 0 C124 1 -0.234077 0.288354 0.640272 11.00000 0.03078 0.02029 = 0.03340 0.00497 -0.00177 -0.00255 AFIX 43 H124 2 -0.225525 0.338212 0.614940 11.00000 -1.20000 AFIX 0 C125 1 -0.185446 0.222683 0.629092 11.00000 0.02543 0.02519 = 0.02535 0.00298 0.00216 -0.00235 AFIX 43 H125 2 -0.142629 0.228331 0.595588 11.00000 -1.20000 AFIX 0 C131 1 -0.354681 0.080758 0.870769 11.00000 0.02501 0.02247 = 0.02534 0.00035 0.00304 0.00298 N3 3 -0.421169 0.052837 0.903499 11.00000 0.03722 0.03151 = 0.04164 -0.00890 0.01763 -0.00269 C135 1 -0.444590 0.092464 0.966289 11.00000 0.04247 0.04132 = 0.04736 -0.00838 0.02345 0.00043 AFIX 43 H135 2 -0.490567 0.072467 0.990184 11.00000 -1.20000 AFIX 0 C134 1 -0.406559 0.159946 0.998285 11.00000 0.04432 0.03915 = 0.03268 -0.01087 0.01222 0.00718 AFIX 43 H134 2 -0.425697 0.185791 1.042771 11.00000 -1.20000 AFIX 0 C133 1 -0.339617 0.189031 0.963733 11.00000 0.04171 0.02973 = 0.03303 -0.00786 0.00182 0.00116 AFIX 43 H133 2 -0.312300 0.236219 0.983396 11.00000 -1.20000 AFIX 0 C141 1 -0.314333 -0.119856 0.837626 11.00000 0.02553 0.01899 = 0.02085 0.00020 0.00040 -0.00124 C142 1 -0.381421 -0.131173 0.881085 11.00000 0.02663 0.02743 = 0.03051 0.00357 0.00577 -0.00069 AFIX 43 H142 2 -0.424985 -0.093435 0.877679 11.00000 -1.20000 AFIX 0 C143 1 -0.383718 -0.197615 0.928905 11.00000 0.03387 0.03408 = 0.03528 0.00806 0.00615 -0.00542 AFIX 43 H143 2 -0.428617 -0.205665 0.959445 11.00000 -1.20000 AFIX 0 C144 1 -0.320424 -0.252687 0.932385 11.00000 0.04031 0.02936 = 0.03675 0.01279 -0.00050 -0.00409 AFIX 43 H144 2 -0.321002 -0.299121 0.964831 11.00000 -1.20000 AFIX 0 C145 1 -0.256594 -0.238070 0.887349 11.00000 0.03485 0.02508 = 0.04196 0.00639 0.00079 0.00424 AFIX 43 H145 2 -0.213120 -0.275883 0.889574 11.00000 -1.20000 AFIX 0 N1 3 -0.155802 -0.037453 0.631107 11.00000 0.02334 0.02271 = 0.02048 -0.00154 0.00283 0.00134 N2 3 -0.195692 0.150275 0.663602 11.00000 0.02141 0.02043 = 0.02114 0.00103 0.00128 -0.00036 C132 1 -0.313120 0.148702 0.900500 11.00000 0.02866 0.02777 = 0.02485 -0.00209 0.00298 0.00019 AFIX 43 H132 2 -0.266308 0.167228 0.876998 11.00000 -1.20000 AFIX 0 N4 3 -0.251994 -0.173319 0.840234 11.00000 0.02958 0.02418 = 0.03083 0.00292 0.00331 0.00282 O1 4 0.082714 -0.142937 0.674824 11.00000 0.07122 0.03864 = 0.03075 -0.00216 0.00015 0.01175 O2 4 0.016981 -0.196596 0.811496 11.00000 0.02800 0.03517 = 0.04553 -0.00002 -0.00380 0.00117 O3 4 0.042124 -0.107638 0.948290 11.00000 0.04787 0.02807 = 0.03950 0.00487 0.01549 0.00179 O4 4 0.183791 -0.016066 0.961442 11.00000 0.04691 0.03663 = 0.03139 -0.00734 0.00037 0.00384 O5 4 0.223708 0.066966 0.826426 11.00000 0.03229 0.04468 = 0.05940 0.00300 0.01344 -0.00371 O6 4 0.202451 -0.022579 0.686160 11.00000 0.06008 0.04543 = 0.04201 0.01205 0.01750 0.00752 CL1 5 -0.018899 0.105818 0.574305 11.00000 0.03979 0.02995 = 0.03665 0.00033 0.02112 -0.00129 CL2 5 -0.043053 0.058904 0.785624 11.00000 0.03482 0.03944 = 0.02448 -0.00291 -0.00395 0.00919 K1 6 0.103043 -0.052115 0.810920 11.00000 0.02979 0.02949 = 0.02807 0.00159 0.00369 0.00178 FE1 7 -0.374141 0.001187 0.699911 11.00000 0.01937 0.01938 = 0.02238 0.00183 0.00011 -0.00090 ZN1 8 -0.104336 0.068998 0.663428 11.00000 0.02167 0.02233 = 0.02042 -0.00038 0.00448 0.00097 HKLF 4 REM bab1 in P2(1)/c REM R1 = 0.0336 for 8008 Fo > 4sig(Fo) and 0.0407 for all 9169 data REM 550 parameters refined using 0 restraints END WGHT 0.0469 1.6174 REM Highest difference peak 0.506, deepest hole -0.393, 1-sigma level 0.057 Q1 1 -0.4983 0.1733 0.6928 11.00000 0.05 0.51 Q2 1 -0.5810 0.1225 0.6904 11.00000 0.05 0.46 Q3 1 -0.3135 -0.0810 0.5329 11.00000 0.05 0.43 Q4 1 -0.5183 0.1195 0.7668 11.00000 0.05 0.42 Q5 1 -0.5382 -0.0359 0.8047 11.00000 0.05 0.42 Q6 1 -0.3376 0.0168 0.5002 11.00000 0.05 0.40 Q7 1 -0.5256 -0.1343 0.7618 11.00000 0.05 0.39 Q8 1 -0.4028 -0.0697 0.4709 11.00000 0.05 0.36 Q9 1 -0.4617 0.0006 0.7055 11.00000 0.05 0.33 Q10 1 -0.6047 -0.0599 0.7313 11.00000 0.05 0.33 Q11 1 -0.0170 0.0703 0.6490 11.00000 0.05 0.31 Q12 1 -0.4014 0.1751 0.6046 11.00000 0.05 0.31 Q13 1 -0.4645 -0.1830 0.6858 11.00000 0.05 0.30 Q14 1 -0.4217 0.0142 0.5911 11.00000 0.05 0.28 Q15 1 -0.2864 0.0011 0.7007 11.00000 0.05 0.27 Q16 1 -0.4707 0.1434 0.5281 11.00000 0.05 0.26 Q17 1 -0.3192 -0.0120 0.8107 11.00000 0.05 0.26 Q18 1 -0.3026 0.0592 0.7806 11.00000 0.05 0.25 Q19 1 -0.0847 0.0608 0.7405 11.00000 0.05 0.25 Q20 1 -0.1857 0.0637 0.6649 11.00000 0.05 0.25 Q21 1 -0.3714 0.1200 0.5226 11.00000 0.05 0.24 Q22 1 -0.3831 -0.1561 0.9010 11.00000 0.05 0.23 Q23 1 -0.1045 0.0938 0.5994 11.00000 0.05 0.23 Q24 1 -0.4610 0.0612 0.6412 11.00000 0.05 0.23 Q25 1 -0.2612 0.0954 0.7251 11.00000 0.05 0.23 ; _shelx_res_checksum 14639 _shelx_hkl_file ; 0 0 2 410.62 5.48 0 0 -2 408.79 5.32 0 0 -3 0.01 0.06 0 0 3 0.06 0.08 0 0 -4 80.23 1.51 0 0 4 77.21 1.71 0 0 -5 0.04 0.08 0 0 5 0.02 0.13 0 0 -6 149.91 2.69 0 0 6 145.80 3.04 0 0 7 0.15 0.18 0 0 -7 -0.03 0.12 0 0 8 259.52 5.00 0 0 -8 253.64 4.39 0 0 -9 -0.17 0.17 0 0 9 0.00 0.23 0 0 -10 21.24 1.06 0 0 10 20.77 1.32 0 0 11 0.24 0.27 0 0 -11 0.11 0.22 0 0 12 0.33 0.30 0 0 -12 0.30 0.21 0 0 -13 -0.13 0.14 0 0 13 0.21 0.25 0 0 14 1.78 0.50 0 0 -14 2.47 0.33 0 0 -15 0.08 0.19 0 0 -16 0.61 0.21 0 0 -17 -0.01 0.18 0 0 -18 0.32 0.16 0 0 -20 0.66 0.16 0 0 -21 0.12 0.08 0 -1 -1 17.24 0.38 0 1 1 15.66 0.44 0 1 -2 91.48 1.41 0 1 -2 93.79 1.34 0 1 -3 388.12 5.22 0 1 -3 403.64 5.29 0 -1 -3 400.94 5.45 0 1 3 393.28 5.62 0 -1 4 15.69 0.69 0 1 4 15.86 0.69 0 1 -4 15.79 0.52 0 1 -4 16.49 0.54 0 -1 -4 16.03 0.61 0 1 5 1.80 0.28 0 -1 -5 1.67 0.22 0 1 -5 2.01 0.21 0 -1 5 1.59 0.25 0 -1 -6 7.06 0.48 0 1 -6 6.62 0.41 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32.67 2.25 0 13 5 55.42 1.51 0 -13 -5 55.16 1.57 0 13 5 56.11 3.05 0 13 -5 52.22 1.53 0 13 5 51.18 1.50 0 13 -6 -0.10 0.20 0 -13 -6 0.06 0.15 0 13 6 0.01 0.15 0 13 6 0.15 0.16 0 13 7 0.28 0.18 0 13 7 0.44 0.17 0 13 -7 0.22 0.19 0 -13 -7 0.36 0.18 0 13 8 5.80 0.53 0 13 -8 5.22 0.49 0 13 8 5.38 0.45 0 -13 -8 5.98 0.53 0 13 -9 24.55 1.06 0 13 9 23.60 1.04 0 -13 -9 26.52 1.13 0 13 9 24.17 0.95 0 -13 -10 1.00 0.29 0 13 -10 0.65 0.23 0 13 10 0.54 0.16 0 13 10 0.90 0.27 0 13 -11 1.31 0.29 0 13 11 1.50 0.29 0 -13 -11 1.55 0.31 0 13 -12 1.56 0.28 0 13 12 1.65 0.31 0 13 -13 0.66 0.20 0 13 13 0.69 0.24 0 13 -14 0.14 0.16 0 13 14 0.37 0.19 0 13 15 0.42 0.16 0 -13 -15 0.46 0.15 0 13 16 -0.29 0.15 0 -13 -16 -0.10 0.10 0 14 0 43.87 1.34 0 14 -1 2.52 0.30 0 14 -1 2.62 0.31 0 14 1 2.58 0.33 0 14 -2 68.04 1.70 0 14 -2 68.23 1.72 0 14 3 0.13 0.16 0 14 -3 0.14 0.15 0 14 -3 -0.05 0.15 0 14 4 2.40 0.32 0 14 -4 2.48 0.33 0 14 5 3.78 0.40 0 14 5 3.19 0.36 0 14 -5 2.95 0.37 0 14 6 24.21 0.99 0 -14 -6 22.89 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21.85 0.78 -19 2 0 20.46 0.64 -19 -2 0 21.33 0.64 19 2 1 -0.01 0.10 -19 2 -1 0.19 0.11 -19 -2 -1 0.11 0.10 19 2 2 2.55 0.25 -19 2 -2 2.34 0.21 -19 -2 -2 2.43 0.21 19 2 3 1.25 0.17 -19 2 -3 1.42 0.15 -19 -2 -3 1.16 0.14 -19 2 -4 1.61 0.16 19 2 4 1.52 0.17 -19 -2 -4 1.50 0.15 19 2 5 0.19 0.08 -19 -2 -5 0.07 0.06 19 3 -8 5.20 0.25 19 3 -7 0.66 0.12 -19 3 7 0.35 0.08 19 3 -6 0.53 0.12 -19 3 6 0.55 0.11 19 3 -5 1.17 0.16 -19 3 5 0.89 0.13 19 3 -4 10.35 0.51 19 3 -4 9.36 0.44 -19 3 4 8.88 0.39 19 3 -3 0.15 0.13 -19 3 3 -0.08 0.11 -19 -3 3 -0.11 0.08 19 3 -2 8.29 0.47 -19 3 2 7.14 0.36 -19 -3 2 7.55 0.33 19 3 -1 -0.01 0.12 -19 3 1 0.13 0.11 -19 -3 1 0.01 0.09 19 3 0 1.83 0.23 -19 3 0 1.29 0.17 -19 -3 0 1.46 0.16 19 3 1 7.99 0.45 -19 3 -1 7.55 0.35 -19 -3 -1 8.49 0.37 -19 3 -2 1.67 0.17 19 3 2 1.46 0.20 -19 -3 -2 1.54 0.17 19 3 3 4.08 0.30 -19 3 -3 3.62 0.22 -19 -3 -3 3.82 0.23 19 3 4 12.59 0.49 -19 3 -4 11.49 0.38 -19 -3 -4 12.34 0.41 -19 -3 -5 1.72 0.14 19 3 5 1.55 0.16 19 4 -8 1.90 0.15 19 4 -7 0.02 0.06 -19 4 7 0.08 0.07 19 4 -6 1.73 0.18 -19 4 6 1.42 0.14 19 4 -5 -0.03 0.08 -19 4 5 0.27 0.10 19 4 -4 3.14 0.29 19 4 -4 2.73 0.23 -19 4 4 2.66 0.21 19 4 -3 4.49 0.33 -19 4 3 4.21 0.27 19 4 -2 0.68 0.16 -19 4 2 0.95 0.14 -19 -4 2 0.50 0.09 19 4 -1 2.96 0.29 -19 4 1 2.45 0.20 -19 -4 1 2.36 0.18 -19 4 0 1.86 0.18 -19 -4 0 1.94 0.17 19 4 0 1.93 0.23 19 4 1 0.10 0.12 -19 4 -1 0.44 0.11 -19 -4 -1 0.38 0.10 19 4 2 0.24 0.12 -19 4 -2 0.05 0.08 -19 -4 -2 0.20 0.09 19 4 3 2.76 0.24 -19 4 -3 2.35 0.17 -19 -4 -3 2.67 0.19 19 4 4 1.31 0.16 -19 -4 -4 1.00 0.11 -19 -4 -5 2.12 0.15 19 5 -7 11.56 0.40 19 5 -6 -0.04 0.07 -19 5 6 0.15 0.07 19 5 -5 1.14 0.15 -19 5 5 1.34 0.14 19 5 -4 2.94 0.26 19 5 -4 3.01 0.24 -19 5 4 2.68 0.20 19 5 -3 2.95 0.26 -19 5 3 2.55 0.20 19 5 -2 1.28 0.19 -19 5 2 1.30 0.15 19 5 -1 0.16 0.12 -19 5 1 0.28 0.10 19 5 0 -0.07 0.11 -19 5 0 0.02 0.08 -19 -5 0 0.20 0.07 19 5 1 1.42 0.20 -19 5 -1 1.16 0.14 -19 -5 -1 1.28 0.13 19 5 2 0.06 0.09 -19 5 -2 0.10 0.08 -19 -5 -2 0.06 0.06 -19 -5 -3 1.92 0.15 19 5 3 1.80 0.19 19 5 4 0.48 0.09 19 6 -6 4.83 0.25 -19 6 6 4.28 0.21 19 6 -5 0.01 0.07 -19 6 5 0.13 0.08 19 6 -4 5.40 0.29 -19 6 4 5.24 0.26 19 6 -3 0.30 0.10 19 6 -3 0.44 0.12 -19 6 3 0.38 0.10 19 6 -2 1.51 0.19 -19 6 2 0.98 0.12 -19 6 1 0.12 0.08 -19 6 1 0.20 0.08 -19 6 0 0.58 0.12 19 6 0 0.97 0.16 -19 6 0 0.91 0.12 -19 6 -1 0.07 0.07 19 6 1 0.01 0.08 -19 6 -1 -0.12 0.07 19 6 2 0.06 0.08 19 6 3 0.24 0.09 19 7 -5 2.34 0.17 -19 7 5 2.06 0.14 19 7 -4 0.65 0.10 -19 7 4 0.38 0.09 -19 7 4 0.44 0.09 -19 7 3 0.76 0.12 19 7 -3 1.10 0.13 -19 7 3 0.98 0.11 -19 7 2 0.03 0.08 19 7 -2 0.00 0.06 19 7 -2 -0.04 0.07 -19 7 2 0.15 0.07 19 7 -1 2.23 0.19 19 7 -1 2.31 0.18 -19 7 1 1.86 0.14 -19 7 0 0.40 0.09 19 7 0 0.39 0.10 -19 7 0 0.53 0.08 19 7 1 0.90 0.12 -20 0 3 0.19 0.08 -20 0 2 3.94 0.22 -20 0 1 0.12 0.08 -20 0 0 2.01 0.16 -20 0 -1 0.16 0.08 -20 0 -2 0.46 0.08 -20 1 4 2.99 0.17 20 1 -3 1.34 0.13 -20 1 3 1.67 0.14 20 1 -2 0.20 0.07 -20 1 2 0.30 0.09 -20 -1 2 0.32 0.08 20 1 -1 0.46 0.10 -20 1 1 0.32 0.08 -20 -1 1 0.36 0.09 20 1 0 0.00 0.07 -20 1 0 -0.03 0.07 -20 1 -1 0.12 0.07 -20 -1 -1 0.07 0.07 -20 1 -2 0.23 0.07 -20 -1 -2 0.14 0.07 20 2 -4 -0.04 0.06 -20 2 4 0.05 0.05 20 2 -3 0.16 0.07 -20 2 3 -0.07 0.07 20 2 -2 3.09 0.23 -20 2 2 2.94 0.19 20 2 -1 0.13 0.08 -20 2 1 -0.05 0.07 -20 -2 1 0.04 0.06 20 2 0 0.06 0.07 -20 2 0 0.26 0.08 -20 -2 0 0.13 0.07 -20 2 -1 1.08 0.12 -20 -2 -1 1.03 0.11 -20 2 -2 0.79 0.10 -20 -2 -2 1.06 0.11 20 3 -4 7.39 0.30 -20 3 4 7.45 0.28 20 3 -3 0.39 0.09 -20 3 3 0.28 0.08 20 3 -2 2.66 0.21 20 3 -2 2.80 0.19 -20 3 2 2.49 0.17 20 3 -1 0.24 0.08 -20 3 1 0.28 0.08 20 3 0 0.16 0.08 -20 3 0 0.34 0.08 -20 3 -1 0.07 0.06 20 4 -3 0.46 0.09 -20 4 3 0.53 0.09 20 4 -2 0.96 0.13 20 4 -2 0.84 0.11 -20 4 2 0.86 0.10 20 4 -1 0.41 0.09 -20 4 1 0.33 0.07 -20 4 0 0.47 0.08 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 3570 _database_code_depnum_ccdc_archive 'CCDC 962753' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cpd_3 _audit_creation_date 2013-09-16 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:59:47, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C46 H55 Cl2 Fe2 K N4 O6' _chemical_formula_sum 'C46 H55 Cl2 Fe2 K N4 O6' _chemical_formula_weight 981.64 _chemical_melting_point ? _chemical_oxdiff_formula 'C44 H55 Fe2 N4 K O6 Cl2' 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' 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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 16.4365(9) _cell_length_b 16.5146(8) _cell_length_c 17.1501(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.109(5) _cell_angle_gamma 90.00 _cell_volume 4636.8(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7934 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 73.4010 _cell_measurement_theta_min 3.6950 _exptl_absorpt_coefficient_mu 7.295 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.43085 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dull dark red' _exptl_crystal_colour_lustre dull _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 2048 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.143 _exptl_crystal_size_min 0.039 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_unetI/netI 0.0474 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 19283 _diffrn_reflns_theta_full 74.18 _diffrn_reflns_theta_max 74.18 _diffrn_reflns_theta_min 3.72 _diffrn_ambient_temperature 123(2) _diffrn_detector_area_resol_mean 10.3546 _diffrn_measured_fraction_theta_full 0.9946 _diffrn_measured_fraction_theta_max 0.9638 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 26.00 113.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 41.2064 37.0000 -120.0000 87 #__ type_ start__ end____ width___ exp.time_ 2 omega 39.00 116.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 41.2064 37.0000 150.0000 77 #__ type_ start__ end____ width___ exp.time_ 3 omega 92.00 158.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 125.0000 -90.0000 66 #__ type_ start__ end____ width___ exp.time_ 4 omega 39.00 109.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -94.0000 90.0000 70 #__ type_ start__ end____ width___ exp.time_ 5 omega 87.00 158.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 45.0000 -180.0000 71 #__ type_ start__ end____ width___ exp.time_ 6 omega 31.00 63.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -30.0000 -90.0000 32 #__ type_ start__ end____ width___ exp.time_ 7 omega 41.00 69.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -45.0000 -120.0000 28 #__ type_ start__ end____ width___ exp.time_ 8 omega 31.00 60.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -30.0000 -150.0000 29 #__ type_ start__ end____ width___ exp.time_ 9 omega 88.00 158.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 61.0000 30.0000 70 #__ type_ start__ end____ width___ exp.time_ 10 omega 32.00 64.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -30.0000 -60.0000 32 #__ type_ start__ end____ width___ exp.time_ 11 omega 34.00 77.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -45.0000 60.0000 43 #__ type_ start__ end____ width___ exp.time_ 12 omega -98.00 -57.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 125.0000 30.0000 41 #__ type_ start__ end____ width___ exp.time_ 13 omega 12.00 115.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 41.2064 57.0000 0.0000 103 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0562667000 _diffrn_orient_matrix_UB_12 -0.0437746000 _diffrn_orient_matrix_UB_13 0.0629355000 _diffrn_orient_matrix_UB_21 0.0722704000 _diffrn_orient_matrix_UB_22 0.0113639000 _diffrn_orient_matrix_UB_23 -0.0499980000 _diffrn_orient_matrix_UB_31 0.0200718000 _diffrn_orient_matrix_UB_32 0.0814050000 _diffrn_orient_matrix_UB_33 0.0408009000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 7592 _reflns_number_total 9059 _reflns_odcompleteness_completeness 99.46 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2\s(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.417 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.067 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 550 _refine_ls_number_reflns 9059 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0419 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+1.3049P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1053 _refine_ls_wR_factor_ref 0.1146 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _olex2_refinement_description ; 1. Others Fixed Uiso: H6A(0.055) H6B(0.055) H6C(0.055) H7A(0.06) H7B(0.06) H7C(0.06) H8A(0.072) H8B(0.072) H8C(0.072) H9A(0.069) H9B(0.069) H9C(0.069) H10A(0.063) H10B(0.063) H10C(0.063) H112(0.032) H113(0.035) H114(0.034) H115(0.033) H122(0.032) H123(0.036) H124(0.038) H125(0.035) H132(0.033) H133(0.042) H134(0.044) H135(0.041) H143(0.052) H144(0.047) H145(0.043) H146(0.033) H20A(0.069) H20B(0.069) H20C(0.07) H20D(0.07) H20E(0.079) H20F(0.079) H20G(0.08) H20H(0.08) H20I(0.077) H20J(0.077) H20K(0.08) H20L(0.08) H20M(0.075) H20N(0.075) H20O(0.074) H20P(0.074) H20Q(0.062) H20R(0.062) H20S(0.063) H20T(0.063) H21A(0.063) H21B(0.063) H21C(0.071) H21D(0.071) Fixed X: H6A(0.059) H6B(0.0588) H6C(0.1415) H7A(-0.0549) H7B(-0.0633) H7C(0.0171) H8A(-0.0688) H8B(-0.0105) H8C(-0.0886) H9A(0.0268) H9B(0.1133) H9C(0.0309) H10A(0.1442) H10B(0.1895) H10C(0.1086) H112(0.1472) H113(0.1685) H114(0.2721) H115(0.3547) H122(0.2305) H123(0.2916) H124(0.3834) H125(0.4153) H132(0.0747) H133(0.072) H134(0.1801) H135(0.2886) H143(0.0083) H144(0.0722) H145(0.1859) H146(0.2321) H20A(0.4454) H20B(0.4596) H20C(0.5972) H20D(0.533) H20E(0.6252) H20F(0.6943) H20G(0.706) H20H(0.6181) H20I(0.6661) H20J(0.7473) H20K(0.821) H20L(0.784) H20M(0.8099) H20N(0.8159) H20O(0.7613) H20P(0.6859) H20Q(0.5949) H20R(0.6704) H20S(0.6353) H20T(0.5608) H21A(0.4496) H21B(0.5254) H21C(0.418) H21D(0.4232) Fixed Y: H6A(0.1777) H6B(0.1269) H6C(0.1364) H7A(0.1015) H7B(0.1485) H7C(0.1595) H8A(-0.0212) H8B(-0.0989) H8C(-0.0993) H9A(-0.192) H9B(-0.186) H9C(-0.1895) H10A(-0.1034) H10B(-0.0179) H10C(-0.026) H112(0.2008) H113(0.3251) H114(0.3382) H115(0.2284) H122(-0.1806) H123(-0.2544) H124(- 0.1896) H125(-0.0547) H132(-0.0943) H133(-0.2067) H134(-0.2989) H135(-0.2753) H143(0.0727) H144(0.1872) H145(0.2375) H146(0.169) H20A(-0.1768) H20B(-0.2707) H20C(-0.2567) H20D(-0.2413) H20E(-0.1574) H20F(-0.1666) H20G(-0.0426) H20H(- 0.0165) H20I(0.0927) H20J(0.0795) H20K(0.0527) H20L(0.1425) H20M(0.1169) H20N(0.0201) H20O(0.0629) H20P(0.1034) H20Q(0.0178) H20R(-0.0232) H20S(- 0.1501) H20T(-0.1146) H21A(-0.1711) H21B(-0.2257) H21C(-0.2321) H21D(-0.1358) Fixed Z: H6A(0.0847) H6B(0.0052) H6C(0.0612) H7A(0.2484) H7B(0.1665) H7C(0.2253) H8A(0.2759) H8B(0.2851) H8C(0.2223) H9A(0.1764) H9B(0.1406) H9C(0.0835) H10A(0.0156) H10B(0.0266) H10C(-0.0321) H112(0.2552) H113(0.1977) H114(0.1112) H115(0.093) H122(0.193) H123(0.0987) H124(0.0209) H125(0.0447) H132(0.375) H133(0.4569) H134(0.4646) H135(0.3904) H143(0.4869) H144(0.5391) H145(0.4801) H146(0.3741) H20A(0.2139) H20B(0.235) H20C(0.2053) H20D(0.1306) H20E(0.0714) H20F(0.1431) H20G(0.0742) H20H(0.0997) H20I(0.1875) H20J(0.1436) H20K(0.2662) H20L(0.2627) H20M(0.405) H20N(0.4001) H20O(0.517) H20P(0.4653) H20Q(0.5258) H20R(0.577) H20S(0.5198) H20T(0.5639) H21A(0.4793) H21B(0.458) H21C(0.3575) H21D(0.3464) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.06186(15) 0.05563(17) 0.10238(15) 0.0281(5) Uani 1 1 d . . . C2 C 0.01339(14) 0.05178(17) 0.16744(16) 0.0289(5) Uani 1 1 d . . . C3 C 0.00588(16) -0.03222(19) 0.18762(17) 0.0340(6) Uani 1 1 d . . . C4 C 0.05057(17) -0.07876(17) 0.13548(17) 0.0334(6) Uani 1 1 d . . . C5 C 0.08505(16) -0.02420(18) 0.08320(15) 0.0307(6) Uani 1 1 d . . . C6 C 0.08202(18) 0.13056(19) 0.05971(17) 0.0369(6) Uani 1 1 d . . . H6A H 0.0590 0.1777 0.0847 0.055 Uiso 1 1 calc R . . H6B H 0.0588 0.1269 0.0052 0.055 Uiso 1 1 calc R . . H6C H 0.1415 0.1364 0.0612 0.055 Uiso 1 1 calc R . . C7 C -0.02522(17) 0.1212(2) 0.20511(19) 0.0402(7) Uani 1 1 d . . . H7A H -0.0549 0.1015 0.2484 0.060 Uiso 1 1 calc R . . H7B H -0.0633 0.1485 0.1665 0.060 Uiso 1 1 calc R . . H7C H 0.0171 0.1595 0.2253 0.060 Uiso 1 1 calc R . . C8 C -0.04486(18) -0.0658(2) 0.2479(2) 0.0482(8) Uani 1 1 d . . . H8A H -0.0688 -0.0212 0.2759 0.072 Uiso 1 1 calc R . . H8B H -0.0105 -0.0989 0.2851 0.072 Uiso 1 1 calc R . . H8C H -0.0886 -0.0993 0.2223 0.072 Uiso 1 1 calc R . . C9 C 0.0559(2) -0.16941(19) 0.1339(2) 0.0458(8) Uani 1 1 d . . . H9A H 0.0268 -0.1920 0.1764 0.069 Uiso 1 1 calc R . . H9B H 0.1133 -0.1860 0.1406 0.069 Uiso 1 1 calc R . . H9C H 0.0309 -0.1895 0.0835 0.069 Uiso 1 1 calc R . . C10 C 0.1363(2) -0.0446(2) 0.01763(17) 0.0419(7) Uani 1 1 d . . . H10A H 0.1442 -0.1034 0.0156 0.063 Uiso 1 1 calc R . . H10B H 0.1895 -0.0179 0.0266 0.063 Uiso 1 1 calc R . . H10C H 0.1086 -0.0260 -0.0321 0.063 Uiso 1 1 calc R . . C11 C 0.22704(13) 0.06223(15) 0.24171(13) 0.0201(5) Uani 1 1 d . . . C12 C 0.24577(14) -0.02412(15) 0.22791(13) 0.0205(4) Uani 1 1 d . . . C13 C 0.19279(14) -0.04771(15) 0.28888(14) 0.0219(5) Uani 1 1 d . . . C14 C 0.17396(14) 0.03813(15) 0.30296(14) 0.0214(5) Uani 1 1 d . . . C111 C 0.24054(13) 0.13975(15) 0.20763(13) 0.0203(4) Uani 1 1 d . . . C112 C 0.18989(15) 0.20688(16) 0.22169(15) 0.0265(5) Uani 1 1 d . . . H112 H 0.1472 0.2008 0.2552 0.032 Uiso 1 1 calc R . . C113 C 0.20201(16) 0.28011(16) 0.18744(16) 0.0293(5) Uani 1 1 d . . . H113 H 0.1685 0.3251 0.1977 0.035 Uiso 1 1 calc R . . C114 C 0.26395(16) 0.28851(16) 0.13722(15) 0.0281(5) Uani 1 1 d . . . H114 H 0.2721 0.3382 0.1112 0.034 Uiso 1 1 calc R . . C115 C 0.31222(15) 0.22301(16) 0.12678(15) 0.0276(5) Uani 1 1 d . . . H115 H 0.3547 0.2284 0.0930 0.033 Uiso 1 1 calc R . . C121 C 0.28602(14) -0.07210(15) 0.17246(13) 0.0215(5) Uani 1 1 d . . . C122 C 0.26784(15) -0.15491(16) 0.16172(15) 0.0267(5) Uani 1 1 d . . . H122 H 0.2305 -0.1806 0.1930 0.032 Uiso 1 1 calc R . . C123 C 0.30403(16) -0.19856(17) 0.10618(15) 0.0300(5) Uani 1 1 d . . . H123 H 0.2916 -0.2544 0.0987 0.036 Uiso 1 1 calc R . . C124 C 0.35910(17) -0.16070(18) 0.06072(16) 0.0319(6) Uani 1 1 d . . . H124 H 0.3834 -0.1896 0.0209 0.038 Uiso 1 1 calc R . . C125 C 0.37723(16) -0.08064(17) 0.07501(15) 0.0289(5) Uani 1 1 d . . . H125 H 0.4153 -0.0547 0.0447 0.035 Uiso 1 1 calc R . . C131 C 0.18638(14) -0.11997(15) 0.33688(14) 0.0221(5) Uani 1 1 d . . . C132 C 0.11885(15) -0.13167(16) 0.37919(15) 0.0276(5) Uani 1 1 d . . . H132 H 0.0747 -0.0943 0.3750 0.033 Uiso 1 1 calc R . . C133 C 0.11720(17) -0.19826(18) 0.42703(17) 0.0348(6) Uani 1 1 d . . . H133 H 0.0720 -0.2067 0.4569 0.042 Uiso 1 1 calc R . . C134 C 0.18053(19) -0.25255(18) 0.43185(18) 0.0368(6) Uani 1 1 d . . . H134 H 0.1801 -0.2989 0.4646 0.044 Uiso 1 1 calc R . . C135 C 0.24480(18) -0.23762(17) 0.38760(17) 0.0341(6) Uani 1 1 d . . . H135 H 0.2886 -0.2753 0.3904 0.041 Uiso 1 1 calc R . . C141 C 0.14463(15) 0.08148(16) 0.36924(14) 0.0241(5) Uani 1 1 d . . . C143 C 0.0543(2) 0.0929(2) 0.4633(2) 0.0433(7) Uani 1 1 d . . . H143 H 0.0083 0.0727 0.4869 0.052 Uiso 1 1 calc R . . C144 C 0.09165(19) 0.16094(19) 0.49502(17) 0.0389(7) Uani 1 1 d . . . H144 H 0.0722 0.1872 0.5391 0.047 Uiso 1 1 calc R . . C145 C 0.15871(19) 0.19002(18) 0.46049(17) 0.0356(6) Uani 1 1 d . . . H145 H 0.1859 0.2375 0.4801 0.043 Uiso 1 1 calc R . . C146 C 0.18567(16) 0.14993(16) 0.39779(15) 0.0278(5) Uani 1 1 d . . . H146 H 0.2321 0.1690 0.3741 0.033 Uiso 1 1 calc R . . C200 C 0.4866(2) -0.2171(2) 0.2341(2) 0.0578(10) Uani 1 1 d . . . H20A H 0.4454 -0.1768 0.2139 0.069 Uiso 1 1 calc R . . H20B H 0.4596 -0.2707 0.2350 0.069 Uiso 1 1 calc R . . C201 C 0.5534(3) -0.2203(2) 0.1828(2) 0.0579(10) Uani 1 1 d . . . H20C H 0.5972 -0.2567 0.2053 0.070 Uiso 1 1 calc R . . H20D H 0.5330 -0.2413 0.1306 0.070 Uiso 1 1 calc R . . C202 C 0.6457(3) -0.1351(3) 0.1230(2) 0.0658(12) Uani 1 1 d . . . H20E H 0.6252 -0.1574 0.0714 0.079 Uiso 1 1 calc R . . H20F H 0.6943 -0.1666 0.1431 0.079 Uiso 1 1 calc R . . C203 C 0.6677(3) -0.0489(3) 0.1151(2) 0.0670(12) Uani 1 1 d . . . H20G H 0.7060 -0.0426 0.0742 0.080 Uiso 1 1 calc R . . H20H H 0.6181 -0.0165 0.0997 0.080 Uiso 1 1 calc R . . C204 C 0.7188(3) 0.0634(2) 0.1897(3) 0.0644(11) Uani 1 1 d . . . H20I H 0.6661 0.0927 0.1875 0.077 Uiso 1 1 calc R . . H20J H 0.7473 0.0795 0.1436 0.077 Uiso 1 1 calc R . . C205 C 0.7697(2) 0.0843(2) 0.2631(3) 0.0670(12) Uani 1 1 d . . . H20K H 0.8210 0.0527 0.2662 0.080 Uiso 1 1 calc R . . H20L H 0.7840 0.1425 0.2627 0.080 Uiso 1 1 calc R . . C206 C 0.7775(2) 0.0663(3) 0.4000(3) 0.0625(11) Uani 1 1 d . . . H20M H 0.8099 0.1169 0.4050 0.075 Uiso 1 1 calc R . . H20N H 0.8159 0.0201 0.4001 0.075 Uiso 1 1 calc R . . C207 C 0.7263(3) 0.0589(3) 0.4671(3) 0.0619(10) Uani 1 1 d . . . H20O H 0.7613 0.0629 0.5170 0.074 Uiso 1 1 calc R . . H20P H 0.6859 0.1034 0.4653 0.074 Uiso 1 1 calc R . . C208 C 0.6359(3) -0.0262(2) 0.52673(18) 0.0516(9) Uani 1 1 d . . . H20Q H 0.5949 0.0178 0.5258 0.062 Uiso 1 1 calc R . . H20R H 0.6704 -0.0232 0.5770 0.062 Uiso 1 1 calc R . . C209 C 0.5942(3) -0.1062(2) 0.51932(18) 0.0529(9) Uani 1 1 d . . . H20S H 0.6353 -0.1501 0.5198 0.063 Uiso 1 1 calc R . . H20T H 0.5608 -0.1146 0.5639 0.063 Uiso 1 1 calc R . . C210 C 0.4928(2) -0.1768(2) 0.4430(2) 0.0527(9) Uani 1 1 d . . . H21A H 0.4496 -0.1711 0.4793 0.063 Uiso 1 1 calc R . . H21B H 0.5254 -0.2257 0.4580 0.063 Uiso 1 1 calc R . . C211 C 0.4553(2) -0.1849(2) 0.3615(3) 0.0592(11) Uani 1 1 d . . . H21C H 0.4180 -0.2321 0.3575 0.071 Uiso 1 1 calc R . . H21D H 0.4232 -0.1358 0.3464 0.071 Uiso 1 1 calc R . . N1 N 0.30295(12) 0.15054(13) 0.16200(12) 0.0220(4) Uani 1 1 d . . . N2 N 0.34309(12) -0.03707(13) 0.13063(12) 0.0234(4) Uani 1 1 d . . . N3 N 0.24912(14) -0.17269(14) 0.34056(13) 0.0300(5) Uani 1 1 d . . . N4 N 0.07826(15) 0.05297(15) 0.40128(15) 0.0368(5) Uani 1 1 d . . . O1 O 0.51802(12) -0.19554(13) 0.31068(13) 0.0411(5) Uani 1 1 d . . . O2 O 0.58430(17) -0.14049(15) 0.17582(13) 0.0525(6) Uani 1 1 d . . . O3 O 0.70508(17) -0.02112(16) 0.18888(15) 0.0538(6) Uani 1 1 d . . . O4 O 0.72656(13) 0.06722(14) 0.32936(16) 0.0488(6) Uani 1 1 d . . . O5 O 0.68538(15) -0.01673(14) 0.46310(13) 0.0423(5) Uani 1 1 d . . . O6 O 0.54363(14) -0.10771(13) 0.44791(13) 0.0417(5) Uani 1 1 d . . . Cl1 Cl 0.48382(4) 0.10682(4) 0.07322(4) 0.03945(17) Uani 1 1 d . . . Cl2 Cl 0.46260(4) 0.06046(5) 0.28795(4) 0.03945(17) Uani 1 1 d . . . K1 K 0.60712(3) -0.05284(4) 0.31291(3) 0.03061(13) Uani 1 1 d . . . Fe1 Fe 0.12573(2) 0.00085(2) 0.19916(2) 0.02043(10) Uani 1 1 d . . . Fe2 Fe 0.39897(2) 0.06989(2) 0.16533(2) 0.02179(10) 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 C1 0.0202(11) 0.0313(13) 0.0312(12) 0.0064(11) -0.0059(9) -0.0021(10) C2 0.0142(10) 0.0353(14) 0.0365(13) 0.0063(11) -0.0010(9) 0.0014(10) C3 0.0187(11) 0.0370(15) 0.0449(15) 0.0111(13) -0.0052(10) -0.0087(11) C4 0.0274(12) 0.0292(14) 0.0407(14) 0.0025(12) -0.0126(11) -0.0047(11) C5 0.0267(12) 0.0345(14) 0.0288(12) -0.0004(11) -0.0083(10) -0.0024(11) C6 0.0343(14) 0.0378(16) 0.0368(14) 0.0116(12) -0.0063(11) -0.0054(12) C7 0.0214(12) 0.0474(18) 0.0518(17) 0.0045(14) 0.0031(11) 0.0100(12) C8 0.0202(12) 0.061(2) 0.063(2) 0.0237(18) 0.0015(13) -0.0099(14) C9 0.0471(17) 0.0286(15) 0.0572(19) 0.0037(14) -0.0211(15) -0.0099(14) C10 0.0430(16) 0.0484(18) 0.0329(14) -0.0066(13) -0.0039(12) 0.0066(15) C11 0.0135(9) 0.0231(12) 0.0238(11) -0.0016(9) 0.0016(8) -0.0009(9) C12 0.0171(10) 0.0204(11) 0.0237(11) 0.0016(9) 0.0001(8) 0.0014(9) C13 0.0159(10) 0.0237(12) 0.0263(11) -0.0007(10) 0.0030(9) 0.0016(9) C14 0.0176(10) 0.0217(12) 0.0253(11) 0.0010(9) 0.0040(9) -0.0008(9) C111 0.0154(9) 0.0214(11) 0.0237(11) -0.0018(9) -0.0008(8) 0.0001(9) C112 0.0219(11) 0.0259(13) 0.0318(12) -0.0003(10) 0.0036(9) 0.0020(10) C113 0.0265(12) 0.0230(12) 0.0380(13) -0.0004(11) -0.0001(10) 0.0032(10) C114 0.0281(12) 0.0220(12) 0.0335(13) 0.0047(10) -0.0008(10) -0.0023(10) C115 0.0225(11) 0.0281(13) 0.0319(12) 0.0039(11) 0.0016(9) -0.0025(10) C121 0.0164(10) 0.0252(12) 0.0226(11) 0.0002(9) 0.0004(8) 0.0023(9) C122 0.0256(11) 0.0254(13) 0.0289(12) -0.0007(10) 0.0008(9) -0.0008(10) C123 0.0305(12) 0.0253(13) 0.0333(13) -0.0090(11) -0.0022(10) 0.0041(11) C124 0.0317(13) 0.0337(14) 0.0304(12) -0.0090(11) 0.0029(10) 0.0047(12) C125 0.0255(11) 0.0335(14) 0.0278(12) -0.0020(11) 0.0032(10) 0.0051(11) C131 0.0195(10) 0.0207(11) 0.0256(11) -0.0012(9) -0.0005(9) -0.0015(9) C132 0.0234(11) 0.0274(13) 0.0323(12) 0.0054(11) 0.0044(10) 0.0007(10) C133 0.0287(13) 0.0343(15) 0.0419(15) 0.0083(13) 0.0050(11) -0.0065(12) C134 0.0404(15) 0.0279(14) 0.0415(15) 0.0126(12) -0.0003(12) -0.0021(12) C135 0.0319(13) 0.0255(13) 0.0443(15) 0.0076(12) 0.0008(11) 0.0036(11) C141 0.0207(10) 0.0246(12) 0.0272(11) -0.0005(10) 0.0036(9) 0.0040(10) C143 0.0400(15) 0.0408(17) 0.0523(18) -0.0072(15) 0.0218(14) 0.0020(14) C144 0.0403(15) 0.0404(16) 0.0373(14) -0.0100(13) 0.0111(12) 0.0081(13) C145 0.0388(15) 0.0329(14) 0.0350(14) -0.0085(12) 0.0021(12) 0.0008(12) C146 0.0268(12) 0.0272(13) 0.0296(12) -0.0012(11) 0.0039(10) -0.0007(11) C200 0.0446(18) 0.0445(19) 0.078(3) -0.0093(18) -0.0278(18) -0.0004(16) C201 0.074(3) 0.0427(19) 0.052(2) -0.0134(16) -0.0220(19) 0.0094(19) C202 0.090(3) 0.074(3) 0.0341(16) -0.0037(18) 0.0095(18) 0.029(3) C203 0.088(3) 0.081(3) 0.0342(16) 0.0130(19) 0.0193(18) 0.023(3) C204 0.065(2) 0.053(2) 0.081(3) 0.024(2) 0.037(2) 0.009(2) C205 0.049(2) 0.046(2) 0.113(4) 0.012(2) 0.044(2) -0.0040(17) C206 0.0338(17) 0.055(2) 0.097(3) -0.022(2) -0.0002(18) -0.0110(16) C207 0.057(2) 0.054(2) 0.072(2) -0.025(2) -0.0047(19) -0.0099(19) C208 0.076(2) 0.0475(19) 0.0309(14) -0.0067(14) 0.0055(15) 0.0195(19) C209 0.085(3) 0.0459(19) 0.0308(15) 0.0077(14) 0.0224(16) 0.0186(19) C210 0.0497(19) 0.0317(16) 0.083(3) 0.0038(17) 0.0409(19) 0.0037(15) C211 0.0260(14) 0.0337(17) 0.120(4) 0.000(2) 0.0197(18) 0.0027(13) N1 0.0169(8) 0.0220(10) 0.0269(10) 0.0006(8) 0.0021(7) -0.0012(8) N2 0.0225(9) 0.0244(10) 0.0238(9) -0.0018(8) 0.0048(8) 0.0022(8) N3 0.0259(10) 0.0269(11) 0.0370(12) 0.0036(9) 0.0025(9) 0.0039(9) N4 0.0330(12) 0.0321(12) 0.0478(14) -0.0086(11) 0.0170(10) -0.0027(10) O1 0.0253(9) 0.0385(11) 0.0583(13) -0.0013(10) -0.0027(9) 0.0019(9) O2 0.0738(17) 0.0474(13) 0.0349(11) -0.0038(10) -0.0029(11) 0.0155(13) O3 0.0593(15) 0.0529(14) 0.0522(13) 0.0166(12) 0.0214(11) 0.0112(13) O4 0.0299(10) 0.0451(13) 0.0736(16) 0.0049(12) 0.0163(11) -0.0018(10) O5 0.0496(12) 0.0377(11) 0.0382(11) -0.0078(9) -0.0031(9) 0.0056(10) O6 0.0504(12) 0.0307(10) 0.0465(11) 0.0055(9) 0.0187(10) 0.0045(10) Cl1 0.0433(4) 0.0328(3) 0.0463(4) 0.0005(3) 0.0269(3) -0.0008(3) Cl2 0.0342(3) 0.0534(4) 0.0295(3) -0.0035(3) -0.0045(2) 0.0127(3) K1 0.0269(3) 0.0328(3) 0.0324(3) 0.0018(2) 0.0040(2) 0.0006(2) Fe1 0.01475(16) 0.02050(19) 0.02562(19) 0.00223(14) -0.00053(13) -0.00076(14) Fe2 0.01672(17) 0.0242(2) 0.02476(19) -0.00022(15) 0.00382(13) 0.00115(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C2 1.429(4) . ? C1 C5 1.419(4) . ? C1 C6 1.490(4) . ? C1 Fe1 2.089(2) . ? C2 C3 1.438(4) . ? C2 C7 1.486(4) . ? C2 Fe1 2.058(2) . ? C3 C4 1.431(4) . ? C3 C8 1.492(4) . ? C3 Fe1 2.037(3) . ? C4 C5 1.424(4) . ? C4 C9 1.500(4) . ? C4 Fe1 2.051(3) . ? C5 C10 1.502(4) . ? C5 Fe1 2.082(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.482(3) . ? C11 C14 1.479(3) . ? C11 C111 1.433(3) . ? C11 Fe1 2.029(2) . ? C12 C13 1.472(3) . ? C12 C121 1.443(3) . ? C12 Fe1 2.033(2) . ? C13 C14 1.476(3) . ? C13 C131 1.459(3) . ? C13 Fe1 1.981(2) . ? C14 C141 1.461(3) . ? C14 Fe1 1.981(2) . ? C111 C112 1.420(3) . ? C111 N1 1.356(3) . ? C112 H112 0.9500 . ? C112 C113 1.367(4) . ? C113 H113 0.9500 . ? C113 C114 1.398(4) . ? C114 H114 0.9500 . ? C114 C115 1.363(4) . ? C114 K1 3.430(3) 2_655 ? C115 H115 0.9500 . ? C115 N1 1.355(3) . ? C121 C122 1.408(4) . ? C121 N2 1.360(3) . ? C122 H122 0.9500 . ? C122 C123 1.372(4) . ? C123 H123 0.9500 . ? C123 C124 1.394(4) . ? C124 H124 0.9500 . ? C124 C125 1.373(4) . ? C125 H125 0.9500 . ? C125 N2 1.356(3) . ? C131 C132 1.393(3) . ? C131 N3 1.347(3) . ? C132 H132 0.9500 . ? C132 C133 1.374(4) . ? C133 H133 0.9500 . ? C133 C134 1.371(4) . ? C134 H134 0.9500 . ? C134 C135 1.377(4) . ? C135 H135 0.9500 . ? C135 N3 1.347(4) . ? C141 C146 1.383(4) . ? C141 N4 1.349(3) . ? C143 H143 0.9500 . ? C143 C144 1.369(5) . ? C143 N4 1.341(4) . ? C144 H144 0.9500 . ? C144 C145 1.383(4) . ? C145 H145 0.9500 . ? C145 C146 1.370(4) . ? C146 H146 0.9500 . ? C200 H20A 0.9900 . ? C200 H20B 0.9900 . ? C200 C201 1.468(6) . ? C200 O1 1.413(4) . ? C201 H20C 0.9900 . ? C201 H20D 0.9900 . ? C201 O2 1.421(5) . ? C202 H20E 0.9900 . ? C202 H20F 0.9900 . ? C202 C203 1.478(7) . ? C202 O2 1.418(5) . ? C203 H20G 0.9900 . ? C203 H20H 0.9900 . ? C203 O3 1.432(5) . ? C204 H20I 0.9900 . ? C204 H20J 0.9900 . ? C204 C205 1.488(7) . ? C204 O3 1.415(5) . ? C204 K1 3.495(4) . ? C205 H20K 0.9900 . ? C205 H20L 0.9900 . ? C205 O4 1.421(5) . ? C206 H20M 0.9900 . ? C206 H20N 0.9900 . ? C206 C207 1.490(6) . ? C206 O4 1.410(5) . ? C207 H20O 0.9900 . ? C207 H20P 0.9900 . ? C207 O5 1.417(5) . ? C208 H20Q 0.9900 . ? C208 H20R 0.9900 . ? C208 C209 1.489(6) . ? C208 O5 1.426(4) . ? C209 H20S 0.9900 . ? C209 H20T 0.9900 . ? C209 O6 1.418(4) . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C210 C211 1.483(6) . ? C210 O6 1.412(4) . ? C211 H21C 0.9900 . ? C211 H21D 0.9900 . ? C211 O1 1.418(4) . ? C211 K1 3.471(4) . ? N1 Fe2 2.062(2) . ? N2 Fe2 2.054(2) . ? O1 K1 2.773(2) . ? O2 K1 2.758(2) . ? O3 K1 2.829(2) . ? O4 K1 2.787(2) . ? O5 K1 2.838(2) . ? O6 K1 2.775(2) . ? Cl1 Fe2 2.2814(7) . ? Cl2 K1 3.0243(9) . ? Cl2 Fe2 2.2690(7) . ? K1 C114 3.430(3) 2_645 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 125.8(3) . . ? C2 C1 Fe1 68.65(14) . . ? C5 C1 C2 108.6(2) . . ? C5 C1 C6 125.6(3) . . ? C5 C1 Fe1 69.85(14) . . ? C6 C1 Fe1 129.19(18) . . ? C1 C2 C3 107.3(3) . . ? C1 C2 C7 126.5(3) . . ? C1 C2 Fe1 71.04(14) . . ? C3 C2 C7 126.2(3) . . ? C3 C2 Fe1 68.66(14) . . ? C7 C2 Fe1 127.5(2) . . ? C2 C3 C8 126.2(3) . . ? C2 C3 Fe1 70.23(14) . . ? C4 C3 C2 107.9(2) . . ? C4 C3 C8 125.7(3) . . ? C4 C3 Fe1 70.05(15) . . ? C8 C3 Fe1 128.9(2) . . ? C3 C4 C9 125.6(3) . . ? C3 C4 Fe1 68.98(15) . . ? C5 C4 C3 108.0(2) . . ? C5 C4 C9 126.4(3) . . ? C5 C4 Fe1 71.04(15) . . ? C9 C4 Fe1 128.05(19) . . ? C1 C5 C4 108.2(3) . . ? C1 C5 C10 124.2(3) . . ? C1 C5 Fe1 70.38(15) . . ? C4 C5 C10 127.6(3) . . ? C4 C5 Fe1 68.67(15) . . ? C10 C5 Fe1 127.28(19) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 Fe1 68.74(12) . . ? C14 C11 C12 89.92(19) . . ? C14 C11 Fe1 66.66(13) . . ? C111 C11 C12 138.8(2) . . ? C111 C11 C14 130.8(2) . . ? C111 C11 Fe1 116.85(16) . . ? C11 C12 Fe1 68.45(12) . . ? C13 C12 C11 89.82(19) . . ? C13 C12 Fe1 66.62(12) . . ? C121 C12 C11 138.4(2) . . ? C121 C12 C13 131.1(2) . . ? C121 C12 Fe1 116.34(16) . . ? C12 C13 Fe1 70.38(13) . . ? C14 C13 C12 90.45(19) . . ? C14 C13 Fe1 68.15(13) . . ? C131 C13 C12 134.0(2) . . ? C131 C13 C14 131.8(2) . . ? C131 C13 Fe1 134.94(17) . . ? C11 C14 Fe1 70.09(13) . . ? C13 C14 C11 89.81(18) . . ? C13 C14 Fe1 68.12(13) . . ? C141 C14 C11 132.6(2) . . ? C141 C14 C13 133.4(2) . . ? C141 C14 Fe1 135.89(17) . . ? C112 C111 C11 120.9(2) . . ? N1 C111 C11 120.4(2) . . ? N1 C111 C112 118.7(2) . . ? C111 C112 H112 119.7 . . ? C113 C112 C111 120.5(2) . . ? C113 C112 H112 119.7 . . ? C112 C113 H113 120.2 . . ? C112 C113 C114 119.7(2) . . ? C114 C113 H113 120.2 . . ? C113 C114 H114 121.1 . . ? C113 C114 K1 112.95(18) . 2_655 ? C115 C114 C113 117.8(2) . . ? C115 C114 H114 121.1 . . ? C115 C114 K1 106.56(17) . 2_655 ? K1 C114 H114 49.2 2_655 . ? C114 C115 H115 118.2 . . ? N1 C115 C114 123.5(2) . . ? N1 C115 H115 118.2 . . ? C122 C121 C12 121.0(2) . . ? N2 C121 C12 119.5(2) . . ? N2 C121 C122 119.5(2) . . ? C121 C122 H122 120.0 . . ? C123 C122 C121 120.1(2) . . ? C123 C122 H122 120.0 . . ? C122 C123 H123 120.1 . . ? C122 C123 C124 119.7(3) . . ? C124 C123 H123 120.1 . . ? C123 C124 H124 120.9 . . ? C125 C124 C123 118.3(2) . . ? C125 C124 H124 120.9 . . ? C124 C125 H125 118.7 . . ? N2 C125 C124 122.7(3) . . ? N2 C125 H125 118.7 . . ? C132 C131 C13 120.6(2) . . ? N3 C131 C13 117.5(2) . . ? N3 C131 C132 121.9(2) . . ? C131 C132 H132 120.6 . . ? C133 C132 C131 118.8(2) . . ? C133 C132 H132 120.6 . . ? C132 C133 H133 119.9 . . ? C134 C133 C132 120.3(3) . . ? C134 C133 H133 119.9 . . ? C133 C134 H134 121.1 . . ? C133 C134 C135 117.7(3) . . ? C135 C134 H134 121.1 . . ? C134 C135 H135 118.1 . . ? N3 C135 C134 123.8(3) . . ? N3 C135 H135 118.1 . . ? C146 C141 C14 119.4(2) . . ? N4 C141 C14 118.7(2) . . ? N4 C141 C146 121.8(2) . . ? C144 C143 H143 117.7 . . ? N4 C143 H143 117.7 . . ? N4 C143 C144 124.5(3) . . ? C143 C144 H144 121.3 . . ? C143 C144 C145 117.4(3) . . ? C145 C144 H144 121.3 . . ? C144 C145 H145 120.2 . . ? C146 C145 C144 119.6(3) . . ? C146 C145 H145 120.2 . . ? C141 C146 H146 120.3 . . ? C145 C146 C141 119.4(3) . . ? C145 C146 H146 120.3 . . ? H20A C200 H20B 108.2 . . ? C201 C200 H20A 109.8 . . ? C201 C200 H20B 109.7 . . ? O1 C200 H20A 109.8 . . ? O1 C200 H20B 109.8 . . ? O1 C200 C201 109.6(3) . . ? C200 C201 H20C 110.1 . . ? C200 C201 H20D 110.1 . . ? H20C C201 H20D 108.4 . . ? O2 C201 C200 108.1(3) . . ? O2 C201 H20C 110.1 . . ? O2 C201 H20D 110.1 . . ? H20E C202 H20F 108.4 . . ? C203 C202 H20E 110.1 . . ? C203 C202 H20F 110.1 . . ? O2 C202 H20E 110.1 . . ? O2 C202 H20F 110.1 . . ? O2 C202 C203 108.2(3) . . ? C202 C203 H20G 110.0 . . ? C202 C203 H20H 110.0 . . ? H20G C203 H20H 108.4 . . ? O3 C203 C202 108.4(3) . . ? O3 C203 H20G 110.0 . . ? O3 C203 H20H 110.0 . . ? H20I C204 H20J 108.4 . . ? C205 C204 H20I 110.0 . . ? C205 C204 H20J 110.0 . . ? C205 C204 K1 84.4(2) . . ? O3 C204 H20I 110.0 . . ? O3 C204 H20J 110.0 . . ? O3 C204 C205 108.3(3) . . ? O3 C204 K1 51.06(16) . . ? K1 C204 H20I 77.6 . . ? K1 C204 H20J 160.2 . . ? C204 C205 H20K 109.6 . . ? C204 C205 H20L 109.6 . . ? H20K C205 H20L 108.1 . . ? O4 C205 C204 110.4(3) . . ? O4 C205 H20K 109.6 . . ? O4 C205 H20L 109.6 . . ? H20M C206 H20N 108.3 . . ? C207 C206 H20M 109.8 . . ? C207 C206 H20N 109.8 . . ? O4 C206 H20M 109.8 . . ? O4 C206 H20N 109.8 . . ? O4 C206 C207 109.3(3) . . ? C206 C207 H20O 109.8 . . ? C206 C207 H20P 109.8 . . ? H20O C207 H20P 108.2 . . ? O5 C207 C206 109.5(3) . . ? O5 C207 H20O 109.8 . . ? O5 C207 H20P 109.8 . . ? H20Q C208 H20R 108.3 . . ? C209 C208 H20Q 109.9 . . ? C209 C208 H20R 109.9 . . ? O5 C208 H20Q 109.9 . . ? O5 C208 H20R 109.9 . . ? O5 C208 C209 108.7(3) . . ? C208 C209 H20S 110.0 . . ? C208 C209 H20T 110.0 . . ? H20S C209 H20T 108.3 . . ? O6 C209 C208 108.6(3) . . ? O6 C209 H20S 110.0 . . ? O6 C209 H20T 110.0 . . ? H21A C210 H21B 108.3 . . ? C211 C210 H21A 109.9 . . ? C211 C210 H21B 109.9 . . ? O6 C210 H21A 109.9 . . ? O6 C210 H21B 109.9 . . ? O6 C210 C211 108.9(3) . . ? C210 C211 H21C 109.9 . . ? C210 C211 H21D 109.9 . . ? C210 C211 K1 85.53(19) . . ? H21C C211 H21D 108.3 . . ? O1 C211 C210 109.1(3) . . ? O1 C211 H21C 109.9 . . ? O1 C211 H21D 109.9 . . ? O1 C211 K1 49.69(15) . . ? K1 C211 H21C 158.7 . . ? K1 C211 H21D 78.5 . . ? C111 N1 C115 119.6(2) . . ? C111 N1 Fe2 121.03(16) . . ? C115 N1 Fe2 117.81(16) . . ? C121 N2 Fe2 121.63(16) . . ? C125 N2 C121 119.6(2) . . ? C125 N2 Fe2 117.25(17) . . ? C135 N3 C131 117.5(2) . . ? C143 N4 C141 117.2(3) . . ? C200 O1 C211 112.1(3) . . ? C200 O1 K1 112.1(2) . . ? C211 O1 K1 107.35(19) . . ? C201 O2 C202 113.1(3) . . ? C201 O2 K1 115.9(2) . . ? C202 O2 K1 117.4(2) . . ? C203 O3 K1 112.1(2) . . ? C204 O3 C203 112.3(3) . . ? C204 O3 K1 106.0(2) . . ? C205 O4 K1 117.2(2) . . ? C206 O4 C205 112.9(3) . . ? C206 O4 K1 116.0(2) . . ? C207 O5 C208 111.1(3) . . ? C207 O5 K1 113.8(2) . . ? C208 O5 K1 115.4(2) . . ? C209 O6 K1 118.7(2) . . ? C210 O6 C209 111.3(3) . . ? C210 O6 K1 118.6(2) . . ? Fe2 Cl2 K1 117.72(3) . . ? C114 K1 C204 102.97(8) 2_645 . ? C114 K1 C211 84.34(7) 2_645 . ? C211 K1 C204 156.63(12) . . ? O1 K1 C114 70.62(6) . 2_645 ? O1 K1 C204 139.80(10) . . ? O1 K1 C211 22.95(8) . . ? O1 K1 O3 118.84(8) . . ? O1 K1 O4 166.52(7) . . ? O1 K1 O5 112.78(7) . . ? O1 K1 O6 59.78(7) . . ? O1 K1 Cl2 96.70(5) . . ? O2 K1 C114 81.13(7) . 2_645 ? O2 K1 C204 79.16(10) . . ? O2 K1 C211 80.13(10) . . ? O2 K1 O1 60.70(8) . . ? O2 K1 O3 59.97(9) . . ? O2 K1 O4 120.06(8) . . ? O2 K1 O5 154.19(7) . . ? O2 K1 O6 120.47(8) . . ? O2 K1 Cl2 99.12(6) . . ? O3 K1 C114 87.05(7) . 2_645 ? O3 K1 C204 22.89(9) . . ? O3 K1 C211 140.03(10) . . ? O3 K1 O5 113.66(8) . . ? O3 K1 Cl2 105.75(6) . . ? O4 K1 C114 95.98(7) . 2_645 ? O4 K1 C204 42.87(10) . . ? O4 K1 C211 159.68(10) . . ? O4 K1 O3 60.09(8) . . ? O4 K1 O5 60.02(8) . . ? O4 K1 Cl2 96.40(5) . . ? O5 K1 C114 73.39(6) . 2_645 ? O5 K1 C204 102.31(10) . . ? O5 K1 C211 101.05(9) . . ? O5 K1 Cl2 106.57(5) . . ? O6 K1 C114 79.19(7) . 2_645 ? O6 K1 C204 160.17(10) . . ? O6 K1 C211 42.50(9) . . ? O6 K1 O3 165.79(7) . . ? O6 K1 O4 117.50(8) . . ? O6 K1 O5 59.01(7) . . ? O6 K1 Cl2 88.34(5) . . ? Cl2 K1 C114 165.46(5) . 2_645 ? Cl2 K1 C204 91.30(7) . . ? Cl2 K1 C211 81.40(6) . . ? C2 Fe1 C1 40.30(11) . . ? C2 Fe1 C5 67.94(11) . . ? C3 Fe1 C1 68.02(11) . . ? C3 Fe1 C2 41.11(11) . . ? C3 Fe1 C4 40.97(13) . . ? C3 Fe1 C5 68.18(12) . . ? C4 Fe1 C1 67.57(11) . . ? C4 Fe1 C2 68.75(11) . . ? C4 Fe1 C5 40.29(11) . . ? C5 Fe1 C1 39.78(11) . . ? C11 Fe1 C1 114.05(10) . . ? C11 Fe1 C2 125.40(11) . . ? C11 Fe1 C3 157.61(12) . . ? C11 Fe1 C4 161.42(11) . . ? C11 Fe1 C5 128.77(10) . . ? C11 Fe1 C12 42.81(9) . . ? C12 Fe1 C1 133.52(10) . . ? C12 Fe1 C2 167.35(11) . . ? C12 Fe1 C3 151.47(11) . . ? C12 Fe1 C4 121.64(11) . . ? C12 Fe1 C5 114.43(10) . . ? C13 Fe1 C1 176.29(10) . . ? C13 Fe1 C2 142.66(10) . . ? C13 Fe1 C3 115.68(11) . . ? C13 Fe1 C4 114.91(11) . . ? C13 Fe1 C5 140.41(11) . . ? C13 Fe1 C11 62.67(10) . . ? C13 Fe1 C12 43.00(9) . . ? C13 Fe1 C14 43.73(10) . . ? C14 Fe1 C1 135.38(11) . . ? C14 Fe1 C2 112.85(11) . . ? C14 Fe1 C3 118.48(11) . . ? C14 Fe1 C4 148.37(11) . . ? C14 Fe1 C5 171.34(11) . . ? C14 Fe1 C11 43.25(9) . . ? C14 Fe1 C12 62.81(9) . . ? N1 Fe2 Cl1 108.76(6) . . ? N1 Fe2 Cl2 111.01(6) . . ? N2 Fe2 N1 103.06(8) . . ? N2 Fe2 Cl1 108.32(6) . . ? N2 Fe2 Cl2 111.52(6) . . ? Cl2 Fe2 Cl1 113.60(3) . . ? _database_code_depnum_ccdc_archive 'CCDC 962754' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cpd_4 _audit_creation_date 2013-09-20 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:59:47, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C8 H16 O2, C34 H31 Cl4 Fe N4 Zn2, C12 H24 K O6' _chemical_formula_sum 'C54 H71 Cl4 Fe K N4 O8 Zn2' _chemical_formula_weight 1271.64 _chemical_melting_point ? _chemical_oxdiff_formula 'C46 H41 Fe K O6 N4 Zn Cl' 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' 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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 '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' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_H-M_alt 'P 1 21/m 1' _space_group_name_Hall '-P 2yb' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z' 3 '-x, -y, -z' 4 'x, -y-1/2, z' _cell_length_a 13.8686(8) _cell_length_b 14.3500(5) _cell_length_c 16.1195(7) _cell_angle_alpha 90.00 _cell_angle_beta 114.168(6) _cell_angle_gamma 90.00 _cell_volume 2926.8(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4733 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 73.2670 _cell_measurement_theta_min 3.4650 _exptl_absorpt_coefficient_mu 5.669 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.48008 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dull dark violet' _exptl_crystal_colour_lustre dull _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary violet _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1320 _exptl_crystal_size_max 0.191 _exptl_crystal_size_mid 0.098 _exptl_crystal_size_min 0.026 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_unetI/netI 0.0550 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 15832 _diffrn_reflns_theta_full 66.59 _diffrn_reflns_theta_max 66.59 _diffrn_reflns_theta_min 8.89 _diffrn_ambient_temperature 123(2) _diffrn_detector_area_resol_mean 10.3546 _diffrn_measured_fraction_theta_full 0.9927 _diffrn_measured_fraction_theta_max 0.9648 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -98.00 -2.00 0.5000 10.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 125.0000 90.0000 192 #__ type_ start__ end____ width___ exp.time_ 2 omega -25.00 67.00 0.5000 10.0000 omega____ theta____ kappa____ phi______ frames - 41.2064 -37.0000 -90.0000 184 #__ type_ start__ end____ width___ exp.time_ 3 omega 32.00 73.00 0.5000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -45.0000 30.0000 82 #__ type_ start__ end____ width___ exp.time_ 4 omega 29.00 69.00 0.5000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -30.0000 90.0000 80 #__ type_ start__ end____ width___ exp.time_ 5 omega 93.00 154.00 0.5000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 45.0000 -120.0000 122 #__ type_ start__ end____ width___ exp.time_ 6 omega 77.00 153.00 0.5000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 30.0000 -60.0000 152 #__ type_ start__ end____ width___ exp.time_ 7 omega 32.00 141.00 0.5000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -77.0000 -150.0000 218 #__ type_ start__ end____ width___ exp.time_ 8 omega 80.00 158.00 0.5000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 90.0000 -31.0000 156 #__ type_ start__ end____ width___ exp.time_ 9 omega 41.00 68.00 0.5000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -45.0000 -30.0000 54 #__ type_ start__ end____ width___ exp.time_ 10 omega 12.00 115.00 0.5000 10.0000 omega____ theta____ kappa____ phi______ frames - 41.2064 57.0000 60.0000 206 #__ type_ start__ end____ width___ exp.time_ 11 omega 12.00 115.00 0.5000 10.0000 omega____ theta____ kappa____ phi______ frames - 41.2064 57.0000 -120.0000 206 #__ type_ start__ end____ width___ exp.time_ 12 omega 46.00 158.00 0.5000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 15.0000 -180.0000 224 #__ type_ start__ end____ width___ exp.time_ 13 omega 76.00 158.00 0.5000 50.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 30.0000 60.0000 164 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0113926000 _diffrn_orient_matrix_UB_12 -0.0021657000 _diffrn_orient_matrix_UB_13 -0.0991442000 _diffrn_orient_matrix_UB_21 -0.0497018000 _diffrn_orient_matrix_UB_22 0.0979994000 _diffrn_orient_matrix_UB_23 -0.0156038000 _diffrn_orient_matrix_UB_31 0.1105797000 _diffrn_orient_matrix_UB_32 0.0437559000 _diffrn_orient_matrix_UB_33 0.0301101000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4027 _reflns_number_total 5331 _reflns_odcompleteness_completeness 99.27 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2\s(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 1.910 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.104 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 366 _refine_ls_number_reflns 5331 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_gt 0.0654 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+6.4409P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1678 _refine_ls_wR_factor_ref 0.1864 _refine_special_details ; A THF molecule coordinate to K1 was partially disordered over two sites. The disorder was refined using a split model. Restraints (SADI, DFIX, and SIMU) were used to obtain a reasonable geometry and reasonable adps on some of the atoms affected by this disorder (O4, C401, C402, C403). Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _olex2_refinement_description ; 1. Others Fixed Sof: O4(0.5) C400(0.5) H11E(0.5) H11F(0.5) C401(0.5) H11H(0.5) C402(0.5) H11C(0.5) H11D(0.5) C403(0.5) H11A(0.5) H11B(0.5) H6A(0.5) H6B(0.5) H6C(0.5) O1(0.67) O2(0.67) O3(0.67) C201(0.67) H10A(0.67) H10B(0.67) C202(0.67) H10C(0.67) H10D(0.67) C203(0.67) H10E(0.67) H10F(0.67) C204(0.67) H10G(0.67) H10H(0.67) C205(0.67) H10I(0.67) H10J(0.67) C206(0.67) H10K(0.67) H10L(0.67) O11(0.33) O12(0.33) O13(0.33) C221(0.33) H12A(0.33) H12B(0.33) C222(0.33) H12C(0.33) H12D(0.33) C223(0.33) H12E(0.33) H12F(0.33) C224(0.33) H12X(0.33) H12Y(0.33) C225(0.33) H12G(0.33) H12H(0.33) C226(0.33) H12I(0.33) H12J(0.33) Fixed U12: C3(0) C6(0) Cl1(0) Cl2(0) Cl3(0) Cl4(0) Fe1(0) Zn1(0) Zn2(0) O5(0) Fixed U23: C3(0) C6(0) Cl1(0) Cl2(0) Cl3(0) Cl4(0) Fe1(0) Zn1(0) Zn2(0) O5(0) Fixed Uiso: H11E(0.103) H11F(0.103) H11G(0.132) H11H(0.132) H11C(0.155) H11D(0.155) H11A(0.196) H11B(0.196) H4A(0.081) H4B(0.081) H4C(0.081) H5A(0.078) H5B(0.078) H5C(0.078) H6A(0.077) H6B(0.077) H6C(0.077) H72(0.042) H73(0.052) H74(0.058) H75(0.046) H82(0.045) H83(0.057) H84(0.054) H85(0.051) H10A(0.058) H10B(0.058) H10C(0.103) H10D(0.103) H10E(0.079) H10F(0.079) H10G(0.09) H10H(0.09) H10I(0.097) H10J(0.097) H10K(0.069) H10L(0.069) H12A(0.061) H12B(0.061) H12C(0.061) H12D(0.061) H12E(0.045) H12F(0.045) H12X(0.032) H12Y(0.032) H12G(0.035) H12H(0.035) H12I(0.041) H12J(0.041) H20A(0.157) H20B(0.157) H20C(0.152) H20D(0.152) Fixed X: H11E(0.1564) H11F(0.0626) H11G(0.1081) H11H(0.1247) H11C(-0.045) H11D(-0.0673) H11A(-0.1185) H11B(-0.1025) H4A(0.6763) H4B(0.7635) H4C(0.6703) H5A(0.557) H5B(0.4408) H5C(0.5211) H6A(0.3898) H6B(0.3457) H6C(0.4214) H72(0.7304) H73(0.8208) H74(0.9903) H75(1.0622) H82(0.7908) H83(0.7157) H84(0.5465) H85(0.4664) K1(0) H10A(0.1961) H10B(0.2252) H10C(0.0507) H10D(0.0653) H10E(-0.117) H10F(-0.127) H10G(-0.2641) H10H(-0.1958) H10I(- 0.2876) H10J(-0.3426) H10K(0.3262) H10L(0.2958) H12A(0.3366) H12B(0.2371) H12C(0.2462) H12D(0.2326) H12E(0.0779) H12F(0.0862) H12X(-0.0905) H12Y(- 0.1024) H12G(-0.243) H12H(-0.2308) H12I(-0.3378) H12J(-0.2455) H20A(0.4384) H20B(0.3462) H20C(0.555) H20D(0.46) Fixed Y: H11E(0.3543) H11F(0.3886) H11G(0.2498) H11H(0.1994) H11C(0.1601) H11D(0.2421) H11A(0.3309) H11B(0.2478) C3(0.25) H4A(0.4241) H4B(0.3466) H4C(0.3465) H5A(0.4714) H5B(0.4379) H5C(0.4441) C6(0.25) H6A(0.3128) H6B(0.2238) H6C(0.2134) H72(0.4722) H73(0.5865) H74(0.5564) H75(0.4132) H82(0.4649) H83(0.5935) H84(0.5812) H85(0.4377) Cl1(0.25) Cl2(0.25) Cl3(0.25) Cl4(0.25) Fe1(0.25) Zn1(0.25) Zn2(0.25) K1(0.5) H10A(0.5657) H10B(0.6678) H10C(0.7092) H10D(0.6615) H10E(0.634) H10F(0.6794) H10G(0.5899) H10H(0.507) H10I(0.4156) H10J(0.508) H10K(0.6082) H10L(0.507) H12A(0.6024) H12B(0.6662) H12C(0.6207) H12D(0.5158) H12E(0.5217) H12F(0.6296) H12X(0.6504) H12Y(0.5885) H12G(0.5192) H12H(0.5889) H12I(0.4562) H12J(0.3874) O5(0.25) H20A(0.3275) H20B(0.3275) H20C(0.352) H20D(0.3801) Fixed Z: H11E(0.4076) H11F(0.318) H11G(0.2715) H11H(0.3639) H11C(0.2906) H11D(0.2196) H11A(0.3023) H11B(0.3699) H4A(1.0752) H4B(1.1101) H4C(1.1414) H5A(0.9462) H5B(0.8892) H5C(0.8437) H6A(0.7609) H6B(0.7899) H6C(0.7401) H72(0.9247) H73(1.0277) H74(1.1361) H75(1.1389) H82(0.8056) H83(0.7154) H84(0.6) H85(0.5714) K1(0.5) H10A(0.3884) H10B(0.4248) H10C(0.3736) H10D(0.2922) H10E(0.2266) H10F(0.3108) H10G(0.2472) H10H(0.2382) H10I(0.3177) H10J(0.3259) H10K(0.5696) H10L(0.5319) H12A(0.574) H12B(0.5551) H12C(0.4105) H12D(0.4329) H12E(0.3012) H12F(0.2889) H12X(0.2954) H12Y(0.2112) H12G(0.2141) H12H(0.2928) H12I(0.3009) H12J(0.3105) H20A(0.0496) H20B(0.083) H20C(0.1828) H20D(0.2076) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O4 O 0.0161(7) 0.3326(6) 0.4066(6) 0.057(2) Uani 0.50 1 d PD A -1 C400 C 0.0856(13) 0.3399(12) 0.3636(11) 0.086(5) Uani 0.50 1 d PDU A -1 H11E H 0.1564 0.3543 0.4076 0.103 Uiso 0.50 1 calc PR A -1 H11F H 0.0626 0.3886 0.3180 0.103 Uiso 0.50 1 calc PR A -1 C401 C 0.0834(12) 0.2456(16) 0.3197(11) 0.110(6) Uani 0.50 1 d PDU A -1 H11G H 0.1081 0.2498 0.2715 0.132 Uiso 1 2 calc SR A -1 H11H H 0.1247 0.1994 0.3639 0.132 Uiso 0.50 1 calc PR A -1 C402 C -0.0320(14) 0.2254(15) 0.2833(13) 0.129(9) Uani 0.50 1 d PDU A -1 H11C H -0.0450 0.1601 0.2906 0.155 Uiso 0.50 1 calc PR A -1 H11D H -0.0673 0.2421 0.2196 0.155 Uiso 0.50 1 calc PR A -1 C403 C -0.0676(13) 0.2859(18) 0.3408(16) 0.163(12) Uani 0.50 1 d PDU A -1 H11A H -0.1185 0.3309 0.3023 0.196 Uiso 0.50 1 calc PR A -1 H11B H -0.1025 0.2478 0.3699 0.196 Uiso 1 2 calc SR A -1 C1 C 0.6254(4) 0.2994(4) 1.0115(4) 0.0421(13) Uani 1 1 d . . . C2 C 0.5467(4) 0.3309(4) 0.9263(4) 0.0398(12) Uani 1 1 d . . . C3 C 0.4988(6) 0.2500 0.8726(5) 0.0402(17) Uani 1 2 d S . . C4 C 0.6897(5) 0.3596(5) 1.0919(4) 0.0539(16) Uani 1 1 d . . . H4A H 0.6763 0.4241 1.0752 0.081 Uiso 1 1 calc R . . H4B H 0.7635 0.3466 1.1101 0.081 Uiso 1 1 calc R . . H4C H 0.6703 0.3465 1.1414 0.081 Uiso 1 1 calc R . . C5 C 0.5134(5) 0.4301(5) 0.8989(5) 0.0522(15) Uani 1 1 d . . . H5A H 0.5570 0.4714 0.9462 0.078 Uiso 1 1 calc R . . H5B H 0.4408 0.4379 0.8892 0.078 Uiso 1 1 calc R . . H5C H 0.5211 0.4441 0.8437 0.078 Uiso 1 1 calc R . . C6 C 0.4056(7) 0.2500 0.7828(6) 0.051(2) Uani 1 2 d S . . H6A H 0.3898 0.3128 0.7609 0.077 Uiso 0.50 1 calc PR . . H6B H 0.3457 0.2238 0.7899 0.077 Uiso 0.50 1 calc PR . . H6C H 0.4214 0.2134 0.7401 0.077 Uiso 0.50 1 calc PR . . C7 C 0.7926(4) 0.3010(3) 0.9046(3) 0.0273(10) Uani 1 1 d . . . C8 C 0.7071(4) 0.3019(3) 0.8122(3) 0.0291(10) Uani 1 1 d . . . C71 C 0.8466(4) 0.3747(3) 0.9688(3) 0.0287(10) Uani 1 1 d . . . C72 C 0.7987(4) 0.4609(3) 0.9675(3) 0.0350(11) Uani 1 1 d . . . H72 H 0.7304 0.4722 0.9247 0.042 Uiso 1 1 calc R . . C73 C 0.8523(4) 0.5288(4) 1.0293(4) 0.0437(13) Uani 1 1 d . . . H73 H 0.8208 0.5865 1.0277 0.052 Uiso 1 1 calc R . . C74 C 0.9529(5) 0.5112(4) 1.0938(4) 0.0480(15) Uani 1 1 d . . . H74 H 0.9903 0.5564 1.1361 0.058 Uiso 1 1 calc R . . C75 C 0.9957(4) 0.4263(4) 1.0939(3) 0.0383(12) Uani 1 1 d . . . H75 H 1.0622 0.4132 1.1389 0.046 Uiso 1 1 calc R . . C81 C 0.6658(4) 0.3774(4) 0.7469(3) 0.0316(11) Uani 1 1 d . . . C82 C 0.7228(5) 0.4610(4) 0.7599(3) 0.0379(12) Uani 1 1 d . . . H82 H 0.7908 0.4649 0.8056 0.045 Uiso 1 1 calc R . . C83 C 0.6787(5) 0.5376(4) 0.7053(4) 0.0471(14) Uani 1 1 d . . . H83 H 0.7157 0.5935 0.7154 0.057 Uiso 1 1 calc R . . C84 C 0.5795(5) 0.5301(4) 0.6358(4) 0.0453(14) Uani 1 1 d . . . H84 H 0.5465 0.5812 0.6000 0.054 Uiso 1 1 calc R . . C85 C 0.5310(5) 0.4442(4) 0.6212(3) 0.0423(13) Uani 1 1 d . . . H85 H 0.4664 0.4377 0.5714 0.051 Uiso 1 1 calc R . . N1 N 0.9462(3) 0.3594(3) 1.0313(3) 0.0283(8) Uani 1 1 d . . . N2 N 0.5711(3) 0.3691(3) 0.6744(3) 0.0351(10) Uani 1 1 d . . . Cl1 Cl 1.18495(15) 0.2500 1.14364(14) 0.0450(5) Uani 1 2 d S . . Cl2 Cl 1.04549(17) 0.2500 0.88751(12) 0.0389(4) Uani 1 2 d S . . Cl3 Cl 0.56214(17) 0.2500 0.49302(12) 0.0414(4) Uani 1 2 d S . . Cl4 Cl 0.33098(18) 0.2500 0.54624(17) 0.0693(7) Uani 1 2 d S . . Fe1 Fe 0.65658(9) 0.2500 0.90276(7) 0.0292(3) Uani 1 2 d S . . Zn1 Zn 1.03153(7) 0.2500 1.02095(6) 0.0291(2) Uani 1 2 d S . . Zn2 Zn 0.50633(8) 0.2500 0.60759(6) 0.0370(3) Uani 1 2 d S . . K1 K 0.0000 0.5000 0.5000 0.0527(5) Uani 1 2 d S . . O1 O 0.1786(6) 0.5906(6) 0.4983(5) 0.0679(19) Uiso 0.67 1 d P B 1 O2 O -0.0116(5) 0.5914(5) 0.3421(4) 0.0507(15) Uiso 0.67 1 d P B 1 O3 O -0.1940(5) 0.5213(4) 0.3552(4) 0.0476(14) Uiso 0.67 1 d P B 1 C201 C 0.1751(8) 0.6176(7) 0.4159(6) 0.048(2) Uiso 0.67 1 d P B 1 H10A H 0.1961 0.5657 0.3884 0.058 Uiso 0.67 1 calc PR B 1 H10B H 0.2252 0.6678 0.4248 0.058 Uiso 0.67 1 calc PR B 1 C202 C 0.0653(11) 0.6503(11) 0.3515(10) 0.086(4) Uiso 0.67 1 d P B 1 H10C H 0.0507 0.7092 0.3736 0.103 Uiso 0.67 1 calc PR B 1 H10D H 0.0653 0.6615 0.2922 0.103 Uiso 0.67 1 calc PR B 1 C203 C -0.1139(10) 0.6212(9) 0.2867(8) 0.066(3) Uiso 0.67 1 d P B 1 H10E H -0.1170 0.6340 0.2266 0.079 Uiso 0.67 1 calc PR B 1 H10F H -0.1270 0.6794 0.3108 0.079 Uiso 0.67 1 calc PR B 1 C204 C -0.1972(12) 0.5577(11) 0.2775(10) 0.075(4) Uiso 0.67 1 d P B 1 H10G H -0.2641 0.5899 0.2472 0.090 Uiso 0.67 1 calc PR B 1 H10H H -0.1958 0.5070 0.2382 0.090 Uiso 0.67 1 calc PR B 1 C205 C -0.2794(12) 0.4705(11) 0.3551(10) 0.081(4) Uiso 0.67 1 d P . 1 H10I H -0.2876 0.4156 0.3177 0.097 Uiso 0.67 1 calc PR . 1 H10J H -0.3426 0.5080 0.3259 0.097 Uiso 0.67 1 calc PR . 1 C206 C 0.2747(9) 0.5589(9) 0.5593(7) 0.057(3) Uiso 0.67 1 d P . 1 H10K H 0.3262 0.6082 0.5696 0.069 Uiso 0.67 1 calc PR . 1 H10L H 0.2958 0.5070 0.5319 0.069 Uiso 0.67 1 calc PR . 1 O11 O 0.2179(10) 0.5375(8) 0.5821(8) 0.040(3) Uiso 0.33 1 d P . 2 O12 O 0.1012(10) 0.5931(8) 0.4062(8) 0.044(3) Uiso 0.33 1 d P B 2 O13 O -0.1079(9) 0.5199(8) 0.3113(7) 0.039(2) Uiso 0.33 1 d P B 2 C221 C 0.2600(17) 0.6046(16) 0.5462(14) 0.051(5) Uiso 0.33 1 d P B 2 H12A H 0.3366 0.6024 0.5740 0.061 Uiso 0.33 1 calc PR B 2 H12B H 0.2371 0.6662 0.5551 0.061 Uiso 0.33 1 calc PR B 2 C222 C 0.2159(16) 0.5798(15) 0.4413(13) 0.051(5) Uiso 0.33 1 d P B 2 H12C H 0.2462 0.6207 0.4105 0.061 Uiso 0.33 1 calc PR B 2 H12D H 0.2326 0.5158 0.4329 0.061 Uiso 0.33 1 calc PR B 2 C223 C 0.0589(13) 0.5823(12) 0.3166(11) 0.037(3) Uiso 0.33 1 d P B 2 H12E H 0.0779 0.5217 0.3012 0.045 Uiso 0.33 1 calc PR B 2 H12F H 0.0862 0.6296 0.2889 0.045 Uiso 0.33 1 calc PR B 2 C224 C -0.0714(12) 0.5913(10) 0.2771(9) 0.027(3) Uiso 0.33 1 d P B 2 H12X H -0.0905 0.6504 0.2954 0.032 Uiso 0.33 1 calc PR B 2 H12Y H -0.1024 0.5885 0.2112 0.032 Uiso 0.33 1 calc PR B 2 C225 C -0.2124(14) 0.5272(13) 0.2796(11) 0.029(4) Uiso 0.33 1 d P B 2 H12G H -0.2430 0.5192 0.2141 0.035 Uiso 0.33 1 calc PR B 2 H12H H -0.2308 0.5889 0.2928 0.035 Uiso 0.33 1 calc PR B 2 C226 C -0.2616(14) 0.4496(12) 0.3249(11) 0.034(3) Uiso 0.33 1 d P . 2 H12I H -0.3378 0.4562 0.3009 0.041 Uiso 0.33 1 calc PR . 2 H12J H -0.2455 0.3874 0.3105 0.041 Uiso 0.33 1 calc PR . 2 O5 O 0.5053(18) 0.2500 0.2366(12) 0.203(8) Uani 1 2 d S . 2 C301 C 0.4163(8) 0.3037(10) 0.0954(7) 0.131(6) Uani 1 1 d . . 2 H20A H 0.4384 0.3275 0.0496 0.157 Uiso 1 1 calc R . 2 H20B H 0.3462 0.3275 0.0830 0.157 Uiso 1 1 calc R . 2 C302 C 0.4891(13) 0.3306(8) 0.1839(7) 0.127(5) Uani 1 1 d . . 2 H20C H 0.5550 0.3520 0.1828 0.152 Uiso 1 1 calc R . 2 H20D H 0.4600 0.3801 0.2076 0.152 Uiso 1 1 calc R . 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 O4 0.058(6) 0.052(5) 0.056(5) 0.000(4) 0.018(5) -0.007(4) C400 0.094(13) 0.085(12) 0.075(10) 0.003(9) 0.031(10) 0.012(10) C401 0.112(12) 0.129(14) 0.083(9) -0.050(17) 0.033(9) 0.02(2) C402 0.146(16) 0.15(2) 0.083(11) -0.017(13) 0.038(12) 0.030(17) C403 0.20(2) 0.16(3) 0.120(17) -0.018(16) 0.047(18) 0.05(2) C1 0.033(3) 0.061(3) 0.032(3) -0.008(2) 0.013(2) 0.001(3) C2 0.029(3) 0.052(3) 0.038(3) -0.005(2) 0.013(2) 0.006(2) C3 0.034(4) 0.050(4) 0.037(4) 0.000 0.014(3) 0.000 C4 0.043(3) 0.078(4) 0.038(3) -0.016(3) 0.015(3) -0.004(3) C5 0.042(3) 0.057(4) 0.057(4) -0.002(3) 0.018(3) 0.016(3) C6 0.033(4) 0.069(6) 0.044(4) 0.000 0.006(4) 0.000 C7 0.026(2) 0.028(2) 0.027(2) -0.0002(19) 0.0100(19) 0.003(2) C8 0.025(2) 0.030(3) 0.028(2) -0.0032(19) 0.0065(19) -0.002(2) C71 0.027(2) 0.031(2) 0.025(2) 0.0005(19) 0.0066(19) -0.001(2) C72 0.030(3) 0.032(2) 0.036(3) 0.001(2) 0.006(2) 0.003(2) C73 0.035(3) 0.034(3) 0.049(3) -0.006(2) 0.005(3) 0.005(2) C74 0.039(3) 0.033(3) 0.053(3) -0.016(3) 0.000(3) 0.000(2) C75 0.032(3) 0.037(3) 0.032(2) -0.004(2) -0.001(2) 0.003(2) C81 0.029(3) 0.037(3) 0.024(2) 0.002(2) 0.007(2) 0.007(2) C82 0.040(3) 0.037(3) 0.031(2) 0.006(2) 0.009(2) -0.002(2) C83 0.057(4) 0.039(3) 0.036(3) 0.005(2) 0.009(3) -0.001(3) C84 0.057(4) 0.039(3) 0.034(3) 0.010(2) 0.013(3) 0.010(3) C85 0.042(3) 0.046(3) 0.028(2) 0.004(2) 0.004(2) 0.010(3) N1 0.026(2) 0.0285(19) 0.0258(18) -0.0005(16) 0.0061(16) -0.0024(17) N2 0.034(2) 0.039(2) 0.0248(19) -0.0039(17) 0.0044(18) 0.0033(19) Cl1 0.0279(9) 0.0451(10) 0.0486(10) 0.000 0.0019(8) 0.000 Cl2 0.0567(12) 0.0287(8) 0.0377(9) 0.000 0.0260(9) 0.000 Cl3 0.0520(12) 0.0378(9) 0.0318(8) 0.000 0.0145(8) 0.000 Cl4 0.0308(11) 0.107(2) 0.0525(12) 0.000 -0.0004(9) 0.000 Fe1 0.0235(6) 0.0350(6) 0.0248(5) 0.000 0.0056(4) 0.000 Zn1 0.0260(5) 0.0298(5) 0.0290(5) 0.000 0.0085(4) 0.000 Zn2 0.0304(5) 0.0422(5) 0.0292(5) 0.000 0.0028(4) 0.000 K1 0.0370(9) 0.0786(13) 0.0343(8) 0.0146(9) 0.0063(7) -0.0108(9) O5 0.27(2) 0.189(18) 0.148(14) 0.000 0.082(15) 0.000 C301 0.076(6) 0.228(16) 0.105(7) 0.080(9) 0.054(6) 0.054(8) C302 0.211(15) 0.081(7) 0.077(6) -0.007(5) 0.049(8) 0.037(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O4 C400 1.402(9) . ? O4 C403 1.383(10) . ? O4 K1 2.892(9) . ? C400 H11E 0.9700 . ? C400 H11F 0.9700 . ? C400 C401 1.522(10) . ? C401 H11G 0.9700 . ? C401 H11H 0.9700 . ? C401 C402 1.491(10) . ? C402 H11C 0.9700 . ? C402 H11D 0.9700 . ? C402 C403 1.493(9) . ? C403 H11A 0.9700 . ? C403 H11B 0.9700 . ? C1 C1 1.417(13) 4_565 ? C1 C2 1.434(8) . ? C1 C4 1.508(8) . ? C1 Fe1 2.094(5) . ? C2 C3 1.438(7) . ? C2 C5 1.506(9) . ? C2 Fe1 2.071(6) . ? C3 C2 1.438(7) 4_565 ? C3 C6 1.494(11) . ? C3 Fe1 2.037(8) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C7 1.464(9) 4_565 ? C7 C8 1.476(6) . ? C7 C71 1.454(7) . ? C7 Fe1 2.013(5) . ? C8 C8 1.490(10) 4_565 ? C8 C81 1.454(7) . ? C8 Fe1 2.004(5) . ? C71 C72 1.400(7) . ? C71 N1 1.354(6) . ? C72 H72 0.9300 . ? C72 C73 1.374(8) . ? C73 H73 0.9300 . ? C73 C74 1.380(8) . ? C74 H74 0.9300 . ? C74 C75 1.356(8) . ? C75 H75 0.9300 . ? C75 N1 1.357(6) . ? C81 C82 1.404(8) . ? C81 N2 1.359(6) . ? C82 H82 0.9300 . ? C82 C83 1.385(8) . ? C83 H83 0.9300 . ? C83 C84 1.377(8) . ? C84 H84 0.9300 . ? C84 C85 1.378(9) . ? C85 H85 0.9300 . ? C85 N2 1.349(7) . ? N1 Zn1 2.013(4) . ? N2 Zn2 2.023(4) . ? Cl1 Zn1 2.234(2) . ? Cl2 Zn1 2.2371(19) . ? Cl3 Zn2 2.276(2) . ? Cl4 Zn2 2.219(2) . ? Fe1 C1 2.094(5) 4_565 ? Fe1 C2 2.071(6) 4_565 ? Fe1 C7 2.013(5) 4_565 ? Fe1 C8 2.004(5) 4_565 ? Zn1 N1 2.013(4) 4_565 ? Zn2 N2 2.023(4) 4_565 ? K1 O1 2.807(8) . ? K1 O1 2.807(8) 3_566 ? K1 O2 2.808(6) 3_566 ? K1 O2 2.808(6) . ? K1 O3 2.764(6) . ? K1 O3 2.764(6) 3_566 ? K1 O11 2.811(12) . ? K1 O11 2.811(12) 3_566 ? K1 O12 2.789(13) . ? K1 O12 2.789(13) 3_566 ? K1 O13 2.801(11) . ? K1 O13 2.801(11) 3_566 ? O1 C201 1.366(12) . ? O1 C206 1.370(13) . ? O2 C202 1.320(15) . ? O2 C203 1.399(13) . ? O3 C204 1.341(15) . ? O3 C205 1.391(15) . ? C201 H10A 0.9700 . ? C201 H10B 0.9700 . ? C201 C202 1.524(17) . ? C202 H10C 0.9700 . ? C202 H10D 0.9700 . ? C203 H10E 0.9700 . ? C203 H10F 0.9700 . ? C203 C204 1.430(19) . ? C204 H10G 0.9700 . ? C204 H10H 0.9700 . ? C205 H10I 0.9700 . ? C205 H10J 0.9700 . ? C205 C206 1.418(18) 3_566 ? C206 C205 1.418(18) 3_566 ? C206 H10K 0.9700 . ? C206 H10L 0.9700 . ? O11 C221 1.37(2) . ? O11 C226 1.38(2) 3_566 ? O12 C222 1.47(2) . ? O12 C223 1.33(2) . ? O13 C224 1.356(18) . ? O13 C225 1.33(2) . ? C221 H12A 0.9700 . ? C221 H12B 0.9700 . ? C221 C222 1.58(3) . ? C222 H12C 0.9700 . ? C222 H12D 0.9700 . ? C223 H12E 0.9700 . ? C223 H12F 0.9700 . ? C223 C224 1.66(2) . ? C224 H12X 0.9700 . ? C224 H12Y 0.9700 . ? C225 H12G 0.9700 . ? C225 H12H 0.9700 . ? C225 C226 1.63(2) . ? C226 O11 1.38(2) 3_566 ? C226 H12I 0.9700 . ? C226 H12J 0.9700 . ? O5 C302 1.398(13) . ? O5 C302 1.398(13) 4_565 ? C301 C301 1.54(3) 4_565 ? C301 H20A 0.9700 . ? C301 H20B 0.9700 . ? C301 C302 1.423(15) . ? C302 H20C 0.9700 . ? C302 H20D 0.9700 . ? 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 C400 O4 K1 114.2(8) . . ? C403 O4 C400 100.8(14) . . ? C403 O4 K1 125.6(10) . . ? O4 C400 H11E 110.5 . . ? O4 C400 H11F 110.5 . . ? O4 C400 C401 106.1(11) . . ? H11E C400 H11F 108.7 . . ? C401 C400 H11E 110.5 . . ? C401 C400 H11F 110.5 . . ? C400 C401 H11G 111.8 . . ? C400 C401 H11H 111.8 . . ? H11G C401 H11H 109.6 . . ? C402 C401 C400 99.7(8) . . ? C402 C401 H11G 111.8 . . ? C402 C401 H11H 111.8 . . ? C401 C402 H11C 111.3 . . ? C401 C402 H11D 111.3 . . ? C401 C402 C403 102.6(6) . . ? H11C C402 H11D 109.2 . . ? C403 C402 H11C 111.3 . . ? C403 C402 H11D 111.3 . . ? O4 C403 C402 111.8(11) . . ? O4 C403 H11A 109.3 . . ? O4 C403 H11B 109.3 . . ? C402 C403 H11A 109.3 . . ? C402 C403 H11B 109.3 . . ? H11A C403 H11B 107.9 . . ? C1 C1 C2 108.4(3) 4_565 . ? C1 C1 C4 125.0(4) 4_565 . ? C1 C1 Fe1 70.22(18) 4_565 . ? C2 C1 C4 126.4(6) . . ? C2 C1 Fe1 69.0(3) . . ? C4 C1 Fe1 131.3(4) . . ? C1 C2 C3 107.8(5) . . ? C1 C2 C5 127.0(5) . . ? C1 C2 Fe1 70.7(3) . . ? C3 C2 C5 125.2(5) . . ? C3 C2 Fe1 68.3(4) . . ? C5 C2 Fe1 129.5(4) . . ? C2 C3 C2 107.7(7) . 4_565 ? C2 C3 C6 125.9(3) 4_565 . ? C2 C3 C6 125.9(3) . . ? C2 C3 Fe1 70.8(4) 4_565 . ? C2 C3 Fe1 70.8(4) . . ? C6 C3 Fe1 130.5(6) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C7 C7 C8 90.5(3) 4_565 . ? C7 C7 Fe1 68.67(13) 4_565 . ? C8 C7 Fe1 68.2(3) . . ? C71 C7 C7 136.6(3) . 4_565 ? C71 C7 C8 132.7(4) . . ? C71 C7 Fe1 118.7(3) . . ? C7 C8 C8 89.5(3) . 4_565 ? C7 C8 Fe1 68.7(3) . . ? C8 C8 Fe1 68.18(14) 4_565 . ? C81 C8 C7 130.7(4) . . ? C81 C8 C8 138.1(3) . 4_565 ? C81 C8 Fe1 130.7(4) . . ? C72 C71 C7 121.9(4) . . ? N1 C71 C7 118.9(4) . . ? N1 C71 C72 119.2(4) . . ? C71 C72 H72 119.9 . . ? C73 C72 C71 120.3(5) . . ? C73 C72 H72 119.9 . . ? C72 C73 H73 120.1 . . ? C72 C73 C74 119.7(5) . . ? C74 C73 H73 120.1 . . ? C73 C74 H74 120.9 . . ? C75 C74 C73 118.2(5) . . ? C75 C74 H74 120.9 . . ? C74 C75 H75 118.4 . . ? C74 C75 N1 123.2(5) . . ? N1 C75 H75 118.4 . . ? C82 C81 C8 119.8(4) . . ? N2 C81 C8 120.8(5) . . ? N2 C81 C82 119.4(5) . . ? C81 C82 H82 119.7 . . ? C83 C82 C81 120.5(5) . . ? C83 C82 H82 119.7 . . ? C82 C83 H83 120.4 . . ? C84 C83 C82 119.3(6) . . ? C84 C83 H83 120.4 . . ? C83 C84 H84 121.1 . . ? C83 C84 C85 117.7(5) . . ? C85 C84 H84 121.1 . . ? C84 C85 H85 117.9 . . ? N2 C85 C84 124.1(5) . . ? N2 C85 H85 117.9 . . ? C71 N1 C75 119.3(4) . . ? C71 N1 Zn1 121.3(3) . . ? C75 N1 Zn1 118.5(3) . . ? C81 N2 Zn2 126.4(3) . . ? C85 N2 C81 118.6(5) . . ? C85 N2 Zn2 111.0(3) . . ? C1 Fe1 C1 39.6(4) . 4_565 ? C2 Fe1 C1 40.3(2) . . ? C2 Fe1 C1 67.4(2) 4_565 . ? C2 Fe1 C1 67.4(2) . 4_565 ? C2 Fe1 C1 40.3(2) 4_565 4_565 ? C2 Fe1 C2 68.2(3) . 4_565 ? C3 Fe1 C1 68.3(3) . 4_565 ? C3 Fe1 C1 68.3(3) . . ? C3 Fe1 C2 41.0(2) . 4_565 ? C3 Fe1 C2 41.0(2) . . ? C7 Fe1 C1 112.2(2) 4_565 4_565 ? C7 Fe1 C1 128.7(2) . 4_565 ? C7 Fe1 C1 128.7(2) 4_565 . ? C7 Fe1 C1 112.2(2) . . ? C7 Fe1 C2 123.3(2) 4_565 4_565 ? C7 Fe1 C2 163.2(2) . 4_565 ? C7 Fe1 C2 163.2(2) 4_565 . ? C7 Fe1 C2 123.3(2) . . ? C7 Fe1 C3 155.77(17) . . ? C7 Fe1 C3 155.77(17) 4_565 . ? C7 Fe1 C7 42.7(3) 4_565 . ? C8 Fe1 C1 137.6(2) 4_565 4_565 ? C8 Fe1 C1 171.8(2) . 4_565 ? C8 Fe1 C1 137.6(2) . . ? C8 Fe1 C1 171.8(2) 4_565 . ? C8 Fe1 C2 115.4(2) . . ? C8 Fe1 C2 115.4(2) 4_565 4_565 ? C8 Fe1 C2 147.7(2) 4_565 . ? C8 Fe1 C2 147.7(2) . 4_565 ? C8 Fe1 C3 119.2(2) . . ? C8 Fe1 C3 119.2(2) 4_565 . ? C8 Fe1 C7 43.12(18) 4_565 4_565 ? C8 Fe1 C7 62.64(19) . 4_565 ? C8 Fe1 C7 43.12(18) . . ? C8 Fe1 C7 62.64(19) 4_565 . ? C8 Fe1 C8 43.6(3) 4_565 . ? N1 Zn1 N1 102.5(2) 4_565 . ? N1 Zn1 Cl1 107.80(12) . . ? N1 Zn1 Cl1 107.80(12) 4_565 . ? N1 Zn1 Cl2 111.39(12) . . ? N1 Zn1 Cl2 111.39(12) 4_565 . ? Cl1 Zn1 Cl2 115.16(9) . . ? N2 Zn2 N2 115.2(2) . 4_565 ? N2 Zn2 Cl3 101.97(13) 4_565 . ? N2 Zn2 Cl3 101.97(13) . . ? N2 Zn2 Cl4 113.83(13) 4_565 . ? N2 Zn2 Cl4 113.83(13) . . ? Cl4 Zn2 Cl3 108.25(9) . . ? O1 K1 O1 180.0 . 3_566 ? O1 K1 O2 59.9(2) 3_566 3_566 ? O1 K1 O2 120.1(2) . 3_566 ? O1 K1 O2 120.1(2) 3_566 . ? O1 K1 O2 59.9(2) . . ? O1 K1 O11 150.1(3) . 3_566 ? O1 K1 O11 29.9(3) 3_566 3_566 ? O1 K1 O11 150.1(3) 3_566 . ? O1 K1 O11 29.9(3) . . ? O2 K1 O2 180.000(1) . 3_566 ? O2 K1 O11 89.4(3) 3_566 3_566 ? O2 K1 O11 89.4(3) . . ? O2 K1 O11 90.6(3) 3_566 . ? O2 K1 O11 90.6(3) . 3_566 ? O3 K1 O1 60.1(2) . 3_566 ? O3 K1 O1 119.9(2) 3_566 3_566 ? O3 K1 O1 60.1(2) 3_566 . ? O3 K1 O1 119.9(2) . . ? O3 K1 O2 119.47(19) 3_566 . ? O3 K1 O2 60.53(19) . . ? O3 K1 O2 119.47(19) . 3_566 ? O3 K1 O2 60.53(19) 3_566 3_566 ? O3 K1 O3 180.000(1) . 3_566 ? O3 K1 O11 30.3(3) . 3_566 ? O3 K1 O11 149.7(3) . . ? O3 K1 O11 30.3(3) 3_566 . ? O3 K1 O11 149.7(3) 3_566 3_566 ? O3 K1 O12 91.2(3) 3_566 3_566 ? O3 K1 O12 88.8(3) . 3_566 ? O3 K1 O12 88.8(3) 3_566 . ? O3 K1 O12 91.2(3) . . ? O3 K1 O13 33.8(3) . . ? O3 K1 O13 33.8(3) 3_566 3_566 ? O3 K1 O13 146.2(3) 3_566 . ? O3 K1 O13 146.2(3) . 3_566 ? O11 K1 O11 180.0(3) 3_566 . ? O12 K1 O1 150.3(3) 3_566 . ? O12 K1 O1 29.7(3) . . ? O12 K1 O1 150.3(3) . 3_566 ? O12 K1 O1 29.7(3) 3_566 3_566 ? O12 K1 O2 149.3(3) 3_566 . ? O12 K1 O2 149.3(3) . 3_566 ? O12 K1 O2 30.7(3) 3_566 3_566 ? O12 K1 O2 30.7(3) . . ? O12 K1 O11 58.7(4) 3_566 3_566 ? O12 K1 O11 121.3(3) . 3_566 ? O12 K1 O11 58.7(4) . . ? O12 K1 O11 121.3(4) 3_566 . ? O12 K1 O12 180.000(1) . 3_566 ? O12 K1 O13 118.3(3) 3_566 . ? O12 K1 O13 61.7(3) . . ? O12 K1 O13 61.7(3) 3_566 3_566 ? O12 K1 O13 118.3(3) . 3_566 ? O13 K1 O1 91.4(3) 3_566 3_566 ? O13 K1 O1 88.6(3) . 3_566 ? O13 K1 O1 91.4(3) . . ? O13 K1 O1 88.6(3) 3_566 . ? O13 K1 O2 147.0(3) . 3_566 ? O13 K1 O2 33.0(3) . . ? O13 K1 O2 147.0(3) 3_566 . ? O13 K1 O2 33.0(3) 3_566 3_566 ? O13 K1 O11 61.0(3) . 3_566 ? O13 K1 O11 119.0(3) 3_566 3_566 ? O13 K1 O11 61.0(3) 3_566 . ? O13 K1 O11 119.0(3) . . ? O13 K1 O13 180.000(2) . 3_566 ? C201 O1 K1 117.4(6) . . ? C201 O1 C206 115.4(9) . . ? C206 O1 K1 116.3(7) . . ? C202 O2 K1 116.8(7) . . ? C202 O2 C203 116.0(9) . . ? C203 O2 K1 112.9(6) . . ? C204 O3 K1 118.7(8) . . ? C204 O3 C205 120.1(10) . . ? C205 O3 K1 118.5(7) . . ? O1 C201 H10A 109.2 . . ? O1 C201 H10B 109.2 . . ? O1 C201 C202 112.2(10) . . ? H10A C201 H10B 107.9 . . ? C202 C201 H10A 109.2 . . ? C202 C201 H10B 109.2 . . ? O2 C202 C201 114.6(11) . . ? O2 C202 H10C 108.6 . . ? O2 C202 H10D 108.6 . . ? C201 C202 H10C 108.6 . . ? C201 C202 H10D 108.6 . . ? H10C C202 H10D 107.6 . . ? O2 C203 H10E 108.3 . . ? O2 C203 H10F 108.3 . . ? O2 C203 C204 115.9(11) . . ? H10E C203 H10F 107.4 . . ? C204 C203 H10E 108.3 . . ? C204 C203 H10F 108.3 . . ? O3 C204 C203 115.8(12) . . ? O3 C204 H10G 108.3 . . ? O3 C204 H10H 108.3 . . ? C203 C204 H10G 108.3 . . ? C203 C204 H10H 108.3 . . ? H10G C204 H10H 107.4 . . ? O3 C205 H10I 108.0 . . ? O3 C205 H10J 108.0 . . ? O3 C205 C206 117.1(12) . 3_566 ? H10I C205 H10J 107.3 . . ? C206 C205 H10I 108.0 3_566 . ? C206 C205 H10J 108.0 3_566 . ? O1 C206 C205 116.2(11) . 3_566 ? O1 C206 H10K 108.2 . . ? O1 C206 H10L 108.2 . . ? C205 C206 H10K 108.2 3_566 . ? C205 C206 H10L 108.2 3_566 . ? H10K C206 H10L 107.4 . . ? C221 O11 K1 119.8(11) . . ? C221 O11 C226 106.9(13) . 3_566 ? C226 O11 K1 116.5(10) 3_566 . ? C222 O12 K1 115.8(10) . . ? C223 O12 K1 116.0(10) . . ? C223 O12 C222 109.3(14) . . ? C224 O13 K1 113.3(9) . . ? C225 O13 K1 116.0(9) . . ? C225 O13 C224 108.4(13) . . ? O11 C221 H12A 110.9 . . ? O11 C221 H12B 110.9 . . ? O11 C221 C222 104.4(16) . . ? H12A C221 H12B 108.9 . . ? C222 C221 H12A 110.9 . . ? C222 C221 H12B 110.9 . . ? O12 C222 C221 105.5(16) . . ? O12 C222 H12C 110.6 . . ? O12 C222 H12D 110.6 . . ? C221 C222 H12C 110.6 . . ? C221 C222 H12D 110.7 . . ? H12C C222 H12D 108.8 . . ? O12 C223 H12E 109.8 . . ? O12 C223 H12F 109.8 . . ? O12 C223 C224 109.5(13) . . ? H12E C223 H12F 108.2 . . ? C224 C223 H12E 109.8 . . ? C224 C223 H12F 109.8 . . ? O13 C224 C223 108.4(12) . . ? O13 C224 H12X 110.0 . . ? O13 C224 H12Y 110.0 . . ? C223 C224 H12X 110.0 . . ? C223 C224 H12Y 110.0 . . ? H12X C224 H12Y 108.4 . . ? O13 C225 H12G 109.3 . . ? O13 C225 H12H 109.3 . . ? O13 C225 C226 111.5(14) . . ? H12G C225 H12H 108.0 . . ? C226 C225 H12G 109.3 . . ? C226 C225 H12H 109.3 . . ? O11 C226 C225 108.5(13) 3_566 . ? O11 C226 H12I 110.0 3_566 . ? O11 C226 H12J 110.0 3_566 . ? C225 C226 H12I 110.0 . . ? C225 C226 H12J 110.0 . . ? H12I C226 H12J 108.4 . . ? C302 O5 C302 111.7(15) 4_565 . ? C301 C301 H20A 110.6 4_565 . ? C301 C301 H20B 110.6 4_565 . ? H20A C301 H20B 108.7 . . ? C302 C301 C301 105.7(7) . 4_565 ? C302 C301 H20A 110.6 . . ? C302 C301 H20B 110.6 . . ? O5 C302 C301 104.8(13) . . ? O5 C302 H20C 110.8 . . ? O5 C302 H20D 110.8 . . ? C301 C302 H20C 110.8 . . ? C301 C302 H20D 110.8 . . ? H20C C302 H20D 108.9 . . ? _database_code_depnum_ccdc_archive 'CCDC 962755'