#------------------------------------------------------------------------------ #$Date: 2018-01-26 06:22:00 +0200 (Fri, 26 Jan 2018) $ #$Revision: 205686 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/54/7045408.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7045408 loop_ _publ_author_name 'Lin, Hsiu-Jung' 'Lutz, Sean' 'O'kane, Catherine' 'Zeller, Matthias' 'Chen, Chun-Hsing' 'Al Assil, Talal' 'Lee, Wei-Tsung' _publ_section_title ; Synthesis and characterization of an iron complex bearing a hemilabile NNN-pincer for catalytic hydrosilylation of organic carbonyl compounds ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C7DT04928E _journal_year 2018 _chemical_formula_sum 'C40 H62 Fe N5 O2 Si2' _chemical_formula_weight 756.97 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-01-06 deposited with the CCDC. 2018-01-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 91.099(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.3471(11) _cell_length_b 18.745(3) _cell_length_c 24.074(3) _cell_measurement_reflns_used 1568 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.2419 _cell_measurement_theta_min 2.5641 _cell_volume 4217.3(10) _computing_cell_refinement 'SAINT V8.34A (Bruker, 2014)' _computing_data_collection 'Apex2 v2014.11 (Bruker, 2014)' _computing_data_reduction 'SAINT V8.34A (Bruker, 2014)' _computing_structure_refinement ; SHELXL-2014/7 (Sheldrick, 2014), SHELXLE Rev714 (H\"ubschle et al., 2011) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measurement_device_type 'Bruker AXS D8 Quest CMOS diffractometer' _diffrn_measurement_method 'omega and phi scans' _diffrn_radiation_monochromator 'laterally graded multilayer (Goebel) mirror' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.2010 _diffrn_reflns_av_unetI/netI 0.2624 _diffrn_reflns_Laue_measured_fraction_full 0.988 _diffrn_reflns_Laue_measured_fraction_max 0.978 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 31483 _diffrn_reflns_point_group_measured_fraction_full 0.988 _diffrn_reflns_point_group_measured_fraction_max 0.978 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.296 _diffrn_reflns_theta_min 1.377 _diffrn_source 'I-mu-S microsource X-ray tube' _exptl_absorpt_coefficient_mu 0.453 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6189 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Apex2 v2014.11 (Bruker, 2014)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.192 _exptl_crystal_description block _exptl_crystal_F_000 1628 _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.070 _refine_diff_density_max 0.910 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.100 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.894 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 469 _refine_ls_number_reflns 10249 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.894 _refine_ls_R_factor_all 0.1785 _refine_ls_R_factor_gt 0.0900 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1461 _refine_ls_wR_factor_ref 0.1743 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5499 _reflns_number_total 10249 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt04928e2.cif _cod_data_source_block Quest15mz331_0m _cod_original_cell_volume 4217.3(9) _cod_database_code 7045408 _shelx_shelxl_version_number 2014/7 _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. ; _shelx_estimated_absorpt_t_min 0.948 _shelx_estimated_absorpt_t_max 0.969 _shelx_res_file ; Quest15mz331_0m.res created by SHELXL-2014/7 REM TRY 527 FINAL CC 65.23 TIME 160 SECS REM Fragments: 17 7 4 3 3 2 2 1 1 1 1 1 REM TITL Quest15mz331_0m in P2(1)/n CELL 0.71073 9.3471 18.7454 24.0736 90.000 91.099 90.000 ZERR 4.00 0.0011 0.0030 0.0025 0.000 0.006 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O FE Si UNIT 160 248 20 8 4 8 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.150 SIZE 0.07 0.11 0.12 L.S. 24 BOND $H CONF FMAP 2 PLAN 111 ACTA REM RIGU WGHT 0.000000 FVAR 0.19630 C1 1 0.373483 0.563779 0.253835 11.00000 0.01438 0.00872 = 0.01183 -0.00106 -0.00075 0.00443 AFIX 43 H1 2 0.297147 0.590950 0.268481 11.00000 -1.20000 AFIX 0 C2 1 0.444826 0.578362 0.206139 11.00000 0.01971 0.01328 = 0.00775 -0.00053 -0.00227 0.00133 AFIX 43 H2 2 0.427065 0.616398 0.180856 11.00000 -1.20000 AFIX 0 C3 1 0.550477 0.524911 0.202430 11.00000 0.01271 0.00743 = 0.00769 -0.00322 -0.00038 -0.00083 C4 1 0.665027 0.522973 0.158140 11.00000 0.01151 0.01165 = 0.00940 -0.00126 0.00258 -0.00307 C5 1 0.797971 0.482290 0.178109 11.00000 0.01671 0.01144 = 0.01731 0.00315 0.00989 0.00314 AFIX 137 H5A 2 0.773125 0.432185 0.184401 11.00000 -1.50000 H5B 2 0.834218 0.503361 0.212875 11.00000 -1.50000 H5C 2 0.871850 0.485227 0.149859 11.00000 -1.50000 AFIX 0 C6 1 0.604979 0.489613 0.104084 11.00000 0.02576 0.01782 = 0.01185 -0.00574 0.00671 -0.00591 AFIX 137 H6A 2 0.516269 0.514056 0.092983 11.00000 -1.50000 H6B 2 0.585186 0.438911 0.110216 11.00000 -1.50000 H6C 2 0.675269 0.494643 0.074652 11.00000 -1.50000 AFIX 0 C7 1 0.707410 0.600424 0.146131 11.00000 0.01641 0.01889 = 0.01938 0.00452 0.00210 -0.00076 AFIX 137 H7A 2 0.785070 0.601095 0.119360 11.00000 -1.50000 H7B 2 0.739645 0.623462 0.180705 11.00000 -1.50000 H7C 2 0.624593 0.626200 0.130657 11.00000 -1.50000 AFIX 0 C8 1 0.403941 0.403444 0.341457 11.00000 0.00722 0.00806 = 0.00881 -0.00353 0.00021 -0.00191 C9 1 0.400272 0.476774 0.330211 11.00000 0.00518 0.01234 = 0.00658 0.00111 -0.00045 -0.00001 C10 1 0.359303 0.523735 0.371122 11.00000 0.00531 0.00625 = 0.01558 -0.00423 -0.00023 -0.00038 AFIX 43 H10 2 0.358210 0.573329 0.363002 11.00000 -1.20000 AFIX 0 C11 1 0.319138 0.501215 0.424297 11.00000 0.00853 0.00655 = 0.01250 -0.00157 -0.00008 0.00061 C12 1 0.318114 0.428771 0.435308 11.00000 0.00443 0.01826 = 0.00660 -0.00347 -0.00092 -0.00037 AFIX 43 H12 2 0.289368 0.411835 0.470574 11.00000 -1.20000 AFIX 0 C13 1 0.359662 0.380516 0.394211 11.00000 0.00654 0.01014 = 0.01003 0.00313 -0.00015 0.00142 C14 1 0.370185 0.304172 0.393184 11.00000 0.00739 0.01257 = 0.01198 -0.00077 -0.00103 -0.00185 C15 1 0.338247 0.251772 0.431700 11.00000 0.01320 0.01373 = 0.00859 -0.00203 0.00228 0.00189 AFIX 43 H15 2 0.301936 0.264925 0.466837 11.00000 -1.20000 AFIX 0 C16 1 0.359044 0.180011 0.419216 11.00000 0.01051 0.01254 = 0.01151 0.00180 -0.00218 -0.00082 C17 1 0.414441 0.162956 0.366944 11.00000 0.01376 0.00615 = 0.01221 -0.00259 -0.00187 -0.00025 AFIX 43 H17 2 0.430929 0.114266 0.358185 11.00000 -1.20000 AFIX 0 C18 1 0.446154 0.214930 0.327396 11.00000 0.00525 0.01429 = 0.01172 0.00120 0.00243 -0.00158 C19 1 0.422183 0.286846 0.339703 11.00000 0.00398 0.01072 = 0.00561 0.00039 0.00104 -0.00073 C20 1 0.273137 0.556364 0.467488 11.00000 0.01215 0.00901 = 0.01302 -0.00508 0.00317 -0.00191 C21 1 0.274928 0.524980 0.526716 11.00000 0.03170 0.01362 = 0.01287 -0.00455 0.00929 0.00019 AFIX 137 H21A 2 0.208169 0.484750 0.528276 11.00000 -1.50000 H21B 2 0.246031 0.561790 0.553143 11.00000 -1.50000 H21C 2 0.371722 0.508457 0.536367 11.00000 -1.50000 AFIX 0 C22 1 0.120382 0.582126 0.451988 11.00000 0.01335 0.02707 = 0.02642 -0.01326 0.00021 0.00893 AFIX 137 H22A 2 0.120507 0.604163 0.415074 11.00000 -1.50000 H22B 2 0.089072 0.617191 0.479395 11.00000 -1.50000 H22C 2 0.054748 0.541353 0.451672 11.00000 -1.50000 AFIX 0 C23 1 0.373712 0.621737 0.468335 11.00000 0.02601 0.01141 = 0.01708 -0.00568 0.00247 -0.00045 AFIX 137 H23A 2 0.362998 0.647882 0.433249 11.00000 -1.50000 H23B 2 0.473014 0.605718 0.473020 11.00000 -1.50000 H23C 2 0.348944 0.653093 0.499273 11.00000 -1.50000 AFIX 0 C24 1 0.320880 0.122778 0.461811 11.00000 0.02300 0.01351 = 0.01318 0.00107 0.00269 -0.00045 C25 1 0.416941 0.131296 0.513577 11.00000 0.04325 0.02470 = 0.02015 0.00613 -0.00967 -0.00242 AFIX 137 H25A 2 0.516507 0.121708 0.503951 11.00000 -1.50000 H25B 2 0.386954 0.097530 0.542170 11.00000 -1.50000 H25C 2 0.408879 0.180105 0.527761 11.00000 -1.50000 AFIX 0 C26 1 0.162458 0.133380 0.478125 11.00000 0.03201 0.02227 = 0.02728 0.01006 0.01027 -0.00521 AFIX 137 H26A 2 0.101304 0.132314 0.444611 11.00000 -1.50000 H26B 2 0.151960 0.179498 0.496782 11.00000 -1.50000 H26C 2 0.134077 0.095022 0.503285 11.00000 -1.50000 AFIX 0 C27 1 0.335313 0.047298 0.439698 11.00000 0.05181 0.01519 = 0.02038 0.00489 0.00998 -0.00716 AFIX 137 H27A 2 0.273719 0.041513 0.406603 11.00000 -1.50000 H27B 2 0.306471 0.013246 0.468272 11.00000 -1.50000 H27C 2 0.435061 0.038427 0.429951 11.00000 -1.50000 AFIX 0 C28 1 0.486671 0.125277 0.254049 11.00000 0.01797 0.00662 = 0.01355 0.00073 -0.00082 -0.00214 AFIX 43 H28 2 0.430613 0.087714 0.268738 11.00000 -1.20000 AFIX 0 C29 1 0.568214 0.121825 0.207712 11.00000 0.01381 0.00791 = 0.01407 -0.00564 0.00116 0.00265 AFIX 43 H29 2 0.580094 0.081892 0.183944 11.00000 -1.20000 AFIX 0 C30 1 0.630528 0.189054 0.202453 11.00000 0.00759 0.01544 = 0.00859 -0.00122 0.00192 0.00491 C31 1 0.739316 0.205336 0.157138 11.00000 0.00946 0.01065 = 0.01048 -0.00145 0.00321 0.00315 C32 1 0.863464 0.151274 0.164826 11.00000 0.01746 0.01856 = 0.03415 0.00231 0.01197 0.00932 AFIX 137 H32A 2 0.934455 0.159103 0.136019 11.00000 -1.50000 H32B 2 0.825856 0.102601 0.161784 11.00000 -1.50000 H32C 2 0.908623 0.157916 0.201537 11.00000 -1.50000 AFIX 0 C33 1 0.666412 0.194016 0.100516 11.00000 0.02266 0.03402 = 0.01459 -0.00177 0.00188 -0.00904 AFIX 137 H33A 2 0.734507 0.204169 0.071091 11.00000 -1.50000 H33B 2 0.584099 0.226152 0.096747 11.00000 -1.50000 H33C 2 0.633844 0.144462 0.097370 11.00000 -1.50000 AFIX 0 C34 1 0.801546 0.280097 0.159135 11.00000 0.01287 0.02095 = 0.01681 -0.00446 0.00625 -0.00135 AFIX 137 H34A 2 0.877185 0.284269 0.131691 11.00000 -1.50000 H34B 2 0.841687 0.289417 0.196335 11.00000 -1.50000 H34C 2 0.725948 0.314877 0.150669 11.00000 -1.50000 AFIX 0 C35 1 0.960604 0.431664 0.345511 11.00000 0.02140 0.01177 = 0.02529 -0.00528 -0.00960 -0.00445 AFIX 137 H35A 2 1.013236 0.451421 0.314232 11.00000 -1.50000 H35B 2 1.027064 0.422750 0.376720 11.00000 -1.50000 H35C 2 0.887210 0.465711 0.356903 11.00000 -1.50000 AFIX 0 C36 1 0.778426 0.304347 0.383523 11.00000 0.02245 0.01609 = 0.01196 0.00110 0.00289 0.00179 AFIX 137 H36A 2 0.740346 0.257756 0.372175 11.00000 -1.50000 H36B 2 0.699558 0.335317 0.394695 11.00000 -1.50000 H36C 2 0.845658 0.298154 0.414890 11.00000 -1.50000 AFIX 0 C37 1 1.015639 0.283046 0.301838 11.00000 0.01689 0.01905 = 0.02533 -0.00058 0.00162 0.00606 AFIX 137 H37A 2 0.971554 0.238473 0.288874 11.00000 -1.50000 H37B 2 1.080363 0.273049 0.333388 11.00000 -1.50000 H37C 2 1.069803 0.304478 0.271638 11.00000 -1.50000 AFIX 0 C38 1 0.204263 0.407105 0.183134 11.00000 0.01144 0.01378 = 0.03570 -0.00148 0.00036 0.00255 AFIX 137 H38A 2 0.237708 0.454912 0.173241 11.00000 -1.50000 H38B 2 0.203232 0.402413 0.223668 11.00000 -1.50000 H38C 2 0.107380 0.399818 0.167904 11.00000 -1.50000 AFIX 0 C39 1 0.322595 0.343930 0.076183 11.00000 0.01945 0.03502 = 0.02150 0.00158 -0.00959 -0.00071 AFIX 137 H39A 2 0.392628 0.310705 0.060933 11.00000 -1.50000 H39B 2 0.345743 0.392650 0.064641 11.00000 -1.50000 H39C 2 0.226607 0.331353 0.062325 11.00000 -1.50000 AFIX 0 C40 1 0.261546 0.247940 0.173902 11.00000 0.01330 0.01238 = 0.02776 -0.00464 -0.00291 -0.00248 AFIX 137 H40A 2 0.165880 0.240229 0.157636 11.00000 -1.50000 H40B 2 0.257033 0.244928 0.214472 11.00000 -1.50000 H40C 2 0.326996 0.211361 0.160236 11.00000 -1.50000 AFIX 0 N1 3 0.539806 0.478197 0.244434 11.00000 0.01202 0.00634 = 0.01102 -0.00157 0.00317 0.00146 N2 3 0.430215 0.504146 0.276502 11.00000 0.00668 0.00793 = 0.01082 -0.00001 0.00374 0.00002 N3 3 0.443080 0.346955 0.307584 11.00000 0.01035 0.00308 = 0.01035 -0.00017 0.00434 0.00202 N4 3 0.590210 0.232542 0.243497 11.00000 0.00759 0.00921 = 0.00954 -0.00008 0.00245 -0.00035 N5 3 0.499990 0.191751 0.275298 11.00000 0.01220 0.01257 = 0.00725 -0.00253 0.00291 -0.00209 O1 4 0.761606 0.362396 0.273026 11.00000 0.01105 0.01218 = 0.01371 0.00006 -0.00223 0.00040 O2 4 0.490513 0.351350 0.176960 11.00000 0.01043 0.01023 = 0.00845 0.00073 0.00045 -0.00085 FE1 5 0.577873 0.355099 0.246453 11.00000 0.00601 0.00758 = 0.00606 -0.00076 0.00143 -0.00036 SI1 6 0.873440 0.346040 0.323913 11.00000 0.00958 0.00737 = 0.01222 -0.00081 -0.00094 0.00006 SI2 6 0.327941 0.338374 0.153567 11.00000 0.00888 0.01059 = 0.01351 -0.00111 -0.00255 0.00083 HKLF 4 REM Quest15mz331_0m in P2(1)/n REM R1 = 0.0900 for 5499 Fo > 4sig(Fo) and 0.1785 for all 10249 data REM 469 parameters refined using 0 restraints END WGHT 0.0000 0.0000 REM Highest difference peak 0.910, deepest hole -0.576, 1-sigma level 0.100 Q1 1 0.5982 0.3556 0.2103 11.00000 0.05 0.91 Q2 1 0.9134 0.2764 0.4368 11.00000 0.05 0.76 Q3 1 0.5584 0.3565 0.2835 11.00000 0.05 0.70 Q4 1 0.6278 0.4048 0.2399 11.00000 0.05 0.62 Q5 1 0.6294 0.3045 0.2428 11.00000 0.05 0.57 Q6 1 0.6821 0.3581 0.2372 11.00000 0.05 0.56 Q7 1 0.3545 0.3407 0.1143 11.00000 0.05 0.56 Q8 1 0.5259 0.4029 0.2520 11.00000 0.05 0.56 Q9 1 0.8421 0.3395 0.3653 11.00000 0.05 0.54 Q10 1 0.4561 0.3382 0.2769 11.00000 0.05 0.53 Q11 1 0.9283 0.2982 0.3172 11.00000 0.05 0.52 Q12 1 0.7532 0.3598 0.2976 11.00000 0.05 0.51 Q13 1 0.2801 0.2942 0.1567 11.00000 0.05 0.51 Q14 1 0.5306 0.3065 0.2536 11.00000 0.05 0.47 Q15 1 0.3939 0.3800 0.3147 11.00000 0.05 0.46 Q16 1 0.5004 0.5580 0.2088 11.00000 0.05 0.45 Q17 1 0.4212 0.3549 0.1833 11.00000 0.05 0.44 Q18 1 0.4793 0.3531 0.2552 11.00000 0.05 0.43 Q19 1 0.8233 0.3923 0.3284 11.00000 0.05 0.42 Q20 1 0.4233 0.3577 0.2837 11.00000 0.05 0.42 Q21 1 0.3918 0.2959 0.3741 11.00000 0.05 0.42 Q22 1 0.4924 0.1374 0.2224 11.00000 0.05 0.42 Q23 1 0.6438 0.2014 0.1725 11.00000 0.05 0.41 Q24 1 0.7706 0.1615 0.1635 11.00000 0.05 0.41 Q25 1 0.6721 0.4449 0.2185 11.00000 0.05 0.40 Q26 1 0.4401 0.3032 0.2367 11.00000 0.05 0.39 Q27 1 0.4153 0.6602 0.5284 11.00000 0.05 0.39 Q28 1 0.5772 0.5226 0.2289 11.00000 0.05 0.39 Q29 1 0.2773 0.3892 0.1623 11.00000 0.05 0.39 Q30 1 0.9553 0.3199 0.3078 11.00000 0.05 0.38 Q31 1 0.3869 0.1997 0.3438 11.00000 0.05 0.38 Q32 1 0.4312 0.4038 0.2417 11.00000 0.05 0.38 Q33 1 0.7888 0.3615 0.2293 11.00000 0.05 0.38 Q34 1 0.5780 0.4792 0.2010 11.00000 0.05 0.37 Q35 1 0.6991 0.3582 0.2716 11.00000 0.05 0.37 Q36 1 0.2837 0.5379 0.4957 11.00000 0.05 0.37 Q37 1 0.2745 0.4617 0.4270 11.00000 0.05 0.37 Q38 1 0.3955 0.3263 0.3133 11.00000 0.05 0.36 Q39 1 0.4230 0.5576 0.5950 11.00000 0.05 0.36 Q40 1 0.4810 0.3584 0.3142 11.00000 0.05 0.36 Q41 1 0.3636 0.4781 0.4335 11.00000 0.05 0.36 Q42 1 0.3774 0.0401 0.5396 11.00000 0.05 0.35 Q43 1 0.7224 0.1948 0.1889 11.00000 0.05 0.35 Q44 1 0.5857 0.5267 0.1698 11.00000 0.05 0.35 Q45 1 0.7455 0.4750 0.2217 11.00000 0.05 0.35 Q46 1 0.9766 0.3415 0.3189 11.00000 0.05 0.35 Q47 1 0.6826 0.3581 0.1821 11.00000 0.05 0.35 Q48 1 1.1434 0.3474 0.3093 11.00000 0.05 0.35 Q49 1 0.7198 0.3050 0.2593 11.00000 0.05 0.35 Q50 1 0.3979 0.2593 0.3246 11.00000 0.05 0.35 Q51 1 0.5210 0.4815 0.1755 11.00000 0.05 0.35 Q52 1 0.3601 0.4381 0.3364 11.00000 0.05 0.34 Q53 1 0.7261 0.4047 0.2657 11.00000 0.05 0.34 Q54 1 0.8251 0.5599 0.2257 11.00000 0.05 0.34 Q55 1 0.4482 0.3423 0.1494 11.00000 0.05 0.33 Q56 1 0.4757 0.3587 0.2130 11.00000 0.05 0.33 Q57 1 0.9682 0.2232 0.3267 11.00000 0.05 0.33 Q58 1 0.6026 0.3397 0.3760 11.00000 0.05 0.33 Q59 1 0.9191 0.5544 0.2304 11.00000 0.05 0.33 Q60 1 0.7415 0.5044 0.1792 11.00000 0.05 0.33 Q61 1 0.6647 0.3329 0.3463 11.00000 0.05 0.33 Q62 1 1.0558 0.2421 0.3018 11.00000 0.05 0.32 Q63 1 0.4802 0.3030 0.3281 11.00000 0.05 0.32 Q64 1 0.4174 0.5005 0.3067 11.00000 0.05 0.32 Q65 1 0.2609 0.4385 0.3331 11.00000 0.05 0.32 Q66 1 0.6683 0.1591 0.1995 11.00000 0.05 0.32 Q67 1 0.8189 0.4783 0.1485 11.00000 0.05 0.32 Q68 1 0.3581 0.3016 0.2235 11.00000 0.05 0.32 Q69 1 0.9296 0.3827 0.3553 11.00000 0.05 0.32 Q70 1 0.2010 0.1818 0.3777 11.00000 0.05 0.32 Q71 1 0.4320 0.3048 0.4940 11.00000 0.05 0.32 Q72 1 0.4746 0.5807 0.5678 11.00000 0.05 0.32 Q73 1 0.5506 0.2416 0.1631 11.00000 0.05 0.32 Q74 1 0.1961 0.5659 0.4597 11.00000 0.05 0.31 Q75 1 0.9540 0.3351 0.2160 11.00000 0.05 0.31 Q76 1 0.5521 0.6398 0.1409 11.00000 0.05 0.31 Q77 1 0.4775 0.4830 0.2523 11.00000 0.05 0.31 Q78 1 0.6496 0.5362 0.1905 11.00000 0.05 0.31 Q79 1 0.7530 0.5541 0.1878 11.00000 0.05 0.30 Q80 1 0.7473 0.4220 0.3205 11.00000 0.05 0.30 Q81 1 0.9875 0.2652 0.4062 11.00000 0.05 0.30 Q82 1 1.0611 0.2375 0.3352 11.00000 0.05 0.30 Q83 1 1.0472 0.2600 0.2565 11.00000 0.05 0.30 Q84 1 0.6393 0.4027 0.1668 11.00000 0.05 0.30 Q85 1 0.2499 0.3030 0.4197 11.00000 0.05 0.30 Q86 1 0.4731 0.3936 0.1416 11.00000 0.05 0.29 Q87 1 0.8442 0.1193 0.1894 11.00000 0.05 0.29 Q88 1 0.2787 0.4180 0.0253 11.00000 0.05 0.29 Q89 1 0.5760 0.4478 0.2571 11.00000 0.05 0.29 Q90 1 0.1606 0.4618 0.1469 11.00000 0.05 0.29 Q91 1 0.4794 0.1992 0.3152 11.00000 0.05 0.29 Q92 1 0.7062 0.3848 0.4142 11.00000 0.05 0.29 Q93 1 0.3775 0.1414 0.3549 11.00000 0.05 0.29 Q94 1 0.9392 0.4405 0.3070 11.00000 0.05 0.29 Q95 1 1.0810 0.3374 0.3050 11.00000 0.05 0.29 Q96 1 0.2018 0.3007 0.1807 11.00000 0.05 0.29 Q97 1 0.8641 0.2429 0.2707 11.00000 0.05 0.29 Q98 1 0.5181 0.0211 0.4228 11.00000 0.05 0.28 Q99 1 0.9304 0.3981 0.3184 11.00000 0.05 0.28 Q100 1 0.9747 0.1467 0.1580 11.00000 0.05 0.28 Q101 1 0.5513 0.4207 0.1540 11.00000 0.05 0.28 Q102 1 0.5006 0.1618 0.1612 11.00000 0.05 0.28 Q103 1 0.5367 0.5375 0.3554 11.00000 0.05 0.28 Q104 1 0.5143 0.3211 0.1861 11.00000 0.05 0.28 Q105 1 0.8796 0.3573 0.2496 11.00000 0.05 0.28 Q106 1 0.9348 0.4809 0.3164 11.00000 0.05 0.28 Q107 1 0.3206 0.1874 0.5276 11.00000 0.05 0.28 Q108 1 0.6441 0.4888 0.1246 11.00000 0.05 0.28 Q109 1 0.4974 0.3570 0.1536 11.00000 0.05 0.28 Q110 1 0.1232 0.0407 0.4560 11.00000 0.05 0.28 Q111 1 0.3787 0.5636 0.2787 11.00000 0.05 0.28 ; _shelx_res_checksum 18353 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 C1 C 0.3735(4) 0.5638(2) 0.25383(16) 0.0117(9) Uani 1 1 d . . H1 H 0.2971 0.5910 0.2685 0.014 Uiso 1 1 calc R U C2 C 0.4448(4) 0.5784(3) 0.20614(15) 0.0136(9) Uani 1 1 d . . H2 H 0.4271 0.6164 0.1809 0.016 Uiso 1 1 calc R U C3 C 0.5505(4) 0.5249(2) 0.20243(15) 0.0093(8) Uani 1 1 d . . C4 C 0.6650(4) 0.5230(2) 0.15814(16) 0.0108(9) Uani 1 1 d . . C5 C 0.7980(4) 0.4823(2) 0.17811(17) 0.0150(10) Uani 1 1 d . . H5A H 0.7731 0.4322 0.1844 0.023 Uiso 1 1 calc R U H5B H 0.8342 0.5034 0.2129 0.023 Uiso 1 1 calc R U H5C H 0.8718 0.4852 0.1499 0.023 Uiso 1 1 calc R U C6 C 0.6050(5) 0.4896(3) 0.10408(16) 0.0184(10) Uani 1 1 d . . H6A H 0.5163 0.5141 0.0930 0.028 Uiso 1 1 calc R U H6B H 0.5852 0.4389 0.1102 0.028 Uiso 1 1 calc R U H6C H 0.6753 0.4946 0.0747 0.028 Uiso 1 1 calc R U C7 C 0.7074(5) 0.6004(3) 0.14613(18) 0.0182(10) Uani 1 1 d . . H7A H 0.7851 0.6011 0.1194 0.027 Uiso 1 1 calc R U H7B H 0.7396 0.6235 0.1807 0.027 Uiso 1 1 calc R U H7C H 0.6246 0.6262 0.1307 0.027 Uiso 1 1 calc R U C8 C 0.4039(4) 0.4034(2) 0.34146(15) 0.0080(8) Uani 1 1 d . . C9 C 0.4003(4) 0.4768(2) 0.33021(15) 0.0080(8) Uani 1 1 d . . C10 C 0.3593(4) 0.5237(2) 0.37112(16) 0.0090(8) Uani 1 1 d . . H10 H 0.3582 0.5733 0.3630 0.011 Uiso 1 1 calc R U C11 C 0.3191(4) 0.5012(2) 0.42430(16) 0.0092(8) Uani 1 1 d . . C12 C 0.3181(4) 0.4288(2) 0.43531(15) 0.0098(9) Uani 1 1 d . . H12 H 0.2894 0.4118 0.4706 0.012 Uiso 1 1 calc R U C13 C 0.3597(4) 0.3805(2) 0.39421(16) 0.0089(8) Uani 1 1 d . . C14 C 0.3702(4) 0.3042(2) 0.39318(16) 0.0107(9) Uani 1 1 d . . C15 C 0.3382(4) 0.2518(2) 0.43170(16) 0.0118(9) Uani 1 1 d . . H15 H 0.3019 0.2649 0.4668 0.014 Uiso 1 1 calc R U C16 C 0.3590(4) 0.1800(2) 0.41922(16) 0.0116(9) Uani 1 1 d . . C17 C 0.4144(4) 0.1630(2) 0.36694(15) 0.0107(9) Uani 1 1 d . . H17 H 0.4309 0.1143 0.3582 0.013 Uiso 1 1 calc R U C18 C 0.4462(4) 0.2149(2) 0.32740(16) 0.0104(9) Uani 1 1 d . . C19 C 0.4222(4) 0.2868(2) 0.33970(15) 0.0068(8) Uani 1 1 d . . C20 C 0.2731(4) 0.5564(2) 0.46749(16) 0.0114(9) Uani 1 1 d . . C21 C 0.2749(5) 0.5250(3) 0.52672(16) 0.0193(10) Uani 1 1 d . . H21A H 0.2082 0.4847 0.5283 0.029 Uiso 1 1 calc R U H21B H 0.2460 0.5618 0.5531 0.029 Uiso 1 1 calc R U H21C H 0.3717 0.5085 0.5364 0.029 Uiso 1 1 calc R U C22 C 0.1204(4) 0.5821(3) 0.45199(19) 0.0223(11) Uani 1 1 d . . H22A H 0.1205 0.6042 0.4151 0.033 Uiso 1 1 calc R U H22B H 0.0891 0.6172 0.4794 0.033 Uiso 1 1 calc R U H22C H 0.0547 0.5414 0.4517 0.033 Uiso 1 1 calc R U C23 C 0.3737(5) 0.6217(2) 0.46833(18) 0.0181(10) Uani 1 1 d . . H23A H 0.3630 0.6479 0.4332 0.027 Uiso 1 1 calc R U H23B H 0.4730 0.6057 0.4730 0.027 Uiso 1 1 calc R U H23C H 0.3489 0.6531 0.4993 0.027 Uiso 1 1 calc R U C24 C 0.3209(5) 0.1228(3) 0.46181(17) 0.0165(10) Uani 1 1 d . . C25 C 0.4169(6) 0.1313(3) 0.51358(19) 0.0295(12) Uani 1 1 d . . H25A H 0.5165 0.1217 0.5040 0.044 Uiso 1 1 calc R U H25B H 0.3870 0.0975 0.5422 0.044 Uiso 1 1 calc R U H25C H 0.4089 0.1801 0.5278 0.044 Uiso 1 1 calc R U C26 C 0.1625(5) 0.1334(3) 0.4781(2) 0.0271(12) Uani 1 1 d . . H26A H 0.1013 0.1323 0.4446 0.041 Uiso 1 1 calc R U H26B H 0.1520 0.1795 0.4968 0.041 Uiso 1 1 calc R U H26C H 0.1341 0.0950 0.5033 0.041 Uiso 1 1 calc R U C27 C 0.3353(6) 0.0473(3) 0.43970(19) 0.0290(13) Uani 1 1 d . . H27A H 0.2737 0.0415 0.4066 0.044 Uiso 1 1 calc R U H27B H 0.3065 0.0132 0.4683 0.044 Uiso 1 1 calc R U H27C H 0.4351 0.0384 0.4300 0.044 Uiso 1 1 calc R U C28 C 0.4867(4) 0.1253(2) 0.25405(16) 0.0127(9) Uani 1 1 d . . H28 H 0.4306 0.0877 0.2687 0.015 Uiso 1 1 calc R U C29 C 0.5682(4) 0.1218(2) 0.20771(16) 0.0119(9) Uani 1 1 d . . H29 H 0.5801 0.0819 0.1839 0.014 Uiso 1 1 calc R U C30 C 0.6305(4) 0.1891(2) 0.20245(16) 0.0105(9) Uani 1 1 d . . C31 C 0.7393(4) 0.2053(2) 0.15714(16) 0.0102(9) Uani 1 1 d . . C32 C 0.8635(5) 0.1513(3) 0.1648(2) 0.0232(11) Uani 1 1 d . . H32A H 0.9345 0.1591 0.1360 0.035 Uiso 1 1 calc R U H32B H 0.8259 0.1026 0.1618 0.035 Uiso 1 1 calc R U H32C H 0.9086 0.1579 0.2015 0.035 Uiso 1 1 calc R U C33 C 0.6664(5) 0.1940(3) 0.10052(17) 0.0237(11) Uani 1 1 d . . H33A H 0.7345 0.2042 0.0711 0.036 Uiso 1 1 calc R U H33B H 0.5841 0.2262 0.0967 0.036 Uiso 1 1 calc R U H33C H 0.6338 0.1445 0.0974 0.036 Uiso 1 1 calc R U C34 C 0.8015(4) 0.2801(3) 0.15914(18) 0.0168(10) Uani 1 1 d . . H34A H 0.8772 0.2843 0.1317 0.025 Uiso 1 1 calc R U H34B H 0.8417 0.2894 0.1963 0.025 Uiso 1 1 calc R U H34C H 0.7259 0.3149 0.1507 0.025 Uiso 1 1 calc R U C35 C 0.9606(5) 0.4317(3) 0.34551(19) 0.0196(10) Uani 1 1 d . . H35A H 1.0132 0.4514 0.3142 0.029 Uiso 1 1 calc R U H35B H 1.0271 0.4227 0.3767 0.029 Uiso 1 1 calc R U H35C H 0.8872 0.4657 0.3569 0.029 Uiso 1 1 calc R U C36 C 0.7784(5) 0.3043(3) 0.38352(16) 0.0168(10) Uani 1 1 d . . H36A H 0.7403 0.2578 0.3722 0.025 Uiso 1 1 calc R U H36B H 0.6996 0.3353 0.3947 0.025 Uiso 1 1 calc R U H36C H 0.8457 0.2982 0.4149 0.025 Uiso 1 1 calc R U C37 C 1.0156(5) 0.2830(3) 0.30184(19) 0.0204(10) Uani 1 1 d . . H37A H 0.9716 0.2385 0.2889 0.031 Uiso 1 1 calc R U H37B H 1.0804 0.2730 0.3334 0.031 Uiso 1 1 calc R U H37C H 1.0698 0.3045 0.2716 0.031 Uiso 1 1 calc R U C38 C 0.2043(4) 0.4071(3) 0.18313(19) 0.0203(10) Uani 1 1 d . . H38A H 0.2377 0.4549 0.1732 0.030 Uiso 1 1 calc R U H38B H 0.2032 0.4024 0.2237 0.030 Uiso 1 1 calc R U H38C H 0.1074 0.3998 0.1679 0.030 Uiso 1 1 calc R U C39 C 0.3226(5) 0.3439(3) 0.07618(18) 0.0255(11) Uani 1 1 d . . H39A H 0.3926 0.3107 0.0609 0.038 Uiso 1 1 calc R U H39B H 0.3457 0.3926 0.0646 0.038 Uiso 1 1 calc R U H39C H 0.2266 0.3314 0.0623 0.038 Uiso 1 1 calc R U C40 C 0.2615(4) 0.2479(2) 0.17390(18) 0.0179(10) Uani 1 1 d . . H40A H 0.1659 0.2402 0.1576 0.027 Uiso 1 1 calc R U H40B H 0.2570 0.2449 0.2145 0.027 Uiso 1 1 calc R U H40C H 0.3270 0.2114 0.1602 0.027 Uiso 1 1 calc R U N1 N 0.5398(3) 0.47820(19) 0.24443(13) 0.0098(7) Uani 1 1 d . . N2 N 0.4302(3) 0.50415(19) 0.27650(13) 0.0084(7) Uani 1 1 d . . N3 N 0.4431(3) 0.34695(18) 0.30758(13) 0.0079(7) Uani 1 1 d . . N4 N 0.5902(3) 0.23254(18) 0.24350(13) 0.0087(7) Uani 1 1 d . . N5 N 0.5000(3) 0.1918(2) 0.27530(13) 0.0106(8) Uani 1 1 d . . O1 O 0.7616(3) 0.36240(16) 0.27303(11) 0.0123(6) Uani 1 1 d . . O2 O 0.4905(3) 0.35135(16) 0.17696(10) 0.0097(6) Uani 1 1 d . . Fe1 Fe 0.57787(6) 0.35510(3) 0.24645(2) 0.00653(14) Uani 1 1 d . . Si1 Si 0.87344(11) 0.34604(7) 0.32391(4) 0.0097(2) Uani 1 1 d . . Si2 Si 0.32794(11) 0.33837(7) 0.15357(5) 0.0110(3) Uani 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.014(2) 0.009(2) 0.0118(18) -0.0011(17) -0.0008(17) 0.0044(17) C2 0.020(2) 0.013(3) 0.0078(18) -0.0005(17) -0.0023(17) 0.0013(18) C3 0.0127(19) 0.007(2) 0.0077(18) -0.0032(16) -0.0004(16) -0.0008(16) C4 0.0115(19) 0.012(2) 0.0094(18) -0.0013(16) 0.0026(16) -0.0031(17) C5 0.017(2) 0.011(3) 0.017(2) 0.0032(18) 0.0099(18) 0.0031(18) C6 0.026(2) 0.018(3) 0.012(2) -0.0057(18) 0.0067(19) -0.006(2) C7 0.016(2) 0.019(3) 0.019(2) 0.0045(19) 0.0021(19) -0.0008(19) C8 0.0072(18) 0.008(2) 0.0088(18) -0.0035(16) 0.0002(16) -0.0019(16) C9 0.0052(18) 0.012(2) 0.0066(17) 0.0011(16) -0.0005(15) 0.0000(16) C10 0.0053(18) 0.006(2) 0.0156(19) -0.0042(16) -0.0002(16) -0.0004(15) C11 0.0085(18) 0.007(2) 0.0125(18) -0.0016(16) -0.0001(16) 0.0006(16) C12 0.0044(18) 0.018(3) 0.0066(17) -0.0035(17) -0.0009(15) -0.0004(16) C13 0.0065(18) 0.010(2) 0.0100(18) 0.0031(16) -0.0001(15) 0.0014(16) C14 0.0074(18) 0.013(2) 0.0120(19) -0.0008(17) -0.0010(16) -0.0018(16) C15 0.0132(19) 0.014(3) 0.0086(18) -0.0020(17) 0.0023(16) 0.0019(17) C16 0.0105(19) 0.013(2) 0.0115(19) 0.0018(17) -0.0022(16) -0.0008(17) C17 0.014(2) 0.006(2) 0.0122(18) -0.0026(16) -0.0019(16) -0.0003(17) C18 0.0053(18) 0.014(3) 0.0117(18) 0.0012(17) 0.0024(16) -0.0016(16) C19 0.0040(17) 0.011(2) 0.0056(17) 0.0004(16) 0.0010(14) -0.0007(15) C20 0.012(2) 0.009(2) 0.0130(19) -0.0051(17) 0.0032(17) -0.0019(17) C21 0.032(3) 0.014(3) 0.013(2) -0.0046(18) 0.009(2) 0.000(2) C22 0.013(2) 0.027(3) 0.026(2) -0.013(2) 0.000(2) 0.009(2) C23 0.026(2) 0.011(3) 0.017(2) -0.0057(18) 0.0025(19) -0.0005(19) C24 0.023(2) 0.014(3) 0.0132(19) 0.0011(18) 0.0027(19) -0.0005(19) C25 0.043(3) 0.025(3) 0.020(2) 0.006(2) -0.010(2) -0.002(2) C26 0.032(3) 0.022(3) 0.027(2) 0.010(2) 0.010(2) -0.005(2) C27 0.052(3) 0.015(3) 0.020(2) 0.005(2) 0.010(2) -0.007(2) C28 0.018(2) 0.007(2) 0.0136(19) 0.0007(17) -0.0008(17) -0.0021(17) C29 0.014(2) 0.008(2) 0.0141(19) -0.0056(17) 0.0012(17) 0.0026(17) C30 0.0076(18) 0.015(3) 0.0086(18) -0.0012(17) 0.0019(16) 0.0049(16) C31 0.0095(19) 0.011(2) 0.0105(18) -0.0015(17) 0.0032(16) 0.0031(17) C32 0.017(2) 0.019(3) 0.034(2) 0.002(2) 0.012(2) 0.009(2) C33 0.023(2) 0.034(3) 0.015(2) -0.002(2) 0.0019(19) -0.009(2) C34 0.013(2) 0.021(3) 0.017(2) -0.0045(19) 0.0062(18) -0.0014(18) C35 0.021(2) 0.012(3) 0.025(2) -0.005(2) -0.010(2) -0.0045(19) C36 0.022(2) 0.016(3) 0.0120(19) 0.0011(18) 0.0029(18) 0.0018(19) C37 0.017(2) 0.019(3) 0.025(2) -0.001(2) 0.002(2) 0.0061(19) C38 0.011(2) 0.014(3) 0.036(3) -0.001(2) 0.000(2) 0.0025(18) C39 0.019(2) 0.035(3) 0.022(2) 0.002(2) -0.0096(19) -0.001(2) C40 0.013(2) 0.012(3) 0.028(2) -0.005(2) -0.0029(19) -0.0025(18) N1 0.0120(17) 0.006(2) 0.0110(16) -0.0016(14) 0.0032(14) 0.0015(14) N2 0.0067(16) 0.008(2) 0.0108(15) 0.0000(14) 0.0037(13) 0.0000(13) N3 0.0103(16) 0.0031(19) 0.0103(14) -0.0002(14) 0.0043(13) 0.0020(13) N4 0.0076(15) 0.0092(19) 0.0095(15) -0.0001(14) 0.0025(13) -0.0003(14) N5 0.0122(16) 0.013(2) 0.0072(15) -0.0025(14) 0.0029(14) -0.0021(14) O1 0.0110(13) 0.0122(18) 0.0137(13) 0.0001(12) -0.0022(11) 0.0004(12) O2 0.0104(13) 0.0102(16) 0.0084(12) 0.0007(12) 0.0005(11) -0.0009(12) Fe1 0.0060(3) 0.0076(3) 0.0061(2) -0.0008(2) 0.0014(2) -0.0004(2) Si1 0.0096(5) 0.0074(6) 0.0122(5) -0.0008(5) -0.0009(4) 0.0001(5) Si2 0.0089(5) 0.0106(7) 0.0135(5) -0.0011(5) -0.0026(4) 0.0008(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N2 C1 C2 108.1(4) N2 C1 H1 125.9 C2 C1 H1 125.9 C1 C2 C3 105.3(4) C1 C2 H2 127.3 C3 C2 H2 127.3 N1 C3 C2 110.7(3) N1 C3 C4 125.0(4) C2 C3 C4 124.2(4) C3 C4 C5 111.7(3) C3 C4 C7 107.2(3) C5 C4 C7 108.7(3) C3 C4 C6 110.5(3) C5 C4 C6 110.1(4) C7 C4 C6 108.4(3) C4 C5 H5A 109.5 C4 C5 H5B 109.5 H5A C5 H5B 109.5 C4 C5 H5C 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 C4 C6 H6A 109.5 C4 C6 H6B 109.5 H6A C6 H6B 109.5 C4 C6 H6C 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.5 C4 C7 H7A 109.5 C4 C7 H7B 109.5 H7A C7 H7B 109.5 C4 C7 H7C 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 N3 C8 C9 129.8(3) N3 C8 C13 112.4(4) C9 C8 C13 117.8(4) C10 C9 C8 119.6(3) C10 C9 N2 118.7(4) C8 C9 N2 121.6(3) C9 C10 C11 122.7(4) C9 C10 H10 118.6 C11 C10 H10 118.6 C12 C11 C10 118.2(4) C12 C11 C20 121.9(3) C10 C11 C20 119.9(4) C11 C12 C13 119.7(3) C11 C12 H12 120.2 C13 C12 H12 120.2 C12 C13 C8 122.0(4) C12 C13 C14 132.6(4) C8 C13 C14 105.5(3) C15 C14 C19 121.7(4) C15 C14 C13 132.8(4) C19 C14 C13 105.6(4) C14 C15 C16 120.5(3) C14 C15 H15 119.8 C16 C15 H15 119.8 C15 C16 C17 117.9(4) C15 C16 C24 119.8(3) C17 C16 C24 122.3(4) C18 C17 C16 122.5(4) C18 C17 H17 118.7 C16 C17 H17 118.7 C17 C18 C19 119.4(3) C17 C18 N5 118.0(4) C19 C18 N5 122.7(4) N3 C19 C18 129.9(3) N3 C19 C14 112.0(4) C18 C19 C14 118.1(4) C11 C20 C21 111.8(4) C11 C20 C23 111.4(3) C21 C20 C23 107.1(4) C11 C20 C22 108.5(3) C21 C20 C22 109.6(3) C23 C20 C22 108.3(4) C20 C21 H21A 109.5 C20 C21 H21B 109.5 H21A C21 H21B 109.5 C20 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C20 C22 H22A 109.5 C20 C22 H22B 109.5 H22A C22 H22B 109.5 C20 C22 H22C 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 C20 C23 H23A 109.5 C20 C23 H23B 109.5 H23A C23 H23B 109.5 C20 C23 H23C 109.5 H23A C23 H23C 109.5 H23B C23 H23C 109.5 C27 C24 C25 109.1(4) C27 C24 C16 113.2(3) C25 C24 C16 109.4(4) C27 C24 C26 107.4(4) C25 C24 C26 109.2(3) C16 C24 C26 108.4(4) C24 C25 H25A 109.5 C24 C25 H25B 109.5 H25A C25 H25B 109.5 C24 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C24 C26 H26A 109.5 C24 C26 H26B 109.5 H26A C26 H26B 109.5 C24 C26 H26C 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 C24 C27 H27A 109.5 C24 C27 H27B 109.5 H27A C27 H27B 109.5 C24 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 N5 C28 C29 107.7(4) N5 C28 H28 126.1 C29 C28 H28 126.1 C28 C29 C30 105.8(4) C28 C29 H29 127.1 C30 C29 H29 127.1 N4 C30 C29 111.0(3) N4 C30 C31 127.0(4) C29 C30 C31 121.8(4) C34 C31 C33 108.7(4) C34 C31 C30 114.8(3) C33 C31 C30 108.4(3) C34 C31 C32 108.3(4) C33 C31 C32 109.6(4) C30 C31 C32 106.8(3) C31 C32 H32A 109.5 C31 C32 H32B 109.5 H32A C32 H32B 109.5 C31 C32 H32C 109.5 H32A C32 H32C 109.5 H32B C32 H32C 109.5 C31 C33 H33A 109.5 C31 C33 H33B 109.5 H33A C33 H33B 109.5 C31 C33 H33C 109.5 H33A C33 H33C 109.5 H33B C33 H33C 109.5 C31 C34 H34A 109.5 C31 C34 H34B 109.5 H34A C34 H34B 109.5 C31 C34 H34C 109.5 H34A C34 H34C 109.5 H34B C34 H34C 109.5 Si1 C35 H35A 109.5 Si1 C35 H35B 109.5 H35A C35 H35B 109.5 Si1 C35 H35C 109.5 H35A C35 H35C 109.5 H35B C35 H35C 109.5 Si1 C36 H36A 109.5 Si1 C36 H36B 109.5 H36A C36 H36B 109.5 Si1 C36 H36C 109.5 H36A C36 H36C 109.5 H36B C36 H36C 109.5 Si1 C37 H37A 109.5 Si1 C37 H37B 109.5 H37A C37 H37B 109.5 Si1 C37 H37C 109.5 H37A C37 H37C 109.5 H37B C37 H37C 109.5 Si2 C38 H38A 109.5 Si2 C38 H38B 109.5 H38A C38 H38B 109.5 Si2 C38 H38C 109.5 H38A C38 H38C 109.5 H38B C38 H38C 109.5 Si2 C39 H39A 109.5 Si2 C39 H39B 109.5 H39A C39 H39B 109.5 Si2 C39 H39C 109.5 H39A C39 H39C 109.5 H39B C39 H39C 109.5 Si2 C40 H40A 109.5 Si2 C40 H40B 109.5 H40A C40 H40B 109.5 Si2 C40 H40C 109.5 H40A C40 H40C 109.5 H40B C40 H40C 109.5 C3 N1 N2 104.9(3) C3 N1 Fe1 130.3(2) N2 N1 Fe1 116.8(2) C1 N2 N1 110.8(3) C1 N2 C9 125.7(3) N1 N2 C9 122.7(3) C19 N3 C8 104.5(3) C19 N3 Fe1 125.6(2) C8 N3 Fe1 124.1(3) C30 N4 N5 104.8(3) C30 N4 Fe1 130.1(3) N5 N4 Fe1 120.3(2) C28 N5 N4 110.7(3) C28 N5 C18 125.5(3) N4 N5 C18 123.2(3) Si1 O1 Fe1 146.86(17) Si2 O2 Fe1 135.36(15) O1 Fe1 O2 135.72(11) O1 Fe1 N3 110.87(13) O2 Fe1 N3 113.39(13) O1 Fe1 N4 92.19(13) O2 Fe1 N4 87.46(13) N3 Fe1 N4 88.78(13) O1 Fe1 N1 94.31(13) O2 Fe1 N1 87.38(13) N3 Fe1 N1 89.58(12) N4 Fe1 N1 173.46(12) O1 Si1 C37 110.91(18) O1 Si1 C35 108.6(2) C37 Si1 C35 108.3(2) O1 Si1 C36 110.42(17) C37 Si1 C36 107.8(2) C35 Si1 C36 110.8(2) O2 Si2 C39 110.11(17) O2 Si2 C40 110.87(19) C39 Si2 C40 108.0(2) O2 Si2 C38 110.07(19) C39 Si2 C38 109.6(2) C40 Si2 C38 108.18(19) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N2 1.348(5) C1 C2 1.366(5) C1 H1 0.9500 C2 C3 1.411(6) C2 H2 0.9500 C3 N1 1.343(5) C3 C4 1.526(5) C4 C5 1.528(6) C4 C7 1.534(6) C4 C6 1.540(6) C5 H5A 0.9800 C5 H5B 0.9800 C5 H5C 0.9800 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 N3 1.390(5) C8 C9 1.401(6) C8 C13 1.410(5) C9 C10 1.381(5) C9 N2 1.424(5) C10 C11 1.406(5) C10 H10 0.9500 C11 C12 1.384(6) C11 C20 1.534(5) C12 C13 1.401(5) C12 H12 0.9500 C13 C14 1.435(6) C14 C15 1.387(6) C14 C19 1.422(5) C15 C16 1.393(6) C15 H15 0.9500 C16 C17 1.407(5) C16 C24 1.531(6) C17 C18 1.398(6) C17 H17 0.9500 C18 C19 1.399(6) C18 N5 1.428(5) C19 N3 1.383(5) C20 C21 1.542(6) C20 C23 1.544(6) C20 C22 1.546(6) C21 H21A 0.9800 C21 H21B 0.9800 C21 H21C 0.9800 C22 H22A 0.9800 C22 H22B 0.9800 C22 H22C 0.9800 C23 H23A 0.9800 C23 H23B 0.9800 C23 H23C 0.9800 C24 C27 1.519(7) C24 C25 1.530(6) C24 C26 1.552(6) C25 H25A 0.9800 C25 H25B 0.9800 C25 H25C 0.9800 C26 H26A 0.9800 C26 H26B 0.9800 C26 H26C 0.9800 C27 H27A 0.9800 C27 H27B 0.9800 C27 H27C 0.9800 C28 N5 1.352(6) C28 C29 1.365(5) C28 H28 0.9500 C29 C30 1.395(6) C29 H29 0.9500 C30 N4 1.341(5) C30 C31 1.536(5) C31 C34 1.518(6) C31 C33 1.527(6) C31 C32 1.549(6) C32 H32A 0.9800 C32 H32B 0.9800 C32 H32C 0.9800 C33 H33A 0.9800 C33 H33B 0.9800 C33 H33C 0.9800 C34 H34A 0.9800 C34 H34B 0.9800 C34 H34C 0.9800 C35 Si1 1.869(5) C35 H35A 0.9800 C35 H35B 0.9800 C35 H35C 0.9800 C36 Si1 1.873(4) C36 H36A 0.9800 C36 H36B 0.9800 C36 H36C 0.9800 C37 Si1 1.863(4) C37 H37A 0.9800 C37 H37B 0.9800 C37 H37C 0.9800 C38 Si2 1.880(4) C38 H38A 0.9800 C38 H38B 0.9800 C38 H38C 0.9800 C39 Si2 1.866(4) C39 H39A 0.9800 C39 H39B 0.9800 C39 H39C 0.9800 C40 Si2 1.874(5) C40 H40A 0.9800 C40 H40B 0.9800 C40 H40C 0.9800 N1 N2 1.383(4) N1 Fe1 2.335(4) N3 Fe1 1.962(3) N4 N5 1.381(4) N4 Fe1 2.301(4) O1 Si1 1.624(3) O1 Fe1 1.826(3) O2 Si2 1.629(3) O2 Fe1 1.849(3) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion N2 C1 C2 C3 -1.6(5) C1 C2 C3 N1 2.7(5) C1 C2 C3 C4 -174.7(4) N1 C3 C4 C5 -22.6(6) C2 C3 C4 C5 154.4(4) N1 C3 C4 C7 -141.5(4) C2 C3 C4 C7 35.4(5) N1 C3 C4 C6 100.4(5) C2 C3 C4 C6 -82.6(5) N3 C8 C9 C10 -179.0(4) C13 C8 C9 C10 2.4(6) N3 C8 C9 N2 4.6(6) C13 C8 C9 N2 -174.1(4) C8 C9 C10 C11 -0.6(6) N2 C9 C10 C11 176.0(4) C9 C10 C11 C12 -1.4(6) C9 C10 C11 C20 -179.3(4) C10 C11 C12 C13 1.4(6) C20 C11 C12 C13 179.3(4) C11 C12 C13 C8 0.4(6) C11 C12 C13 C14 179.7(4) N3 C8 C13 C12 178.8(3) C9 C8 C13 C12 -2.4(6) N3 C8 C13 C14 -0.7(5) C9 C8 C13 C14 178.2(3) C12 C13 C14 C15 2.6(8) C8 C13 C14 C15 -178.0(4) C12 C13 C14 C19 -178.7(4) C8 C13 C14 C19 0.7(4) C19 C14 C15 C16 1.2(6) C13 C14 C15 C16 179.8(4) C14 C15 C16 C17 0.7(6) C14 C15 C16 C24 -179.0(4) C15 C16 C17 C18 -1.2(6) C24 C16 C17 C18 178.4(4) C16 C17 C18 C19 -0.1(6) C16 C17 C18 N5 -179.1(4) C17 C18 C19 N3 -179.1(4) N5 C18 C19 N3 -0.1(7) C17 C18 C19 C14 1.9(6) N5 C18 C19 C14 -179.1(4) C15 C14 C19 N3 178.3(4) C13 C14 C19 N3 -0.6(5) C15 C14 C19 C18 -2.5(6) C13 C14 C19 C18 178.6(3) C12 C11 C20 C21 18.4(5) C10 C11 C20 C21 -163.8(4) C12 C11 C20 C23 138.3(4) C10 C11 C20 C23 -43.9(5) C12 C11 C20 C22 -102.6(4) C10 C11 C20 C22 75.2(5) C15 C16 C24 C27 174.1(4) C17 C16 C24 C27 -5.6(6) C15 C16 C24 C25 -64.0(5) C17 C16 C24 C25 116.4(4) C15 C16 C24 C26 55.0(5) C17 C16 C24 C26 -124.7(4) N5 C28 C29 C30 0.1(5) C28 C29 C30 N4 0.1(5) C28 C29 C30 C31 175.7(4) N4 C30 C31 C34 -2.4(6) C29 C30 C31 C34 -177.3(4) N4 C30 C31 C33 -124.1(5) C29 C30 C31 C33 61.0(5) N4 C30 C31 C32 117.8(5) C29 C30 C31 C32 -57.1(5) C2 C3 N1 N2 -2.6(4) C4 C3 N1 N2 174.7(4) C2 C3 N1 Fe1 144.2(3) C4 C3 N1 Fe1 -38.5(6) C2 C1 N2 N1 0.0(5) C2 C1 N2 C9 170.5(4) C3 N1 N2 C1 1.6(4) Fe1 N1 N2 C1 -150.5(3) C3 N1 N2 C9 -169.2(4) Fe1 N1 N2 C9 38.7(4) C10 C9 N2 C1 -27.4(6) C8 C9 N2 C1 149.1(4) C10 C9 N2 N1 142.0(4) C8 C9 N2 N1 -41.5(5) C18 C19 N3 C8 -178.9(4) C14 C19 N3 C8 0.2(4) C18 C19 N3 Fe1 -24.8(6) C14 C19 N3 Fe1 154.2(3) C9 C8 N3 C19 -178.4(4) C13 C8 N3 C19 0.3(4) C9 C8 N3 Fe1 27.1(6) C13 C8 N3 Fe1 -154.2(3) C29 C30 N4 N5 -0.2(4) C31 C30 N4 N5 -175.5(4) C29 C30 N4 Fe1 -155.0(3) C31 C30 N4 Fe1 29.7(6) C29 C28 N5 N4 -0.2(5) C29 C28 N5 C18 -171.9(4) C30 N4 N5 C28 0.2(4) Fe1 N4 N5 C28 158.1(3) C30 N4 N5 C18 172.1(4) Fe1 N4 N5 C18 -30.0(5) C17 C18 N5 C28 19.7(6) C19 C18 N5 C28 -159.2(4) C17 C18 N5 N4 -151.0(4) C19 C18 N5 N4 30.0(6) Si1 O1 Fe1 O2 -153.8(3) Si1 O1 Fe1 N3 24.3(4) Si1 O1 Fe1 N4 -65.2(3) Si1 O1 Fe1 N1 115.5(3) Si2 O2 Fe1 O1 173.9(2) Si2 O2 Fe1 N3 -4.2(3) Si2 O2 Fe1 N4 83.4(3) Si2 O2 Fe1 N1 -92.6(3) Fe1 O1 Si1 C37 116.1(3) Fe1 O1 Si1 C35 -125.0(3) Fe1 O1 Si1 C36 -3.3(4) Fe1 O2 Si2 C39 179.0(3) Fe1 O2 Si2 C40 -61.5(3) Fe1 O2 Si2 C38 58.1(3)