#------------------------------------------------------------------------------ #$Date: 2020-10-06 11:48:21 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257536 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/51/7705162.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_7705162 loop_ _publ_author_name 'He, Zhiyuan' 'Xue, Xiaolian' 'Liu, Yilan' 'Yu, Na' 'Krogman, Jeremy P.' _publ_section_title ; Aminolysis of bis[bis(trimethylsilyl)amido]-manganese, -iron, and -cobalt for the synthesis of mono- and bis-silylene complexes. ; _journal_issue 36 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 12586 _journal_page_last 12591 _journal_paper_doi 10.1039/d0dt00570c _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C60 H120 Cl2 Fe2 N8 Si10' _chemical_formula_sum 'C60 H120 Cl2 Fe2 N8 Si10' _chemical_formula_weight 1417.13 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-07-14 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-07-26 deposited with the CCDC. 2020-08-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 110.4720(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 37.0728(13) _cell_length_b 13.2937(5) _cell_length_c 17.4231(6) _cell_measurement_reflns_used 9993 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 74.52 _cell_measurement_theta_min 5.08 _cell_volume 8044.4(5) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 149.87 _diffrn_measured_fraction_theta_full 0.966 _diffrn_measured_fraction_theta_max 0.966 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_unetI/netI 0.0679 _diffrn_reflns_Laue_measured_fraction_full 0.966 _diffrn_reflns_Laue_measured_fraction_max 0.966 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 18524 _diffrn_reflns_point_group_measured_fraction_full 0.966 _diffrn_reflns_point_group_measured_fraction_max 0.966 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.238 _diffrn_reflns_theta_min 2.544 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 5.223 _exptl_absorpt_correction_T_max 0.7538 _exptl_absorpt_correction_T_min 0.4917 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1079 before and 0.0628 after correction. The Ratio of minimum to maximum transmission is 0.6523. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear yellowish yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier yellowish _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.170 _exptl_crystal_description block _exptl_crystal_F_000 3048 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.312 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.067 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 388 _refine_ls_number_reflns 7108 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.077 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0415 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+3.0977P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1159 _refine_ls_wR_factor_ref 0.1190 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6272 _reflns_number_total 7108 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt00570c2.cif _cod_data_source_block 11 _cod_depositor_comments 'Adding full bibliography for 7705159--7705168.cif.' _cod_database_code 7705162 _shelx_shelxl_version_number 2018/3 _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_max 0.573 _shelx_estimated_absorpt_t_min 0.421 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C8(H8), C5(H5), C7(H7), C6(H6) 2.b Idealised Me refined as rotating group: C25(H25A,H25B,H25C), C24(H24A,H24B,H24C), C16(H16A,H16B,H16C), C23(H23A,H23B, H23C), C13(H13A,H13B,H13C), C19(H19A,H19B,H19C), C14(H14A,H14B,H14C), C20(H20A, H20B,H20C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C17(H17A,H17B,H17C), C00Z(H00A,H00B,H00C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C), C012(H01A,H01B, H01C), C22(H22A,H22B,H22C), C12(H12A,H12B,H12C), C21(H21A,H21B,H21C) ; _shelx_res_file ; TITL cu_hzy2962_0m_a.res in C2/c cu_hzy2962_0m.res created by SHELXL-2018/3 at 14:05:42 on 14-Jul-2020 REM Old TITL cu_hzy2962_0m in C2/c REM SHELXT solution in C2/c: R1 0.131, Rweak 0.009, Alpha 0.040 REM 0.418 for 322 systematic absences, Orientation as input REM Formula found by SHELXT: C30 N4 Si5 Cl Fe CELL 1.54178 37.0728 13.2937 17.4231 90 110.472 90 ZERR 4 0.0013 0.0005 0.0006 0 0.001 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Cl Fe N Si UNIT 240 480 8 8 32 40 L.S. 9 0 0 PLAN 20 SIZE 0.18 0.2 0.12 TEMP -123.28 list 4 fmap 2 53 acta OMIT -33 9 2 OMIT 12 14 5 REM REM REM WGHT 0.057900 3.097700 FVAR 0.26077 FE1 4 0.654953 0.506077 0.289742 11.00000 0.01834 0.01858 = 0.02556 -0.00008 0.00762 -0.00283 SI4 6 0.720688 0.629409 0.251811 11.00000 0.01967 0.02354 = 0.02787 -0.00242 0.01089 -0.00275 SI1 6 0.604919 0.640164 0.277845 11.00000 0.01940 0.02094 = 0.02935 -0.00080 0.01135 -0.00031 CL1 3 0.569260 0.626119 0.348689 11.00000 0.04096 0.04592 = 0.05760 0.00734 0.03557 0.00156 SI2 6 0.626814 0.314533 0.182038 11.00000 0.02516 0.02090 = 0.04331 -0.00726 0.00275 0.00190 SI5 6 0.741032 0.495224 0.400585 11.00000 0.02189 0.03633 = 0.03170 0.00634 0.00384 0.00014 SI3 6 0.614399 0.336699 0.347526 11.00000 0.04853 0.03388 = 0.05400 0.00663 0.02445 -0.01358 N3 5 0.708077 0.546246 0.313096 11.00000 0.01955 0.02469 = 0.02600 -0.00121 0.00624 -0.00145 N1 5 0.610672 0.776362 0.278364 11.00000 0.02298 0.01995 = 0.02762 -0.00397 0.00949 0.00063 N2 5 0.571071 0.691697 0.181720 11.00000 0.01788 0.02202 = 0.03161 -0.00467 0.00641 0.00108 N4 5 0.628888 0.376657 0.269530 11.00000 0.02876 0.01980 = 0.03956 -0.00042 0.01036 -0.00586 C10 1 0.584778 0.784705 0.202151 11.00000 0.01744 0.02388 = 0.02896 -0.00288 0.01315 0.00114 C2 1 0.523111 0.943254 0.199927 11.00000 0.01897 0.02382 = 0.04074 -0.00052 0.01241 0.00109 C4 1 0.546756 0.946075 0.145934 11.00000 0.02301 0.02293 = 0.03684 0.00110 0.01097 -0.00148 C1 1 0.511195 1.032721 0.225546 11.00000 0.03310 0.01746 = 0.05563 0.00344 0.02243 -0.00257 AFIX 43 H1 2 0.518645 1.095079 0.208984 11.00000 -1.20000 AFIX 0 C15 1 0.546063 0.645169 0.103635 11.00000 0.01869 0.03278 = 0.03624 -0.01255 0.00405 -0.00022 C9 1 0.575337 0.874822 0.148413 11.00000 0.02267 0.02462 = 0.03150 0.00017 0.01183 -0.00034 C11 1 0.634241 0.851765 0.337814 11.00000 0.02599 0.02798 = 0.03465 -0.01053 0.00980 -0.00366 C3 1 0.511253 0.853544 0.225703 11.00000 0.02358 0.01975 = 0.05244 -0.00045 0.01916 0.00209 AFIX 43 H3 2 0.518850 0.791201 0.209426 11.00000 -1.20000 AFIX 0 C25 1 0.676774 0.684970 0.172526 11.00000 0.02733 0.03397 = 0.03152 0.00466 0.01225 0.00015 AFIX 137 H25A 2 0.661695 0.631313 0.137136 11.00000 -1.50000 H25B 2 0.684676 0.733808 0.139327 11.00000 -1.50000 H25C 2 0.661050 0.718765 0.199765 11.00000 -1.50000 AFIX 0 C24 1 0.748750 0.569711 0.193283 11.00000 0.03543 0.03987 = 0.04672 -0.00680 0.02560 -0.00507 AFIX 137 H24A 2 0.773768 0.547304 0.231507 11.00000 -1.50000 H24B 2 0.752711 0.618767 0.154995 11.00000 -1.50000 H24C 2 0.734483 0.511764 0.162663 11.00000 -1.50000 AFIX 0 C8 1 0.596149 0.883947 0.096108 11.00000 0.03284 0.04056 = 0.03859 0.00551 0.01860 0.00652 AFIX 43 H8 2 0.615707 0.836295 0.099218 11.00000 -1.20000 AFIX 0 C16 1 0.571231 0.608073 0.056678 11.00000 0.03189 0.04910 = 0.03770 -0.01063 0.01179 -0.00139 AFIX 137 H16A 2 0.584012 0.665517 0.041827 11.00000 -1.50000 H16B 2 0.555196 0.573273 0.006836 11.00000 -1.50000 H16C 2 0.590687 0.561546 0.091139 11.00000 -1.50000 AFIX 0 C23 1 0.749312 0.738558 0.310644 11.00000 0.03013 0.03231 = 0.04664 -0.00862 0.01510 -0.00806 AFIX 137 H23A 2 0.735443 0.769918 0.343064 11.00000 -1.50000 H23B 2 0.752985 0.788015 0.272315 11.00000 -1.50000 H23C 2 0.774457 0.714742 0.347278 11.00000 -1.50000 AFIX 0 C5 1 0.540119 1.022731 0.087886 11.00000 0.03017 0.02972 = 0.04388 0.00520 0.01358 0.00390 AFIX 43 H5 2 0.520868 1.071437 0.084482 11.00000 -1.20000 AFIX 0 C7 1 0.588877 0.960866 0.039922 11.00000 0.04694 0.04842 = 0.04136 0.01254 0.02637 0.00556 AFIX 43 H7 2 0.603283 0.966233 0.004473 11.00000 -1.20000 AFIX 0 C13 1 0.662099 0.789396 0.407166 11.00000 0.04401 0.04376 = 0.03143 -0.00438 0.00361 -0.01214 AFIX 137 H13A 2 0.647447 0.746826 0.431697 11.00000 -1.50000 H13B 2 0.678876 0.834496 0.448998 11.00000 -1.50000 H13C 2 0.677817 0.746921 0.385222 11.00000 -1.50000 AFIX 0 C19 1 0.655175 0.385311 0.129351 11.00000 0.05221 0.03650 = 0.03866 -0.00372 0.01686 0.00913 AFIX 137 H19A 2 0.643425 0.451437 0.112269 11.00000 -1.50000 H19B 2 0.655243 0.347537 0.081100 11.00000 -1.50000 H19C 2 0.681695 0.393987 0.167119 11.00000 -1.50000 AFIX 0 C6 1 0.560398 1.030431 0.035412 11.00000 0.04619 0.03865 = 0.04166 0.01275 0.01749 0.00448 AFIX 43 H6 2 0.554891 1.083234 -0.003747 11.00000 -1.20000 AFIX 0 C14 1 0.656994 0.917962 0.299962 11.00000 0.04400 0.02922 = 0.04759 -0.00314 0.00880 -0.01481 AFIX 137 H14A 2 0.674059 0.875919 0.281395 11.00000 -1.50000 H14B 2 0.672415 0.966121 0.340910 11.00000 -1.50000 H14C 2 0.639181 0.954530 0.253175 11.00000 -1.50000 AFIX 0 C20 1 0.635249 0.423440 0.437960 11.00000 0.04938 0.06733 = 0.03665 0.00989 0.02021 -0.00601 AFIX 137 H20A 2 0.659195 0.394618 0.475819 11.00000 -1.50000 H20B 2 0.616759 0.431623 0.466227 11.00000 -1.50000 H20C 2 0.640626 0.489147 0.418821 11.00000 -1.50000 AFIX 0 C18 1 0.526846 0.556100 0.129471 11.00000 0.03528 0.04673 = 0.05817 -0.02123 0.02020 -0.01655 AFIX 137 H18A 2 0.546671 0.511046 0.164723 11.00000 -1.50000 H18B 2 0.510838 0.519393 0.080665 11.00000 -1.50000 H18C 2 0.510707 0.580756 0.159589 11.00000 -1.50000 AFIX 0 C27 1 0.792185 0.496214 0.403564 11.00000 0.02404 0.06238 = 0.05500 0.01309 0.00720 0.00847 AFIX 137 H27A 2 0.793919 0.458478 0.356660 11.00000 -1.50000 H27B 2 0.808874 0.464892 0.454530 11.00000 -1.50000 H27C 2 0.800441 0.565789 0.401057 11.00000 -1.50000 AFIX 0 C17 1 0.515271 0.716340 0.049688 11.00000 0.03947 0.05847 = 0.05135 -0.01635 -0.01514 0.01458 AFIX 137 H17A 2 0.500313 0.743888 0.081369 11.00000 -1.50000 H17B 2 0.498108 0.679386 0.002299 11.00000 -1.50000 H17C 2 0.527627 0.771428 0.030769 11.00000 -1.50000 AFIX 0 C00Z 1 0.646201 0.184229 0.200548 11.00000 0.04640 0.02688 = 0.07645 -0.00407 0.01360 0.00933 AFIX 137 H00A 2 0.671437 0.184828 0.244486 11.00000 -1.50000 H00B 2 0.648878 0.157754 0.150317 11.00000 -1.50000 H00C 2 0.628503 0.141445 0.216594 11.00000 -1.50000 AFIX 0 C28 1 0.730914 0.359351 0.413244 11.00000 0.04428 0.03995 = 0.07432 0.02466 0.00663 0.00381 AFIX 137 H28A 2 0.704704 0.352326 0.413874 11.00000 -1.50000 H28B 2 0.749368 0.334174 0.464943 11.00000 -1.50000 H28C 2 0.733375 0.320480 0.367536 11.00000 -1.50000 AFIX 0 C26 1 0.740135 0.567540 0.492447 11.00000 0.03774 0.07317 = 0.02794 0.00347 0.00515 -0.00623 AFIX 137 H26A 2 0.745372 0.638699 0.486003 11.00000 -1.50000 H26B 2 0.759840 0.540856 0.541844 11.00000 -1.50000 H26C 2 0.714726 0.560816 0.497451 11.00000 -1.50000 AFIX 0 C012 1 0.576242 0.303112 0.106883 11.00000 0.03555 0.04306 = 0.07257 -0.02215 -0.00895 0.00747 AFIX 137 H01A 2 0.561054 0.261034 0.130456 11.00000 -1.50000 H01B 2 0.576730 0.272249 0.056175 11.00000 -1.50000 H01C 2 0.564584 0.370101 0.094847 11.00000 -1.50000 AFIX 0 C22 1 0.560628 0.335925 0.318666 11.00000 0.05575 0.08787 = 0.07948 -0.01292 0.03776 -0.03770 AFIX 137 H22A 2 0.550727 0.404546 0.305558 11.00000 -1.50000 H22B 2 0.553887 0.310211 0.364622 11.00000 -1.50000 H22C 2 0.549205 0.292614 0.270754 11.00000 -1.50000 AFIX 0 C12 1 0.608623 0.915906 0.369380 11.00000 0.04050 0.07059 = 0.07668 -0.05168 0.02008 -0.00201 AFIX 137 H12A 2 0.591300 0.955994 0.324305 11.00000 -1.50000 H12B 2 0.624602 0.960859 0.412460 11.00000 -1.50000 H12C 2 0.593400 0.872340 0.391787 11.00000 -1.50000 AFIX 0 C21 1 0.631452 0.207227 0.386414 11.00000 0.14217 0.04127 = 0.10580 0.02818 0.06461 -0.00331 AFIX 137 H21A 2 0.617632 0.157283 0.345264 11.00000 -1.50000 H21B 2 0.626489 0.194940 0.437292 11.00000 -1.50000 H21C 2 0.659140 0.201843 0.396995 11.00000 -1.50000 AFIX 0 HKLF 4 REM cu_hzy2962_0m_a.res in C2/c REM wR2 = 0.1190, GooF = S = 1.077, Restrained GooF = 1.077 for all data REM R1 = 0.0415 for 6272 Fo > 4sig(Fo) and 0.0464 for all 7108 data REM 388 parameters refined using 0 restraints END WGHT 0.0578 3.1141 REM Highest difference peak 0.312, deepest hole -0.298, 1-sigma level 0.067 Q1 1 0.5392 0.9429 0.1750 11.00000 0.05 0.31 Q2 1 0.6389 0.4365 0.2820 11.00000 0.05 0.28 Q3 1 0.5609 0.9097 0.1556 11.00000 0.05 0.28 Q4 1 0.6365 0.2964 0.2657 11.00000 0.05 0.27 Q5 1 0.6990 0.6403 0.2069 11.00000 0.05 0.27 Q6 1 0.6168 0.7291 0.2930 11.00000 0.05 0.26 Q7 1 0.5626 0.5061 0.2812 11.00000 0.05 0.26 Q8 1 0.6393 0.6001 0.3010 11.00000 0.05 0.25 Q9 1 0.6183 0.4821 0.4380 11.00000 0.05 0.24 Q10 1 0.6749 0.7330 0.2790 11.00000 0.05 0.23 Q11 1 0.7234 0.5146 0.3249 11.00000 0.05 0.23 Q12 1 0.7377 0.6935 0.2805 11.00000 0.05 0.23 Q13 1 0.5582 0.3600 0.1631 11.00000 0.05 0.23 Q14 1 0.5209 0.5064 0.0489 11.00000 0.05 0.22 Q15 1 0.6374 0.9185 0.4764 11.00000 0.05 0.22 Q16 1 0.6409 0.8143 0.4159 11.00000 0.05 0.22 Q17 1 0.6245 0.8931 0.3382 11.00000 0.05 0.22 Q18 1 0.5651 0.7381 0.1910 11.00000 0.05 0.21 Q19 1 0.5000 0.4979 0.2500 10.50000 0.05 0.21 Q20 1 0.5785 0.8210 0.1783 11.00000 0.05 0.21 ; _shelx_res_checksum 5077 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.65495(2) 0.50608(3) 0.28974(2) 0.02084(12) Uani 1 1 d . . . . . Si4 Si 0.72069(2) 0.62941(5) 0.25181(3) 0.02301(15) Uani 1 1 d . . . . . Si1 Si 0.60492(2) 0.64016(5) 0.27785(3) 0.02247(15) Uani 1 1 d . . . . . Cl1 Cl 0.56926(2) 0.62612(6) 0.34869(4) 0.04329(18) Uani 1 1 d . . . . . Si2 Si 0.62681(2) 0.31453(5) 0.18204(4) 0.03224(17) Uani 1 1 d . . . . . Si5 Si 0.74103(2) 0.49522(5) 0.40058(4) 0.03144(18) Uani 1 1 d . . . . . Si3 Si 0.61440(2) 0.33670(7) 0.34753(5) 0.0437(2) Uani 1 1 d . . . . . N3 N 0.70808(5) 0.54625(15) 0.31310(10) 0.0239(4) Uani 1 1 d . . . . . N1 N 0.61067(5) 0.77636(15) 0.27836(10) 0.0233(4) Uani 1 1 d . . . . . N2 N 0.57107(5) 0.69170(15) 0.18172(11) 0.0244(4) Uani 1 1 d . . . . . N4 N 0.62889(6) 0.37666(15) 0.26953(11) 0.0298(4) Uani 1 1 d . . . . . C10 C 0.58478(6) 0.78471(18) 0.20215(12) 0.0221(5) Uani 1 1 d . . . . . C2 C 0.52311(6) 0.94325(19) 0.19993(14) 0.0273(5) Uani 1 1 d . . . . . C4 C 0.54676(6) 0.94607(19) 0.14593(13) 0.0275(5) Uani 1 1 d . . . . . C1 C 0.51119(7) 1.0327(2) 0.22555(16) 0.0336(5) Uani 1 1 d . . . . . H1 H 0.518645 1.095079 0.208984 0.040 Uiso 1 1 calc R . . . . C15 C 0.54606(6) 0.6452(2) 0.10363(14) 0.0307(5) Uani 1 1 d . . . . . C9 C 0.57534(6) 0.87482(18) 0.14841(13) 0.0256(5) Uani 1 1 d . . . . . C11 C 0.63424(7) 0.85176(19) 0.33781(13) 0.0298(5) Uani 1 1 d . . . . . C3 C 0.51125(6) 0.85354(18) 0.22570(15) 0.0304(5) Uani 1 1 d . . . . . H3 H 0.518850 0.791201 0.209426 0.036 Uiso 1 1 calc R . . . . C25 C 0.67677(7) 0.6850(2) 0.17253(13) 0.0304(5) Uani 1 1 d . . . . . H25A H 0.661695 0.631313 0.137136 0.046 Uiso 1 1 calc GR . . . . H25B H 0.684676 0.733808 0.139327 0.046 Uiso 1 1 calc GR . . . . H25C H 0.661050 0.718765 0.199765 0.046 Uiso 1 1 calc GR . . . . C24 C 0.74875(7) 0.5697(2) 0.19328(15) 0.0377(6) Uani 1 1 d . . . . . H24A H 0.773768 0.547304 0.231507 0.057 Uiso 1 1 calc GR . . . . H24B H 0.752711 0.618767 0.154995 0.057 Uiso 1 1 calc GR . . . . H24C H 0.734483 0.511764 0.162663 0.057 Uiso 1 1 calc GR . . . . C8 C 0.59615(7) 0.8839(2) 0.09611(14) 0.0357(6) Uani 1 1 d . . . . . H8 H 0.615707 0.836295 0.099218 0.043 Uiso 1 1 calc R . . . . C16 C 0.57123(7) 0.6081(2) 0.05668(15) 0.0397(6) Uani 1 1 d . . . . . H16A H 0.584012 0.665517 0.041827 0.059 Uiso 1 1 calc GR . . . . H16B H 0.555196 0.573273 0.006836 0.059 Uiso 1 1 calc GR . . . . H16C H 0.590687 0.561546 0.091139 0.059 Uiso 1 1 calc GR . . . . C23 C 0.74931(7) 0.7386(2) 0.31064(15) 0.0359(6) Uani 1 1 d . . . . . H23A H 0.735443 0.769918 0.343064 0.054 Uiso 1 1 calc GR . . . . H23B H 0.752985 0.788015 0.272315 0.054 Uiso 1 1 calc GR . . . . H23C H 0.774457 0.714742 0.347278 0.054 Uiso 1 1 calc GR . . . . C5 C 0.54012(7) 1.0227(2) 0.08789(15) 0.0344(6) Uani 1 1 d . . . . . H5 H 0.520868 1.071437 0.084482 0.041 Uiso 1 1 calc R . . . . C7 C 0.58888(8) 0.9609(2) 0.03992(16) 0.0427(7) Uani 1 1 d . . . . . H7 H 0.603283 0.966233 0.004473 0.051 Uiso 1 1 calc R . . . . C13 C 0.66210(8) 0.7894(2) 0.40717(14) 0.0423(7) Uani 1 1 d . . . . . H13A H 0.647447 0.746826 0.431697 0.063 Uiso 1 1 calc GR . . . . H13B H 0.678876 0.834496 0.448998 0.063 Uiso 1 1 calc GR . . . . H13C H 0.677817 0.746921 0.385222 0.063 Uiso 1 1 calc GR . . . . C19 C 0.65518(8) 0.3853(2) 0.12935(15) 0.0422(7) Uani 1 1 d . . . . . H19A H 0.643425 0.451437 0.112269 0.063 Uiso 1 1 calc GR . . . . H19B H 0.655243 0.347537 0.081100 0.063 Uiso 1 1 calc GR . . . . H19C H 0.681695 0.393987 0.167119 0.063 Uiso 1 1 calc GR . . . . C6 C 0.56040(8) 1.0304(2) 0.03541(16) 0.0416(6) Uani 1 1 d . . . . . H6 H 0.554891 1.083234 -0.003747 0.050 Uiso 1 1 calc R . . . . C14 C 0.65699(8) 0.9180(2) 0.29996(16) 0.0422(7) Uani 1 1 d . . . . . H14A H 0.674059 0.875919 0.281395 0.063 Uiso 1 1 calc GR . . . . H14B H 0.672415 0.966121 0.340910 0.063 Uiso 1 1 calc GR . . . . H14C H 0.639181 0.954530 0.253175 0.063 Uiso 1 1 calc GR . . . . C20 C 0.63525(9) 0.4234(3) 0.43796(15) 0.0497(8) Uani 1 1 d . . . . . H20A H 0.659195 0.394618 0.475819 0.075 Uiso 1 1 calc GR . . . . H20B H 0.616759 0.431623 0.466227 0.075 Uiso 1 1 calc GR . . . . H20C H 0.640626 0.489147 0.418821 0.075 Uiso 1 1 calc GR . . . . C18 C 0.52685(8) 0.5561(2) 0.12947(18) 0.0457(7) Uani 1 1 d . . . . . H18A H 0.546671 0.511046 0.164723 0.069 Uiso 1 1 calc GR . . . . H18B H 0.510838 0.519393 0.080665 0.069 Uiso 1 1 calc GR . . . . H18C H 0.510707 0.580756 0.159589 0.069 Uiso 1 1 calc GR . . . . C27 C 0.79218(8) 0.4962(2) 0.40356(19) 0.0489(8) Uani 1 1 d . . . . . H27A H 0.793919 0.458478 0.356660 0.073 Uiso 1 1 calc GR . . . . H27B H 0.808874 0.464892 0.454530 0.073 Uiso 1 1 calc GR . . . . H27C H 0.800441 0.565789 0.401057 0.073 Uiso 1 1 calc GR . . . . C17 C 0.51527(8) 0.7163(3) 0.04969(18) 0.0580(9) Uani 1 1 d . . . . . H17A H 0.500313 0.743888 0.081369 0.087 Uiso 1 1 calc GR . . . . H17B H 0.498108 0.679386 0.002299 0.087 Uiso 1 1 calc GR . . . . H17C H 0.527627 0.771428 0.030769 0.087 Uiso 1 1 calc GR . . . . C00Z C 0.64620(9) 0.1842(2) 0.2005(2) 0.0520(8) Uani 1 1 d . . . . . H00A H 0.671437 0.184828 0.244486 0.078 Uiso 1 1 calc GR . . . . H00B H 0.648878 0.157754 0.150317 0.078 Uiso 1 1 calc GR . . . . H00C H 0.628503 0.141445 0.216594 0.078 Uiso 1 1 calc GR . . . . C28 C 0.73091(9) 0.3594(2) 0.4132(2) 0.0566(9) Uani 1 1 d . . . . . H28A H 0.704704 0.352326 0.413874 0.085 Uiso 1 1 calc GR . . . . H28B H 0.749368 0.334174 0.464943 0.085 Uiso 1 1 calc GR . . . . H28C H 0.733375 0.320480 0.367536 0.085 Uiso 1 1 calc GR . . . . C26 C 0.74014(8) 0.5675(3) 0.49245(14) 0.0480(8) Uani 1 1 d . . . . . H26A H 0.745372 0.638699 0.486003 0.072 Uiso 1 1 calc GR . . . . H26B H 0.759840 0.540856 0.541844 0.072 Uiso 1 1 calc GR . . . . H26C H 0.714726 0.560816 0.497451 0.072 Uiso 1 1 calc GR . . . . C012 C 0.57624(8) 0.3031(2) 0.1069(2) 0.0578(9) Uani 1 1 d . . . . . H01A H 0.561054 0.261034 0.130456 0.087 Uiso 1 1 calc GR . . . . H01B H 0.576730 0.272249 0.056175 0.087 Uiso 1 1 calc GR . . . . H01C H 0.564584 0.370101 0.094847 0.087 Uiso 1 1 calc GR . . . . C22 C 0.56063(10) 0.3359(3) 0.3187(2) 0.0706(11) Uani 1 1 d . . . . . H22A H 0.550727 0.404546 0.305558 0.106 Uiso 1 1 calc GR . . . . H22B H 0.553887 0.310211 0.364622 0.106 Uiso 1 1 calc GR . . . . H22C H 0.549205 0.292614 0.270754 0.106 Uiso 1 1 calc GR . . . . C12 C 0.60862(9) 0.9159(3) 0.3694(2) 0.0627(10) Uani 1 1 d . . . . . H12A H 0.591300 0.955994 0.324305 0.094 Uiso 1 1 calc GR . . . . H12B H 0.624602 0.960859 0.412460 0.094 Uiso 1 1 calc GR . . . . H12C H 0.593400 0.872340 0.391787 0.094 Uiso 1 1 calc GR . . . . C21 C 0.63145(16) 0.2072(3) 0.3864(3) 0.0908(15) Uani 1 1 d . . . . . H21A H 0.617632 0.157283 0.345264 0.136 Uiso 1 1 calc GR . . . . H21B H 0.626489 0.194940 0.437292 0.136 Uiso 1 1 calc GR . . . . H21C H 0.659140 0.201843 0.396995 0.136 Uiso 1 1 calc GR . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01834(19) 0.0186(2) 0.02556(18) -0.00008(12) 0.00762(14) -0.00283(13) Si4 0.0197(3) 0.0235(3) 0.0279(3) -0.0024(2) 0.0109(2) -0.0027(2) Si1 0.0194(3) 0.0209(3) 0.0293(3) -0.0008(2) 0.0114(2) -0.0003(2) Cl1 0.0410(3) 0.0459(4) 0.0576(4) 0.0073(3) 0.0356(3) 0.0016(3) Si2 0.0252(3) 0.0209(4) 0.0433(3) -0.0073(3) 0.0028(3) 0.0019(3) Si5 0.0219(3) 0.0363(4) 0.0317(3) 0.0063(3) 0.0038(3) 0.0001(2) Si3 0.0485(4) 0.0339(5) 0.0540(4) 0.0066(3) 0.0244(3) -0.0136(3) N3 0.0196(8) 0.0247(11) 0.0260(8) -0.0012(7) 0.0062(7) -0.0015(8) N1 0.0230(9) 0.0200(10) 0.0276(8) -0.0040(7) 0.0095(7) 0.0006(7) N2 0.0179(8) 0.0220(11) 0.0316(8) -0.0047(8) 0.0064(7) 0.0011(7) N4 0.0288(10) 0.0198(11) 0.0396(10) -0.0004(8) 0.0104(8) -0.0059(8) C10 0.0174(9) 0.0239(13) 0.0290(10) -0.0029(8) 0.0132(8) 0.0011(8) C2 0.0190(10) 0.0238(13) 0.0407(11) -0.0005(10) 0.0124(9) 0.0011(9) C4 0.0230(10) 0.0229(13) 0.0368(11) 0.0011(9) 0.0110(9) -0.0015(9) C1 0.0331(12) 0.0175(13) 0.0556(14) 0.0034(11) 0.0224(11) -0.0026(10) C15 0.0187(10) 0.0328(15) 0.0362(11) -0.0126(10) 0.0040(9) -0.0002(10) C9 0.0227(10) 0.0246(13) 0.0315(10) 0.0002(9) 0.0118(9) -0.0003(9) C11 0.0260(11) 0.0280(14) 0.0346(11) -0.0105(10) 0.0098(9) -0.0037(10) C3 0.0236(11) 0.0198(13) 0.0524(13) -0.0004(10) 0.0192(10) 0.0021(9) C25 0.0273(11) 0.0340(15) 0.0315(10) 0.0047(10) 0.0123(9) 0.0001(10) C24 0.0354(13) 0.0399(16) 0.0467(13) -0.0068(11) 0.0256(11) -0.0051(11) C8 0.0328(13) 0.0406(17) 0.0386(12) 0.0055(11) 0.0186(10) 0.0065(11) C16 0.0319(13) 0.0491(18) 0.0377(12) -0.0106(12) 0.0118(10) -0.0014(12) C23 0.0301(12) 0.0323(15) 0.0466(12) -0.0086(11) 0.0151(10) -0.0081(11) C5 0.0302(12) 0.0297(14) 0.0439(13) 0.0052(11) 0.0136(10) 0.0039(11) C7 0.0469(15) 0.0484(19) 0.0414(13) 0.0125(12) 0.0264(12) 0.0056(14) C13 0.0440(15) 0.0438(18) 0.0314(11) -0.0044(11) 0.0036(11) -0.0121(13) C19 0.0522(16) 0.0365(17) 0.0387(12) -0.0037(11) 0.0169(12) 0.0091(13) C6 0.0462(15) 0.0387(17) 0.0417(13) 0.0127(12) 0.0175(12) 0.0045(13) C14 0.0440(15) 0.0292(16) 0.0476(13) -0.0031(11) 0.0088(12) -0.0148(12) C20 0.0494(16) 0.067(2) 0.0367(12) 0.0099(13) 0.0202(12) -0.0060(15) C18 0.0353(14) 0.0467(19) 0.0582(15) -0.0212(14) 0.0202(12) -0.0165(13) C27 0.0240(13) 0.062(2) 0.0550(17) 0.0131(13) 0.0072(12) 0.0085(12) C17 0.0395(15) 0.058(2) 0.0514(15) -0.0164(14) -0.0151(13) 0.0146(15) C00Z 0.0464(16) 0.0269(16) 0.0764(19) -0.0041(14) 0.0136(15) 0.0093(13) C28 0.0443(16) 0.0399(19) 0.0743(19) 0.0247(15) 0.0066(15) 0.0038(14) C26 0.0377(14) 0.073(2) 0.0279(11) 0.0035(13) 0.0051(10) -0.0062(14) C012 0.0355(15) 0.0431(19) 0.0726(18) -0.0222(15) -0.0089(14) 0.0075(13) C22 0.056(2) 0.088(3) 0.079(2) -0.013(2) 0.0378(18) -0.038(2) C12 0.0405(15) 0.071(3) 0.0767(19) -0.0517(19) 0.0201(14) -0.0020(16) C21 0.142(4) 0.041(2) 0.106(3) 0.028(2) 0.065(3) -0.003(3) 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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Fe1 Si1 118.99(6) . . ? N3 Fe1 N4 133.23(9) . . ? N4 Fe1 Si1 107.77(6) . . ? N3 Si4 C25 110.92(10) . . ? N3 Si4 C24 113.06(12) . . ? N3 Si4 C23 112.60(10) . . ? C24 Si4 C25 105.68(11) . . ? C24 Si4 C23 108.06(12) . . ? C23 Si4 C25 106.06(12) . . ? Cl1 Si1 Fe1 118.80(3) . . ? Cl1 Si1 C10 105.37(6) . . ? N1 Si1 Fe1 128.22(6) . . ? N1 Si1 Cl1 100.44(7) . . ? N1 Si1 N2 71.08(8) . . ? N1 Si1 C10 35.68(7) . . ? N2 Si1 Fe1 125.80(6) . . ? N2 Si1 Cl1 101.44(7) . . ? N2 Si1 C10 35.48(8) . . ? C10 Si1 Fe1 135.81(6) . . ? N4 Si2 C19 109.64(11) . . ? N4 Si2 C00Z 113.62(13) . . ? N4 Si2 C012 112.48(13) . . ? C19 Si2 C012 107.05(15) . . ? C00Z Si2 C19 107.68(15) . . ? C00Z Si2 C012 106.04(14) . . ? N3 Si5 C27 114.70(12) . . ? N3 Si5 C28 111.97(12) . . ? N3 Si5 C26 109.51(11) . . ? C28 Si5 C27 104.19(15) . . ? C28 Si5 C26 109.23(16) . . ? C26 Si5 C27 106.95(14) . . ? N4 Si3 C20 108.84(12) . . ? N4 Si3 C22 112.82(14) . . ? N4 Si3 C21 114.32(17) . . ? C22 Si3 C20 108.27(16) . . ? C21 Si3 C20 105.74(19) . . ? C21 Si3 C22 106.5(2) . . ? Si4 N3 Fe1 121.69(9) . . ? Si4 N3 Si5 122.81(11) . . ? Si5 N3 Fe1 115.48(10) . . ? C10 N1 Si1 92.02(14) . . ? C10 N1 C11 132.5(2) . . ? C11 N1 Si1 135.46(15) . . ? C10 N2 Si1 91.56(13) . . ? C10 N2 C15 133.3(2) . . ? C15 N2 Si1 133.40(16) . . ? Si2 N4 Fe1 116.93(11) . . ? Si3 N4 Fe1 113.89(11) . . ? Si3 N4 Si2 128.95(13) . . ? N1 C10 Si1 52.30(12) . . ? N1 C10 C9 128.2(2) . . ? N2 C10 Si1 52.95(11) . . ? N2 C10 N1 105.10(19) . . ? N2 C10 C9 126.47(18) . . ? C9 C10 Si1 172.85(16) . . ? C1 C2 C4 120.1(2) . . ? C1 C2 C3 117.0(2) . . ? C3 C2 C4 122.9(2) . . ? C9 C4 C2 124.3(2) . . ? C5 C4 C2 118.8(2) . . ? C5 C4 C9 116.9(2) . . ? C1 C1 C2 121.53(15) 2_655 . ? N2 C15 C16 108.86(18) . . ? N2 C15 C18 105.0(2) . . ? N2 C15 C17 113.5(2) . . ? C16 C15 C18 110.1(2) . . ? C16 C15 C17 109.7(2) . . ? C17 C15 C18 109.6(2) . . ? C4 C9 C10 124.7(2) . . ? C8 C9 C10 114.9(2) . . ? C8 C9 C4 120.3(2) . . ? N1 C11 C13 104.8(2) . . ? N1 C11 C14 111.62(19) . . ? N1 C11 C12 110.01(19) . . ? C14 C11 C13 109.4(2) . . ? C12 C11 C13 110.7(2) . . ? C12 C11 C14 110.2(3) . . ? C3 C3 C2 121.48(14) 2_655 . ? C7 C8 C9 121.1(3) . . ? C6 C5 C4 122.5(3) . . ? C8 C7 C6 119.5(3) . . ? C5 C6 C7 119.7(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 Si1 2.5282(7) . ? Fe1 N3 1.9414(18) . ? Fe1 N4 1.944(2) . ? Si4 N3 1.712(2) . ? Si4 C25 1.879(2) . ? Si4 C24 1.869(3) . ? Si4 C23 1.877(3) . ? Si1 Cl1 2.1089(8) . ? Si1 N1 1.823(2) . ? Si1 N2 1.8382(18) . ? Si1 C10 2.302(2) . ? Si2 N4 1.712(2) . ? Si2 C19 1.873(3) . ? Si2 C00Z 1.860(3) . ? Si2 C012 1.880(3) . ? Si5 N3 1.7244(17) . ? Si5 C27 1.879(3) . ? Si5 C28 1.873(3) . ? Si5 C26 1.877(3) . ? Si3 N4 1.711(2) . ? Si3 C20 1.886(3) . ? Si3 C22 1.878(4) . ? Si3 C21 1.877(4) . ? N1 C10 1.344(3) . ? N1 C11 1.486(3) . ? N2 C10 1.337(3) . ? N2 C15 1.487(3) . ? C10 C9 1.485(3) . ? C2 C4 1.494(3) . ? C2 C1 1.395(4) . ? C2 C3 1.398(3) . ? C4 C9 1.411(3) . ? C4 C5 1.396(4) . ? C1 C1 1.382(5) 2_655 ? C15 C16 1.522(4) . ? C15 C18 1.529(4) . ? C15 C17 1.527(4) . ? C9 C8 1.390(3) . ? C11 C13 1.530(3) . ? C11 C14 1.520(4) . ? C11 C12 1.516(4) . ? C3 C3 1.381(5) 2_655 ? C8 C7 1.375(4) . ? C5 C6 1.376(4) . ? C7 C6 1.385(4) . ?