#------------------------------------------------------------------------------ #$Date: 2020-10-06 11:48:21 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257536 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/51/7705164.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_7705164 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 'C27 H59 Cl Fe N4 Si5' _chemical_formula_sum 'C27 H59 Cl Fe N4 Si5' _chemical_formula_weight 671.53 _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-10-15 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-02-14 deposited with the CCDC. 2020-08-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 26.9482(14) _cell_length_b 16.5518(8) _cell_length_c 8.8695(4) _cell_measurement_reflns_used 9332 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.36 _cell_measurement_theta_min 2.575 _cell_volume 3956.2(3) _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 149.96 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_unetI/netI 0.0468 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 47547 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.433 _diffrn_reflns_theta_min 2.461 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.621 _exptl_absorpt_correction_T_max 0.0276 _exptl_absorpt_correction_T_min 0.0108 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1091 before and 0.0873 after correction. The Ratio of minimum to maximum transmission is 0.3913. The \l/2 correction factor is Not present.' _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.127 _exptl_crystal_description block _exptl_crystal_F_000 1448 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Pentane' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.17 _refine_diff_density_max 0.583 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.058 _refine_ls_abs_structure_details ; Flack x determined using 2868 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.045(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 361 _refine_ls_number_reflns 8032 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0431 _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^)+(0.0625P)^2^+1.6383P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1163 _refine_ls_wR_factor_ref 0.1220 _reflns_Friedel_coverage 0.854 _reflns_Friedel_fraction_full 0.980 _reflns_Friedel_fraction_max 0.974 _reflns_number_gt 7021 _reflns_number_total 8032 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt00570c2.cif _cod_data_source_block 9 _cod_depositor_comments 'Adding full bibliography for 7705159--7705168.cif.' _cod_database_code 7705164 _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 0.902 _shelx_estimated_absorpt_t_min 0.870 _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: C3(H3), C4(H4), C5(H5), C7(H7), C6(H6) 2.b Idealised Me refined as rotating group: C25(H25A,H25B,H25C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C26(H26A,H26B, H26C), C17(H17A,H17B,H17C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C18(H18A, H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C00S(H00A,H00B,H00C), C20(H20A,H20B,H20C), C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C15(H15A,H15B, H15C), C22(H22A,H22B,H22C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C) ; _shelx_res_file ; TITL mo_hzy240_0ma_a.res in Pna2(1) mo_hzy240_0ma.res created by SHELXL-2018/3 at 13:19:18 on 15-Oct-2019 REM Old TITL mo_HZY240_0ma in Pna2(1) REM SHELXT solution in Pna2(1): R1 0.098, Rweak 0.016, Alpha 0.004 REM 1.087 for 252 systematic absences, Orientation as input REM Flack x = 0.093 ( 0.010 ) from 2935 Parsons' quotients REM Formula found by SHELXT: C27 N4 Si5 Cl Fe CELL 0.71073 26.9482 16.5518 8.8695 90 90 90 ZERR 4 0.0014 0.0008 0.0004 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,+Z SYMM 0.5-X,0.5+Y,0.5+Z SFAC C H Cl Fe N Si UNIT 108 236 4 4 16 20 L.S. 10 PLAN 20 SIZE 0.17 0.2 0.23 TEMP -123.19 list 4 fmap 2 53 acta REM REM REM WGHT 0.062500 1.638300 FVAR 0.43784 FE1 4 0.663618 0.653386 0.548230 11.00000 0.03126 0.03494 = 0.04055 0.00089 -0.00001 -0.00172 CL1 3 0.637422 0.880003 0.663737 11.00000 0.04889 0.03739 = 0.06182 -0.01606 -0.00690 0.00309 SI1 6 0.613598 0.780248 0.529710 11.00000 0.03532 0.03420 = 0.04672 -0.00051 0.00150 0.00024 SI5 6 0.583988 0.523837 0.443951 11.00000 0.03749 0.03922 = 0.05015 -0.00612 0.00265 -0.00417 SI2 6 0.763862 0.729954 0.671184 11.00000 0.03754 0.05401 = 0.05491 0.00227 -0.00570 -0.00641 SI3 6 0.762098 0.639751 0.371872 11.00000 0.03632 0.04973 = 0.04969 0.00617 0.00613 0.00365 SI4 6 0.639988 0.503683 0.741426 11.00000 0.03921 0.04754 = 0.05663 0.01517 -0.00053 -0.00037 N1 5 0.593444 0.832222 0.355612 11.00000 0.03745 0.04134 = 0.04259 0.00680 0.00281 0.00002 N2 5 0.545611 0.790111 0.532180 11.00000 0.03332 0.03754 = 0.04697 0.00352 0.00353 0.00096 N3 5 0.734043 0.676616 0.531099 11.00000 0.03337 0.04192 = 0.04744 0.00443 0.00249 -0.00137 N4 5 0.624550 0.555451 0.579855 11.00000 0.03462 0.03611 = 0.04851 0.00120 0.00466 -0.00086 C1 1 0.545427 0.823833 0.396052 11.00000 0.03831 0.03267 = 0.05885 -0.00203 0.00317 0.00290 C25 1 0.571237 0.607759 0.305080 11.00000 0.04720 0.05050 = 0.05451 -0.00322 -0.00522 -0.00268 AFIX 137 H25A 2 0.555490 0.653142 0.357484 11.00000 -1.50000 H25B 2 0.549064 0.587936 0.225700 11.00000 -1.50000 H25C 2 0.602540 0.625758 0.259975 11.00000 -1.50000 AFIX 0 C11 1 0.617361 0.866709 0.220524 11.00000 0.04041 0.05366 = 0.05961 0.02041 0.00870 0.00185 C2 1 0.501286 0.846673 0.303665 11.00000 0.03728 0.04821 = 0.06431 0.02052 0.00645 0.00424 C8 1 0.504404 0.772461 0.639162 11.00000 0.04116 0.04319 = 0.05463 0.00506 0.01519 -0.00074 C9 1 0.527294 0.715319 0.756748 11.00000 0.05547 0.05885 = 0.04742 0.00484 0.00552 -0.00519 AFIX 137 H9A 2 0.540340 0.667173 0.706107 11.00000 -1.50000 H9B 2 0.501810 0.699265 0.829657 11.00000 -1.50000 H9C 2 0.554326 0.743089 0.809449 11.00000 -1.50000 AFIX 0 C3 1 0.480796 0.791932 0.202579 11.00000 0.04798 0.06846 = 0.05360 0.01556 -0.00030 -0.00206 AFIX 43 H3 2 0.495345 0.740074 0.190214 11.00000 -1.20000 AFIX 0 C10 1 0.460748 0.729613 0.561145 11.00000 0.04133 0.06475 = 0.08041 0.01303 0.00896 -0.00809 AFIX 137 H10A 2 0.442914 0.768295 0.497419 11.00000 -1.50000 H10B 2 0.438126 0.707928 0.637607 11.00000 -1.50000 H10C 2 0.473391 0.685315 0.498701 11.00000 -1.50000 AFIX 0 C26 1 0.521084 0.493048 0.518196 11.00000 0.03961 0.06313 = 0.07898 -0.00141 0.00033 -0.00909 AFIX 137 H26A 2 0.522625 0.437366 0.555466 11.00000 -1.50000 H26B 2 0.496532 0.496618 0.436959 11.00000 -1.50000 H26C 2 0.511453 0.529182 0.600688 11.00000 -1.50000 AFIX 0 C17 1 0.725173 0.730368 0.847428 11.00000 0.06179 0.07336 = 0.04901 0.00263 -0.00168 -0.00619 AFIX 137 H17A 2 0.692098 0.751694 0.824500 11.00000 -1.50000 H17B 2 0.741083 0.764515 0.923659 11.00000 -1.50000 H17C 2 0.722161 0.675111 0.886046 11.00000 -1.50000 AFIX 0 C23 1 0.623358 0.564849 0.910583 11.00000 0.05447 0.08264 = 0.05773 0.01065 -0.00682 -0.00989 AFIX 137 H23A 2 0.640377 0.617114 0.905987 11.00000 -1.50000 H23B 2 0.633559 0.535993 1.001950 11.00000 -1.50000 H23C 2 0.587397 0.573586 0.912718 11.00000 -1.50000 AFIX 0 C24 1 0.607598 0.434863 0.332062 11.00000 0.07328 0.04883 = 0.07851 -0.01542 0.01241 -0.00341 AFIX 137 H24A 2 0.638241 0.450034 0.279728 11.00000 -1.50000 H24B 2 0.582518 0.418704 0.257949 11.00000 -1.50000 H24C 2 0.614301 0.389627 0.400380 11.00000 -1.50000 AFIX 0 C18 1 0.801236 0.717756 0.272694 11.00000 0.05170 0.06830 = 0.07675 0.00857 0.01973 -0.00437 AFIX 137 H18A 2 0.781354 0.766361 0.254475 11.00000 -1.50000 H18B 2 0.812842 0.695918 0.176237 11.00000 -1.50000 H18C 2 0.829859 0.731544 0.335806 11.00000 -1.50000 AFIX 0 C4 1 0.439235 0.812889 0.119954 11.00000 0.04487 0.09762 = 0.07723 0.03164 -0.00543 -0.01251 AFIX 43 H4 2 0.424766 0.775348 0.051899 11.00000 -1.20000 AFIX 0 C19 1 0.802836 0.550427 0.409376 11.00000 0.07181 0.06876 = 0.07202 0.00301 0.00964 0.02835 AFIX 137 H19A 2 0.829662 0.566147 0.477965 11.00000 -1.50000 H19B 2 0.817023 0.531127 0.314228 11.00000 -1.50000 H19C 2 0.783157 0.507227 0.455575 11.00000 -1.50000 AFIX 0 C21 1 0.708129 0.483677 0.747747 11.00000 0.04847 0.08129 = 0.08589 0.03962 0.00216 0.01080 AFIX 137 H21A 2 0.717320 0.447839 0.664348 11.00000 -1.50000 H21B 2 0.716630 0.457884 0.843790 11.00000 -1.50000 H21C 2 0.726208 0.534806 0.738422 11.00000 -1.50000 AFIX 0 C00S 1 0.488627 0.851771 0.715382 11.00000 0.07814 0.05769 = 0.09381 -0.00234 0.03738 0.00885 AFIX 137 H00A 2 0.517975 0.879144 0.755978 11.00000 -1.50000 H00B 2 0.465443 0.839958 0.797603 11.00000 -1.50000 H00C 2 0.472402 0.886795 0.641178 11.00000 -1.50000 AFIX 0 C20 1 0.713729 0.605940 0.235484 11.00000 0.05525 0.07512 = 0.05839 -0.00851 0.00362 -0.00393 AFIX 137 H20A 2 0.693165 0.564022 0.282233 11.00000 -1.50000 H20B 2 0.729765 0.584031 0.145137 11.00000 -1.50000 H20C 2 0.692829 0.651995 0.207385 11.00000 -1.50000 AFIX 0 C5 1 0.418733 0.889872 0.137588 11.00000 0.03817 0.10947 = 0.11128 0.05354 -0.00332 0.00326 AFIX 43 H5 2 0.390475 0.904873 0.079992 11.00000 -1.20000 AFIX 0 C16 1 0.825453 0.685119 0.723290 11.00000 0.04902 0.09721 = 0.08532 0.00053 -0.01943 -0.00057 AFIX 137 H16A 2 0.821203 0.627727 0.747182 11.00000 -1.50000 H16B 2 0.838839 0.713390 0.811441 11.00000 -1.50000 H16C 2 0.848492 0.690817 0.638466 11.00000 -1.50000 AFIX 0 C7 1 0.480384 0.923101 0.322014 11.00000 0.04825 0.05145 = 0.10482 0.01674 0.00465 0.00810 AFIX 43 H7 2 0.494100 0.960679 0.391425 11.00000 -1.20000 AFIX 0 C12 1 0.672513 0.862162 0.246193 11.00000 0.04632 0.11205 = 0.07544 0.02368 0.00863 -0.00947 AFIX 137 H12A 2 0.682190 0.902038 0.322392 11.00000 -1.50000 H12B 2 0.689919 0.873591 0.151553 11.00000 -1.50000 H12C 2 0.681332 0.807897 0.281343 11.00000 -1.50000 AFIX 0 C15 1 0.776281 0.838184 0.617811 11.00000 0.06552 0.06062 = 0.08028 -0.00055 -0.00802 -0.02473 AFIX 137 H15A 2 0.801404 0.839984 0.537995 11.00000 -1.50000 H15B 2 0.788356 0.867772 0.706205 11.00000 -1.50000 H15C 2 0.745547 0.863128 0.581453 11.00000 -1.50000 AFIX 0 C22 1 0.606983 0.403633 0.764570 11.00000 0.07092 0.05525 = 0.09045 0.02349 0.00629 -0.00304 AFIX 137 H22A 2 0.571157 0.412932 0.772200 11.00000 -1.50000 H22B 2 0.618786 0.376876 0.856380 11.00000 -1.50000 H22C 2 0.613903 0.369239 0.677125 11.00000 -1.50000 AFIX 0 C6 1 0.438667 0.943085 0.235571 11.00000 0.04511 0.06596 = 0.16434 0.04770 -0.00043 0.01352 AFIX 43 H6 2 0.424140 0.995074 0.246128 11.00000 -1.20000 AFIX 0 C13 1 0.603987 0.817271 0.083040 11.00000 0.08770 0.18307 = 0.05960 -0.00206 0.02453 -0.03811 AFIX 137 H13A 2 0.616614 0.762123 0.095092 11.00000 -1.50000 H13B 2 0.618856 0.841849 -0.006759 11.00000 -1.50000 H13C 2 0.567825 0.815801 0.071683 11.00000 -1.50000 AFIX 0 C14 1 0.601252 0.953024 0.199473 11.00000 0.11331 0.07866 = 0.18454 0.07539 0.08695 0.02909 AFIX 137 H14A 2 0.564977 0.956222 0.204556 11.00000 -1.50000 H14B 2 0.612557 0.972505 0.100949 11.00000 -1.50000 H14C 2 0.615730 0.986558 0.279204 11.00000 -1.50000 AFIX 0 HKLF 4 REM mo_hzy240_0ma_a.res in Pna2(1) REM wR2 = 0.1220, GooF = S = 1.056, Restrained GooF = 1.056 for all data REM R1 = 0.0431 for 7021 Fo > 4sig(Fo) and 0.0519 for all 8032 data REM 361 parameters refined using 1 restraints END WGHT 0.0624 1.6356 REM Highest difference peak 0.583, deepest hole -0.256, 1-sigma level 0.058 Q1 1 0.7400 0.7257 0.7571 11.00000 0.05 0.23 Q2 1 0.5774 0.5800 0.4023 11.00000 0.05 0.22 Q3 1 0.6068 0.8417 0.5502 11.00000 0.05 0.21 Q4 1 0.6930 0.8545 0.3346 11.00000 0.05 0.20 Q5 1 0.6377 0.8776 0.8137 11.00000 0.05 0.20 Q6 1 0.6388 0.5942 0.5426 11.00000 0.05 0.20 Q7 1 0.6883 0.8355 0.3274 11.00000 0.05 0.20 Q8 1 0.5595 0.8387 0.5393 11.00000 0.05 0.19 Q9 1 0.7413 0.8318 0.2082 11.00000 0.05 0.18 Q10 1 0.6595 0.7139 0.5708 11.00000 0.05 0.18 Q11 1 0.7487 0.7195 0.5685 11.00000 0.05 0.18 Q12 1 0.4589 0.9424 0.1762 11.00000 0.05 0.17 Q13 1 0.7582 0.6795 0.5723 11.00000 0.05 0.17 Q14 1 0.7933 0.5217 0.5338 11.00000 0.05 0.17 Q15 1 0.7013 0.6802 0.5325 11.00000 0.05 0.17 Q16 1 0.6424 0.8858 0.2621 11.00000 0.05 0.17 Q17 1 0.6323 0.3407 0.7738 11.00000 0.05 0.17 Q18 1 0.7734 0.7971 0.6881 11.00000 0.05 0.17 Q19 1 0.6254 0.3271 0.7569 11.00000 0.05 0.17 Q20 1 0.6174 0.7242 0.4355 11.00000 0.05 0.17 ; _shelx_res_checksum 93341 _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' 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 0.66362(2) 0.65339(4) 0.54823(8) 0.03558(16) Uani 1 1 d . . . . . Cl1 Cl 0.63742(5) 0.88000(7) 0.66374(17) 0.0494(3) Uani 1 1 d . . . . . Si1 Si 0.61360(4) 0.78025(7) 0.52971(17) 0.0387(3) Uani 1 1 d . . . . . Si5 Si 0.58399(5) 0.52384(8) 0.44395(17) 0.0423(3) Uani 1 1 d . . . . . Si2 Si 0.76386(5) 0.72995(10) 0.67118(19) 0.0488(3) Uani 1 1 d . . . . . Si3 Si 0.76210(5) 0.63975(9) 0.37187(18) 0.0452(3) Uani 1 1 d . . . . . Si4 Si 0.63999(5) 0.50368(9) 0.74143(19) 0.0478(4) Uani 1 1 d . . . . . N1 N 0.59344(15) 0.8322(2) 0.3556(5) 0.0405(9) Uani 1 1 d . . . . . N2 N 0.54561(13) 0.7901(2) 0.5322(5) 0.0393(8) Uani 1 1 d . . . . . N3 N 0.73404(13) 0.6766(2) 0.5311(5) 0.0409(9) Uani 1 1 d . . . . . N4 N 0.62455(14) 0.5555(2) 0.5799(5) 0.0397(9) Uani 1 1 d . . . . . C1 C 0.54543(18) 0.8238(3) 0.3961(7) 0.0433(12) Uani 1 1 d . . . . . C25 C 0.5712(2) 0.6078(3) 0.3051(7) 0.0507(13) Uani 1 1 d . . . . . H25A H 0.555490 0.653142 0.357484 0.076 Uiso 1 1 calc GR . . . . H25B H 0.549064 0.587936 0.225700 0.076 Uiso 1 1 calc GR . . . . H25C H 0.602540 0.625758 0.259975 0.076 Uiso 1 1 calc GR . . . . C11 C 0.6174(2) 0.8667(3) 0.2205(7) 0.0512(13) Uani 1 1 d . . . . . C2 C 0.50129(19) 0.8467(3) 0.3037(7) 0.0499(14) Uani 1 1 d . . . . . C8 C 0.50440(19) 0.7725(3) 0.6392(7) 0.0463(12) Uani 1 1 d . . . . . C9 C 0.5273(2) 0.7153(4) 0.7567(7) 0.0539(14) Uani 1 1 d . . . . . H9A H 0.540340 0.667173 0.706107 0.081 Uiso 1 1 calc GR . . . . H9B H 0.501810 0.699265 0.829657 0.081 Uiso 1 1 calc GR . . . . H9C H 0.554326 0.743089 0.809449 0.081 Uiso 1 1 calc GR . . . . C3 C 0.4808(2) 0.7919(4) 0.2026(7) 0.0567(15) Uani 1 1 d . . . . . H3 H 0.495345 0.740074 0.190214 0.068 Uiso 1 1 calc R . . . . C10 C 0.4607(2) 0.7296(4) 0.5611(9) 0.0622(16) Uani 1 1 d . . . . . H10A H 0.442914 0.768295 0.497419 0.093 Uiso 1 1 calc GR . . . . H10B H 0.438126 0.707928 0.637607 0.093 Uiso 1 1 calc GR . . . . H10C H 0.473391 0.685315 0.498701 0.093 Uiso 1 1 calc GR . . . . C26 C 0.52108(19) 0.4930(4) 0.5182(9) 0.0606(15) Uani 1 1 d . . . . . H26A H 0.522625 0.437366 0.555466 0.091 Uiso 1 1 calc GR . . . . H26B H 0.496532 0.496618 0.436959 0.091 Uiso 1 1 calc GR . . . . H26C H 0.511453 0.529182 0.600688 0.091 Uiso 1 1 calc GR . . . . C17 C 0.7252(2) 0.7304(4) 0.8474(7) 0.0614(15) Uani 1 1 d . . . . . H17A H 0.692098 0.751694 0.824500 0.092 Uiso 1 1 calc GR . . . . H17B H 0.741083 0.764515 0.923659 0.092 Uiso 1 1 calc GR . . . . H17C H 0.722161 0.675111 0.886046 0.092 Uiso 1 1 calc GR . . . . C23 C 0.6234(2) 0.5648(4) 0.9106(8) 0.0649(17) Uani 1 1 d . . . . . H23A H 0.640377 0.617114 0.905987 0.097 Uiso 1 1 calc GR . . . . H23B H 0.633559 0.535993 1.001950 0.097 Uiso 1 1 calc GR . . . . H23C H 0.587397 0.573586 0.912718 0.097 Uiso 1 1 calc GR . . . . C24 C 0.6076(3) 0.4349(4) 0.3321(9) 0.0669(18) Uani 1 1 d . . . . . H24A H 0.638241 0.450034 0.279728 0.100 Uiso 1 1 calc GR . . . . H24B H 0.582518 0.418704 0.257949 0.100 Uiso 1 1 calc GR . . . . H24C H 0.614301 0.389627 0.400380 0.100 Uiso 1 1 calc GR . . . . C18 C 0.8012(2) 0.7178(4) 0.2727(9) 0.0656(17) Uani 1 1 d . . . . . H18A H 0.781354 0.766361 0.254475 0.098 Uiso 1 1 calc GR . . . . H18B H 0.812842 0.695918 0.176237 0.098 Uiso 1 1 calc GR . . . . H18C H 0.829859 0.731544 0.335806 0.098 Uiso 1 1 calc GR . . . . C4 C 0.4392(2) 0.8129(5) 0.1200(9) 0.073(2) Uani 1 1 d . . . . . H4 H 0.424766 0.775348 0.051899 0.088 Uiso 1 1 calc R . . . . C19 C 0.8028(3) 0.5504(4) 0.4094(9) 0.0709(19) Uani 1 1 d . . . . . H19A H 0.829662 0.566147 0.477965 0.106 Uiso 1 1 calc GR . . . . H19B H 0.817023 0.531127 0.314228 0.106 Uiso 1 1 calc GR . . . . H19C H 0.783157 0.507227 0.455575 0.106 Uiso 1 1 calc GR . . . . C21 C 0.7081(2) 0.4837(5) 0.7477(9) 0.072(2) Uani 1 1 d . . . . . H21A H 0.717320 0.447839 0.664348 0.108 Uiso 1 1 calc GR . . . . H21B H 0.716630 0.457884 0.843790 0.108 Uiso 1 1 calc GR . . . . H21C H 0.726208 0.534806 0.738422 0.108 Uiso 1 1 calc GR . . . . C00S C 0.4886(3) 0.8518(4) 0.7154(10) 0.077(2) Uani 1 1 d . . . . . H00A H 0.517975 0.879144 0.755978 0.115 Uiso 1 1 calc GR . . . . H00B H 0.465443 0.839958 0.797603 0.115 Uiso 1 1 calc GR . . . . H00C H 0.472402 0.886795 0.641178 0.115 Uiso 1 1 calc GR . . . . C20 C 0.7137(2) 0.6059(4) 0.2355(8) 0.0629(16) Uani 1 1 d . . . . . H20A H 0.693165 0.564022 0.282233 0.094 Uiso 1 1 calc GR . . . . H20B H 0.729765 0.584031 0.145137 0.094 Uiso 1 1 calc GR . . . . H20C H 0.692829 0.651995 0.207385 0.094 Uiso 1 1 calc GR . . . . C5 C 0.4187(2) 0.8899(6) 0.1376(11) 0.086(3) Uani 1 1 d . . . . . H5 H 0.390475 0.904873 0.079992 0.104 Uiso 1 1 calc R . . . . C16 C 0.8255(2) 0.6851(5) 0.7233(10) 0.077(2) Uani 1 1 d . . . . . H16A H 0.821203 0.627727 0.747182 0.116 Uiso 1 1 calc GR . . . . H16B H 0.838839 0.713390 0.811441 0.116 Uiso 1 1 calc GR . . . . H16C H 0.848492 0.690817 0.638466 0.116 Uiso 1 1 calc GR . . . . C7 C 0.4804(2) 0.9231(4) 0.3220(10) 0.0682(19) Uani 1 1 d . . . . . H7 H 0.494100 0.960679 0.391425 0.082 Uiso 1 1 calc R . . . . C12 C 0.6725(2) 0.8622(5) 0.2462(10) 0.078(2) Uani 1 1 d . . . . . H12A H 0.682190 0.902038 0.322392 0.117 Uiso 1 1 calc GR . . . . H12B H 0.689919 0.873591 0.151553 0.117 Uiso 1 1 calc GR . . . . H12C H 0.681332 0.807897 0.281343 0.117 Uiso 1 1 calc GR . . . . C15 C 0.7763(3) 0.8382(4) 0.6178(9) 0.0688(18) Uani 1 1 d . . . . . H15A H 0.801404 0.839984 0.537995 0.103 Uiso 1 1 calc GR . . . . H15B H 0.788356 0.867772 0.706205 0.103 Uiso 1 1 calc GR . . . . H15C H 0.745547 0.863128 0.581453 0.103 Uiso 1 1 calc GR . . . . C22 C 0.6070(3) 0.4036(4) 0.7646(10) 0.0722(19) Uani 1 1 d . . . . . H22A H 0.571157 0.412932 0.772200 0.108 Uiso 1 1 calc GR . . . . H22B H 0.618786 0.376876 0.856380 0.108 Uiso 1 1 calc GR . . . . H22C H 0.613903 0.369239 0.677125 0.108 Uiso 1 1 calc GR . . . . C6 C 0.4387(2) 0.9431(5) 0.2356(13) 0.092(3) Uani 1 1 d . . . . . H6 H 0.424140 0.995074 0.246128 0.110 Uiso 1 1 calc R . . . . C13 C 0.6040(3) 0.8173(8) 0.0830(9) 0.110(4) Uani 1 1 d . . . . . H13A H 0.616614 0.762123 0.095092 0.165 Uiso 1 1 calc GR . . . . H13B H 0.618856 0.841849 -0.006759 0.165 Uiso 1 1 calc GR . . . . H13C H 0.567825 0.815801 0.071683 0.165 Uiso 1 1 calc GR . . . . C14 C 0.6013(4) 0.9530(5) 0.1995(15) 0.126(5) Uani 1 1 d . . . . . H14A H 0.564977 0.956222 0.204556 0.188 Uiso 1 1 calc GR . . . . H14B H 0.612557 0.972505 0.100949 0.188 Uiso 1 1 calc GR . . . . H14C H 0.615730 0.986558 0.279204 0.188 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 0.0313(3) 0.0349(3) 0.0405(3) 0.0009(3) 0.0000(3) -0.0017(2) Cl1 0.0489(6) 0.0374(6) 0.0618(8) -0.0161(6) -0.0069(6) 0.0031(5) Si1 0.0353(6) 0.0342(6) 0.0467(8) -0.0005(6) 0.0015(6) 0.0002(5) Si5 0.0375(6) 0.0392(7) 0.0502(8) -0.0061(6) 0.0026(6) -0.0042(5) Si2 0.0375(7) 0.0540(8) 0.0549(9) 0.0023(7) -0.0057(6) -0.0064(6) Si3 0.0363(7) 0.0497(7) 0.0497(8) 0.0062(7) 0.0061(6) 0.0037(6) Si4 0.0392(7) 0.0475(8) 0.0566(9) 0.0152(7) -0.0005(7) -0.0004(6) N1 0.037(2) 0.041(2) 0.043(2) 0.0068(18) 0.0028(18) 0.0000(16) N2 0.0333(18) 0.0375(18) 0.047(2) 0.004(2) 0.0035(19) 0.0010(14) N3 0.0334(18) 0.042(2) 0.047(2) 0.004(2) 0.0025(19) -0.0014(15) N4 0.0346(19) 0.0361(19) 0.049(3) 0.0012(17) 0.0047(17) -0.0009(15) C1 0.038(2) 0.033(2) 0.059(3) -0.002(2) 0.003(2) 0.0029(19) C25 0.047(3) 0.050(3) 0.055(3) -0.003(3) -0.005(2) -0.003(2) C11 0.040(3) 0.054(3) 0.060(3) 0.020(3) 0.009(2) 0.002(2) C2 0.037(3) 0.048(3) 0.064(4) 0.021(3) 0.006(2) 0.004(2) C8 0.041(3) 0.043(3) 0.055(3) 0.005(2) 0.015(2) -0.001(2) C9 0.055(3) 0.059(3) 0.047(3) 0.005(3) 0.006(3) -0.005(3) C3 0.048(3) 0.068(4) 0.054(3) 0.016(3) 0.000(3) -0.002(3) C10 0.041(3) 0.065(3) 0.080(4) 0.013(4) 0.009(3) -0.008(2) C26 0.040(3) 0.063(3) 0.079(4) -0.001(3) 0.000(3) -0.009(2) C17 0.062(3) 0.073(4) 0.049(3) 0.003(3) -0.002(3) -0.006(3) C23 0.054(3) 0.083(4) 0.058(4) 0.011(3) -0.007(3) -0.010(3) C24 0.073(4) 0.049(3) 0.079(5) -0.015(3) 0.012(4) -0.003(3) C18 0.052(3) 0.068(4) 0.077(4) 0.009(3) 0.020(3) -0.004(3) C4 0.045(3) 0.098(5) 0.077(5) 0.032(4) -0.005(3) -0.013(3) C19 0.072(4) 0.069(4) 0.072(4) 0.003(3) 0.010(3) 0.028(3) C21 0.048(3) 0.081(5) 0.086(5) 0.040(4) 0.002(3) 0.011(3) C00S 0.078(5) 0.058(4) 0.094(6) -0.002(4) 0.037(4) 0.009(3) C20 0.055(3) 0.075(4) 0.058(4) -0.009(3) 0.004(3) -0.004(3) C5 0.038(3) 0.109(6) 0.111(7) 0.054(6) -0.003(4) 0.003(4) C16 0.049(3) 0.097(5) 0.085(5) 0.001(4) -0.019(4) -0.001(3) C7 0.048(3) 0.051(3) 0.105(6) 0.017(4) 0.005(3) 0.008(3) C12 0.046(3) 0.112(6) 0.075(5) 0.024(4) 0.009(3) -0.009(4) C15 0.066(4) 0.061(4) 0.080(5) -0.001(3) -0.008(3) -0.025(3) C22 0.071(4) 0.055(4) 0.090(5) 0.023(4) 0.006(4) -0.003(3) C6 0.045(3) 0.066(4) 0.164(9) 0.048(6) 0.000(5) 0.014(3) C13 0.088(6) 0.183(10) 0.060(5) -0.002(5) 0.025(4) -0.038(6) C14 0.113(7) 0.079(5) 0.185(11) 0.075(7) 0.087(8) 0.029(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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Fe1 Si1 110.81(12) . . ? N3 Fe1 N4 134.60(17) . . ? N4 Fe1 Si1 114.57(12) . . ? Cl1 Si1 Fe1 116.81(7) . . ? Cl1 Si1 C1 106.53(14) . . ? N1 Si1 Fe1 127.14(15) . . ? N1 Si1 Cl1 101.16(15) . . ? N1 Si1 C1 35.89(18) . . ? N2 Si1 Fe1 127.63(13) . . ? N2 Si1 Cl1 102.97(14) . . ? N2 Si1 N1 71.10(19) . . ? N2 Si1 C1 35.27(19) . . ? C1 Si1 Fe1 136.64(14) . . ? N4 Si5 C25 110.6(2) . . ? N4 Si5 C26 114.2(3) . . ? N4 Si5 C24 113.2(3) . . ? C25 Si5 C26 105.2(3) . . ? C24 Si5 C25 107.0(3) . . ? C24 Si5 C26 106.0(3) . . ? N3 Si2 C17 110.1(2) . . ? N3 Si2 C16 112.8(3) . . ? N3 Si2 C15 112.9(3) . . ? C17 Si2 C15 107.7(3) . . ? C16 Si2 C17 106.7(4) . . ? C16 Si2 C15 106.3(4) . . ? N3 Si3 C18 112.8(3) . . ? N3 Si3 C19 113.2(3) . . ? N3 Si3 C20 109.5(3) . . ? C19 Si3 C18 107.2(3) . . ? C20 Si3 C18 107.1(3) . . ? C20 Si3 C19 106.8(3) . . ? N4 Si4 C23 110.0(3) . . ? N4 Si4 C21 110.6(3) . . ? N4 Si4 C22 114.4(3) . . ? C23 Si4 C21 108.0(4) . . ? C23 Si4 C22 106.0(3) . . ? C21 Si4 C22 107.7(3) . . ? C1 N1 Si1 90.7(3) . . ? C1 N1 C11 132.4(4) . . ? C11 N1 Si1 136.9(3) . . ? C1 N2 Si1 91.7(3) . . ? C1 N2 C8 131.1(4) . . ? C8 N2 Si1 137.1(4) . . ? Si2 N3 Fe1 120.0(3) . . ? Si3 N3 Fe1 115.1(2) . . ? Si3 N3 Si2 124.8(2) . . ? Si5 N4 Fe1 119.8(2) . . ? Si5 N4 Si4 126.1(2) . . ? Si4 N4 Fe1 113.7(2) . . ? N1 C1 Si1 53.4(3) . . ? N1 C1 C2 126.3(5) . . ? N2 C1 Si1 53.0(2) . . ? N2 C1 N1 106.3(4) . . ? N2 C1 C2 127.4(5) . . ? C2 C1 Si1 176.0(4) . . ? N1 C11 C12 106.8(5) . . ? N1 C11 C13 110.0(5) . . ? N1 C11 C14 110.0(6) . . ? C12 C11 C13 109.3(7) . . ? C14 C11 C12 110.6(7) . . ? C14 C11 C13 110.2(8) . . ? C3 C2 C1 120.4(5) . . ? C3 C2 C7 120.4(6) . . ? C7 C2 C1 119.2(6) . . ? N2 C8 C9 104.7(4) . . ? N2 C8 C10 112.0(5) . . ? N2 C8 C00S 108.6(4) . . ? C9 C8 C10 109.2(4) . . ? C00S C8 C9 109.8(6) . . ? C00S C8 C10 112.3(5) . . ? C4 C3 C2 120.0(6) . . ? C3 C4 C5 119.3(8) . . ? C6 C5 C4 120.7(7) . . ? C2 C7 C6 118.3(7) . . ? C5 C6 C7 121.2(7) . . ? 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 2.5006(14) . ? Fe1 N3 1.942(4) . ? Fe1 N4 1.953(4) . ? Cl1 Si1 2.1334(18) . ? Si1 N1 1.849(4) . ? Si1 N2 1.840(4) . ? Si1 C1 2.302(5) . ? Si5 N4 1.709(4) . ? Si5 C25 1.888(6) . ? Si5 C26 1.889(5) . ? Si5 C24 1.886(6) . ? Si2 N3 1.723(5) . ? Si2 C17 1.879(6) . ? Si2 C16 1.876(7) . ? Si2 C15 1.883(7) . ? Si3 N3 1.714(5) . ? Si3 C18 1.885(6) . ? Si3 C19 1.871(6) . ? Si3 C20 1.864(7) . ? Si4 N4 1.721(4) . ? Si4 C23 1.865(7) . ? Si4 C21 1.867(6) . ? Si4 C22 1.891(7) . ? N1 C1 1.350(6) . ? N1 C11 1.475(7) . ? N2 C1 1.330(7) . ? N2 C8 1.490(6) . ? C1 C2 1.493(8) . ? C11 C12 1.505(8) . ? C11 C13 1.512(11) . ? C11 C14 1.505(9) . ? C2 C3 1.389(9) . ? C2 C7 1.394(8) . ? C8 C9 1.537(8) . ? C8 C10 1.538(8) . ? C8 C00S 1.537(8) . ? C3 C4 1.383(8) . ? C4 C5 1.398(12) . ? C5 C6 1.349(14) . ? C7 C6 1.400(10) . ?