#------------------------------------------------------------------------------ #$Date: 2020-08-15 04:54:03 +0300 (Sat, 15 Aug 2020) $ #$Revision: 255334 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/51/7705161.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_7705161 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_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT00570C _journal_year 2020 _chemical_formula_moiety 'C42 H82 Cl4 Fe2 N6 Si6' _chemical_formula_sum 'C42 H82 Cl4 Fe2 N6 Si6' _chemical_formula_weight 1093.17 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-10-11 _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 67.489(4) _cell_angle_beta 85.051(5) _cell_angle_gamma 67.086(4) _cell_formula_units_Z 1 _cell_length_a 10.0727(9) _cell_length_b 12.8695(12) _cell_length_c 13.2383(11) _cell_measurement_reflns_used 5167 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.355 _cell_measurement_theta_min 2.201 _cell_volume 1456.3(2) _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 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 149.99 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.991 _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 0.1060 _diffrn_reflns_av_unetI/netI 0.0786 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 27756 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.021 _diffrn_reflns_theta_min 2.201 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.838 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6598 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0807 before and 0.0603 after correction. The Ratio of minimum to maximum transmission is 0.8852. The \l/2 correction factor is Not present.' _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.247 _exptl_crystal_description block _exptl_crystal_F_000 580 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Diethyl Ether' _exptl_crystal_size_max 0.422 _exptl_crystal_size_mid 0.282 _exptl_crystal_size_min 0.125 _refine_diff_density_max 0.808 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.099 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 283 _refine_ls_number_reflns 5688 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.020 _refine_ls_R_factor_all 0.0994 _refine_ls_R_factor_gt 0.0540 _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^)+(0.0577P)^2^+2.1400P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1199 _refine_ls_wR_factor_ref 0.1393 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3741 _reflns_number_total 5688 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt00570c2.cif _cod_data_source_block 7 _cod_database_code 7705161 _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_max 0.902 _shelx_estimated_absorpt_t_min 0.719 _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), C7(H7), C4(H4), C6(H6), C5(H5) 2.b Idealised Me refined as rotating group: C21(H21A,H21B,H21C), C16(H16A,H16B,H16C), C14(H14A,H14B,H14C), C17(H17A,H17B, H17C), C13(H13A,H13B,H13C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C19(H19A, H19B,H19C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C10(H10A,H10B,H10C) ; _shelx_res_file ; mo_hzy2372_0m.res created by SHELXL-2014/7 TITL mo_hzy2372_0m_a.res in P-1 REM Old TITL mo_HZY2372_0m in P-1 REM SHELXT solution in P-1: R1 0.142, Rweak 0.014, Alpha 0.052 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C21 N3 Si3 Cl2 Fe CELL 0.71073 10.0727 12.8695 13.2383 67.489 85.051 67.086 ZERR 1 0.0009 0.0012 0.0011 0.004 0.005 0.004 LATT 1 SFAC C H Cl Fe N Si UNIT 42 82 4 2 6 6 L.S. 4 0 0 PLAN 20 SIZE 0.125 0.282 0.422 TEMP -123.16 list 4 fmap 2 53 acta REM REM REM WGHT 0.057700 2.140000 FVAR 0.68058 FE1 4 0.589581 0.846629 0.580000 11.00000 0.02460 0.01984 = 0.01873 -0.00510 0.00250 -0.00728 CL1 3 0.380197 0.965862 0.448299 11.00000 0.02204 0.01547 = 0.02422 -0.00382 -0.00387 -0.00662 SI1 6 0.774368 0.734566 0.483416 11.00000 0.02482 0.02546 = 0.02086 -0.00847 0.00352 -0.00842 CL2 3 0.903594 0.561223 0.592213 11.00000 0.04390 0.02990 = 0.03070 -0.00523 0.00301 0.00334 SI3 6 0.710310 0.730428 0.827322 11.00000 0.03215 0.02718 = 0.01978 -0.00666 0.00028 -0.01227 SI2 6 0.496346 0.651990 0.763033 11.00000 0.02919 0.02674 = 0.02861 -0.00489 0.00260 -0.01447 N3 5 0.599635 0.737789 0.730012 11.00000 0.02543 0.02318 = 0.01966 -0.00510 0.00149 -0.01222 N1 5 0.755155 0.713985 0.356423 11.00000 0.03090 0.03017 = 0.02628 -0.01238 0.00731 -0.01690 N2 5 0.896884 0.787702 0.386500 11.00000 0.02310 0.03640 = 0.02343 -0.01393 0.00357 -0.01311 C1 1 0.841723 0.772325 0.307324 11.00000 0.02170 0.02113 = 0.02784 -0.01081 0.00146 -0.00614 C2 1 0.866373 0.817865 0.188880 11.00000 0.02942 0.03242 = 0.02229 -0.01161 0.00345 -0.01848 C12 1 0.989497 0.856250 0.379920 11.00000 0.02656 0.04425 = 0.03058 -0.01957 0.00627 -0.01911 C8 1 0.659761 0.675646 0.310649 11.00000 0.03144 0.03025 = 0.03408 -0.01528 0.00628 -0.01817 C3 1 0.983193 0.746517 0.147673 11.00000 0.03993 0.03683 = 0.02909 -0.01462 0.01221 -0.01344 AFIX 43 H3 2 1.045301 0.667607 0.195203 11.00000 -1.20000 AFIX 0 C21 1 0.869581 0.766114 0.767767 11.00000 0.03480 0.04817 = 0.03166 -0.01129 -0.00452 -0.02036 AFIX 137 H21A 2 0.922838 0.711657 0.729884 11.00000 -1.50000 H21B 2 0.933076 0.754430 0.826636 11.00000 -1.50000 H21C 2 0.836444 0.850989 0.715513 11.00000 -1.50000 AFIX 0 C7 1 0.775965 0.930979 0.119516 11.00000 0.03297 0.03724 = 0.03211 -0.01432 -0.00166 -0.01254 AFIX 43 H7 2 0.695366 0.978934 0.146951 11.00000 -1.20000 AFIX 0 C16 1 0.364975 0.700477 0.647625 11.00000 0.04033 0.03509 = 0.05129 -0.00876 -0.00092 -0.02471 AFIX 137 H16A 2 0.297564 0.784940 0.631403 11.00000 -1.50000 H16B 2 0.311074 0.647214 0.667959 11.00000 -1.50000 H16C 2 0.416979 0.694858 0.582627 11.00000 -1.50000 AFIX 0 C14 1 0.908367 0.991191 0.314175 11.00000 0.05185 0.04147 = 0.04465 -0.02119 0.00872 -0.02750 AFIX 137 H14A 2 0.898499 1.004852 0.236631 11.00000 -1.50000 H14B 2 0.961958 1.037157 0.322310 11.00000 -1.50000 H14C 2 0.812234 1.018736 0.341112 11.00000 -1.50000 AFIX 0 C17 1 0.607212 0.485876 0.795826 11.00000 0.03858 0.03401 = 0.05001 -0.01213 0.00099 -0.01796 AFIX 137 H17A 2 0.659698 0.475766 0.732157 11.00000 -1.50000 H17B 2 0.543462 0.440957 0.813898 11.00000 -1.50000 H17C 2 0.676387 0.454134 0.858555 11.00000 -1.50000 AFIX 0 C13 1 1.017110 0.838303 0.498597 11.00000 0.03968 0.07263 = 0.03892 -0.02545 -0.00013 -0.03284 AFIX 137 H13A 2 0.924802 0.871329 0.528574 11.00000 -1.50000 H13B 2 1.078335 0.881026 0.500476 11.00000 -1.50000 H13C 2 1.065858 0.751073 0.542666 11.00000 -1.50000 AFIX 0 C18 1 0.384158 0.669236 0.880384 11.00000 0.04784 0.04412 = 0.04175 -0.00701 0.01394 -0.02208 AFIX 137 H18A 2 0.447678 0.637363 0.946468 11.00000 -1.50000 H18B 2 0.321776 0.623645 0.893184 11.00000 -1.50000 H18C 2 0.324298 0.755728 0.862924 11.00000 -1.50000 AFIX 0 C20 1 0.608924 0.840025 0.893768 11.00000 0.05003 0.04961 = 0.04671 -0.03075 0.00732 -0.02126 AFIX 137 H20A 2 0.566736 0.922522 0.837497 11.00000 -1.50000 H20B 2 0.675077 0.838178 0.945132 11.00000 -1.50000 H20C 2 0.531694 0.816955 0.933583 11.00000 -1.50000 AFIX 0 C19 1 0.789712 0.575516 0.940275 11.00000 0.05171 0.04015 = 0.03708 -0.00249 -0.01471 -0.01726 AFIX 137 H19A 2 0.711732 0.549763 0.974788 11.00000 -1.50000 H19B 2 0.845128 0.579268 0.995194 11.00000 -1.50000 H19C 2 0.853678 0.516739 0.909740 11.00000 -1.50000 AFIX 0 C4 1 1.008512 0.790174 0.038564 11.00000 0.05229 0.05669 = 0.03525 -0.02371 0.01776 -0.03060 AFIX 43 H4 2 1.088317 0.742042 0.010665 11.00000 -1.20000 AFIX 0 C11 1 0.740469 0.608443 0.237655 11.00000 0.03975 0.05173 = 0.04890 -0.03313 0.00569 -0.01965 AFIX 137 H11A 2 0.764768 0.664867 0.172043 11.00000 -1.50000 H11B 2 0.679370 0.575862 0.215985 11.00000 -1.50000 H11C 2 0.829428 0.541171 0.277765 11.00000 -1.50000 AFIX 0 C6 1 0.801300 0.975875 0.009661 11.00000 0.06248 0.04859 = 0.02587 -0.00187 -0.00605 -0.03062 AFIX 43 H6 2 0.739781 1.054963 -0.037984 11.00000 -1.20000 AFIX 0 C9 1 0.527515 0.784745 0.248748 11.00000 0.03058 0.05471 = 0.08368 -0.03949 -0.00434 -0.01430 AFIX 137 H9A 2 0.480799 0.830251 0.295512 11.00000 -1.50000 H9B 2 0.459907 0.757353 0.227714 11.00000 -1.50000 H9C 2 0.555788 0.837622 0.182741 11.00000 -1.50000 AFIX 0 C5 1 0.917238 0.904113 -0.029720 11.00000 0.06979 0.06835 = 0.02638 -0.01768 0.01131 -0.04742 AFIX 43 H5 2 0.934112 0.934018 -0.105195 11.00000 -1.20000 AFIX 0 C15 1 1.132655 0.803637 0.332928 11.00000 0.03537 0.08583 = 0.07884 -0.05332 0.02254 -0.03368 AFIX 137 H15A 2 1.176903 0.715190 0.373362 11.00000 -1.50000 H15B 2 1.197857 0.840949 0.339899 11.00000 -1.50000 H15C 2 1.115069 0.821011 0.255366 11.00000 -1.50000 AFIX 0 C10 1 0.616544 0.588869 0.411238 11.00000 0.10964 0.09022 = 0.04598 -0.03063 0.02538 -0.08340 AFIX 137 H10A 2 0.703253 0.518132 0.450777 11.00000 -1.50000 H10B 2 0.551032 0.561434 0.387546 11.00000 -1.50000 H10C 2 0.567717 0.631562 0.459699 11.00000 -1.50000 AFIX 0 HKLF 4 REM mo_hzy2372_0m_a.res in P-1 REM R1 = 0.0540 for 3741 Fo > 4sig(Fo) and 0.0994 for all 5688 data REM 283 parameters refined using 0 restraints END WGHT 0.0577 2.1497 REM Highest difference peak 0.808, deepest hole -0.462, 1-sigma level 0.099 Q1 1 0.3460 0.9641 0.4283 11.00000 0.05 0.81 Q2 1 0.3600 0.9534 0.4802 11.00000 0.05 0.76 Q3 1 0.4106 0.9282 0.4466 11.00000 0.05 0.76 Q4 1 0.4129 0.9725 0.4231 11.00000 0.05 0.71 Q5 1 0.3778 1.0025 0.4347 11.00000 0.05 0.64 Q6 1 0.4322 0.6531 0.8250 11.00000 0.05 0.40 Q7 1 0.5240 0.9420 0.4784 11.00000 0.05 0.37 Q8 1 0.2991 0.5780 0.8353 11.00000 0.05 0.36 Q9 1 0.4142 0.7018 0.7043 11.00000 0.05 0.36 Q10 1 1.0582 0.7801 0.7655 11.00000 0.05 0.35 Q11 1 0.7948 0.9994 0.3803 11.00000 0.05 0.34 Q12 1 0.2282 0.6736 0.7116 11.00000 0.05 0.34 Q13 1 0.2043 0.7414 0.6072 11.00000 0.05 0.34 Q14 1 0.6256 0.7521 0.6807 11.00000 0.05 0.34 Q15 1 0.2381 0.6970 0.7097 11.00000 0.05 0.34 Q16 1 0.6022 0.7242 0.6699 11.00000 0.05 0.33 Q17 1 1.1888 0.7384 0.2770 11.00000 0.05 0.33 Q18 1 0.8754 0.5960 0.7344 11.00000 0.05 0.33 Q19 1 1.0962 0.8549 0.0742 11.00000 0.05 0.32 Q20 1 1.2079 0.8053 0.4359 11.00000 0.05 0.32 ; _shelx_res_checksum 5664 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 0.58958(6) 0.84663(6) 0.58000(5) 0.02228(17) Uani 1 1 d . . . . . Cl1 Cl 0.38020(10) 0.96586(9) 0.44830(8) 0.0216(2) Uani 1 1 d . . . . . Si1 Si 0.77437(13) 0.73457(11) 0.48342(9) 0.0244(3) Uani 1 1 d . . . . . Cl2 Cl 0.90359(14) 0.56122(11) 0.59221(9) 0.0427(3) Uani 1 1 d . . . . . Si3 Si 0.71031(14) 0.73043(12) 0.82732(9) 0.0267(3) Uani 1 1 d . . . . . Si2 Si 0.49635(14) 0.65199(12) 0.76303(10) 0.0288(3) Uani 1 1 d . . . . . N3 N 0.5996(4) 0.7378(3) 0.7300(3) 0.0228(8) Uani 1 1 d . . . . . N1 N 0.7552(4) 0.7140(3) 0.3564(3) 0.0273(8) Uani 1 1 d . . . . . N2 N 0.8969(4) 0.7877(3) 0.3865(3) 0.0264(8) Uani 1 1 d . . . . . C1 C 0.8417(4) 0.7723(4) 0.3073(3) 0.0238(9) Uani 1 1 d . . . . . C2 C 0.8664(5) 0.8179(4) 0.1889(3) 0.0256(10) Uani 1 1 d . . . . . C12 C 0.9895(5) 0.8563(4) 0.3799(4) 0.0306(11) Uani 1 1 d . . . . . C8 C 0.6598(5) 0.6756(4) 0.3106(4) 0.0291(10) Uani 1 1 d . . . . . C3 C 0.9832(5) 0.7465(5) 0.1477(4) 0.0357(11) Uani 1 1 d . . . . . H3 H 1.0453 0.6676 0.1952 0.043 Uiso 1 1 calc R . . . . C21 C 0.8696(5) 0.7661(5) 0.7678(4) 0.0376(12) Uani 1 1 d . . . . . H21A H 0.9228 0.7117 0.7299 0.056 Uiso 1 1 calc GR . . . . H21B H 0.9331 0.7544 0.8266 0.056 Uiso 1 1 calc GR . . . . H21C H 0.8364 0.8510 0.7155 0.056 Uiso 1 1 calc GR . . . . C7 C 0.7760(5) 0.9310(4) 0.1195(4) 0.0338(11) Uani 1 1 d . . . . . H7 H 0.6954 0.9789 0.1470 0.041 Uiso 1 1 calc R . . . . C16 C 0.3650(5) 0.7005(5) 0.6476(4) 0.0411(12) Uani 1 1 d . . . . . H16A H 0.2976 0.7849 0.6314 0.062 Uiso 1 1 calc GR . . . . H16B H 0.3111 0.6472 0.6680 0.062 Uiso 1 1 calc GR . . . . H16C H 0.4170 0.6949 0.5826 0.062 Uiso 1 1 calc GR . . . . C14 C 0.9084(6) 0.9912(5) 0.3142(4) 0.0416(12) Uani 1 1 d . . . . . H14A H 0.8985 1.0049 0.2366 0.062 Uiso 1 1 calc GR . . . . H14B H 0.9620 1.0372 0.3223 0.062 Uiso 1 1 calc GR . . . . H14C H 0.8122 1.0187 0.3411 0.062 Uiso 1 1 calc GR . . . . C17 C 0.6072(5) 0.4859(4) 0.7958(4) 0.0407(12) Uani 1 1 d . . . . . H17A H 0.6597 0.4758 0.7322 0.061 Uiso 1 1 calc GR . . . . H17B H 0.5435 0.4410 0.8139 0.061 Uiso 1 1 calc GR . . . . H17C H 0.6764 0.4541 0.8586 0.061 Uiso 1 1 calc GR . . . . C13 C 1.0171(6) 0.8383(6) 0.4986(4) 0.0451(14) Uani 1 1 d . . . . . H13A H 0.9248 0.8713 0.5286 0.068 Uiso 1 1 calc GR . . . . H13B H 1.0783 0.8810 0.5005 0.068 Uiso 1 1 calc GR . . . . H13C H 1.0659 0.7511 0.5427 0.068 Uiso 1 1 calc GR . . . . C18 C 0.3842(6) 0.6692(5) 0.8804(4) 0.0469(14) Uani 1 1 d . . . . . H18A H 0.4477 0.6374 0.9465 0.070 Uiso 1 1 calc GR . . . . H18B H 0.3218 0.6236 0.8932 0.070 Uiso 1 1 calc GR . . . . H18C H 0.3243 0.7557 0.8629 0.070 Uiso 1 1 calc GR . . . . C20 C 0.6089(6) 0.8400(5) 0.8938(4) 0.0443(13) Uani 1 1 d . . . . . H20A H 0.5667 0.9225 0.8375 0.067 Uiso 1 1 calc GR . . . . H20B H 0.6751 0.8382 0.9451 0.067 Uiso 1 1 calc GR . . . . H20C H 0.5317 0.8170 0.9336 0.067 Uiso 1 1 calc GR . . . . C19 C 0.7897(6) 0.5755(5) 0.9403(4) 0.0459(13) Uani 1 1 d . . . . . H19A H 0.7117 0.5498 0.9748 0.069 Uiso 1 1 calc GR . . . . H19B H 0.8451 0.5793 0.9952 0.069 Uiso 1 1 calc GR . . . . H19C H 0.8537 0.5167 0.9097 0.069 Uiso 1 1 calc GR . . . . C4 C 1.0085(6) 0.7902(5) 0.0386(4) 0.0439(13) Uani 1 1 d . . . . . H4 H 1.0883 0.7420 0.0107 0.053 Uiso 1 1 calc R . . . . C11 C 0.7405(5) 0.6084(5) 0.2377(4) 0.0418(13) Uani 1 1 d . . . . . H11A H 0.7648 0.6649 0.1720 0.063 Uiso 1 1 calc GR . . . . H11B H 0.6794 0.5759 0.2160 0.063 Uiso 1 1 calc GR . . . . H11C H 0.8294 0.5412 0.2778 0.063 Uiso 1 1 calc GR . . . . C6 C 0.8013(6) 0.9759(5) 0.0097(4) 0.0460(14) Uani 1 1 d . . . . . H6 H 0.7398 1.0550 -0.0380 0.055 Uiso 1 1 calc R . . . . C9 C 0.5275(5) 0.7847(5) 0.2487(5) 0.0522(15) Uani 1 1 d . . . . . H9A H 0.4808 0.8303 0.2955 0.078 Uiso 1 1 calc GR . . . . H9B H 0.4599 0.7574 0.2277 0.078 Uiso 1 1 calc GR . . . . H9C H 0.5558 0.8376 0.1827 0.078 Uiso 1 1 calc GR . . . . C5 C 0.9172(7) 0.9041(6) -0.0297(4) 0.0486(15) Uani 1 1 d . . . . . H5 H 0.9341 0.9340 -0.1052 0.058 Uiso 1 1 calc R . . . . C15 C 1.1327(6) 0.8036(6) 0.3329(5) 0.0574(17) Uani 1 1 d . . . . . H15A H 1.1769 0.7152 0.3734 0.086 Uiso 1 1 calc GR . . . . H15B H 1.1979 0.8409 0.3399 0.086 Uiso 1 1 calc GR . . . . H15C H 1.1151 0.8210 0.2554 0.086 Uiso 1 1 calc GR . . . . C10 C 0.6165(8) 0.5889(6) 0.4112(4) 0.067(2) Uani 1 1 d . . . . . H10A H 0.7033 0.5181 0.4508 0.100 Uiso 1 1 calc GR . . . . H10B H 0.5510 0.5614 0.3875 0.100 Uiso 1 1 calc GR . . . . H10C H 0.5677 0.6316 0.4597 0.100 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 0.0246(3) 0.0198(3) 0.0187(3) -0.0051(3) 0.0025(2) -0.0073(3) Cl1 0.0220(5) 0.0155(5) 0.0242(5) -0.0038(4) -0.0039(4) -0.0066(4) Si1 0.0248(6) 0.0255(7) 0.0209(6) -0.0085(5) 0.0035(5) -0.0084(5) Cl2 0.0439(7) 0.0299(7) 0.0307(6) -0.0052(5) 0.0030(5) 0.0033(6) Si3 0.0321(7) 0.0272(7) 0.0198(6) -0.0067(5) 0.0003(5) -0.0123(6) Si2 0.0292(7) 0.0267(7) 0.0286(6) -0.0049(5) 0.0026(5) -0.0145(6) N3 0.0254(19) 0.023(2) 0.0197(17) -0.0051(15) 0.0015(14) -0.0122(16) N1 0.031(2) 0.030(2) 0.0263(19) -0.0124(17) 0.0073(16) -0.0169(18) N2 0.023(2) 0.036(2) 0.0234(18) -0.0139(17) 0.0036(15) -0.0131(17) C1 0.022(2) 0.021(2) 0.028(2) -0.0108(19) 0.0015(18) -0.0061(19) C2 0.029(2) 0.032(3) 0.022(2) -0.012(2) 0.0034(18) -0.018(2) C12 0.027(2) 0.044(3) 0.031(2) -0.020(2) 0.0063(19) -0.019(2) C8 0.031(3) 0.030(3) 0.034(2) -0.015(2) 0.006(2) -0.018(2) C3 0.040(3) 0.037(3) 0.029(2) -0.015(2) 0.012(2) -0.013(2) C21 0.035(3) 0.048(3) 0.032(3) -0.011(2) -0.005(2) -0.020(2) C7 0.033(3) 0.037(3) 0.032(3) -0.014(2) -0.002(2) -0.013(2) C16 0.040(3) 0.035(3) 0.051(3) -0.009(2) -0.001(2) -0.025(3) C14 0.052(3) 0.041(3) 0.045(3) -0.021(3) 0.009(2) -0.028(3) C17 0.039(3) 0.034(3) 0.050(3) -0.012(2) 0.001(2) -0.018(2) C13 0.040(3) 0.073(4) 0.039(3) -0.025(3) 0.000(2) -0.033(3) C18 0.048(3) 0.044(3) 0.042(3) -0.007(3) 0.014(2) -0.022(3) C20 0.050(3) 0.050(3) 0.047(3) -0.031(3) 0.007(3) -0.021(3) C19 0.052(3) 0.040(3) 0.037(3) -0.002(2) -0.015(2) -0.017(3) C4 0.052(3) 0.057(4) 0.035(3) -0.024(3) 0.018(3) -0.031(3) C11 0.040(3) 0.052(3) 0.049(3) -0.033(3) 0.006(2) -0.020(3) C6 0.062(4) 0.049(3) 0.026(3) -0.002(2) -0.006(2) -0.031(3) C9 0.031(3) 0.055(4) 0.084(4) -0.039(3) -0.004(3) -0.014(3) C5 0.070(4) 0.068(4) 0.026(3) -0.018(3) 0.011(3) -0.047(4) C15 0.035(3) 0.086(5) 0.079(4) -0.053(4) 0.023(3) -0.034(3) C10 0.110(6) 0.090(5) 0.046(3) -0.031(3) 0.025(3) -0.083(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 Cl1 Fe1 Cl1 88.97(4) . 2_676 ? Cl1 Fe1 Si1 103.98(4) . . ? Cl1 Fe1 Si1 108.70(4) 2_676 . ? N3 Fe1 Cl1 116.35(11) . 2_676 ? N3 Fe1 Cl1 128.11(11) . . ? N3 Fe1 Si1 108.47(11) . . ? Fe1 Cl1 Fe1 91.03(4) . 2_676 ? Cl2 Si1 Fe1 110.90(6) . . ? Cl2 Si1 C1 112.40(12) . . ? N1 Si1 Fe1 129.75(13) . . ? N1 Si1 Cl2 104.70(13) . . ? N1 Si1 C1 35.67(15) . . ? N2 Si1 Fe1 128.08(13) . . ? N2 Si1 Cl2 105.35(13) . . ? N2 Si1 N1 71.06(16) . . ? N2 Si1 C1 35.74(15) . . ? C1 Si1 Fe1 136.70(12) . . ? N3 Si3 C21 112.37(19) . . ? N3 Si3 C20 110.8(2) . . ? N3 Si3 C19 113.7(2) . . ? C21 Si3 C19 104.8(2) . . ? C20 Si3 C21 107.8(2) . . ? C20 Si3 C19 106.9(2) . . ? N3 Si2 C16 111.62(19) . . ? N3 Si2 C17 112.6(2) . . ? N3 Si2 C18 112.0(2) . . ? C16 Si2 C17 105.7(2) . . ? C16 Si2 C18 105.3(2) . . ? C18 Si2 C17 109.1(2) . . ? Si3 N3 Fe1 119.37(18) . . ? Si2 N3 Fe1 118.68(18) . . ? Si2 N3 Si3 122.0(2) . . ? C1 N1 Si1 91.1(3) . . ? C1 N1 C8 130.9(3) . . ? C8 N1 Si1 136.8(3) . . ? C1 N2 Si1 91.3(3) . . ? C1 N2 C12 130.3(4) . . ? C12 N2 Si1 136.2(3) . . ? N1 C1 Si1 53.3(2) . . ? N1 C1 N2 105.6(3) . . ? N1 C1 C2 127.9(4) . . ? N2 C1 Si1 53.0(2) . . ? N2 C1 C2 126.4(4) . . ? C2 C1 Si1 170.3(3) . . ? C3 C2 C1 120.3(4) . . ? C7 C2 C1 120.2(4) . . ? C7 C2 C3 119.6(4) . . ? N2 C12 C14 110.2(4) . . ? N2 C12 C13 105.0(4) . . ? N2 C12 C15 110.6(4) . . ? C14 C12 C13 108.7(4) . . ? C14 C12 C15 112.2(4) . . ? C15 C12 C13 109.9(4) . . ? N1 C8 C11 111.2(4) . . ? N1 C8 C9 110.3(4) . . ? N1 C8 C10 104.8(4) . . ? C11 C8 C10 109.6(4) . . ? C9 C8 C11 110.7(4) . . ? C9 C8 C10 110.1(5) . . ? C4 C3 C2 120.3(5) . . ? C2 C7 C6 120.5(5) . . ? C5 C4 C3 119.4(5) . . ? C5 C6 C7 119.2(5) . . ? C4 C5 C6 121.1(5) . . ? 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 Cl1 2.4307(11) . ? Fe1 Cl1 2.4324(12) 2_676 ? Fe1 Si1 2.4678(13) . ? Fe1 N3 1.926(3) . ? Cl1 Fe1 2.4323(12) 2_676 ? Si1 Cl2 2.0850(17) . ? Si1 N1 1.836(4) . ? Si1 N2 1.830(4) . ? Si1 C1 2.291(4) . ? Si3 N3 1.727(3) . ? Si3 C21 1.867(5) . ? Si3 C20 1.865(5) . ? Si3 C19 1.879(5) . ? Si2 N3 1.714(3) . ? Si2 C16 1.858(5) . ? Si2 C17 1.876(5) . ? Si2 C18 1.872(5) . ? N1 C1 1.336(5) . ? N1 C8 1.494(5) . ? N2 C1 1.338(5) . ? N2 C12 1.491(5) . ? C1 C2 1.485(5) . ? C2 C3 1.399(6) . ? C2 C7 1.371(6) . ? C12 C14 1.517(7) . ? C12 C13 1.532(6) . ? C12 C15 1.527(6) . ? C8 C11 1.516(6) . ? C8 C9 1.506(7) . ? C8 C10 1.533(6) . ? C3 C4 1.376(6) . ? C7 C6 1.386(6) . ? C4 C5 1.375(8) . ? C6 C5 1.383(8) . ?