#------------------------------------------------------------------------------ #$Date: 2020-08-15 04:54:03 +0300 (Sat, 15 Aug 2020) $ #$Revision: 255334 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/51/7705168.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_7705168 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 Co2 N6 Si6' _chemical_formula_sum 'C42 H82 Cl4 Co2 N6 Si6' _chemical_formula_weight 1099.33 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-10-12 _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 100.479(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.9455(12) _cell_length_b 14.6642(16) _cell_length_c 18.3130(19) _cell_measurement_reflns_used 9983 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.41 _cell_measurement_theta_min 2.35 _cell_volume 2890.3(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 150.0 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _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 0.1031 _diffrn_reflns_av_unetI/netI 0.0388 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 66630 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.020 _diffrn_reflns_theta_min 2.452 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.916 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6931 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0859 before and 0.0704 after correction. The Ratio of minimum to maximum transmission is 0.9298. The \l/2 correction factor is Not present. ; _exptl_crystal_colour green _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.263 _exptl_crystal_description block _exptl_crystal_F_000 1164 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Benzene and Diethyl Ether' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _refine_diff_density_max 1.063 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.104 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 283 _refine_ls_number_reflns 5657 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.108 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_gt 0.0562 _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^)+(0.0602P)^2^+8.5208P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1272 _refine_ls_wR_factor_ref 0.1489 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4178 _reflns_number_total 5657 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL mo_hzy2232_0m_a.res in P2(1)/c mo_hzy2232_0m.res created by SHELXL-2018/3 at 13:04:16 on 12-Oct-2019 REM Old TITL mo_hzy2232_0m in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.126, Rweak 0.008, Alpha 0.040 REM 0.396 for 237 systematic absences, Orientation as input REM Formula found by SHELXT: C21 N3 Si3 Cl2 Co CELL 0.71073 10.9455 14.6642 18.313 90 100.479 90 ZERR 2 0.0012 0.0016 0.0019 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Co N Si UNIT 84 164 8 4 12 12 L.S. 10 PLAN 20 SIZE 0.15 0.24 0.26 TEMP -123.15 list 4 fmap 2 53 acta OMIT 0 0 2 OMIT 3 0 2 OMIT -4 10 3 OMIT 5 1 16 OMIT 7 12 9 OMIT 1 1 0 OMIT 0 2 0 REM REM REM WGHT 0.060200 8.520802 FVAR 0.49555 CO1 4 0.644229 0.531941 0.544179 11.00000 0.02357 0.02182 = 0.02194 -0.00304 0.00483 -0.00105 CL1 3 0.802236 0.430917 0.579637 11.00000 0.02307 0.02191 = 0.02600 0.00494 0.01092 0.00399 CL2 3 0.541354 0.524992 0.419344 11.00000 0.02111 0.02653 = 0.01753 -0.00333 0.00371 -0.00387 SI1 6 0.705825 0.676743 0.604097 11.00000 0.02024 0.02057 = 0.02285 -0.00179 0.00367 -0.00097 SI3 6 0.933704 0.698109 0.536920 11.00000 0.02136 0.03075 = 0.03132 0.00473 0.00569 -0.00174 SI2 6 0.878989 0.843307 0.645779 11.00000 0.02923 0.02357 = 0.04479 -0.00231 -0.00122 -0.00638 N1 5 0.571656 0.746239 0.616875 11.00000 0.02414 0.02092 = 0.02140 -0.00109 0.00206 0.00205 N2 5 0.680538 0.663978 0.701152 11.00000 0.02602 0.02142 = 0.02349 -0.00065 0.00399 0.00043 N3 5 0.833078 0.742211 0.595247 11.00000 0.02474 0.02488 = 0.02907 0.00065 0.00296 -0.00372 C1 1 0.571175 0.707940 0.684000 11.00000 0.02611 0.01860 = 0.02186 -0.00695 0.00127 0.00002 C2 1 0.470768 0.709522 0.728173 11.00000 0.02775 0.02840 = 0.01985 -0.00183 0.00615 0.00167 C8 1 0.733215 0.606113 0.765795 11.00000 0.03374 0.02912 = 0.01960 -0.00047 0.00070 0.00178 C12 1 0.473825 0.796948 0.565935 11.00000 0.02822 0.02750 = 0.02979 0.00178 0.00408 0.00438 C3 1 0.460303 0.781956 0.776208 11.00000 0.03690 0.02293 = 0.02488 0.00048 0.00465 0.00168 AFIX 43 H3 2 0.515845 0.832157 0.779147 11.00000 -1.20000 AFIX 0 C7 1 0.388084 0.636560 0.723903 11.00000 0.03283 0.03145 = 0.03053 -0.00790 0.00900 -0.00267 AFIX 43 H7 2 0.394253 0.587372 0.691009 11.00000 -1.20000 AFIX 0 C6 1 0.296694 0.635493 0.767563 11.00000 0.03333 0.03797 = 0.03349 0.00285 0.00752 -0.00050 AFIX 43 H6 2 0.240611 0.585628 0.764670 11.00000 -1.20000 AFIX 0 C21 1 0.845765 0.633961 0.456610 11.00000 0.03175 0.03864 = 0.03185 0.00454 0.01332 -0.00283 AFIX 137 H21A 2 0.827548 0.572450 0.472604 11.00000 -1.50000 H21B 2 0.895659 0.629859 0.417390 11.00000 -1.50000 H21C 2 0.767752 0.665775 0.437520 11.00000 -1.50000 AFIX 0 C4 1 0.368978 0.780591 0.819540 11.00000 0.04168 0.03551 = 0.02342 -0.00100 0.00883 0.00992 AFIX 43 H4 2 0.362089 0.829899 0.852193 11.00000 -1.20000 AFIX 0 C10 1 0.680055 0.509468 0.755553 11.00000 0.03749 0.03183 = 0.03205 0.00397 0.00787 -0.00187 AFIX 137 H10A 2 0.590097 0.511481 0.753894 11.00000 -1.50000 H10B 2 0.718966 0.471184 0.797212 11.00000 -1.50000 H10C 2 0.697062 0.483857 0.708994 11.00000 -1.50000 AFIX 0 C19 1 1.053428 0.622231 0.591269 11.00000 0.03020 0.04076 = 0.04059 -0.00138 0.00868 -0.00016 AFIX 137 H19A 2 1.098067 0.655430 0.634445 11.00000 -1.50000 H19B 2 1.112233 0.602814 0.559879 11.00000 -1.50000 H19C 2 1.012955 0.568539 0.608069 11.00000 -1.50000 AFIX 0 C5 1 0.287673 0.707669 0.815473 11.00000 0.03270 0.04891 = 0.02555 0.00300 0.01074 0.00642 AFIX 43 H5 2 0.225506 0.706970 0.845537 11.00000 -1.20000 AFIX 0 C9 1 0.872382 0.603252 0.767415 11.00000 0.03214 0.03894 = 0.04201 0.00607 -0.00386 -0.00040 AFIX 137 H9A 2 0.888548 0.577641 0.720666 11.00000 -1.50000 H9B 2 0.912148 0.565069 0.808922 11.00000 -1.50000 H9C 2 0.906253 0.665200 0.773703 11.00000 -1.50000 AFIX 0 C11 1 0.706898 0.645565 0.838957 11.00000 0.05886 0.04073 = 0.02101 -0.00640 -0.00132 0.01287 AFIX 137 H11A 2 0.736546 0.708692 0.844375 11.00000 -1.50000 H11B 2 0.750049 0.609061 0.880609 11.00000 -1.50000 H11C 2 0.617285 0.644144 0.838628 11.00000 -1.50000 AFIX 0 C16 1 0.794087 0.865802 0.723858 11.00000 0.05675 0.03012 = 0.04941 -0.01403 0.00596 -0.00866 AFIX 137 H16A 2 0.706701 0.879035 0.703693 11.00000 -1.50000 H16B 2 0.831659 0.918180 0.752782 11.00000 -1.50000 H16C 2 0.799428 0.811974 0.755998 11.00000 -1.50000 AFIX 0 C13 1 0.523121 0.810743 0.494818 11.00000 0.04180 0.06769 = 0.02727 0.00630 0.00568 0.01513 AFIX 137 H13A 2 0.605472 0.839100 0.506137 11.00000 -1.50000 H13B 2 0.466454 0.850446 0.461385 11.00000 -1.50000 H13C 2 0.529402 0.751629 0.470814 11.00000 -1.50000 AFIX 0 C20 1 1.011303 0.792804 0.493248 11.00000 0.02931 0.04471 = 0.04707 0.01201 0.00995 -0.00454 AFIX 137 H20A 2 0.947916 0.831043 0.463156 11.00000 -1.50000 H20B 2 1.065566 0.766770 0.461570 11.00000 -1.50000 H20C 2 1.060866 0.829948 0.532260 11.00000 -1.50000 AFIX 0 C18 1 0.852030 0.945738 0.583826 11.00000 0.05194 0.02798 = 0.06115 0.00425 0.00172 -0.00340 AFIX 137 H18A 2 0.905632 0.942321 0.546481 11.00000 -1.50000 H18B 2 0.871516 1.001134 0.613601 11.00000 -1.50000 H18C 2 0.764838 0.947349 0.558984 11.00000 -1.50000 AFIX 0 C17 1 1.045736 0.836232 0.691374 11.00000 0.04011 0.03481 = 0.06570 -0.00382 -0.00722 -0.00709 AFIX 137 H17A 2 1.059587 0.780105 0.720764 11.00000 -1.50000 H17B 2 1.067018 0.889059 0.723984 11.00000 -1.50000 H17C 2 1.098143 0.835817 0.653311 11.00000 -1.50000 AFIX 0 C14 1 0.456470 0.890687 0.599154 11.00000 0.12905 0.04822 = 0.03553 0.00141 -0.00026 0.05477 AFIX 137 H14A 2 0.426416 0.883174 0.646042 11.00000 -1.50000 H14B 2 0.395764 0.925890 0.564338 11.00000 -1.50000 H14C 2 0.536107 0.923080 0.608373 11.00000 -1.50000 AFIX 0 C15 1 0.353605 0.743061 0.549592 11.00000 0.03179 0.09498 = 0.08381 0.04447 -0.01897 -0.01191 AFIX 137 H15A 2 0.370402 0.681923 0.532194 11.00000 -1.50000 H15B 2 0.294483 0.774379 0.511111 11.00000 -1.50000 H15C 2 0.318284 0.738077 0.594914 11.00000 -1.50000 AFIX 0 HKLF 4 REM mo_hzy2232_0m_a.res in P2(1)/c REM wR2 = 0.1489, GooF = S = 1.108, Restrained GooF = 1.108 for all data REM R1 = 0.0562 for 4178 Fo > 4sig(Fo) and 0.0893 for all 5657 data REM 283 parameters refined using 0 restraints END WGHT 0.0596 8.5888 REM Highest difference peak 1.063, deepest hole -0.536, 1-sigma level 0.104 Q1 1 0.8335 0.4283 0.5855 11.00000 0.05 1.06 Q2 1 0.7870 0.4168 0.5677 11.00000 0.05 1.04 Q3 1 0.7693 0.4335 0.5765 11.00000 0.05 1.01 Q4 1 0.7054 0.3784 0.6008 11.00000 0.05 0.50 Q5 1 0.8811 1.1003 0.6418 11.00000 0.05 0.40 Q6 1 0.8201 0.4639 0.5014 11.00000 0.05 0.40 Q7 1 1.0000 0.5000 0.5000 10.50000 0.05 0.40 Q8 1 0.4042 0.8387 0.4401 11.00000 0.05 0.39 Q9 1 0.7749 0.3427 0.5185 11.00000 0.05 0.38 Q10 1 0.8460 0.4809 0.5153 11.00000 0.05 0.37 Q11 1 0.6590 0.4365 0.5541 11.00000 0.05 0.36 Q12 1 0.5923 0.6782 0.4782 11.00000 0.05 0.36 Q13 1 0.7939 0.6312 0.5803 11.00000 0.05 0.35 Q14 1 1.0487 0.6383 0.4601 11.00000 0.05 0.34 Q15 1 0.6061 0.5711 0.6014 11.00000 0.05 0.34 Q16 1 1.1116 0.6720 0.4292 11.00000 0.05 0.34 Q17 1 0.6768 0.5643 0.9012 11.00000 0.05 0.33 Q18 1 0.5579 0.6858 0.8597 11.00000 0.05 0.33 Q19 1 0.3865 0.8593 0.6007 11.00000 0.05 0.33 Q20 1 0.6175 0.7171 0.6001 11.00000 0.05 0.33 REM The information below was added by Olex2. REM REM R1 = 0.0562 for 4178 Fo > 4sig(Fo) and 0.0893 for all 68100 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.06, deepest hole -0.54 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0893 REM R1_gt = 0.0562 REM wR_ref = 0.1489 REM GOOF = 1.108 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 68100 REM Reflections_gt = 4178 REM Parameters = n/a REM Hole = -0.54 REM Peak = 1.06 REM Flack = n/a ; _cod_data_source_file d0dt00570c2.cif _cod_data_source_block 6 _cod_database_code 7705168 _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 0.875 _shelx_estimated_absorpt_t_min 0.797 _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), C6(H6), C4(H4), C5(H5) 2.b Idealised Me refined as rotating group: C21(H21A,H21B,H21C), C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C9(H9A,H9B, H9C), C11(H11A,H11B,H11C), C16(H16A,H16B,H16C), C13(H13A,H13B,H13C), C20(H20A, H20B,H20C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 Co1 Co 0.64423(5) 0.53194(4) 0.54418(3) 0.02236(16) Uani 1 1 d . . . . . Cl1 Cl 0.80224(9) 0.43092(7) 0.57964(5) 0.0229(2) Uani 1 1 d . . . . . Cl2 Cl 0.54135(9) 0.52499(7) 0.41934(5) 0.0217(2) Uani 1 1 d . . . . . Si1 Si 0.70583(11) 0.67674(8) 0.60410(6) 0.0213(3) Uani 1 1 d . . . . . Si3 Si 0.93370(11) 0.69811(9) 0.53692(7) 0.0277(3) Uani 1 1 d . . . . . Si2 Si 0.87899(12) 0.84331(9) 0.64578(8) 0.0335(3) Uani 1 1 d . . . . . N1 N 0.5717(3) 0.7462(2) 0.61688(18) 0.0224(7) Uani 1 1 d . . . . . N2 N 0.6805(3) 0.6640(2) 0.70115(19) 0.0237(8) Uani 1 1 d . . . . . N3 N 0.8331(3) 0.7422(2) 0.5952(2) 0.0265(8) Uani 1 1 d . . . . . C1 C 0.5712(4) 0.7079(3) 0.6840(2) 0.0226(9) Uani 1 1 d . . . . . C2 C 0.4708(4) 0.7095(3) 0.7282(2) 0.0251(9) Uani 1 1 d . . . . . C8 C 0.7332(4) 0.6061(3) 0.7658(2) 0.0280(10) Uani 1 1 d . . . . . C12 C 0.4738(4) 0.7969(3) 0.5659(2) 0.0287(10) Uani 1 1 d . . . . . C3 C 0.4603(4) 0.7820(3) 0.7762(2) 0.0284(10) Uani 1 1 d . . . . . H3 H 0.515845 0.832157 0.779147 0.034 Uiso 1 1 calc R . . . . C7 C 0.3881(4) 0.6366(3) 0.7239(2) 0.0312(10) Uani 1 1 d . . . . . H7 H 0.394253 0.587372 0.691009 0.037 Uiso 1 1 calc R . . . . C6 C 0.2967(5) 0.6355(4) 0.7676(3) 0.0347(11) Uani 1 1 d . . . . . H6 H 0.240611 0.585628 0.764670 0.042 Uiso 1 1 calc R . . . . C21 C 0.8458(4) 0.6340(3) 0.4566(2) 0.0331(11) Uani 1 1 d . . . . . H21A H 0.827548 0.572450 0.472604 0.050 Uiso 1 1 calc GR . . . . H21B H 0.895659 0.629859 0.417390 0.050 Uiso 1 1 calc GR . . . . H21C H 0.767752 0.665775 0.437520 0.050 Uiso 1 1 calc GR . . . . C4 C 0.3690(5) 0.7806(3) 0.8195(2) 0.0332(11) Uani 1 1 d . . . . . H4 H 0.362089 0.829899 0.852193 0.040 Uiso 1 1 calc R . . . . C10 C 0.6801(5) 0.5095(3) 0.7556(3) 0.0336(11) Uani 1 1 d . . . . . H10A H 0.590097 0.511481 0.753894 0.050 Uiso 1 1 calc GR . . . . H10B H 0.718966 0.471184 0.797212 0.050 Uiso 1 1 calc GR . . . . H10C H 0.697062 0.483857 0.708994 0.050 Uiso 1 1 calc GR . . . . C19 C 1.0534(4) 0.6222(4) 0.5913(3) 0.0369(11) Uani 1 1 d . . . . . H19A H 1.098067 0.655430 0.634445 0.055 Uiso 1 1 calc GR . . . . H19B H 1.112233 0.602814 0.559879 0.055 Uiso 1 1 calc GR . . . . H19C H 1.012955 0.568539 0.608069 0.055 Uiso 1 1 calc GR . . . . C5 C 0.2877(4) 0.7077(4) 0.8155(2) 0.0350(11) Uani 1 1 d . . . . . H5 H 0.225506 0.706970 0.845537 0.042 Uiso 1 1 calc R . . . . C9 C 0.8724(4) 0.6033(4) 0.7674(3) 0.0390(12) Uani 1 1 d . . . . . H9A H 0.888548 0.577641 0.720666 0.059 Uiso 1 1 calc GR . . . . H9B H 0.912148 0.565069 0.808922 0.059 Uiso 1 1 calc GR . . . . H9C H 0.906253 0.665200 0.773703 0.059 Uiso 1 1 calc GR . . . . C11 C 0.7069(5) 0.6456(4) 0.8390(3) 0.0413(13) Uani 1 1 d . . . . . H11A H 0.736546 0.708692 0.844375 0.062 Uiso 1 1 calc GR . . . . H11B H 0.750049 0.609061 0.880609 0.062 Uiso 1 1 calc GR . . . . H11C H 0.617285 0.644144 0.838628 0.062 Uiso 1 1 calc GR . . . . C16 C 0.7941(5) 0.8658(4) 0.7239(3) 0.0459(13) Uani 1 1 d . . . . . H16A H 0.706701 0.879035 0.703693 0.069 Uiso 1 1 calc GR . . . . H16B H 0.831659 0.918180 0.752782 0.069 Uiso 1 1 calc GR . . . . H16C H 0.799428 0.811974 0.755998 0.069 Uiso 1 1 calc GR . . . . C13 C 0.5231(5) 0.8107(4) 0.4948(3) 0.0457(14) Uani 1 1 d . . . . . H13A H 0.605472 0.839100 0.506137 0.068 Uiso 1 1 calc GR . . . . H13B H 0.466454 0.850446 0.461385 0.068 Uiso 1 1 calc GR . . . . H13C H 0.529402 0.751629 0.470814 0.068 Uiso 1 1 calc GR . . . . C20 C 1.0113(5) 0.7928(4) 0.4932(3) 0.0400(12) Uani 1 1 d . . . . . H20A H 0.947916 0.831043 0.463156 0.060 Uiso 1 1 calc GR . . . . H20B H 1.065566 0.766770 0.461570 0.060 Uiso 1 1 calc GR . . . . H20C H 1.060866 0.829948 0.532260 0.060 Uiso 1 1 calc GR . . . . C18 C 0.8520(6) 0.9457(4) 0.5838(3) 0.0481(14) Uani 1 1 d . . . . . H18A H 0.905632 0.942321 0.546481 0.072 Uiso 1 1 calc GR . . . . H18B H 0.871516 1.001134 0.613601 0.072 Uiso 1 1 calc GR . . . . H18C H 0.764838 0.947349 0.558984 0.072 Uiso 1 1 calc GR . . . . C17 C 1.0457(5) 0.8362(4) 0.6914(3) 0.0490(14) Uani 1 1 d . . . . . H17A H 1.059587 0.780105 0.720764 0.073 Uiso 1 1 calc GR . . . . H17B H 1.067018 0.889059 0.723984 0.073 Uiso 1 1 calc GR . . . . H17C H 1.098143 0.835817 0.653311 0.073 Uiso 1 1 calc GR . . . . C14 C 0.4565(8) 0.8907(4) 0.5992(3) 0.073(2) Uani 1 1 d . . . . . H14A H 0.426416 0.883174 0.646042 0.109 Uiso 1 1 calc GR . . . . H14B H 0.395764 0.925890 0.564338 0.109 Uiso 1 1 calc GR . . . . H14C H 0.536107 0.923080 0.608373 0.109 Uiso 1 1 calc GR . . . . C15 C 0.3536(5) 0.7431(5) 0.5496(4) 0.074(2) Uani 1 1 d . . . . . H15A H 0.370402 0.681923 0.532194 0.111 Uiso 1 1 calc GR . . . . H15B H 0.294483 0.774379 0.511111 0.111 Uiso 1 1 calc GR . . . . H15C H 0.318284 0.738077 0.594914 0.111 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 Co1 0.0236(3) 0.0218(3) 0.0219(3) -0.0030(2) 0.0048(2) -0.0010(2) Cl1 0.0231(5) 0.0219(5) 0.0260(5) 0.0049(4) 0.0109(4) 0.0040(4) Cl2 0.0211(5) 0.0265(5) 0.0175(5) -0.0033(4) 0.0037(4) -0.0039(4) Si1 0.0202(6) 0.0206(6) 0.0228(6) -0.0018(5) 0.0037(4) -0.0010(5) Si3 0.0214(6) 0.0308(7) 0.0313(6) 0.0047(5) 0.0057(5) -0.0017(5) Si2 0.0292(7) 0.0236(6) 0.0448(8) -0.0023(6) -0.0012(6) -0.0064(5) N1 0.0241(18) 0.0209(18) 0.0214(17) -0.0011(14) 0.0021(14) 0.0020(14) N2 0.0260(19) 0.0214(18) 0.0235(18) -0.0006(14) 0.0040(15) 0.0004(15) N3 0.0247(19) 0.0249(19) 0.0291(19) 0.0007(15) 0.0030(15) -0.0037(15) C1 0.026(2) 0.019(2) 0.022(2) -0.0070(16) 0.0013(17) 0.0000(17) C2 0.028(2) 0.028(2) 0.020(2) -0.0018(17) 0.0061(17) 0.0017(19) C8 0.034(2) 0.029(2) 0.020(2) -0.0005(18) 0.0007(18) 0.0018(19) C12 0.028(2) 0.028(2) 0.030(2) 0.0018(19) 0.0041(19) 0.0044(19) C3 0.037(3) 0.023(2) 0.025(2) 0.0005(18) 0.0046(19) 0.0017(19) C7 0.033(2) 0.031(2) 0.031(2) -0.008(2) 0.009(2) -0.003(2) C6 0.033(3) 0.038(3) 0.033(3) 0.003(2) 0.008(2) -0.001(2) C21 0.032(3) 0.039(3) 0.032(2) 0.005(2) 0.013(2) -0.003(2) C4 0.042(3) 0.036(3) 0.023(2) -0.0010(19) 0.009(2) 0.010(2) C10 0.037(3) 0.032(3) 0.032(2) 0.004(2) 0.008(2) -0.002(2) C19 0.030(3) 0.041(3) 0.041(3) -0.001(2) 0.009(2) 0.000(2) C5 0.033(3) 0.049(3) 0.026(2) 0.003(2) 0.011(2) 0.006(2) C9 0.032(3) 0.039(3) 0.042(3) 0.006(2) -0.004(2) 0.000(2) C11 0.059(3) 0.041(3) 0.021(2) -0.006(2) -0.001(2) 0.013(3) C16 0.057(3) 0.030(3) 0.049(3) -0.014(2) 0.006(3) -0.009(2) C13 0.042(3) 0.068(4) 0.027(2) 0.006(3) 0.006(2) 0.015(3) C20 0.029(3) 0.045(3) 0.047(3) 0.012(2) 0.010(2) -0.005(2) C18 0.052(3) 0.028(3) 0.061(4) 0.004(2) 0.002(3) -0.003(2) C17 0.040(3) 0.035(3) 0.066(4) -0.004(3) -0.007(3) -0.007(2) C14 0.129(6) 0.048(4) 0.036(3) 0.001(3) 0.000(4) 0.055(4) C15 0.032(3) 0.095(6) 0.084(5) 0.044(4) -0.019(3) -0.012(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Co Co 0.3494 0.9721 '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 Co1 Cl2 116.84(4) . . ? Cl1 Co1 Cl2 109.34(4) . 3_666 ? Cl1 Co1 Si1 107.79(4) . . ? Cl2 Co1 Cl2 88.61(4) . 3_666 ? Cl2 Co1 Si1 110.96(4) 3_666 . ? Cl2 Co1 Si1 121.32(4) . . ? Co1 Cl2 Co1 91.39(4) . 3_666 ? N1 Si1 Co1 112.33(12) . . ? N1 Si1 N2 70.87(16) . . ? N1 Si1 C1 35.94(15) . . ? N2 Si1 Co1 105.47(12) . . ? N2 Si1 C1 35.73(15) . . ? N3 Si1 Co1 127.39(14) . . ? N3 Si1 N1 112.42(18) . . ? N3 Si1 N2 114.19(17) . . ? N3 Si1 C1 124.78(17) . . ? C1 Si1 Co1 107.67(11) . . ? N3 Si3 C21 111.64(19) . . ? N3 Si3 C19 110.3(2) . . ? N3 Si3 C20 111.2(2) . . ? C21 Si3 C19 109.4(2) . . ? C21 Si3 C20 104.2(2) . . ? C19 Si3 C20 109.9(2) . . ? N3 Si2 C16 114.4(2) . . ? N3 Si2 C18 110.9(2) . . ? N3 Si2 C17 110.4(2) . . ? C16 Si2 C18 106.0(3) . . ? C17 Si2 C16 104.4(3) . . ? C17 Si2 C18 110.4(3) . . ? C1 N1 Si1 91.2(3) . . ? C1 N1 C12 131.1(4) . . ? C12 N1 Si1 134.4(3) . . ? C1 N2 Si1 90.5(3) . . ? C1 N2 C8 131.3(4) . . ? C8 N2 Si1 135.8(3) . . ? Si1 N3 Si3 116.8(2) . . ? Si1 N3 Si2 125.1(2) . . ? Si2 N3 Si3 117.9(2) . . ? N1 C1 Si1 52.9(2) . . ? N1 C1 C2 128.1(4) . . ? N2 C1 Si1 53.7(2) . . ? N2 C1 N1 105.1(4) . . ? N2 C1 C2 126.7(4) . . ? C2 C1 Si1 167.3(3) . . ? C3 C2 C1 120.7(4) . . ? C7 C2 C1 119.8(4) . . ? C7 C2 C3 119.5(4) . . ? N2 C8 C10 110.3(3) . . ? N2 C8 C9 105.9(4) . . ? N2 C8 C11 111.9(4) . . ? C10 C8 C11 109.2(4) . . ? C9 C8 C10 109.5(4) . . ? C9 C8 C11 109.9(4) . . ? N1 C12 C13 106.2(4) . . ? N1 C12 C14 109.1(4) . . ? N1 C12 C15 111.3(4) . . ? C13 C12 C14 108.2(5) . . ? C13 C12 C15 109.4(5) . . ? C15 C12 C14 112.4(6) . . ? C4 C3 C2 120.0(4) . . ? C6 C7 C2 120.3(4) . . ? C7 C6 C5 119.7(5) . . ? C5 C4 C3 120.3(4) . . ? C4 C5 C6 120.2(4) . . ? 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 Co1 Cl1 2.2801(11) . ? Co1 Cl2 2.4006(11) 3_666 ? Co1 Cl2 2.3597(11) . ? Co1 Si1 2.4286(13) . ? Si1 N1 1.837(4) . ? Si1 N2 1.857(4) . ? Si1 N3 1.723(4) . ? Si1 C1 2.304(4) . ? Si3 N3 1.789(4) . ? Si3 C21 1.860(5) . ? Si3 C19 1.863(5) . ? Si3 C20 1.881(5) . ? Si2 N3 1.771(4) . ? Si2 C16 1.871(6) . ? Si2 C18 1.873(5) . ? Si2 C17 1.867(5) . ? N1 C1 1.352(5) . ? N1 C12 1.485(5) . ? N2 C1 1.346(5) . ? N2 C8 1.485(5) . ? C1 C2 1.479(6) . ? C2 C3 1.397(6) . ? C2 C7 1.394(6) . ? C8 C10 1.531(6) . ? C8 C9 1.519(7) . ? C8 C11 1.534(6) . ? C12 C13 1.511(6) . ? C12 C14 1.529(7) . ? C12 C15 1.517(7) . ? C3 C4 1.385(6) . ? C7 C6 1.390(6) . ? C6 C5 1.390(7) . ? C4 C5 1.385(7) . ?