# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Moatazedi, Zohreh' 'Katz, Michael' 'Leznoff, Daniel' _publ_contact_author_name 'Leznoff, Daniel' _publ_contact_author_email dleznoff@sfu.ca _publ_section_title ; Synthesis and characterization of a series of halide-bridged, multinuclear iron(II) and cobalt(II) diamido complexes and a dinuclear, high-spin cobalt(II) alkyl derivative ; # Attachment '- dleznoff NONM2X2.cif' #============================================================================= data_{[(tBut)2NON]Fe2Br2}2 _database_code_depnum_ccdc_archive 'CCDC 778589' #TrackingRef '- dleznoff NONM2X2.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C24 H60 Br4 Fe4 N4 O2 Si4' _chemical_formula_moiety 'C24 H60 Br4 Fe4 N4 O2 Si4' _chemical_formula_weight 1092.12 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 #------------------------------------------------ _cell_length_a 9.9613(16) _cell_length_b 14.460(2) _cell_length_c 15.729(2) _cell_angle_alpha 90 _cell_angle_beta 104.525(2) _cell_angle_gamma 90 _cell_volume 2193.2(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9911 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 28.13 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour 'light green' _exptl_crystal_size_min 0.25 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.50 _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_meas ? # non-dispersive F(000): _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 5.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5241 _exptl_absorpt_correction_T_max 0.7457 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.70930 _diffrn_measurement_device_type 'Bruker Smart APEX II' _diffrn_detector_type 'APEX II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w and \f scans' _diffrn_ambient_temperature 293 _diffrn_reflns_number 25725 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_theta_min 1.942 _diffrn_reflns_theta_max 28.515 _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 27.089 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 #========================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _reflns_number_total 5236 # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 3727 _refine_ls_number_restraints 0 _refine_ls_number_parameters 191 _oxford_refine_ls_R_factor_ref 0.0255 _refine_ls_wR_factor_ref 0.0247 _refine_ls_goodness_of_fit_ref 2.6652 _refine_ls_shift/su_max 0.0008992 _refine_ls_shift/su_mean 0.0012309 _refine_diff_density_min -0.62 _refine_diff_density_max 0.73 # The values computed from all data _oxford_reflns_number_all 5236 _refine_ls_R_factor_all 0.0402 _refine_ls_wR_factor_all 0.0279 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3900 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_gt 0.0248 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F)] ; _reflns_limit_h_min -13 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _oxford_refine_ls_scale 0.10211(8) _oxford_diffrn_Wilson_B_factor 3.16 _oxford_diffrn_Wilson_scale 127.91 # Number of reflections without Friedels Law is 5236 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 5568 #--------------------------------------------------------- _chemical_name_systematic ; ; # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type Full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment constr # none if no extinction, _refine_ls_extinction_method none #========================================================== # 9. General computing _computing_data_collection ' Bruker SMART APEX II' _computing_data_reduction ' Bruker SMART APEX II' _computing_cell_refinement ' Bruker SMART APEX II' _computing_structure_solution ' SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Si 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' #============================================================================== # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Fe1 Fe 0.53519(4) 0.60328(2) 0.44150(2) 0.0342 1.0000 Uani . . . . . . . Fe2 Fe 0.67970(4) 0.75159(3) 0.42147(3) 0.0400 1.0000 Uani . . . . . . . Br1 Br 0.34045(3) 0.48839(2) 0.421218(19) 0.0461 1.0000 Uani . . . . . . . Br2 Br 0.81645(4) 0.88091(3) 0.41766(3) 0.0858 1.0000 Uani . . . . . . . Si1 Si 0.37106(8) 0.76729(5) 0.36547(5) 0.0410 1.0000 Uani . . . . . . . Si2 Si 0.52856(8) 0.64546(5) 0.25846(5) 0.0386 1.0000 Uani . . . . . . . N1 N 0.5019(2) 0.74197(14) 0.46100(13) 0.0339 1.0000 Uani . . . . . . . N2 N 0.6591(2) 0.62937(14) 0.35640(13) 0.0330 1.0000 Uani . . . . . . . O1 O 0.40359(17) 0.68531(12) 0.30021(11) 0.0379 1.0000 Uani . . . . . . . C1 C 0.1917(3) 0.7493(2) 0.3742(2) 0.0673 1.0000 Uani . . . . . . . C2 C 0.3869(3) 0.88286(19) 0.3161(2) 0.0661 1.0000 Uani . . . . . . . C3 C 0.4631(3) 0.5383(2) 0.19911(19) 0.0576 1.0000 Uani . . . . . . . C4 C 0.5673(3) 0.7335(2) 0.1816(2) 0.0666 1.0000 Uani . . . . . . . C11 C 0.5040(3) 0.78225(19) 0.54964(19) 0.0464 1.0000 Uani . . . . . . . C21 C 0.6518(3) 0.7789(2) 0.60743(19) 0.0652 1.0000 Uani . . . . . . . C111 C 0.4123(3) 0.7251(2) 0.5934(2) 0.0645 1.0000 Uani . . . . . . . C112 C 0.7939(3) 0.57943(19) 0.35937(19) 0.0438 1.0000 Uani . . . . . . . C113 C 0.4537(4) 0.8826(2) 0.5408(2) 0.0782 1.0000 Uani . . . . . . . C211 C 0.7727(3) 0.47545(19) 0.3601(2) 0.0604 1.0000 Uani . . . . . . . C212 C 0.8475(3) 0.6062(2) 0.2791(2) 0.0661 1.0000 Uani . . . . . . . C213 C 0.9020(3) 0.6083(2) 0.4426(2) 0.0560 1.0000 Uani . . . . . . . H11 H 0.1297 0.7489 0.3172 0.094(2) 1.0000 Uiso R . . . . . . H12 H 0.1862 0.6900 0.4045 0.094(2) 1.0000 Uiso R . . . . . . H13 H 0.1659 0.7974 0.4085 0.094(2) 1.0000 Uiso R . . . . . . H21 H 0.4797 0.8908 0.3118 0.070(2) 1.0000 Uiso R . . . . . . H22 H 0.3646 0.9300 0.3523 0.070(2) 1.0000 Uiso R . . . . . . H23 H 0.3256 0.8865 0.2592 0.070(2) 1.0000 Uiso R . . . . . . H31 H 0.3912 0.5587 0.1487 0.075(2) 1.0000 Uiso R . . . . . . H32 H 0.4240 0.4989 0.2354 0.075(2) 1.0000 Uiso R . . . . . . H33 H 0.5366 0.5100 0.1792 0.075(2) 1.0000 Uiso R . . . . . . H41 H 0.4828 0.7511 0.1415 0.090(2) 1.0000 Uiso R . . . . . . H42 H 0.6279 0.7047 0.1504 0.090(2) 1.0000 Uiso R . . . . . . H43 H 0.6102 0.7842 0.2132 0.090(2) 1.0000 Uiso R . . . . . . H211 H 0.6530 0.8064 0.6636 0.094(2) 1.0000 Uiso R . . . . . . H212 H 0.6846 0.7161 0.6174 0.095(2) 1.0000 Uiso R . . . . . . H213 H 0.7148 0.8156 0.5808 0.095(2) 1.0000 Uiso R . . . . . . H1111 H 0.4148 0.7520 0.6496 0.085(2) 1.0000 Uiso R . . . . . . H1112 H 0.3174 0.7242 0.5586 0.085(2) 1.0000 Uiso R . . . . . . H1113 H 0.4464 0.6625 0.6000 0.085(2) 1.0000 Uiso R . . . . . . H1131 H 0.5113 0.9166 0.5109 0.109(2) 1.0000 Uiso R . . . . . . H1132 H 0.4651 0.9075 0.5991 0.110(2) 1.0000 Uiso R . . . . . . H1133 H 0.3555 0.8868 0.5101 0.109(2) 1.0000 Uiso R . . . . . . H2111 H 0.7355 0.4614 0.4112 0.082(2) 1.0000 Uiso R . . . . . . H2112 H 0.8579 0.4448 0.3668 0.082(2) 1.0000 Uiso R . . . . . . H2113 H 0.7055 0.4564 0.3069 0.082(2) 1.0000 Uiso R . . . . . . H2121 H 0.8551 0.6719 0.2762 0.091(2) 1.0000 Uiso R . . . . . . H2122 H 0.9358 0.5783 0.2818 0.091(2) 1.0000 Uiso R . . . . . . H2123 H 0.7799 0.5866 0.2251 0.090(2) 1.0000 Uiso R . . . . . . H2131 H 0.9141 0.6752 0.4443 0.075(2) 1.0000 Uiso R . . . . . . H2132 H 0.9897 0.5767 0.4451 0.075(2) 1.0000 Uiso R . . . . . . H2133 H 0.8683 0.5910 0.4907 0.075(2) 1.0000 Uiso R . . . . . . 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 0.0390(2) 0.0312(2) 0.0346(2) 0.00243(17) 0.01303(17) -0.00557(17) Fe2 0.0387(2) 0.0366(2) 0.0448(2) 0.00341(19) 0.01047(18) -0.00980(18) Br1 0.04722(17) 0.04523(18) 0.04104(17) 0.01084(14) 0.00200(13) -0.01579(14) Br2 0.0859(3) 0.0641(3) 0.1107(3) 0.0097(2) 0.0308(3) -0.0390(2) Si1 0.0369(4) 0.0386(5) 0.0456(5) -0.0011(4) 0.0069(4) 0.0027(4) Si2 0.0396(4) 0.0451(5) 0.0321(4) 0.0038(4) 0.0107(3) -0.0013(4) N1 0.0394(13) 0.0298(12) 0.0328(12) -0.0028(10) 0.0096(10) -0.0039(10) N2 0.0326(12) 0.0355(13) 0.0328(12) 0.0043(10) 0.0116(10) -0.0010(10) O1 0.0340(10) 0.0420(11) 0.0358(10) -0.0020(9) 0.0052(8) 0.0005(8) C1 0.0416(19) 0.084(3) 0.076(3) -0.016(2) 0.0146(18) 0.0049(18) C2 0.077(2) 0.046(2) 0.067(2) 0.0107(17) 0.0021(19) 0.0130(17) C3 0.059(2) 0.066(2) 0.049(2) -0.0156(17) 0.0145(16) 0.0004(17) C4 0.067(2) 0.084(3) 0.050(2) 0.0260(19) 0.0157(17) -0.0008(19) C11 0.062(2) 0.0372(17) 0.0412(18) -0.0086(14) 0.0161(15) -0.0088(15) C21 0.077(2) 0.073(2) 0.0410(19) -0.0100(17) 0.0044(18) -0.0235(19) C111 0.082(2) 0.067(2) 0.056(2) -0.0155(18) 0.0387(19) -0.0115(19) C112 0.0373(16) 0.0477(18) 0.0498(19) 0.0088(15) 0.0171(14) 0.0049(14) C113 0.127(3) 0.045(2) 0.064(2) -0.0167(18) 0.027(2) 0.003(2) C211 0.057(2) 0.048(2) 0.076(2) 0.0043(18) 0.0167(18) 0.0122(16) C212 0.051(2) 0.094(3) 0.064(2) 0.021(2) 0.0332(17) 0.0150(18) C213 0.0383(17) 0.063(2) 0.065(2) 0.0135(18) 0.0107(16) 0.0023(16) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . Br1 2_666 2.5715(5) yes Fe1 . Fe2 . 2.6453(6) yes Fe1 . Br1 . 2.5129(5) yes Fe1 . N1 . 2.068(2) yes Fe1 . N2 . 2.0702(19) yes Fe1 . O1 . 2.5696(17) yes Fe1 . Fe1 2_666 3.6670(8) yes Fe2 . Br2 . 2.3231(6) yes Fe2 . N1 . 2.024(2) yes Fe2 . N2 . 2.027(2) yes Fe2 . O1 . 3.0806(17) yes Si1 . N1 . 1.763(2) yes Si1 . O1 . 1.6525(18) yes Si1 . C1 . 1.844(3) yes Si1 . C2 . 1.866(3) yes Si2 . N2 . 1.765(2) yes Si2 . O1 . 1.6501(17) yes Si2 . C3 . 1.841(3) yes Si2 . C4 . 1.861(3) yes N1 . C11 . 1.506(3) yes N2 . C112 . 1.515(3) yes C1 . H11 . 0.953 no C1 . H12 . 0.989 no C1 . H13 . 0.954 no C2 . H21 . 0.950 no C2 . H22 . 0.950 no C2 . H23 . 0.950 no C3 . H31 . 0.972 no C3 . H32 . 0.956 no C3 . H33 . 0.958 no C4 . H41 . 0.951 no C4 . H42 . 0.963 no C4 . H43 . 0.927 no C11 . C21 . 1.525(4) yes C11 . C111 . 1.519(4) yes C11 . C113 . 1.529(4) yes C21 . H211 . 0.966 no C21 . H212 . 0.964 no C21 . H213 . 0.992 no C111 . H1111 . 0.959 no C111 . H1112 . 0.966 no C111 . H1113 . 0.963 no C112 . C211 . 1.519(4) yes C112 . C212 . 1.539(4) yes C112 . C213 . 1.530(4) yes C113 . H1131 . 0.963 no C113 . H1132 . 0.964 no C113 . H1133 . 0.979 no C211 . H2111 . 0.987 no C211 . H2112 . 0.939 no C211 . H2113 . 0.971 no C212 . H2121 . 0.954 no C212 . H2122 . 0.959 no C212 . H2123 . 0.984 no C213 . H2131 . 0.975 no C213 . H2132 . 0.978 no C213 . H2133 . 0.935 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Br1 2_666 Fe1 . Fe2 . 110.85(2) yes Br1 2_666 Fe1 . Br1 . 87.695(17) yes Fe2 . Fe1 . Br1 . 161.20(2) yes Br1 2_666 Fe1 . N1 . 115.89(6) yes Fe2 . Fe1 . N1 . 48.99(6) yes Br1 . Fe1 . N1 . 120.83(6) yes Br1 2_666 Fe1 . N2 . 113.39(6) yes Fe2 . Fe1 . N2 . 49.07(6) yes Br1 . Fe1 . N2 . 127.22(6) yes N1 . Fe1 . N2 . 93.61(8) yes Br1 2_666 Fe1 . O1 . 176.38(4) yes Fe2 . Fe1 . O1 . 72.40(4) yes Br1 . Fe1 . O1 . 89.15(4) yes N1 . Fe1 . O1 . 67.34(7) yes N2 . Fe1 . O1 . 67.31(7) yes Br1 2_666 Fe1 . Fe1 2_666 43.213(12) yes Fe2 . Fe1 . Fe1 2_666 153.94(2) yes Br1 . Fe1 . Fe1 2_666 44.482(12) yes N1 . Fe1 . Fe1 2_666 131.10(6) yes N2 . Fe1 . Fe1 2_666 133.86(6) yes O1 . Fe1 . Fe1 2_666 133.61(4) yes Fe1 . Fe2 . Br2 . 174.70(2) yes Fe1 . Fe2 . N1 . 50.46(6) yes Br2 . Fe2 . N1 . 128.85(6) yes Fe1 . Fe2 . N2 . 50.51(5) yes Br2 . Fe2 . N2 . 132.42(6) yes N1 . Fe2 . N2 . 96.29(8) yes Fe1 . Fe2 . O1 . 52.66(3) yes Br2 . Fe2 . O1 . 132.28(4) yes N1 . Fe2 . O1 . 56.94(7) yes N2 . Fe2 . O1 . 56.94(6) yes Fe1 . Br1 . Fe1 2_666 92.305(18) yes N1 . Si1 . O1 . 99.34(10) yes N1 . Si1 . C1 . 115.46(13) yes O1 . Si1 . C1 . 106.85(12) yes N1 . Si1 . C2 . 114.76(13) yes O1 . Si1 . C2 . 109.50(12) yes C1 . Si1 . C2 . 110.00(16) yes N2 . Si2 . O1 . 99.38(9) yes N2 . Si2 . C3 . 114.93(13) yes O1 . Si2 . C3 . 106.79(11) yes N2 . Si2 . C4 . 115.45(13) yes O1 . Si2 . C4 . 108.63(13) yes C3 . Si2 . C4 . 110.55(15) yes Fe1 . N1 . Fe2 . 80.55(7) yes Fe1 . N1 . Si1 . 100.76(10) yes Fe2 . N1 . Si1 . 103.93(10) yes Fe1 . N1 . C11 . 123.15(16) yes Fe2 . N1 . C11 . 116.60(16) yes Si1 . N1 . C11 . 122.98(17) yes Fe1 . N2 . Fe2 . 80.42(7) yes Fe1 . N2 . Si2 . 99.21(9) yes Fe2 . N2 . Si2 . 106.56(10) yes Fe1 . N2 . C112 . 124.11(15) yes Fe2 . N2 . C112 . 115.05(16) yes Si2 . N2 . C112 . 122.90(16) yes Fe1 . O1 . Si1 . 86.04(7) yes Fe1 . O1 . Si2 . 84.89(7) yes Si1 . O1 . Si2 . 141.51(11) yes Fe1 . O1 . Fe2 . 54.94(3) yes Si1 . O1 . Fe2 . 71.09(6) yes Si2 . O1 . Fe2 . 73.12(6) yes Si1 . C1 . H11 . 110.0 no Si1 . C1 . H12 . 109.3 no H11 . C1 . H12 . 110.2 no Si1 . C1 . H13 . 110.1 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 107.7 no Si1 . C2 . H21 . 108.9 no Si1 . C2 . H22 . 109.7 no H21 . C2 . H22 . 109.5 no Si1 . C2 . H23 . 109.8 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 109.5 no Si2 . C3 . H31 . 104.7 no Si2 . C3 . H32 . 110.2 no H31 . C3 . H32 . 110.0 no Si2 . C3 . H33 . 108.8 no H31 . C3 . H33 . 109.3 no H32 . C3 . H33 . 113.5 no Si2 . C4 . H41 . 108.7 no Si2 . C4 . H42 . 107.1 no H41 . C4 . H42 . 109.9 no Si2 . C4 . H43 . 109.6 no H41 . C4 . H43 . 110.8 no H42 . C4 . H43 . 110.5 no N1 . C11 . C21 . 109.1(2) yes N1 . C11 . C111 . 109.8(2) yes C21 . C11 . C111 . 108.2(3) yes N1 . C11 . C113 . 110.8(2) yes C21 . C11 . C113 . 109.2(3) yes C111 . C11 . C113 . 109.6(3) yes C11 . C21 . H211 . 108.7 no C11 . C21 . H212 . 111.4 no H211 . C21 . H212 . 108.2 no C11 . C21 . H213 . 110.5 no H211 . C21 . H213 . 107.6 no H212 . C21 . H213 . 110.3 no C11 . C111 . H1111 . 108.5 no C11 . C111 . H1112 . 111.4 no H1111 . C111 . H1112 . 108.8 no C11 . C111 . H1113 . 108.9 no H1111 . C111 . H1113 . 110.8 no H1112 . C111 . H1113 . 108.4 no N2 . C112 . C211 . 110.4(2) yes N2 . C112 . C212 . 110.0(2) yes C211 . C112 . C212 . 109.4(3) yes N2 . C112 . C213 . 108.9(2) yes C211 . C112 . C213 . 109.4(2) yes C212 . C112 . C213 . 108.6(2) yes C11 . C113 . H1131 . 107.8 no C11 . C113 . H1132 . 108.1 no H1131 . C113 . H1132 . 109.3 no C11 . C113 . H1133 . 111.6 no H1131 . C113 . H1133 . 111.8 no H1132 . C113 . H1133 . 108.1 no C112 . C211 . H2111 . 106.9 no C112 . C211 . H2112 . 110.2 no H2111 . C211 . H2112 . 108.9 no C112 . C211 . H2113 . 110.0 no H2111 . C211 . H2113 . 108.9 no H2112 . C211 . H2113 . 111.7 no C112 . C212 . H2121 . 109.7 no C112 . C212 . H2122 . 111.2 no H2121 . C212 . H2122 . 109.8 no C112 . C212 . H2123 . 109.4 no H2121 . C212 . H2123 . 107.0 no H2122 . C212 . H2123 . 109.7 no C112 . C213 . H2131 . 110.5 no C112 . C213 . H2132 . 109.6 no H2131 . C213 . H2132 . 111.0 no C112 . C213 . H2133 . 107.5 no H2131 . C213 . H2133 . 108.1 no H2132 . C213 . H2133 . 110.0 no #=============================================================================== data_{[(tBut)2NON]Co2Br2}2 _database_code_depnum_ccdc_archive 'CCDC 778590' #TrackingRef '- dleznoff NONM2X2.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C24 H60 Br4 Co4 N4 O2 Si4' _chemical_formula_moiety 'C24 H60 Br4 Co4 N4 O2 Si4' _chemical_formula_weight 1104.46 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 #------------------------------------------------ _cell_length_a 9.9296(2) _cell_length_b 14.2666(3) _cell_length_c 15.5281(3) _cell_angle_alpha 90 _cell_angle_beta 104.2860(10) _cell_angle_gamma 90 _cell_volume 2131.71(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9935 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 35.34 _cell_measurement_temperature 149(2) _exptl_crystal_description cube _exptl_crystal_colour blue _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_max 0.50 _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_meas ? # non-dispersive F(000): _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 5.417 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4997 _exptl_absorpt_correction_T_max 0.7461 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.70930 _diffrn_measurement_device_type 'Bruker Smart APEX II' _diffrn_detector_type 'APEX II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w and \f scans' _diffrn_ambient_temperature 149(2) _diffrn_reflns_number 88444 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_min 1.967 _diffrn_reflns_theta_max 36.681 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 34.480 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 #========================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _reflns_number_total 10515 # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 6474 _refine_ls_number_restraints 0 _refine_ls_number_parameters 192 _oxford_refine_ls_R_factor_ref 0.0211 _refine_ls_wR_factor_ref 0.0213 _refine_ls_goodness_of_fit_ref 0.7141 _refine_ls_shift/su_max 0.0019217 _refine_ls_shift/su_mean 0.0150124 _refine_diff_density_min -0.63 _refine_diff_density_max 0.74 # The values computed from all data _oxford_reflns_number_all 10515 _refine_ls_R_factor_all 0.0452 _refine_ls_wR_factor_all 0.0257 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6873 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_gt 0.0216 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F)] ; _reflns_limit_h_min -16 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _oxford_refine_ls_scale 0.30235(17) _oxford_diffrn_Wilson_B_factor 1.47 _oxford_diffrn_Wilson_scale 7.02 # Number of reflections without Friedels Law is 10515 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 10602 #--------------------------------------------------------- _chemical_name_systematic ; ; # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type Full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment constr # none if no extinction, _refine_ls_extinction_method 'Larson (1970), Equation 22' _refine_ls_extinction_coef 12.0(20) #========================================================== # 9. General computing _computing_data_collection ' Bruker SMART APEX II' _computing_data_reduction ' Bruker SMART APEX II' _computing_cell_refinement ' Bruker SMART APEX II' _computing_structure_solution ' SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Si 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' #============================================================================== # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Co1 Co 0.53398(2) 0.896771(14) 0.443228(13) 0.0147 1.0000 Uani . . . . . . . Co2 Co 0.67614(2) 0.749726(15) 0.423176(14) 0.0188 1.0000 Uani . . . . . . . Br1 Br 0.343733(15) 1.010829(11) 0.420044(10) 0.0197 1.0000 Uani . . . . . . . Br2 Br 0.80170(2) 0.615982(14) 0.411360(16) 0.0418 1.0000 Uani . . . . . . . Si1 Si 0.52767(4) 0.85582(3) 0.26005(3) 0.0179 1.0000 Uani . . . . . . . Si2 Si 0.36982(4) 0.73333(3) 0.37046(3) 0.0186 1.0000 Uani . . . . . . . N1 N 0.65815(12) 0.87090(9) 0.35919(8) 0.0161 1.0000 Uani . . . . . . . N2 N 0.50334(12) 0.75915(9) 0.46507(8) 0.0162 1.0000 Uani . . . . . . . O1 O 0.40251(10) 0.81541(7) 0.30326(7) 0.0180 1.0000 Uani . . . . . . . C1 C 0.46453(17) 0.96452(13) 0.19972(11) 0.0269 1.0000 Uani . . . . . . . C2 C 0.56702(19) 0.76610(14) 0.18299(12) 0.0337 1.0000 Uani . . . . . . . C3 C 0.19122(16) 0.75198(14) 0.38286(13) 0.0321 1.0000 Uani . . . . . . . C4 C 0.38425(19) 0.61653(12) 0.32066(13) 0.0313 1.0000 Uani . . . . . . . C11 C 0.79425(15) 0.91947(11) 0.36393(11) 0.0200 1.0000 Uani . . . . . . . C21 C 0.51055(17) 0.71987(11) 0.55584(10) 0.0219 1.0000 Uani . . . . . . . C111 C 0.85129(17) 0.89039(14) 0.28459(12) 0.0308 1.0000 Uani . . . . . . . C112 C 0.89833(15) 0.88884(12) 0.44941(11) 0.0244 1.0000 Uani . . . . . . . C113 C 0.77691(17) 1.02535(12) 0.36414(12) 0.0265 1.0000 Uani . . . . . . . C211 C 0.4642(2) 0.61755(12) 0.54901(13) 0.0341 1.0000 Uani . . . . . . . C212 C 0.41852(19) 0.77749(13) 0.60142(12) 0.0294 1.0000 Uani . . . . . . . C213 C 0.66021(18) 0.72457(13) 0.61104(11) 0.0295 1.0000 Uani . . . . . . . H11 H 0.4330 1.0070 0.2378 0.0359(11) 1.0000 Uiso R . . . . . . H12 H 0.5356 0.9920 0.1778 0.0360(11) 1.0000 Uiso R . . . . . . H13 H 0.3879 0.9483 0.1520 0.0363(11) 1.0000 Uiso R . . . . . . H21 H 0.4819 0.7423 0.1467 0.0482(11) 1.0000 Uiso R . . . . . . H22 H 0.6182 0.7147 0.2147 0.0494(11) 1.0000 Uiso R . . . . . . H23 H 0.6208 0.7927 0.1471 0.0479(11) 1.0000 Uiso R . . . . . . H31 H 0.1816 0.8152 0.4063 0.0453(11) 1.0000 Uiso R . . . . . . H32 H 0.1682 0.7057 0.4232 0.0452(11) 1.0000 Uiso R . . . . . . H33 H 0.1259 0.7456 0.3258 0.0455(11) 1.0000 Uiso R . . . . . . H41 H 0.3272 0.6140 0.2602 0.0412(11) 1.0000 Uiso R . . . . . . H42 H 0.4769 0.6027 0.3194 0.0414(11) 1.0000 Uiso R . . . . . . H43 H 0.3559 0.5671 0.3546 0.0425(11) 1.0000 Uiso R . . . . . . H1111 H 0.8598 0.8229 0.2815 0.0444(11) 1.0000 Uiso R . . . . . . H1112 H 0.7880 0.9128 0.2298 0.0434(11) 1.0000 Uiso R . . . . . . H1113 H 0.9428 0.9182 0.2902 0.0430(11) 1.0000 Uiso R . . . . . . H1121 H 0.9843 0.9217 0.4554 0.0312(11) 1.0000 Uiso R . . . . . . H1122 H 0.9123 0.8193 0.4493 0.0306(11) 1.0000 Uiso R . . . . . . H1123 H 0.8642 0.9054 0.5005 0.0300(11) 1.0000 Uiso R . . . . . . H1131 H 0.8653 1.0560 0.3674 0.0351(11) 1.0000 Uiso R . . . . . . H1132 H 0.7404 1.0456 0.4145 0.0352(11) 1.0000 Uiso R . . . . . . H1133 H 0.7121 1.0452 0.3099 0.0361(11) 1.0000 Uiso R . . . . . . H2111 H 0.5191 0.5845 0.5179 0.0486(11) 1.0000 Uiso R . . . . . . H2112 H 0.4770 0.5922 0.6059 0.0473(11) 1.0000 Uiso R . . . . . . H2113 H 0.3683 0.6113 0.5170 0.0467(11) 1.0000 Uiso R . . . . . . H2121 H 0.4518 0.8402 0.6080 0.0408(11) 1.0000 Uiso R . . . . . . H2122 H 0.4250 0.7510 0.6589 0.0417(11) 1.0000 Uiso R . . . . . . H2123 H 0.3239 0.7760 0.5692 0.0422(11) 1.0000 Uiso R . . . . . . H2131 H 0.6648 0.7018 0.6695 0.0383(11) 1.0000 Uiso R . . . . . . H2132 H 0.7186 0.6866 0.5835 0.0391(11) 1.0000 Uiso R . . . . . . H2133 H 0.6934 0.7891 0.6150 0.0388(11) 1.0000 Uiso R . . . . . . 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 0.01712(9) 0.01252(9) 0.01501(9) -0.00073(7) 0.00528(7) 0.00281(7) Co2 0.01805(9) 0.01623(9) 0.02182(10) -0.00194(8) 0.00460(7) 0.00475(8) Br1 0.02145(7) 0.01833(7) 0.01747(7) -0.00382(6) 0.00128(5) 0.00665(6) Br2 0.04119(11) 0.02870(10) 0.05669(14) -0.00804(9) 0.01441(10) 0.01750(8) Si1 0.01834(18) 0.0212(2) 0.01434(18) -0.00243(16) 0.00460(15) 0.00039(16) Si2 0.01724(18) 0.0161(2) 0.0211(2) 0.00115(16) 0.00221(15) -0.00102(15) N1 0.0152(5) 0.0183(6) 0.0152(6) -0.0028(5) 0.0044(4) 0.0002(4) N2 0.0194(6) 0.0134(6) 0.0162(6) 0.0005(5) 0.0051(5) 0.0019(4) O1 0.0171(5) 0.0187(5) 0.0171(5) 0.0009(4) 0.0023(4) -0.0005(4) C1 0.0261(8) 0.0320(9) 0.0217(8) 0.0073(7) 0.0045(6) -0.0016(7) C2 0.0314(9) 0.0445(12) 0.0252(9) -0.0165(8) 0.0067(7) 0.0021(8) C3 0.0195(7) 0.0394(10) 0.0375(10) 0.0094(9) 0.0073(7) -0.0017(7) C4 0.0355(9) 0.0200(8) 0.0328(9) -0.0045(7) -0.0021(7) -0.0037(7) C11 0.0170(6) 0.0225(7) 0.0215(7) -0.0028(6) 0.0067(6) -0.0012(6) C21 0.0299(8) 0.0177(7) 0.0182(7) 0.0049(6) 0.0060(6) 0.0038(6) C111 0.0238(8) 0.0432(11) 0.0294(9) -0.0074(8) 0.0140(7) -0.0036(7) C112 0.0174(7) 0.0268(8) 0.0277(8) -0.0051(7) 0.0031(6) 0.0000(6) C113 0.0269(8) 0.0219(8) 0.0308(9) -0.0005(7) 0.0072(7) -0.0044(6) C211 0.0508(11) 0.0200(8) 0.0306(9) 0.0075(7) 0.0085(8) 0.0007(8) C212 0.0392(10) 0.0287(9) 0.0246(8) 0.0059(7) 0.0160(7) 0.0046(7) C213 0.0361(9) 0.0285(9) 0.0197(8) 0.0032(7) -0.0013(7) 0.0090(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 . Br1 2_676 2.5392(3) yes Co1 . Co2 . 2.5899(3) yes Co1 . Br1 . 2.4516(2) yes Co1 . N1 . 2.0379(12) yes Co1 . N2 . 2.0281(12) yes Co1 . O1 . 2.5248(10) yes Co1 . Co1 2_676 3.5815(4) yes Co2 . Br2 . 2.3112(3) yes Co2 . N1 . 1.9799(13) yes Co2 . N2 . 1.9840(12) yes Co2 . O1 . 3.0382(10) yes Si1 . N1 . 1.7636(13) yes Si1 . O1 . 1.6549(11) yes Si1 . C1 . 1.8402(17) yes Si1 . C2 . 1.8583(17) yes Si2 . N2 . 1.7579(13) yes Si2 . O1 . 1.6531(11) yes Si2 . C3 . 1.8497(16) yes Si2 . C4 . 1.8573(17) yes N1 . C11 . 1.5043(18) yes N2 . C21 . 1.5021(19) yes C1 . H11 . 0.952 no C1 . H12 . 0.942 no C1 . H13 . 0.951 no C2 . H21 . 0.956 no C2 . H22 . 0.956 no C2 . H23 . 0.941 no C3 . H31 . 0.986 no C3 . H32 . 0.975 no C3 . H33 . 0.964 no C4 . H41 . 0.970 no C4 . H42 . 0.946 no C4 . H43 . 0.963 no C11 . C111 . 1.535(2) yes C11 . C112 . 1.531(2) yes C11 . C113 . 1.520(2) yes C21 . C211 . 1.527(2) yes C21 . C212 . 1.527(2) yes C21 . C213 . 1.523(2) yes C111 . H1111 . 0.968 no C111 . H1112 . 0.978 no C111 . H1113 . 0.976 no C112 . H1121 . 0.958 no C112 . H1122 . 1.001 no C112 . H1123 . 0.966 no C113 . H1131 . 0.970 no C113 . H1132 . 0.984 no C113 . H1133 . 0.968 no C211 . H2111 . 0.940 no C211 . H2112 . 0.934 no C211 . H2113 . 0.963 no C212 . H2121 . 0.950 no C212 . H2122 . 0.957 no C212 . H2123 . 0.950 no C213 . H2131 . 0.954 no C213 . H2132 . 0.967 no C213 . H2133 . 0.974 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Br1 2_676 Co1 . Co2 . 111.019(9) yes Br1 2_676 Co1 . Br1 . 88.302(8) yes Co2 . Co1 . Br1 . 160.574(11) yes Br1 2_676 Co1 . N1 . 112.92(3) yes Co2 . Co1 . N1 . 48.89(4) yes Br1 . Co1 . N1 . 126.31(4) yes Br1 2_676 Co1 . N2 . 115.04(4) yes Co2 . Co1 . N2 . 49.05(3) yes Br1 . Co1 . N2 . 121.68(3) yes N1 . Co1 . N2 . 94.08(5) yes Br1 2_676 Co1 . O1 . 175.88(3) yes Co2 . Co1 . O1 . 72.87(2) yes Br1 . Co1 . O1 . 87.87(2) yes N1 . Co1 . O1 . 68.38(4) yes N2 . Co1 . O1 . 68.40(4) yes Br1 2_676 Co1 . Co1 2_676 43.175(6) yes Co2 . Co1 . Co1 2_676 154.140(12) yes Br1 . Co1 . Co1 2_676 45.127(6) yes N1 . Co1 . Co1 2_676 132.95(4) yes N2 . Co1 . Co1 2_676 131.27(4) yes O1 . Co1 . Co1 2_676 132.97(3) yes Co1 . Co2 . Br2 . 177.403(12) yes Co1 . Co2 . N1 . 50.85(3) yes Br2 . Co2 . N1 . 131.66(4) yes Co1 . Co2 . N2 . 50.55(4) yes Br2 . Co2 . N2 . 127.53(4) yes N1 . Co2 . N2 . 97.30(5) yes Co1 . Co2 . O1 . 52.58(2) yes Br2 . Co2 . O1 . 128.63(2) yes N1 . Co2 . O1 . 57.78(4) yes N2 . Co2 . O1 . 57.66(4) yes Co1 2_676 Br1 . Co1 . 91.698(8) yes N1 . Si1 . O1 . 98.74(6) yes N1 . Si1 . C1 . 115.23(7) yes O1 . Si1 . C1 . 107.72(7) yes N1 . Si1 . C2 . 114.85(7) yes O1 . Si1 . C2 . 108.63(8) yes C1 . Si1 . C2 . 110.61(9) yes N2 . Si2 . O1 . 98.86(6) yes N2 . Si2 . C3 . 115.31(8) yes O1 . Si2 . C3 . 107.84(7) yes N2 . Si2 . C4 . 114.60(7) yes O1 . Si2 . C4 . 108.99(7) yes C3 . Si2 . C4 . 110.30(9) yes Co1 . N1 . Co2 . 80.26(5) yes Co1 . N1 . Si1 . 98.68(5) yes Co2 . N1 . Si1 . 106.70(6) yes Co1 . N1 . C11 . 124.30(9) yes Co2 . N1 . C11 . 114.14(9) yes Si1 . N1 . C11 . 123.81(10) yes Co1 . N2 . Co2 . 80.40(5) yes Co1 . N2 . Si2 . 100.17(6) yes Co2 . N2 . Si2 . 104.28(6) yes Co1 . N2 . C21 . 122.94(10) yes Co2 . N2 . C21 . 115.95(9) yes Si2 . N2 . C21 . 123.88(10) yes Co1 . O1 . Si1 . 84.74(4) yes Co1 . O1 . Si2 . 85.57(4) yes Si1 . O1 . Si2 . 141.89(7) yes Co1 . O1 . Co2 . 54.55(2) yes Si1 . O1 . Co2 . 73.05(4) yes Si2 . O1 . Co2 . 71.33(4) yes Si1 . C1 . H11 . 110.1 no Si1 . C1 . H12 . 110.1 no H11 . C1 . H12 . 110.5 no Si1 . C1 . H13 . 107.4 no H11 . C1 . H13 . 108.5 no H12 . C1 . H13 . 110.3 no Si1 . C2 . H21 . 109.2 no Si1 . C2 . H22 . 111.4 no H21 . C2 . H22 . 108.2 no Si1 . C2 . H23 . 110.1 no H21 . C2 . H23 . 110.0 no H22 . C2 . H23 . 107.9 no Si2 . C3 . H31 . 110.6 no Si2 . C3 . H32 . 110.6 no H31 . C3 . H32 . 108.9 no Si2 . C3 . H33 . 109.6 no H31 . C3 . H33 . 108.7 no H32 . C3 . H33 . 108.3 no Si2 . C4 . H41 . 110.5 no Si2 . C4 . H42 . 111.8 no H41 . C4 . H42 . 108.1 no Si2 . C4 . H43 . 111.5 no H41 . C4 . H43 . 108.8 no H42 . C4 . H43 . 106.0 no N1 . C11 . C111 . 109.96(13) yes N1 . C11 . C112 . 108.48(12) yes C111 . C11 . C112 . 108.36(13) yes N1 . C11 . C113 . 110.91(12) yes C111 . C11 . C113 . 109.56(14) yes C112 . C11 . C113 . 109.53(14) yes N2 . C21 . C211 . 110.35(14) yes N2 . C21 . C212 . 109.80(12) yes C211 . C21 . C212 . 110.02(14) yes N2 . C21 . C213 . 109.01(13) yes C211 . C21 . C213 . 108.47(14) yes C212 . C21 . C213 . 109.15(14) yes C11 . C111 . H1111 . 111.2 no C11 . C111 . H1112 . 108.9 no H1111 . C111 . H1112 . 109.1 no C11 . C111 . H1113 . 109.8 no H1111 . C111 . H1113 . 108.6 no H1112 . C111 . H1113 . 109.2 no C11 . C112 . H1121 . 109.8 no C11 . C112 . H1122 . 110.2 no H1121 . C112 . H1122 . 111.3 no C11 . C112 . H1123 . 110.1 no H1121 . C112 . H1123 . 106.6 no H1122 . C112 . H1123 . 108.7 no C11 . C113 . H1131 . 110.3 no C11 . C113 . H1132 . 111.0 no H1131 . C113 . H1132 . 109.4 no C11 . C113 . H1133 . 109.9 no H1131 . C113 . H1133 . 108.2 no H1132 . C113 . H1133 . 108.1 no C21 . C211 . H2111 . 108.2 no C21 . C211 . H2112 . 109.6 no H2111 . C211 . H2112 . 109.4 no C21 . C211 . H2113 . 111.5 no H2111 . C211 . H2113 . 108.3 no H2112 . C211 . H2113 . 109.8 no C21 . C212 . H2121 . 108.9 no C21 . C212 . H2122 . 108.0 no H2121 . C212 . H2122 . 109.3 no C21 . C212 . H2123 . 111.8 no H2121 . C212 . H2123 . 110.6 no H2122 . C212 . H2123 . 108.3 no C21 . C213 . H2131 . 109.4 no C21 . C213 . H2132 . 109.6 no H2131 . C213 . H2132 . 109.7 no C21 . C213 . H2133 . 110.2 no H2131 . C213 . H2133 . 109.0 no H2132 . C213 . H2133 . 109.0 no #=============================================================================== data_{[(tBut)2NON]Fe2Cl2} _database_code_depnum_ccdc_archive 'CCDC 778591' #TrackingRef '- dleznoff NONM2X2.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C12 H30 Cl2 Fe2 N2 O1 Si2' _chemical_formula_moiety 'C12 H30 Cl2 Fe2 N2 O1 Si2' _chemical_formula_weight 457.15 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------ _cell_length_a 8.678(4) _cell_length_b 10.910(5) _cell_length_c 12.131(5) _cell_angle_alpha 73.617(5) _cell_angle_beta 89.898(6) _cell_angle_gamma 68.368(6) _cell_volume 1017.4(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2003 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 24.74 _cell_measurement_temperature 150(2) _exptl_crystal_description cube _exptl_crystal_colour 'dark yellow' _exptl_crystal_size_min 0.25 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_meas ? # non-dispersive F(000): _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 1.805 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6110 _exptl_absorpt_correction_T_max 0.7457 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.70930 _diffrn_measurement_device_type 'Bruker Smart APEX II' _diffrn_detector_type 'APEX II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w and \f scans' _diffrn_ambient_temperature 150(2) _diffrn_reflns_number 4630 _diffrn_reflns_av_R_equivalents 0.123 _diffrn_reflns_theta_min 1.761 _diffrn_reflns_theta_max 28.329 _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 25.497 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 #========================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _reflns_number_total 4630 # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 2147 _refine_ls_number_restraints 0 _refine_ls_number_parameters 192 _oxford_refine_ls_R_factor_ref 0.0694 _refine_ls_wR_factor_ref 0.0776 _refine_ls_goodness_of_fit_ref 1.3226 _refine_ls_shift/su_max 0.0000804 _refine_ls_shift/su_mean 0.0000510 _refine_diff_density_min -0.77 _refine_diff_density_max 1.12 # The values computed from all data _oxford_reflns_number_all 4630 _refine_ls_R_factor_all 0.1585 _refine_ls_wR_factor_all 0.1193 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2396 _refine_ls_R_factor_gt 0.0774 _refine_ls_wR_factor_gt 0.0815 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F) + (0.03P)^2^] ,where P=(max(Fo,0) + 2Fc)/3 ; _refine_special_details ; The data was collected as a single crystal. The solution was passed through ROTAX once a reasonable model was obtained. ROTAX indicated that a twin was present with a 180degree rotation about the 0 1 4 direction (FOM = 1.3). twin law: 1 0 0 0 -1 0.5 0 0 1 The Rvalue decreased from 9.3% to the observed 7% with a concomitant decrease in the residual electron density. ; _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -13 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _oxford_refine_ls_scale 0.1816(6) _oxford_diffrn_Wilson_B_factor 1.37 _oxford_diffrn_Wilson_scale 35.67 loop_ _oxford_twin_element_scale_factors 0.805(4) 0.195(4) # Number of reflections without Friedels Law is 4630 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 4926 #--------------------------------------------------------- _chemical_name_systematic ; ; # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type Full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment constr # none if no extinction, _refine_ls_extinction_method none #========================================================== # 9. General computing _computing_data_collection ' Bruker SMART APEX II' _computing_data_reduction ' Bruker SMART APEX II' _computing_cell_refinement ' Bruker SMART APEX II' _computing_structure_solution ' SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Si 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' #============================================================================== # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Fe1 Fe 0.0650(2) 0.48596(17) 0.14278(14) 0.0192 1.0000 Uani . . . . . . . Fe2 Fe 0.0588(2) 0.49838(17) 0.35834(14) 0.0185 1.0000 Uani . . . . . . . Cl1 Cl 0.1882(4) 0.4750(3) -0.0331(2) 0.0278 1.0000 Uani . . . . . . . Cl2 Cl -0.1828(3) 0.5134(3) 0.4603(2) 0.0259 1.0000 Uani . . . . . . . Si1 Si 0.3759(4) 0.2973(3) 0.2999(3) 0.0218 1.0000 Uani . . . . . . . Si2 Si 0.2737(4) 0.6259(3) 0.2120(3) 0.0214 1.0000 Uani . . . . . . . O1 O 0.3661(9) 0.4572(7) 0.2482(8) 0.0278 1.0000 Uani . . . . . . . N1 N 0.1596(10) 0.3288(8) 0.2962(8) 0.0174 1.0000 Uani . . . . . . . N2 N 0.0602(10) 0.6450(8) 0.2082(8) 0.0156 1.0000 Uani . . . . . . . C1 C 0.4998(15) 0.2167(13) 0.4440(11) 0.0323 1.0000 Uani . . . . . . . C2 C 0.4925(16) 0.2014(13) 0.2039(11) 0.0365 1.0000 Uani . . . . . . . C3 C 0.3499(16) 0.6860(13) 0.3208(11) 0.0360 1.0000 Uani . . . . . . . C4 C 0.3396(15) 0.6987(12) 0.0705(10) 0.0302 1.0000 Uani . . . . . . . C11 C 0.1035(14) 0.2093(11) 0.3401(10) 0.0233 1.0000 Uani . . . . . . . C21 C -0.0765(13) 0.7871(11) 0.1619(10) 0.0227 1.0000 Uani . . . . . . . C111 C 0.2059(15) 0.0863(12) 0.3011(10) 0.0294 1.0000 Uani . . . . . . . C112 C -0.0796(14) 0.2529(11) 0.2949(10) 0.0291 1.0000 Uani . . . . . . . C113 C 0.1192(15) 0.1620(13) 0.4747(9) 0.0287 1.0000 Uani . . . . . . . C211 C -0.0983(15) 0.8358(12) 0.0278(10) 0.0303 1.0000 Uani . . . . . . . C212 C -0.2416(14) 0.7820(12) 0.2026(11) 0.0338 1.0000 Uani . . . . . . . C213 C -0.0409(15) 0.8923(11) 0.2055(10) 0.0276 1.0000 Uani . . . . . . . H11 H 0.4498 0.2695 0.4972 0.039(6) 1.0000 Uiso R . . . . . . H12 H 0.6133 0.2126 0.4404 0.038(6) 1.0000 Uiso R . . . . . . H13 H 0.5043 0.1238 0.4781 0.038(6) 1.0000 Uiso R . . . . . . H21 H 0.5278 0.1001 0.2418 0.041(6) 1.0000 Uiso R . . . . . . H22 H 0.5931 0.2184 0.1882 0.041(6) 1.0000 Uiso R . . . . . . H23 H 0.4270 0.2237 0.1324 0.041(6) 1.0000 Uiso R . . . . . . H31 H 0.2965 0.6716 0.3902 0.044(6) 1.0000 Uiso R . . . . . . H32 H 0.4701 0.6363 0.3415 0.044(6) 1.0000 Uiso R . . . . . . H33 H 0.3286 0.7838 0.2900 0.044(6) 1.0000 Uiso R . . . . . . H41 H 0.2935 0.7974 0.0453 0.041(6) 1.0000 Uiso R . . . . . . H42 H 0.3017 0.6693 0.0099 0.041(6) 1.0000 Uiso R . . . . . . H43 H 0.4585 0.6676 0.0726 0.041(6) 1.0000 Uiso R . . . . . . H1111 H 0.1692 0.0116 0.3288 0.034(6) 1.0000 Uiso R . . . . . . H1112 H 0.2019 0.1114 0.2186 0.034(6) 1.0000 Uiso R . . . . . . H1113 H 0.3248 0.0524 0.3333 0.034(6) 1.0000 Uiso R . . . . . . H1121 H -0.1176 0.1795 0.3252 0.031(6) 1.0000 Uiso R . . . . . . H1122 H -0.0945 0.2785 0.2108 0.031(6) 1.0000 Uiso R . . . . . . H1123 H -0.1504 0.3324 0.3162 0.031(6) 1.0000 Uiso R . . . . . . H1131 H 0.0815 0.0881 0.5025 0.032(6) 1.0000 Uiso R . . . . . . H1132 H 0.2346 0.1337 0.5050 0.032(6) 1.0000 Uiso R . . . . . . H1133 H 0.0509 0.2411 0.5009 0.032(6) 1.0000 Uiso R . . . . . . H2111 H -0.1233 0.7698 -0.0010 0.027(6) 1.0000 Uiso R . . . . . . H2112 H -0.1855 0.9244 -0.0025 0.027(6) 1.0000 Uiso R . . . . . . H2113 H 0.0057 0.8401 -0.0007 0.027(6) 1.0000 Uiso R . . . . . . H2121 H -0.3318 0.8689 0.1697 0.034(6) 1.0000 Uiso R . . . . . . H2122 H -0.2360 0.7585 0.2870 0.034(6) 1.0000 Uiso R . . . . . . H2123 H -0.2651 0.7110 0.1811 0.034(6) 1.0000 Uiso R . . . . . . H2131 H -0.0299 0.8655 0.2895 0.031(6) 1.0000 Uiso R . . . . . . H2132 H 0.0624 0.8996 0.1811 0.031(6) 1.0000 Uiso R . . . . . . H2133 H -0.1290 0.9824 0.1771 0.031(6) 1.0000 Uiso R . . . . . . 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 0.0272(11) 0.0214(10) 0.0099(9) -0.0062(7) -0.0009(7) -0.0091(9) Fe2 0.0265(11) 0.0234(10) 0.0081(9) -0.0065(7) 0.0046(7) -0.0110(9) Cl1 0.0251(17) 0.044(2) 0.0157(16) -0.0125(14) 0.0015(12) -0.0124(15) Cl2 0.0208(17) 0.045(2) 0.0147(16) -0.0121(14) 0.0053(12) -0.0139(15) Si1 0.0199(17) 0.0264(18) 0.0158(17) -0.0081(17) 0.0010(15) -0.0040(14) Si2 0.0228(18) 0.0261(19) 0.0185(18) -0.0069(16) 0.0044(16) -0.0130(15) O1 0.023(4) 0.024(4) 0.038(5) -0.009(4) 0.014(4) -0.011(4) N1 0.025(5) 0.018(5) 0.014(5) -0.005(5) 0.006(5) -0.014(4) N2 0.022(5) 0.021(5) 0.006(5) -0.003(4) 0.001(4) -0.012(4) C1 0.028(8) 0.038(8) 0.032(8) -0.019(7) -0.002(6) -0.008(6) C2 0.034(8) 0.039(8) 0.024(8) -0.006(6) -0.010(6) -0.003(6) C3 0.042(9) 0.040(8) 0.027(8) -0.016(7) 0.004(7) -0.013(7) C4 0.032(8) 0.033(8) 0.025(7) -0.005(6) 0.004(6) -0.015(6) C11 0.030(7) 0.024(7) 0.015(7) -0.009(6) 0.002(6) -0.007(5) C21 0.021(6) 0.023(7) 0.013(7) 0.000(5) -0.001(5) -0.001(5) C111 0.034(8) 0.030(8) 0.023(7) 0.001(6) 0.001(6) -0.018(6) C112 0.039(8) 0.030(7) 0.021(7) 0.002(6) 0.002(6) -0.024(6) C113 0.032(7) 0.038(8) 0.017(7) -0.006(6) 0.015(6) -0.016(6) C211 0.027(7) 0.030(7) 0.018(7) -0.003(6) 0.000(6) 0.005(6) C212 0.035(8) 0.031(8) 0.025(8) -0.002(6) 0.009(6) -0.005(6) C213 0.032(7) 0.016(7) 0.028(7) -0.008(6) 0.010(6) 0.000(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . Cl1 2_565 2.405(3) yes Fe1 . Fe2 . 2.656(2) yes Fe1 . Cl1 . 2.398(3) yes Fe1 . N1 . 2.061(9) yes Fe1 . N2 . 2.089(9) yes Fe1 . Fe1 2_565 3.539(4) yes Fe1 . O1 . 2.782(8) yes Fe2 . Cl2 2_566 2.400(3) yes Fe2 . Cl2 . 2.409(3) yes Fe2 . N1 . 2.085(9) yes Fe2 . N2 . 2.061(8) yes Fe2 . Fe2 2_566 3.590(3) yes Fe2 . O1 . 2.922(7) yes Si1 . O1 . 1.648(7) yes Si1 . N1 . 1.778(8) yes Si1 . C1 . 1.851(12) yes Si1 . C2 . 1.837(12) yes Si2 . O1 . 1.637(7) yes Si2 . N2 . 1.785(8) yes Si2 . C3 . 1.849(12) yes Si2 . C4 . 1.863(12) yes N1 . C11 . 1.515(13) yes N2 . C21 . 1.511(13) yes C1 . H11 . 0.980 no C1 . H12 . 0.971 no C1 . H13 . 0.966 no C2 . H21 . 0.995 no C2 . H22 . 0.966 no C2 . H23 . 0.957 no C3 . H31 . 0.962 no C3 . H32 . 0.976 no C3 . H33 . 0.971 no C4 . H41 . 0.954 no C4 . H42 . 0.981 no C4 . H43 . 0.957 no C11 . C111 . 1.514(15) yes C11 . C112 . 1.533(15) yes C11 . C113 . 1.556(15) yes C21 . C211 . 1.551(15) yes C21 . C212 . 1.529(15) yes C21 . C213 . 1.515(16) yes C111 . H1111 . 0.957 no C111 . H1112 . 0.957 no C111 . H1113 . 0.996 no C112 . H1121 . 0.956 no C112 . H1122 . 0.975 no C112 . H1123 . 0.964 no C113 . H1131 . 0.955 no C113 . H1132 . 0.972 no C113 . H1133 . 0.987 no C211 . H2111 . 0.972 no C211 . H2112 . 0.950 no C211 . H2113 . 0.979 no C212 . H2121 . 0.955 no C212 . H2122 . 0.979 no C212 . H2123 . 0.969 no C213 . H2131 . 0.972 no C213 . H2132 . 0.967 no C213 . H2133 . 0.962 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 2_565 Fe1 . Fe2 . 119.76(11) yes Cl1 2_565 Fe1 . Cl1 . 85.06(13) yes Fe2 . Fe1 . Cl1 . 154.76(11) yes Cl1 2_565 Fe1 . N1 . 122.1(2) yes Fe2 . Fe1 . N1 . 50.6(3) yes Cl1 . Fe1 . N1 . 122.2(3) yes Cl1 2_565 Fe1 . N2 . 115.9(2) yes Fe2 . Fe1 . N2 . 49.7(2) yes Cl1 . Fe1 . N2 . 117.7(3) yes N1 . Fe1 . N2 . 96.0(3) yes Cl1 2_565 Fe1 . Fe1 2_565 42.45(8) yes Fe2 . Fe1 . Fe1 2_565 161.82(10) yes Cl1 . Fe1 . Fe1 2_565 42.60(8) yes N1 . Fe1 . Fe1 2_565 136.2(3) yes N2 . Fe1 . Fe1 2_565 127.7(2) yes Cl1 2_565 Fe1 . O1 . 173.90(19) yes Fe2 . Fe1 . O1 . 64.95(18) yes Cl1 . Fe1 . O1 . 90.0(2) yes N1 . Fe1 . O1 . 63.6(3) yes N2 . Fe1 . O1 . 63.5(3) yes Fe1 2_565 Fe1 . O1 . 132.48(19) yes Cl2 2_566 Fe2 . Fe1 . 153.98(11) yes Cl2 2_566 Fe2 . Cl2 . 83.44(11) yes Fe1 . Fe2 . Cl2 . 122.30(10) yes Cl2 2_566 Fe2 . N1 . 118.3(3) yes Fe1 . Fe2 . N1 . 49.8(3) yes Cl2 . Fe2 . N1 . 116.7(2) yes Cl2 2_566 Fe2 . N2 . 120.5(3) yes Fe1 . Fe2 . N2 . 50.7(3) yes Cl2 . Fe2 . N2 . 123.9(2) yes N1 . Fe2 . N2 . 96.2(4) yes Cl2 2_566 Fe2 . Fe2 2_566 41.82(8) yes Fe1 . Fe2 . Fe2 2_566 163.65(10) yes Cl2 . Fe2 . Fe2 2_566 41.62(8) yes N1 . Fe2 . Fe2 2_566 128.3(3) yes N2 . Fe2 . Fe2 2_566 135.6(3) yes Cl2 2_566 Fe2 . O1 . 94.42(19) yes Fe1 . Fe2 . O1 . 59.62(18) yes Cl2 . Fe2 . O1 . 175.22(18) yes N1 . Fe2 . O1 . 60.6(3) yes N2 . Fe2 . O1 . 60.8(3) yes Fe2 2_566 Fe2 . O1 . 136.08(19) yes Fe1 2_565 Cl1 . Fe1 . 94.94(13) yes Fe2 . Cl2 . Fe2 2_566 96.56(12) yes O1 . Si1 . N1 . 100.0(4) yes O1 . Si1 . C1 . 108.9(5) yes N1 . Si1 . C1 . 116.7(5) yes O1 . Si1 . C2 . 107.0(5) yes N1 . Si1 . C2 . 116.4(5) yes C1 . Si1 . C2 . 107.0(5) yes O1 . Si2 . N2 . 100.3(4) yes O1 . Si2 . C3 . 108.4(5) yes N2 . Si2 . C3 . 116.7(5) yes O1 . Si2 . C4 . 107.6(5) yes N2 . Si2 . C4 . 115.3(5) yes C3 . Si2 . C4 . 107.9(5) yes Si1 . O1 . Si2 . 154.8(5) yes Si1 . O1 . Fe1 . 80.0(3) yes Si2 . O1 . Fe1 . 81.6(3) yes Si1 . O1 . Fe2 . 78.4(3) yes Si2 . O1 . Fe2 . 77.0(3) yes Fe1 . O1 . Fe2 . 55.43(14) yes Fe2 . N1 . Fe1 . 79.7(3) yes Fe2 . N1 . Si1 . 104.1(4) yes Fe1 . N1 . Si1 . 101.4(4) yes Fe2 . N1 . C11 . 118.3(7) yes Fe1 . N1 . C11 . 125.2(7) yes Si1 . N1 . C11 . 120.0(7) yes Fe1 . N2 . Fe2 . 79.6(3) yes Fe1 . N2 . Si2 . 101.8(4) yes Fe2 . N2 . Si2 . 102.9(4) yes Fe1 . N2 . C21 . 120.1(7) yes Fe2 . N2 . C21 . 124.2(7) yes Si2 . N2 . C21 . 119.9(6) yes Si1 . C1 . H11 . 110.9 no Si1 . C1 . H12 . 112.1 no H11 . C1 . H12 . 107.1 no Si1 . C1 . H13 . 111.0 no H11 . C1 . H13 . 107.2 no H12 . C1 . H13 . 108.3 no Si1 . C2 . H21 . 110.1 no Si1 . C2 . H22 . 111.0 no H21 . C2 . H22 . 106.7 no Si1 . C2 . H23 . 112.3 no H21 . C2 . H23 . 107.3 no H22 . C2 . H23 . 109.4 no Si2 . C3 . H31 . 111.4 no Si2 . C3 . H32 . 110.5 no H31 . C3 . H32 . 108.2 no Si2 . C3 . H33 . 110.4 no H31 . C3 . H33 . 108.6 no H32 . C3 . H33 . 107.6 no Si2 . C4 . H41 . 112.2 no Si2 . C4 . H42 . 110.7 no H41 . C4 . H42 . 106.6 no Si2 . C4 . H43 . 112.2 no H41 . C4 . H43 . 108.5 no H42 . C4 . H43 . 106.3 no N1 . C11 . C111 . 111.8(9) yes N1 . C11 . C112 . 110.4(9) yes C111 . C11 . C112 . 107.7(10) yes N1 . C11 . C113 . 110.4(9) yes C111 . C11 . C113 . 108.4(9) yes C112 . C11 . C113 . 108.0(9) yes N2 . C21 . C211 . 110.7(9) yes N2 . C21 . C212 . 109.4(9) yes C211 . C21 . C212 . 108.0(9) yes N2 . C21 . C213 . 111.5(9) yes C211 . C21 . C213 . 109.3(9) yes C212 . C21 . C213 . 107.8(9) yes C11 . C111 . H1111 . 111.2 no C11 . C111 . H1112 . 111.1 no H1111 . C111 . H1112 . 110.0 no C11 . C111 . H1113 . 109.3 no H1111 . C111 . H1113 . 107.5 no H1112 . C111 . H1113 . 107.5 no C11 . C112 . H1121 . 111.0 no C11 . C112 . H1122 . 111.0 no H1121 . C112 . H1122 . 108.2 no C11 . C112 . H1123 . 111.1 no H1121 . C112 . H1123 . 108.4 no H1122 . C112 . H1123 . 107.0 no C11 . C113 . H1131 . 110.6 no C11 . C113 . H1132 . 109.2 no H1131 . C113 . H1132 . 110.7 no C11 . C113 . H1133 . 109.0 no H1131 . C113 . H1133 . 109.4 no H1132 . C113 . H1133 . 107.9 no C21 . C211 . H2111 . 109.9 no C21 . C211 . H2112 . 111.6 no H2111 . C211 . H2112 . 108.9 no C21 . C211 . H2113 . 109.8 no H2111 . C211 . H2113 . 107.6 no H2112 . C211 . H2113 . 108.9 no C21 . C212 . H2121 . 111.1 no C21 . C212 . H2122 . 110.7 no H2121 . C212 . H2122 . 108.5 no C21 . C212 . H2123 . 110.4 no H2121 . C212 . H2123 . 108.9 no H2122 . C212 . H2123 . 107.1 no C21 . C213 . H2131 . 110.9 no C21 . C213 . H2132 . 110.7 no H2131 . C213 . H2132 . 107.6 no C21 . C213 . H2133 . 111.4 no H2131 . C213 . H2133 . 107.7 no H2132 . C213 . H2133 . 108.4 no #=============================================================================== data_{[(tBut)2NON]Co2Cl3LiTHF2}2 _database_code_depnum_ccdc_archive 'CCDC 778592' #TrackingRef '- dleznoff NONM2X2.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C40 H92 Cl6 Co4 Li2 N4 O6 Si4' _chemical_formula_moiety 'C40 H92 Cl6 Co4 Li2 N4 O6 Si4' _chemical_formula_weight 1299.86 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------ _cell_length_a 11.0506(19) _cell_length_b 12.391(2) _cell_length_c 13.330(2) _cell_angle_alpha 89.942(2) _cell_angle_beta 88.776(2) _cell_angle_gamma 64.740(2) _cell_volume 1650.3(5) _cell_formula_units_Z 1 _cell_measurement_reflns_used 7857 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.70 _cell_measurement_temperature 293 _exptl_crystal_description needle _exptl_crystal_colour 'blue green' _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_max 0.50 _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_meas ? # non-dispersive F(000): _exptl_crystal_F_000 680.760 _exptl_absorpt_coefficient_mu 1.342 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6331 _exptl_absorpt_correction_T_max 0.7457 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.70930 _diffrn_measurement_device_type 'Bruker Smart APEX II' _diffrn_detector_type 'APEX II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w and \f scans' _diffrn_ambient_temperature 293 _diffrn_reflns_number 19235 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_theta_min 1.817 _diffrn_reflns_theta_max 28.456 _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 25.895 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 #========================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _reflns_number_total 7580 # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 3637 _refine_ls_number_restraints 99 _refine_ls_number_parameters 299 _oxford_refine_ls_R_factor_ref 0.0503 _refine_ls_wR_factor_ref 0.0587 _refine_ls_goodness_of_fit_ref 2.6647 _refine_ls_shift/su_max 0.0016052 _refine_ls_shift/su_mean 0.3808625 _refine_diff_density_min -0.54 _refine_diff_density_max 0.51 # The values computed from all data _oxford_reflns_number_all 7580 _refine_ls_R_factor_all 0.0947 _refine_ls_wR_factor_all 0.0850 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4148 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_gt 0.0596 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F) + ( 0.01P)^2^] ,where P=(max(Fo,0) + 2Fc)/3 ; _refine_special_details ; One of the tButyl units was found to be rotationally disordered. Both THF moieties were found to be significantly disordered. Adequate geometric and thermal similarity restraints were used in order to achieve an unbiased, and chemically reasonable model. Note that the THF atoms are refined isotropically. The large degree of disorder in such a small space do not allow for reasonable anisotropic displacement parameters to be obtained. ; _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min -16 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _oxford_refine_ls_scale 0.1263(2) _oxford_diffrn_Wilson_B_factor 4.28 _oxford_diffrn_Wilson_scale 46.18 # Number of reflections without Friedels Law is 7580 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 8179 #--------------------------------------------------------- _chemical_name_systematic ; ; # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type Full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment constr # none if no extinction, _refine_ls_extinction_method none #========================================================== # 9. General computing _computing_data_collection ' Bruker SMART APEX II' _computing_data_reduction ' Bruker SMART APEX II' _computing_cell_refinement ' Bruker SMART APEX II' _computing_structure_solution ' SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Li -0.0003 0.0001 1.1282 3.9546 0.7508 1.0524 0.6175 85.3905 0.4653 168.2610 0.0377 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Si 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' #============================================================================== # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Co1 Co 0.59814(8) 0.38873(7) 0.41937(6) 0.0504 1.0000 Uani . . . . . . . Co2 Co 0.71131(9) 0.28108(8) 0.24761(7) 0.0650 1.0000 Uani . . . . . . . Cl1 Cl 0.43991(16) 0.59164(13) 0.40862(12) 0.0643 1.0000 Uani . . . . . . . Cl2 Cl 0.8541(2) 0.12033(18) 0.15347(15) 0.0990 1.0000 Uani . . . . . . . Cl3 Cl 0.6280(3) 0.41007(18) 0.11479(15) 0.1144 1.0000 Uani . . . . . . . Si1 Si 0.65474(18) 0.13107(16) 0.40803(16) 0.0672 1.0000 Uani . . . . . . . Si2 Si 0.88635(17) 0.21493(16) 0.43123(14) 0.0611 1.0000 Uani . . . . . . . N1 N 0.5682(5) 0.2613(4) 0.3397(4) 0.0602 1.0000 Uani . . . . . . . N2 N 0.7878(4) 0.3424(4) 0.3634(3) 0.0522 1.0000 Uani D . . . . . . O1 O 0.7920(4) 0.1441(4) 0.4347(3) 0.0745 1.0000 Uani . . . . . . . O3 O 0.9098(8) 0.2765(9) -0.0511(7) 0.185(3) 1.0000 Uiso D . . . . . . O41 O 0.6745(15) 0.1895(14) -0.0695(11) 0.130(2) 0.476(10) Uiso D . P . 1 . . O42 O 0.7070(14) 0.1999(13) -0.0945(10) 0.130(2) 0.524(10) Uiso D . P . 2 . . C1 C 0.5769(7) 0.1200(6) 0.5307(5) 0.0937 1.0000 Uani . . . . . . . C2 C 0.7033(7) -0.0125(5) 0.3412(6) 0.0960 1.0000 Uani . . . . . . . C3 C 1.0494(6) 0.1138(6) 0.3730(6) 0.0885 1.0000 Uani . . . . . . . C4 C 0.9178(7) 0.2392(6) 0.5636(5) 0.0903 1.0000 Uani . . . . . . . C11 C 0.4377(7) 0.2801(7) 0.2920(7) 0.0913 1.0000 Uani . . . . . . . C21 C 0.8409(6) 0.4340(5) 0.3413(5) 0.0792 1.0000 Uani D U . . . . . C31 C 0.934(2) 0.279(3) -0.1563(10) 0.235(3) 0.499(8) Uiso D . P . 1 . . C32 C 1.050(2) 0.298(3) -0.1682(16) 0.235(3) 0.499(8) Uiso D . P . 1 . . C33 C 1.1213(16) 0.265(3) -0.071(2) 0.235(3) 0.499(8) Uiso D . P . 1 . . C34 C 1.0386(18) 0.234(3) -0.0064(16) 0.235(3) 0.499(8) Uiso D . P . 1 . . C35 C 1.0309(19) 0.1850(16) -0.089(3) 0.235(3) 0.501(8) Uiso D . P . 2 . . C36 C 1.1246(15) 0.235(2) -0.103(2) 0.235(3) 0.501(8) Uiso D . P . 2 . . C37 C 1.060(2) 0.356(2) -0.055(2) 0.235(3) 0.501(8) Uiso D . P . 2 . . C38 C 0.921(2) 0.3869(12) -0.064(2) 0.235(3) 0.501(8) Uiso D . P . 2 . . C41 C 0.5390(17) 0.2502(13) -0.0967(17) 0.130(2) 0.476(10) Uiso D . P . 1 . . C42 C 0.4923(14) 0.1653(17) -0.1226(17) 0.130(2) 0.476(10) Uiso D . P . 1 . . C43 C 0.6044(19) 0.0506(13) -0.1202(17) 0.130(2) 0.476(10) Uiso D . P . 1 . . C44 C 0.7123(17) 0.0657(14) -0.0796(17) 0.130(2) 0.476(10) Uiso D . P . 1 . . C45 C 0.5887(18) 0.2631(12) -0.1464(14) 0.130(2) 0.524(10) Uiso D . P . 2 . . C46 C 0.5381(15) 0.1819(15) -0.1797(14) 0.130(2) 0.524(10) Uiso D . P . 2 . . C47 C 0.6542(18) 0.0662(12) -0.1804(15) 0.130(2) 0.524(10) Uiso D . P . 2 . . C48 C 0.7606(14) 0.0876(14) -0.1423(15) 0.130(2) 0.524(10) Uiso D . P . 2 . . C111 C 0.3553(7) 0.4089(7) 0.2676(7) 0.1341 1.0000 Uani . . . . . . . C112 C 0.4653(9) 0.2088(8) 0.1936(8) 0.1535 1.0000 Uani . . . . . . . C113 C 0.3557(8) 0.2336(8) 0.3573(9) 0.1573 1.0000 Uani . . . . . . . C211 C 0.7380(9) 0.5523(6) 0.3085(8) 0.0700 0.642(9) Uani D U P . 1 . . C212 C 0.9412(9) 0.3803(8) 0.2444(7) 0.0884 0.642(9) Uani D U P . 1 . . C213 C 0.9296(11) 0.4447(10) 0.4210(7) 0.0913 0.642(9) Uani D U P . 1 . . C214 C 0.9860(9) 0.3914(13) 0.3195(15) 0.0890 0.358(9) Uani D U P . 2 . . C215 C 0.8119(18) 0.5139(13) 0.4434(9) 0.0784 0.358(9) Uani D U P . 2 . . C216 C 0.7562(16) 0.5271(12) 0.2651(11) 0.0799 0.358(9) Uani D U P . 2 . . Li1 Li 0.7692(15) 0.2498(15) 0.0162(9) 0.1187 1.0000 Uani D . . . . . . H11 H 0.5504 0.1934 0.5675 0.105(5) 1.0000 Uiso R . . . . . . H12 H 0.6413 0.0557 0.5681 0.105(5) 1.0000 Uiso R . . . . . . H13 H 0.4998 0.1049 0.5200 0.105(5) 1.0000 Uiso R . . . . . . H21 H 0.7427 -0.0086 0.2772 0.109(5) 1.0000 Uiso R . . . . . . H22 H 0.7671 -0.0761 0.3796 0.109(5) 1.0000 Uiso R . . . . . . H23 H 0.6256 -0.0269 0.3315 0.109(5) 1.0000 Uiso R . . . . . . H31 H 1.1107 0.1495 0.3769 0.128(5) 1.0000 Uiso R . . . . . . H32 H 1.0359 0.1000 0.3041 0.128(5) 1.0000 Uiso R . . . . . . H33 H 1.0837 0.0396 0.4085 0.128(5) 1.0000 Uiso R . . . . . . H41 H 0.9428 0.1654 0.5989 0.131(5) 1.0000 Uiso R . . . . . . H42 H 0.8375 0.2987 0.5938 0.131(5) 1.0000 Uiso R . . . . . . H43 H 0.9884 0.2645 0.5658 0.131(5) 1.0000 Uiso R . . . . . . H311 H 0.8862 0.3640 -0.1500 0.55(4) 0.499(8) Uiso R . P . 1 . . H312 H 0.8927 0.2502 -0.2057 0.55(4) 0.499(8) Uiso R . P . 1 . . H321 H 1.0608 0.3653 -0.1960 0.55(4) 0.499(8) Uiso R . P . 1 . . H322 H 1.0810 0.2340 -0.2164 0.55(4) 0.499(8) Uiso R . P . 1 . . H331 H 1.1289 0.3314 -0.0396 0.55(4) 0.499(8) Uiso R . P . 1 . . H332 H 1.2090 0.2036 -0.0861 0.55(4) 0.499(8) Uiso R . P . 1 . . H341 H 1.0433 0.2528 0.0627 0.55(4) 0.499(8) Uiso R . P . 1 . . H342 H 1.0716 0.1486 -0.0141 0.55(4) 0.499(8) Uiso R . P . 1 . . H351 H 0.9977 0.2148 -0.1539 0.55(4) 0.501(8) Uiso R . P . 2 . . H352 H 1.0504 0.1018 -0.0854 0.55(4) 0.501(8) Uiso R . P . 2 . . H361 H 1.1685 0.2405 -0.1639 0.55(4) 0.501(8) Uiso R . P . 2 . . H362 H 1.1859 0.1705 -0.0632 0.55(4) 0.501(8) Uiso R . P . 2 . . H371 H 1.0872 0.4113 -0.0872 0.55(4) 0.501(8) Uiso R . P . 2 . . H372 H 1.0926 0.3425 0.0126 0.55(4) 0.501(8) Uiso R . P . 2 . . H381 H 0.8843 0.4337 -0.1228 0.55(4) 0.501(8) Uiso R . P . 2 . . H382 H 0.8812 0.4339 -0.0052 0.55(4) 0.501(8) Uiso R . P . 2 . . H411 H 0.5388 0.2967 -0.1544 0.44(4) 0.476(10) Uiso R . P . 1 . . H412 H 0.4814 0.3017 -0.0451 0.44(4) 0.476(10) Uiso R . P . 1 . . H421 H 0.4522 0.1816 -0.1874 0.44(4) 0.476(10) Uiso R . P . 1 . . H422 H 0.4284 0.1636 -0.0735 0.44(4) 0.476(10) Uiso R . P . 1 . . H431 H 0.6325 0.0270 -0.1885 0.44(4) 0.476(10) Uiso R . P . 1 . . H432 H 0.5836 -0.0089 -0.0880 0.44(4) 0.476(10) Uiso R . P . 1 . . H441 H 0.7944 0.0325 -0.1184 0.44(4) 0.476(10) Uiso R . P . 1 . . H442 H 0.7256 0.0272 -0.0156 0.44(4) 0.476(10) Uiso R . P . 1 . . H451 H 0.6087 0.3017 -0.2026 0.44(4) 0.524(10) Uiso R . P . 2 . . H452 H 0.5240 0.3221 -0.1027 0.44(4) 0.524(10) Uiso R . P . 2 . . H461 H 0.5009 0.2029 -0.2452 0.44(4) 0.524(10) Uiso R . P . 2 . . H462 H 0.4709 0.1805 -0.1335 0.44(4) 0.524(10) Uiso R . P . 2 . . H471 H 0.6748 0.0380 -0.2484 0.44(4) 0.524(10) Uiso R . P . 2 . . H472 H 0.6358 0.0097 -0.1411 0.44(4) 0.524(10) Uiso R . P . 2 . . H481 H 0.8220 0.0863 -0.1949 0.44(4) 0.524(10) Uiso R . P . 2 . . H482 H 0.8066 0.0259 -0.0950 0.44(4) 0.524(10) Uiso R . P . 2 . . H1111 H 0.3331 0.4558 0.3283 0.144(5) 1.0000 Uiso R . . . . . . H1112 H 0.4068 0.4353 0.2234 0.144(5) 1.0000 Uiso R . . . . . . H1113 H 0.2746 0.4183 0.2355 0.144(5) 1.0000 Uiso R . . . . . . H1121 H 0.5159 0.2368 0.1500 0.164(5) 1.0000 Uiso R . . . . . . H1122 H 0.5169 0.1255 0.2067 0.164(5) 1.0000 Uiso R . . . . . . H1123 H 0.3836 0.2199 0.1620 0.164(5) 1.0000 Uiso R . . . . . . H1131 H 0.3344 0.2768 0.4198 0.173(5) 1.0000 Uiso R . . . . . . H1132 H 0.4078 0.1503 0.3697 0.173(5) 1.0000 Uiso R . . . . . . H1133 H 0.2745 0.2446 0.3250 0.173(5) 1.0000 Uiso R . . . . . . H2111 H 0.6866 0.5403 0.2561 0.086(5) 0.642(9) Uiso R . P . 1 . . H2112 H 0.7799 0.6013 0.2843 0.086(5) 0.642(9) Uiso R . P . 1 . . H2113 H 0.6800 0.5910 0.3648 0.086(5) 0.642(9) Uiso R . P . 1 . . H2121 H 0.8924 0.3714 0.1887 0.105(5) 0.642(9) Uiso R . P . 1 . . H2122 H 0.9798 0.4342 0.2268 0.105(5) 0.642(9) Uiso R . P . 1 . . H2123 H 1.0110 0.3040 0.2608 0.105(5) 0.642(9) Uiso R . P . 1 . . H2131 H 0.8755 0.4758 0.4806 0.105(5) 0.642(9) Uiso R . P . 1 . . H2132 H 0.9683 0.4975 0.4004 0.105(5) 0.642(9) Uiso R . P . 1 . . H2133 H 0.9995 0.3673 0.4345 0.105(5) 0.642(9) Uiso R . P . 1 . . H2141 H 1.0358 0.3907 0.3778 0.105(5) 0.358(9) Uiso R . P . 2 . . H2142 H 1.0002 0.4402 0.2688 0.105(5) 0.358(9) Uiso R . P . 2 . . H2143 H 1.0154 0.3115 0.2942 0.105(5) 0.358(9) Uiso R . P . 2 . . H2151 H 0.8629 0.4629 0.4960 0.090(5) 0.358(9) Uiso R . P . 2 . . H2152 H 0.8406 0.5761 0.4325 0.090(5) 0.358(9) Uiso R . P . 2 . . H2153 H 0.7186 0.5486 0.4622 0.090(5) 0.358(9) Uiso R . P . 2 . . H2161 H 0.7643 0.4879 0.2015 0.092(5) 0.358(9) Uiso R . P . 2 . . H2162 H 0.7862 0.5889 0.2579 0.092(5) 0.358(9) Uiso R . P . 2 . . H2163 H 0.6642 0.5614 0.2876 0.092(5) 0.358(9) Uiso R . P . 2 . . 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 0.0403(5) 0.0468(5) 0.0641(6) -0.0025(4) -0.0018(4) -0.0184(4) Co2 0.0632(6) 0.0631(6) 0.0620(6) -0.0059(5) -0.0063(5) -0.0203(5) Cl1 0.0630(10) 0.0519(10) 0.0654(11) 0.0037(8) 0.0012(8) -0.0126(8) Cl2 0.1081(16) 0.0821(14) 0.0805(14) -0.0175(11) 0.0086(12) -0.0157(12) Cl3 0.154(2) 0.0857(15) 0.0755(14) 0.0067(11) -0.0310(14) -0.0231(15) Si1 0.0542(12) 0.0515(11) 0.0971(16) -0.0013(10) -0.0019(10) -0.0238(10) Si2 0.0412(10) 0.0633(12) 0.0744(13) 0.0056(10) -0.0082(9) -0.0179(9) N1 0.043(3) 0.055(3) 0.083(4) -0.013(3) -0.008(3) -0.022(3) N2 0.042(3) 0.056(3) 0.061(3) 0.000(3) -0.001(2) -0.023(3) O1 0.053(3) 0.072(3) 0.103(4) 0.028(3) -0.020(2) -0.030(2) C1 0.087(6) 0.073(5) 0.128(7) 0.007(5) 0.020(5) -0.042(5) C2 0.091(6) 0.054(5) 0.134(7) -0.007(5) -0.003(5) -0.023(4) C3 0.052(4) 0.076(5) 0.121(7) 0.009(5) -0.003(4) -0.012(4) C4 0.076(5) 0.095(6) 0.086(6) 0.012(4) -0.027(4) -0.021(5) C11 0.063(5) 0.081(6) 0.133(7) -0.006(5) -0.035(5) -0.033(5) C21 0.068(4) 0.085(4) 0.098(5) 0.012(4) -0.002(3) -0.046(3) C111 0.071(6) 0.090(6) 0.228(11) -0.002(7) -0.083(7) -0.018(5) C112 0.143(9) 0.108(7) 0.203(11) -0.027(8) -0.100(8) -0.043(7) C113 0.061(6) 0.150(9) 0.278(15) 0.038(9) -0.036(7) -0.059(6) C211 0.071(6) 0.060(6) 0.085(7) -0.001(5) 0.008(6) -0.034(5) C212 0.071(6) 0.094(7) 0.105(8) 0.026(6) 0.001(6) -0.040(6) C213 0.075(7) 0.102(7) 0.120(8) 0.004(6) -0.014(6) -0.060(6) C214 0.070(8) 0.094(9) 0.116(10) 0.016(9) -0.002(8) -0.047(8) C215 0.065(8) 0.082(9) 0.111(9) 0.012(7) -0.009(8) -0.053(7) C216 0.075(9) 0.072(9) 0.098(10) 0.004(8) 0.002(8) -0.036(8) Li1 0.133(13) 0.154(14) 0.095(11) -0.021(10) -0.010(9) -0.085(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 . Cl1 2_666 2.3164(18) yes Co1 . Co1 2_666 3.4114(16) yes Co1 . Co2 . 2.6543(12) yes Co1 . Cl1 . 2.3785(17) yes Co1 . N1 . 2.048(5) yes Co1 . N2 . 2.046(4) yes Co1 . O1 . 2.881(4) yes Co2 . Cl2 . 2.296(2) yes Co2 . Cl3 . 2.312(2) yes Co2 . N1 . 2.078(5) yes Co2 . N2 . 2.069(4) yes Co2 . O1 . 2.948(4) yes Cl2 . Li1 . 2.363(16) yes Cl3 . Li1 . 2.319(16) yes Si1 . N1 . 1.750(5) yes Si1 . O1 . 1.638(4) yes Si1 . C1 . 1.863(7) yes Si1 . C2 . 1.847(6) yes Si2 . N2 . 1.752(5) yes Si2 . O1 . 1.625(4) yes Si2 . C3 . 1.853(6) yes Si2 . C4 . 1.855(7) yes N1 . C11 . 1.513(8) yes N2 . C21 . 1.510(7) yes O3 . C31 . 1.425(10) yes O3 . C34 . 1.433(10) yes O3 . Li1 . 1.925(13) yes O41 . C41 . 1.415(9) yes O41 . C44 . 1.413(9) yes O41 . Li1 . 1.918(14) yes O42 . C45 . 1.401(9) yes O42 . C48 . 1.405(9) yes O42 . Li1 . 1.857(13) yes C1 . H11 . 0.960 no C1 . H12 . 0.960 no C1 . H13 . 0.960 no C2 . H21 . 0.960 no C2 . H22 . 0.960 no C2 . H23 . 0.960 no C3 . H31 . 0.956 no C3 . H32 . 0.962 no C3 . H33 . 0.960 no C4 . H41 . 0.960 no C4 . H42 . 0.960 no C4 . H43 . 0.958 no C11 . C111 . 1.501(9) yes C11 . C112 . 1.534(11) yes C11 . C113 . 1.523(11) yes C21 . C211 . 1.493(7) yes C21 . C212 . 1.628(7) yes C21 . C213 . 1.504(7) yes C31 . C32 . 1.408(9) yes C31 . H311 . 0.960 no C31 . H312 . 0.960 no C32 . C33 . 1.487(10) yes C32 . H321 . 0.960 no C32 . H322 . 0.960 no C33 . C34 . 1.419(9) yes C33 . H331 . 0.960 no C33 . H332 . 0.960 no C34 . H341 . 0.960 no C34 . H342 . 0.960 no C35 . C36 . 1.423(9) yes C35 . H351 . 0.960 no C35 . H352 . 0.960 no C36 . C37 . 1.494(10) yes C36 . H361 . 0.960 no C36 . H362 . 0.960 no C37 . C38 . 1.423(10) yes C37 . H371 . 0.960 no C37 . H372 . 0.960 no C38 . H381 . 0.960 no C38 . H382 . 0.960 no C41 . C42 . 1.401(9) yes C41 . H411 . 0.960 no C41 . H412 . 0.960 no C42 . C43 . 1.433(9) yes C42 . H421 . 0.960 no C42 . H422 . 0.960 no C43 . C44 . 1.402(9) yes C43 . H431 . 0.960 no C43 . H432 . 0.960 no C44 . H441 . 0.960 no C44 . H442 . 0.960 no C45 . C46 . 1.419(9) yes C45 . H451 . 0.960 no C45 . H452 . 0.960 no C46 . C47 . 1.460(9) yes C46 . H461 . 0.960 no C46 . H462 . 0.960 no C47 . C48 . 1.415(9) yes C47 . H471 . 0.960 no C47 . H472 . 0.960 no C48 . H481 . 0.960 no C48 . H482 . 0.960 no C111 . H1111 . 0.960 no C111 . H1112 . 0.960 no C111 . H1113 . 0.960 no C112 . H1121 . 0.960 no C112 . H1122 . 0.960 no C112 . H1123 . 0.960 no C113 . H1131 . 0.960 no C113 . H1132 . 0.960 no C113 . H1133 . 0.960 no C211 . H2111 . 0.960 no C211 . H2112 . 0.960 no C211 . H2113 . 0.960 no C212 . H2121 . 0.960 no C212 . H2122 . 0.960 no C212 . H2123 . 0.960 no C213 . H2131 . 0.960 no C213 . H2132 . 0.960 no C213 . H2133 . 0.960 no C214 . H2141 . 0.960 no C214 . H2142 . 0.960 no C214 . H2143 . 0.960 no C215 . H2151 . 0.960 no C215 . H2152 . 0.960 no C215 . H2153 . 0.960 no C216 . H2161 . 0.960 no C216 . H2162 . 0.960 no C216 . H2163 . 0.960 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 2_666 Co1 . Co1 2_666 44.12(4) yes Cl1 2_666 Co1 . Co2 . 156.83(5) yes Co1 2_666 Co1 . Co2 . 158.97(5) yes Cl1 2_666 Co1 . Cl1 . 86.80(6) yes Co1 2_666 Co1 . Cl1 . 42.69(4) yes Co2 . Co1 . Cl1 . 116.32(5) yes Cl1 2_666 Co1 . N1 . 120.95(15) yes Co1 2_666 Co1 . N1 . 133.60(14) yes Co2 . Co1 . N1 . 50.46(14) yes Cl1 . Co1 . N1 . 119.22(14) yes Cl1 2_666 Co1 . N2 . 119.07(13) yes Co1 2_666 Co1 . N2 . 131.30(12) yes Co2 . Co1 . N2 . 50.22(12) yes Cl1 . Co1 . N2 . 118.26(13) yes N1 . Co1 . N2 . 95.03(18) yes Cl1 2_666 Co1 . O1 . 92.65(10) yes Co1 2_666 Co1 . O1 . 136.77(10) yes Co2 . Co1 . O1 . 64.20(9) yes Cl1 . Co1 . O1 . 179.11(10) yes N1 . Co1 . O1 . 61.67(16) yes N2 . Co1 . O1 . 61.42(14) yes Co1 . Co2 . Cl2 . 153.18(7) yes Co1 . Co2 . Cl3 . 110.44(7) yes Cl2 . Co2 . Cl3 . 96.38(8) yes Co1 . Co2 . N1 . 49.47(13) yes Cl2 . Co2 . N1 . 118.64(14) yes Cl3 . Co2 . N1 . 115.31(15) yes Co1 . Co2 . N2 . 49.47(12) yes Cl2 . Co2 . N2 . 118.94(13) yes Cl3 . Co2 . N2 . 115.77(13) yes N1 . Co2 . N2 . 93.46(17) yes Co1 . Co2 . O1 . 61.63(9) yes Cl2 . Co2 . O1 . 91.55(11) yes Cl3 . Co2 . O1 . 172.07(11) yes N1 . Co2 . O1 . 60.06(15) yes N2 . Co2 . O1 . 59.86(14) yes Co1 . Cl1 . Co1 2_666 93.20(6) yes Co2 . Cl2 . Li1 . 84.3(4) yes Co2 . Cl3 . Li1 . 84.9(4) yes N1 . Si1 . O1 . 101.5(2) yes N1 . Si1 . C1 . 116.1(3) yes O1 . Si1 . C1 . 106.1(3) yes N1 . Si1 . C2 . 117.0(3) yes O1 . Si1 . C2 . 107.9(3) yes C1 . Si1 . C2 . 107.2(3) yes N2 . Si2 . O1 . 101.5(2) yes N2 . Si2 . C3 . 116.7(3) yes O1 . Si2 . C3 . 107.6(3) yes N2 . Si2 . C4 . 116.5(3) yes O1 . Si2 . C4 . 106.4(3) yes C3 . Si2 . C4 . 107.2(3) yes Co2 . N1 . Co1 . 80.07(17) yes Co2 . N1 . Si1 . 105.7(2) yes Co1 . N1 . Si1 . 103.2(2) yes Co2 . N1 . C11 . 116.8(5) yes Co1 . N1 . C11 . 124.6(4) yes Si1 . N1 . C11 . 119.1(4) yes Co2 . N2 . Co1 . 80.32(15) yes Co2 . N2 . Si2 . 105.2(2) yes Co1 . N2 . Si2 . 103.9(2) yes Co2 . N2 . C21 . 119.1(3) yes Co1 . N2 . C21 . 122.2(3) yes Si2 . N2 . C21 . 119.0(3) yes Si1 . O1 . Si2 . 152.1(3) yes Si1 . O1 . Co1 . 77.26(16) yes Si2 . O1 . Co1 . 77.89(16) yes Si1 . O1 . Co2 . 77.88(16) yes Si2 . O1 . Co2 . 77.47(16) yes Co1 . O1 . Co2 . 54.17(7) yes C31 . O3 . C34 . 105.6(11) yes C31 . O3 . Li1 . 128.1(11) yes C34 . O3 . Li1 . 119.1(11) yes C41 . O41 . C44 . 107.9(7) yes C41 . O41 . Li1 . 126.3(13) yes C44 . O41 . Li1 . 121.3(13) yes C45 . O42 . C48 . 102.9(9) yes C45 . O42 . Li1 . 128.0(13) yes C48 . O42 . Li1 . 128.9(13) yes Si1 . C1 . H11 . 109.4 no Si1 . C1 . H12 . 108.8 no H11 . C1 . H12 . 109.5 no Si1 . C1 . H13 . 110.2 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no Si1 . C2 . H21 . 108.9 no Si1 . C2 . H22 . 109.8 no H21 . C2 . H22 . 109.5 no Si1 . C2 . H23 . 109.8 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 109.5 no Si2 . C3 . H31 . 109.6 no Si2 . C3 . H32 . 108.8 no H31 . C3 . H32 . 110.1 no Si2 . C3 . H33 . 108.7 no H31 . C3 . H33 . 110.0 no H32 . C3 . H33 . 109.6 no Si2 . C4 . H41 . 108.4 no Si2 . C4 . H42 . 109.4 no H41 . C4 . H42 . 109.3 no Si2 . C4 . H43 . 109.5 no H41 . C4 . H43 . 110.1 no H42 . C4 . H43 . 110.1 no N1 . C11 . C111 . 111.7(6) yes N1 . C11 . C112 . 110.1(6) yes C111 . C11 . C112 . 107.4(7) yes N1 . C11 . C113 . 112.1(7) yes C111 . C11 . C113 . 110.0(7) yes C112 . C11 . C113 . 105.2(7) yes N2 . C21 . C211 . 114.7(5) yes N2 . C21 . C212 . 104.7(5) yes C211 . C21 . C212 . 105.2(5) yes N2 . C21 . C213 . 114.1(5) yes C211 . C21 . C213 . 112.8(6) yes C212 . C21 . C213 . 104.0(5) yes O3 . C31 . C32 . 106.8(9) yes O3 . C31 . H311 . 85.8 no C32 . C31 . H311 . 86.4 no O3 . C31 . H312 . 123.4 no C32 . C31 . H312 . 127.7 no H311 . C31 . H312 . 109.5 no C31 . C32 . C33 . 106.5(9) yes C31 . C32 . H321 . 129.7 no C33 . C32 . H321 . 109.2 no C31 . C32 . H322 . 86.9 no C33 . C32 . H322 . 113.3 no H321 . C32 . H322 . 109.5 no C32 . C33 . C34 . 105.9(8) yes C32 . C33 . H331 . 112.6 no C34 . C33 . H331 . 105.8 no C32 . C33 . H332 . 107.1 no C34 . C33 . H332 . 116.1 no H331 . C33 . H332 . 109.5 no O3 . C34 . C33 . 106.9(9) yes O3 . C34 . H341 . 118.6 no C33 . C34 . H341 . 113.3 no O3 . C34 . H342 . 102.5 no C33 . C34 . H342 . 104.8 no H341 . C34 . H342 . 109.5 no O3 . C35 . C36 . 107.7(8) yes O3 . C35 . H351 . 85.6 no C36 . C35 . H351 . 87.7 no O3 . C35 . H352 . 123.0 no C36 . C35 . H352 . 126.8 no H351 . C35 . H352 . 109.5 no C35 . C36 . C37 . 105.3(8) yes C35 . C36 . H361 . 127.7 no C37 . C36 . H361 . 108.5 no C35 . C36 . H362 . 87.9 no C37 . C36 . H362 . 117.6 no H361 . C36 . H362 . 109.5 no C36 . C37 . C38 . 102.8(11) yes C36 . C37 . H371 . 111.8 no C38 . C37 . H371 . 112.7 no C36 . C37 . H372 . 103.8 no C38 . C37 . H372 . 115.7 no H371 . C37 . H372 . 109.5 no O3 . C38 . C37 . 104.5(9) yes O3 . C38 . H381 . 119.0 no C37 . C38 . H381 . 112.8 no O3 . C38 . H382 . 106.0 no C37 . C38 . H382 . 103.7 no H381 . C38 . H382 . 109.5 no O41 . C41 . C42 . 108.5(8) yes O41 . C41 . H411 . 105.8 no C42 . C41 . H411 . 109.9 no O41 . C41 . H412 . 114.1 no C42 . C41 . H412 . 109.0 no H411 . C41 . H412 . 109.5 no C41 . C42 . C43 . 107.2(7) yes C41 . C42 . H421 . 111.0 no C43 . C42 . H421 . 111.7 no C41 . C42 . H422 . 110.9 no C43 . C42 . H422 . 106.4 no H421 . C42 . H422 . 109.5 no C42 . C43 . C44 . 107.9(7) yes C42 . C43 . H431 . 107.1 no C44 . C43 . H431 . 103.9 no C42 . C43 . H432 . 113.0 no C44 . C43 . H432 . 114.8 no H431 . C43 . H432 . 109.5 no O41 . C44 . C43 . 107.9(8) yes O41 . C44 . H441 . 107.4 no C43 . C44 . H441 . 115.8 no O41 . C44 . H442 . 111.8 no C43 . C44 . H442 . 104.7 no H441 . C44 . H442 . 109.5 no O42 . C45 . C46 . 108.9(8) yes O42 . C45 . H451 . 108.6 no C46 . C45 . H451 . 110.3 no O42 . C45 . H452 . 109.7 no C46 . C45 . H452 . 109.9 no H451 . C45 . H452 . 109.5 no C45 . C46 . C47 . 104.2(8) yes C45 . C46 . H461 . 110.9 no C47 . C46 . H461 . 111.8 no C45 . C46 . H462 . 110.7 no C47 . C46 . H462 . 109.7 no H461 . C46 . H462 . 109.5 no C46 . C47 . C48 . 105.8(7) yes C46 . C47 . H471 . 108.7 no C48 . C47 . H471 . 109.6 no C46 . C47 . H472 . 110.6 no C48 . C47 . H472 . 112.6 no H471 . C47 . H472 . 109.5 no C47 . C48 . O42 . 108.7(8) yes C47 . C48 . H481 . 111.5 no O42 . C48 . H481 . 109.4 no C47 . C48 . H482 . 107.6 no O42 . C48 . H482 . 110.3 no H481 . C48 . H482 . 109.5 no C11 . C111 . H1111 . 109.5 no C11 . C111 . H1112 . 108.7 no H1111 . C111 . H1112 . 109.5 no C11 . C111 . H1113 . 110.2 no H1111 . C111 . H1113 . 109.5 no H1112 . C111 . H1113 . 109.5 no C11 . C112 . H1121 . 107.5 no C11 . C112 . H1122 . 109.6 no H1121 . C112 . H1122 . 109.5 no C11 . C112 . H1123 . 111.3 no H1121 . C112 . H1123 . 109.5 no H1122 . C112 . H1123 . 109.5 no C11 . C113 . H1131 . 108.4 no C11 . C113 . H1132 . 109.2 no H1131 . C113 . H1132 . 109.5 no C11 . C113 . H1133 . 110.8 no H1131 . C113 . H1133 . 109.5 no H1132 . C113 . H1133 . 109.5 no C21 . C211 . H2111 . 109.2 no C21 . C211 . H2112 . 110.4 no H2111 . C211 . H2112 . 109.5 no C21 . C211 . H2113 . 108.7 no H2111 . C211 . H2113 . 109.5 no H2112 . C211 . H2113 . 109.5 no C21 . C212 . H2121 . 110.0 no C21 . C212 . H2122 . 109.0 no H2121 . C212 . H2122 . 109.5 no C21 . C212 . H2123 . 109.4 no H2121 . C212 . H2123 . 109.5 no H2122 . C212 . H2123 . 109.5 no C21 . C213 . H2131 . 107.8 no C21 . C213 . H2132 . 111.0 no H2131 . C213 . H2132 . 109.5 no C21 . C213 . H2133 . 109.6 no H2131 . C213 . H2133 . 109.5 no H2132 . C213 . H2133 . 109.5 no C21 . C214 . H2141 . 113.0 no C21 . C214 . H2142 . 109.9 no H2141 . C214 . H2142 . 109.5 no C21 . C214 . H2143 . 105.5 no H2141 . C214 . H2143 . 109.5 no H2142 . C214 . H2143 . 109.5 no C21 . C215 . H2151 . 108.0 no C21 . C215 . H2152 . 108.8 no H2151 . C215 . H2152 . 109.5 no C21 . C215 . H2153 . 111.5 no H2151 . C215 . H2153 . 109.5 no H2152 . C215 . H2153 . 109.5 no C21 . C216 . H2161 . 108.6 no C21 . C216 . H2162 . 110.7 no H2161 . C216 . H2162 . 109.5 no C21 . C216 . H2163 . 109.2 no H2161 . C216 . H2163 . 109.5 no H2162 . C216 . H2163 . 109.5 no O3 . Li1 . Cl3 . 113.5(7) yes O3 . Li1 . Cl2 . 110.6(7) yes Cl3 . Li1 . Cl2 . 94.4(5) yes O3 . Li1 . O41 . 114.1(8) yes Cl3 . Li1 . O41 . 113.0(8) yes Cl2 . Li1 . O41 . 109.6(8) yes #=============================================================================== data_[(tBut)2NON]Co2(CH2SiMe3)2 _database_code_depnum_ccdc_archive 'CCDC 778593' #TrackingRef '- dleznoff NONM2X2.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C20 H52 Co2 N2 O1 Si4' _chemical_formula_moiety 'C20 H52 Co2 N2 O1 Si4' _chemical_formula_weight 566.86 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------ _cell_length_a 10.85(3) _cell_length_b 11.62(3) _cell_length_c 14.67(7) _cell_angle_alpha 100.32(4) _cell_angle_beta 103.76(4) _cell_angle_gamma 113.45(3) _cell_volume 1568(10) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5704 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 28.7 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_min 0.25 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_meas ? # non-dispersive F(000): _exptl_crystal_F_000 608.000 _exptl_absorpt_coefficient_mu 1.223 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6192 _exptl_absorpt_correction_T_max 0.7458 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.70930 _diffrn_measurement_device_type 'Bruker Smart APEX II' _diffrn_detector_type 'APEX II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w and \f scans' _diffrn_ambient_temperature 293 _diffrn_reflns_number 14320 _diffrn_reflns_av_R_equivalents 0.109 _diffrn_reflns_theta_min 1.502 _diffrn_reflns_theta_max 28.812 _diffrn_measured_fraction_theta_max 0.892 _diffrn_reflns_theta_full 25.066 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 #========================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _reflns_number_total 7317 # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 2237 _refine_ls_number_restraints 46 _refine_ls_number_parameters 283 _oxford_refine_ls_R_factor_ref 0.0602 _refine_ls_wR_factor_ref 0.0535 _refine_ls_goodness_of_fit_ref 1.3142 _refine_ls_shift/su_max 0.0002551 _refine_ls_shift/su_mean 0.0000853 _refine_diff_density_min -0.50 _refine_diff_density_max 0.56 # The values computed from all data _oxford_reflns_number_all 7317 _refine_ls_R_factor_all 0.2378 _refine_ls_wR_factor_all 0.1254 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2567 _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_gt 0.0600 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F) + ( 0.02P)^2^] ,where P=(max(Fo,0) + 2Fc)/3 ; _refine_special_details ; One of the two CH2Si(CH3) was found to be disordered. Adequate geometric restraints as well as thermal similarity restraints were used to produce an unbiased chemically consistant solution. ; _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_refine_ls_scale 0.1577(4) _oxford_diffrn_Wilson_B_factor 1.98 _oxford_diffrn_Wilson_scale 74.24 # Number of reflections without Friedels Law is 7317 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 7871 #--------------------------------------------------------- _chemical_name_systematic ; ; # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type Full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment constr # none if no extinction, _refine_ls_extinction_method none #========================================================== # 9. General computing _computing_data_collection ' Bruker SMART APEX II' _computing_data_reduction ' Bruker SMART APEX II' _computing_cell_refinement ' Bruker SMART APEX II' _computing_structure_solution ' SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Si 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' #============================================================================== # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Co1 Co 0.38992(13) 0.16003(12) 0.71652(9) 0.0466 1.0000 Uani . . . . . . . Co2 Co 0.51257(12) 0.41138(12) 0.79918(9) 0.0449 1.0000 Uani . . . . . . . Si1 Si 0.6506(3) 0.3253(3) 0.6830(2) 0.0670 1.0000 Uani . . . . . . . Si2 Si 0.3660(3) 0.3304(3) 0.5932(2) 0.0621 1.0000 Uani . . . . . . . Si4 Si 0.7251(3) 0.7387(3) 0.8938(2) 0.0624 1.0000 Uani . . . . . . . Si30 Si 0.2071(7) -0.1649(6) 0.6913(4) 0.0525 0.609(15) Uani D U P . 1 . . Si31 Si 0.2372(10) -0.1718(9) 0.6876(7) 0.0525 0.391(15) Uani D U P . 2 . . N1 N 0.5953(7) 0.2884(6) 0.7794(6) 0.0481 1.0000 Uani . . . . . . . N2 N 0.3235(7) 0.2930(6) 0.6937(5) 0.0419 1.0000 Uani . . . . . . . O1 O 0.5371(6) 0.3756(6) 0.6346(4) 0.0581 1.0000 Uani . . . . . . . C1 C 0.6297(12) 0.1839(10) 0.5902(9) 0.1091 1.0000 Uani . . . . . . . C2 C 0.8296(10) 0.4623(10) 0.7150(9) 0.0957 1.0000 Uani . . . . . . . C3 C 0.3431(11) 0.4682(10) 0.5619(8) 0.0953 1.0000 Uani . . . . . . . C4 C 0.2807(11) 0.1879(11) 0.4798(7) 0.1012 1.0000 Uani . . . . . . . C11 C 0.6747(11) 0.2628(10) 0.8641(9) 0.0711 1.0000 Uani . . . . . . . C21 C 0.1890(10) 0.2717(10) 0.7106(8) 0.0585 1.0000 Uani . . . . . . . C31 C 0.2919(9) -0.0293(7) 0.6458(6) 0.0710 1.0000 Uani D . . . . . . C32 C 0.1157(10) -0.3245(8) 0.5907(6) 0.1016 1.0000 Uani D . . . . . . C33 C 0.0667(15) -0.1515(12) 0.7318(12) 0.0785 0.609(15) Uani D U P . 1 . . C34 C 0.3230(17) -0.1780(12) 0.7923(8) 0.0918 0.609(15) Uani D U P . 1 . . C35 C 0.159(2) -0.1558(14) 0.7821(9) 0.0771 0.391(15) Uani D U P . 2 . . C36 C 0.3915(14) -0.1923(14) 0.7488(13) 0.0708 0.391(15) Uani D U P . 2 . . C41 C 0.5777(9) 0.5879(8) 0.8883(7) 0.0581 1.0000 Uani . . . . . . . C42 C 0.9002(9) 0.7459(10) 0.9514(7) 0.0857 1.0000 Uani . . . . . . . C43 C 0.7090(11) 0.7530(11) 0.7688(7) 0.0951 1.0000 Uani . . . . . . . C44 C 0.7281(11) 0.8894(9) 0.9679(8) 0.0912 1.0000 Uani . . . . . . . C111 C 0.7227(13) 0.1617(12) 0.8305(10) 0.1236 1.0000 Uani . . . . . . . C112 C 0.8007(11) 0.3880(11) 0.9358(8) 0.1130 1.0000 Uani . . . . . . . C113 C 0.5776(11) 0.2087(10) 0.9200(7) 0.0856 1.0000 Uani . . . . . . . C211 C 0.1893(10) 0.2236(11) 0.7987(8) 0.0869 1.0000 Uani . . . . . . . C212 C 0.0610(9) 0.1675(11) 0.6242(8) 0.0919 1.0000 Uani . . . . . . . C213 C 0.1750(11) 0.3965(11) 0.7310(9) 0.1064 1.0000 Uani . . . . . . . H11 H 0.6493 0.2103 0.5347 0.134(12) 1.0000 Uiso R . . . . . . H12 H 0.5337 0.1148 0.5693 0.134(12) 1.0000 Uiso R . . . . . . H13 H 0.6953 0.1535 0.6187 0.134(12) 1.0000 Uiso R . . . . . . H21 H 0.8529 0.4692 0.6565 0.119(12) 1.0000 Uiso R . . . . . . H22 H 0.8327 0.5432 0.7474 0.119(12) 1.0000 Uiso R . . . . . . H23 H 0.8976 0.4458 0.7583 0.119(12) 1.0000 Uiso R . . . . . . H31 H 0.3785 0.4848 0.5092 0.115(12) 1.0000 Uiso R . . . . . . H32 H 0.2435 0.4460 0.5417 0.116(12) 1.0000 Uiso R . . . . . . H33 H 0.3958 0.5450 0.6189 0.115(12) 1.0000 Uiso R . . . . . . H41 H 0.3146 0.2155 0.4290 0.119(12) 1.0000 Uiso R . . . . . . H42 H 0.1789 0.1547 0.4592 0.119(12) 1.0000 Uiso R . . . . . . H43 H 0.3052 0.1205 0.4934 0.119(12) 1.0000 Uiso R . . . . . . H311 H 0.3629 -0.0461 0.6261 0.091(17) 0.609(15) Uiso R . P . 1 . . H312 H 0.2185 -0.0399 0.5886 0.091(17) 0.609(15) Uiso R . P . 1 . . H313 H 0.3542 -0.0405 0.6122 0.091(17) 0.391(15) Uiso R . P . 2 . . H314 H 0.2056 -0.0424 0.5986 0.091(17) 0.391(15) Uiso R . P . 2 . . H321 H 0.0441 -0.3236 0.5383 0.142(12) 0.609(15) Uiso R . P . 1 . . H322 H 0.0717 -0.3949 0.6163 0.142(12) 0.609(15) Uiso R . P . 1 . . H323 H 0.1851 -0.3375 0.5660 0.142(12) 0.609(15) Uiso R . P . 1 . . H324 H 0.0339 -0.3180 0.5544 0.142(12) 0.391(15) Uiso R . P . 2 . . H325 H 0.0853 -0.3959 0.6180 0.142(12) 0.391(15) Uiso R . P . 2 . . H326 H 0.1650 -0.3404 0.5474 0.142(12) 0.391(15) Uiso R . P . 2 . . H331 H 0.1066 -0.1016 0.8015 0.126(12) 0.609(15) Uiso R . P . 1 . . H332 H -0.0075 -0.2390 0.7211 0.126(12) 0.609(15) Uiso R . P . 1 . . H333 H 0.0269 -0.1067 0.6936 0.126(12) 0.609(15) Uiso R . P . 1 . . H341 H 0.3183 -0.1363 0.8535 0.140(12) 0.609(15) Uiso R . P . 1 . . H342 H 0.2952 -0.2696 0.7858 0.140(12) 0.609(15) Uiso R . P . 1 . . H343 H 0.4191 -0.1343 0.7918 0.140(12) 0.609(15) Uiso R . P . 1 . . H351 H 0.0769 -0.1452 0.7520 0.126(12) 0.391(15) Uiso R . P . 2 . . H352 H 0.1290 -0.2334 0.8028 0.126(12) 0.391(15) Uiso R . P . 2 . . H353 H 0.2240 -0.0801 0.8383 0.126(12) 0.391(15) Uiso R . P . 2 . . H361 H 0.3582 -0.2794 0.7555 0.128(12) 0.391(15) Uiso R . P . 2 . . H362 H 0.4550 -0.1807 0.7115 0.128(12) 0.391(15) Uiso R . P . 2 . . H363 H 0.4411 -0.1273 0.8131 0.128(12) 0.391(15) Uiso R . P . 2 . . H411 H 0.6014 0.5804 0.9536 0.077(17) 1.0000 Uiso R . . . . . . H412 H 0.4959 0.6038 0.8746 0.077(17) 1.0000 Uiso R . . . . . . H421 H 0.9744 0.8258 0.9510 0.152(12) 1.0000 Uiso R . . . . . . H422 H 0.9120 0.7447 1.0182 0.152(12) 1.0000 Uiso R . . . . . . H423 H 0.9048 0.6712 0.9148 0.152(12) 1.0000 Uiso R . . . . . . H431 H 0.7854 0.8352 0.7736 0.165(12) 1.0000 Uiso R . . . . . . H432 H 0.6189 0.7509 0.7394 0.165(12) 1.0000 Uiso R . . . . . . H433 H 0.7149 0.6813 0.7295 0.165(12) 1.0000 Uiso R . . . . . . H441 H 0.7362 0.8860 1.0338 0.130(12) 1.0000 Uiso R . . . . . . H442 H 0.8081 0.9668 0.9697 0.130(12) 1.0000 Uiso R . . . . . . H443 H 0.6411 0.8925 0.9380 0.130(12) 1.0000 Uiso R . . . . . . H1111 H 0.7674 0.1413 0.8857 0.139(10) 1.0000 Uiso R . . . . . . H1112 H 0.7892 0.1978 0.7979 0.139(10) 1.0000 Uiso R . . . . . . H1113 H 0.6404 0.0837 0.7852 0.139(10) 1.0000 Uiso R . . . . . . H1121 H 0.8534 0.3695 0.9887 0.129(10) 1.0000 Uiso R . . . . . . H1122 H 0.7666 0.4465 0.9621 0.129(10) 1.0000 Uiso R . . . . . . H1123 H 0.8615 0.4281 0.9007 0.129(10) 1.0000 Uiso R . . . . . . H1131 H 0.5496 0.2734 0.9446 0.090(10) 1.0000 Uiso R . . . . . . H1132 H 0.6258 0.1891 0.9743 0.090(10) 1.0000 Uiso R . . . . . . H1133 H 0.4946 0.1297 0.8763 0.090(10) 1.0000 Uiso R . . . . . . H2111 H 0.2659 0.2914 0.8559 0.095(10) 1.0000 Uiso R . . . . . . H2112 H 0.0998 0.2015 0.8092 0.095(10) 1.0000 Uiso R . . . . . . H2113 H 0.2036 0.1465 0.7870 0.095(10) 1.0000 Uiso R . . . . . . H2121 H 0.0703 0.0880 0.6109 0.103(10) 1.0000 Uiso R . . . . . . H2122 H -0.0253 0.1502 0.6385 0.103(10) 1.0000 Uiso R . . . . . . H2123 H 0.0580 0.1988 0.5679 0.103(10) 1.0000 Uiso R . . . . . . H2131 H 0.2608 0.4658 0.7812 0.119(10) 1.0000 Uiso R . . . . . . H2132 H 0.0949 0.3839 0.7523 0.119(10) 1.0000 Uiso R . . . . . . H2133 H 0.1612 0.4199 0.6710 0.119(10) 1.0000 Uiso R . . . . . . 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 0.0443(9) 0.0372(8) 0.0518(10) 0.0120(7) 0.0126(7) 0.0157(7) Co2 0.0375(8) 0.0389(8) 0.0464(9) 0.0084(7) 0.0066(7) 0.0127(7) Si1 0.060(2) 0.058(2) 0.087(3) 0.020(2) 0.037(2) 0.0255(18) Si2 0.061(2) 0.063(2) 0.054(2) 0.0256(18) 0.0106(17) 0.0217(17) Si4 0.063(2) 0.0491(19) 0.052(2) 0.0115(16) 0.0130(16) 0.0096(16) Si30 0.0527(11) 0.0527(11) 0.0527(11) 0.0164(11) 0.0183(11) 0.0245(11) Si31 0.0527(11) 0.0527(11) 0.0527(11) 0.0164(11) 0.0183(11) 0.0245(11) N1 0.045(5) 0.041(5) 0.058(6) 0.020(4) 0.012(4) 0.020(4) N2 0.032(5) 0.045(5) 0.043(5) 0.011(4) 0.008(4) 0.017(4) O1 0.064(5) 0.063(5) 0.058(5) 0.030(4) 0.029(4) 0.029(4) C1 0.125(11) 0.081(9) 0.138(12) 0.020(9) 0.075(10) 0.052(8) C2 0.063(8) 0.091(9) 0.149(12) 0.044(9) 0.056(8) 0.036(7) C3 0.082(9) 0.090(9) 0.111(10) 0.065(9) 0.016(7) 0.032(7) C4 0.119(10) 0.117(11) 0.042(7) 0.027(8) 0.024(7) 0.030(9) C11 0.046(7) 0.058(8) 0.099(10) 0.035(8) 0.015(7) 0.014(7) C21 0.041(7) 0.055(7) 0.075(9) 0.022(7) 0.011(6) 0.022(6) C31 0.084(8) 0.042(7) 0.072(8) 0.001(6) 0.037(7) 0.016(6) C32 0.126(11) 0.048(7) 0.109(10) 0.026(7) 0.024(8) 0.027(7) C33 0.061(8) 0.070(8) 0.086(8) 0.014(7) 0.024(7) 0.018(7) C34 0.085(8) 0.075(8) 0.083(8) 0.022(7) 0.009(7) 0.018(7) C35 0.069(9) 0.065(9) 0.069(9) 0.012(8) 0.012(8) 0.014(8) C36 0.060(8) 0.060(9) 0.082(9) 0.010(8) 0.010(8) 0.031(7) C41 0.053(7) 0.042(6) 0.054(7) 0.000(5) 0.009(5) 0.011(5) C42 0.044(7) 0.084(9) 0.087(9) 0.008(7) 0.003(6) 0.008(6) C43 0.096(9) 0.103(10) 0.074(9) 0.043(8) 0.030(7) 0.028(8) C44 0.102(9) 0.052(7) 0.088(9) 0.011(7) 0.014(7) 0.020(7) C111 0.115(11) 0.115(12) 0.189(15) 0.079(11) 0.045(11) 0.089(10) C112 0.067(9) 0.102(11) 0.121(12) 0.041(9) -0.025(8) 0.022(8) C113 0.086(9) 0.097(10) 0.060(8) 0.031(7) 0.000(7) 0.042(8) C211 0.055(8) 0.128(11) 0.093(10) 0.041(9) 0.041(7) 0.045(8) C212 0.034(7) 0.104(10) 0.101(10) 0.022(8) 0.004(7) 0.011(7) C213 0.068(9) 0.090(10) 0.172(14) 0.033(10) 0.040(9) 0.051(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 . Co2 . 2.576(8) yes Co1 . N1 . 1.982(8) yes Co1 . N2 . 1.993(8) yes Co1 . C31 . 1.959(9) yes Co1 . O1 . 3.012(9) yes Co2 . N1 . 1.982(8) yes Co2 . N2 . 1.995(8) yes Co2 . O1 . 2.471(12) yes Co2 . C41 . 1.965(10) yes Si1 . N1 . 1.720(10) yes Si1 . O1 . 1.634(7) yes Si1 . C1 . 1.832(11) yes Si1 . C2 . 1.835(10) yes Si2 . N2 . 1.722(10) yes Si2 . O1 . 1.633(8) yes Si2 . C3 . 1.834(10) yes Si2 . C4 . 1.851(12) yes Si4 . C41 . 1.815(9) yes Si4 . C42 . 1.849(11) yes Si4 . C43 . 1.843(13) yes Si4 . C44 . 1.871(11) yes Si30 . C31 . 1.813(8) yes Si30 . C32 . 1.859(11) yes Si30 . C33 . 1.813(8) yes Si30 . C34 . 1.775(9) yes Si31 . C31 . 1.795(9) yes Si31 . C32 . 1.802(12) yes Si31 . C35 . 1.809(10) yes Si31 . C36 . 1.829(9) yes N1 . C11 . 1.485(12) yes N2 . C21 . 1.470(11) yes C1 . H11 . 0.961 no C1 . H12 . 0.958 no C1 . H13 . 0.958 no C2 . H21 . 0.958 no C2 . H22 . 0.958 no C2 . H23 . 0.958 no C3 . H31 . 0.959 no C3 . H32 . 0.960 no C3 . H33 . 0.960 no C4 . H41 . 0.958 no C4 . H42 . 0.960 no C4 . H43 . 0.960 no C11 . C111 . 1.515(14) yes C11 . C112 . 1.509(13) yes C11 . C113 . 1.499(13) yes C21 . C211 . 1.496(13) yes C21 . C212 . 1.509(12) yes C21 . C213 . 1.502(13) yes C31 . H311 . 0.960 no C31 . H312 . 0.960 no C32 . H321 . 0.960 no C32 . H322 . 0.960 no C32 . H323 . 0.960 no C33 . H331 . 0.973 no C33 . H332 . 0.969 no C33 . H333 . 0.969 no C34 . H341 . 0.963 no C34 . H342 . 0.962 no C34 . H343 . 0.964 no C35 . H351 . 0.960 no C35 . H352 . 0.960 no C35 . H353 . 0.960 no C36 . H361 . 0.962 no C36 . H362 . 0.962 no C36 . H363 . 0.965 no C41 . H411 . 0.960 no C41 . H412 . 0.960 no C42 . H421 . 0.959 no C42 . H422 . 0.961 no C42 . H423 . 0.961 no C43 . H431 . 0.960 no C43 . H432 . 0.959 no C43 . H433 . 0.959 no C44 . H441 . 0.960 no C44 . H442 . 0.960 no C44 . H443 . 0.960 no C111 . H1111 . 0.960 no C111 . H1112 . 0.960 no C111 . H1113 . 0.958 no C112 . H1121 . 0.959 no C112 . H1122 . 0.960 no C112 . H1123 . 0.960 no C113 . H1131 . 0.962 no C113 . H1132 . 0.959 no C113 . H1133 . 0.960 no C211 . H2111 . 0.962 no C211 . H2112 . 0.959 no C211 . H2113 . 0.961 no C212 . H2121 . 0.959 no C212 . H2122 . 0.959 no C212 . H2123 . 0.959 no C213 . H2131 . 0.961 no C213 . H2132 . 0.959 no C213 . H2133 . 0.961 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Co2 . Co1 . N1 . 49.5(2) yes Co2 . Co1 . N2 . 49.8(3) yes N1 . Co1 . N2 . 95.6(3) yes Co2 . Co1 . C31 . 176.4(2) yes N1 . Co1 . C31 . 132.1(4) yes N2 . Co1 . C31 . 127.3(4) yes Co2 . Co1 . O1 . 51.8(2) yes N1 . Co1 . O1 . 57.4(3) yes N2 . Co1 . O1 . 57.1(3) yes C31 . Co1 . O1 . 125.4(3) yes Co1 . Co2 . N1 . 49.5(2) yes Co1 . Co2 . N2 . 49.7(2) yes N1 . Co2 . N2 . 95.6(4) yes Co1 . Co2 . O1 . 73.2(3) yes N1 . Co2 . O1 . 69.3(3) yes N2 . Co2 . O1 . 68.9(4) yes Co1 . Co2 . C41 . 163.7(3) yes N1 . Co2 . C41 . 135.8(4) yes N2 . Co2 . C41 . 128.6(4) yes O1 . Co2 . C41 . 122.6(3) yes N1 . Si1 . O1 . 99.7(4) yes N1 . Si1 . C1 . 114.8(5) yes O1 . Si1 . C1 . 108.9(5) yes N1 . Si1 . C2 . 116.9(5) yes O1 . Si1 . C2 . 106.5(5) yes C1 . Si1 . C2 . 109.1(5) yes N2 . Si2 . O1 . 99.2(5) yes N2 . Si2 . C3 . 116.9(5) yes O1 . Si2 . C3 . 107.9(4) yes N2 . Si2 . C4 . 114.5(5) yes O1 . Si2 . C4 . 108.9(5) yes C3 . Si2 . C4 . 108.7(5) yes C41 . Si4 . C42 . 111.9(5) yes C41 . Si4 . C43 . 110.2(5) yes C42 . Si4 . C43 . 109.2(6) yes C41 . Si4 . C44 . 112.3(5) yes C42 . Si4 . C44 . 106.4(5) yes C43 . Si4 . C44 . 106.6(5) yes C31 . Si30 . C32 . 110.6(6) yes C31 . Si30 . C33 . 111.0(5) yes C32 . Si30 . C33 . 105.0(5) yes C31 . Si30 . C34 . 115.1(6) yes C32 . Si30 . C34 . 108.4(6) yes C33 . Si30 . C34 . 106.2(5) yes C31 . Si31 . C32 . 114.2(7) yes C31 . Si31 . C35 . 112.5(7) yes C32 . Si31 . C35 . 108.7(6) yes C31 . Si31 . C36 . 110.9(6) yes C32 . Si31 . C36 . 106.4(6) yes C35 . Si31 . C36 . 103.5(7) yes Co1 . N1 . Co2 . 81.1(3) yes Co1 . N1 . Si1 . 104.6(4) yes Co2 . N1 . Si1 . 98.9(4) yes Co1 . N1 . C11 . 115.0(6) yes Co2 . N1 . C11 . 121.4(7) yes Si1 . N1 . C11 . 126.0(7) yes Co2 . N2 . Co1 . 80.5(3) yes Co2 . N2 . Si2 . 99.2(5) yes Co1 . N2 . Si2 . 105.0(4) yes Co2 . N2 . C21 . 121.4(7) yes Co1 . N2 . C21 . 115.4(6) yes Si2 . N2 . C21 . 125.6(6) yes Co2 . O1 . Si1 . 84.1(3) yes Co2 . O1 . Si2 . 84.9(5) yes Si1 . O1 . Si2 . 141.6(4) yes Co2 . O1 . Co1 . 54.99(14) yes Si1 . O1 . Co1 . 71.4(4) yes Si2 . O1 . Co1 . 72.1(2) yes Si1 . C1 . H11 . 109.4 no Si1 . C1 . H12 . 109.3 no H11 . C1 . H12 . 109.6 no Si1 . C1 . H13 . 109.1 no H11 . C1 . H13 . 109.8 no H12 . C1 . H13 . 109.6 no Si1 . C2 . H21 . 110.0 no Si1 . C2 . H22 . 109.9 no H21 . C2 . H22 . 109.3 no Si1 . C2 . H23 . 108.9 no H21 . C2 . H23 . 109.4 no H22 . C2 . H23 . 109.4 no Si2 . C3 . H31 . 109.2 no Si2 . C3 . H32 . 109.3 no H31 . C3 . H32 . 109.8 no Si2 . C3 . H33 . 109.0 no H31 . C3 . H33 . 109.8 no H32 . C3 . H33 . 109.8 no Si2 . C4 . H41 . 109.3 no Si2 . C4 . H42 . 109.3 no H41 . C4 . H42 . 109.8 no Si2 . C4 . H43 . 109.0 no H41 . C4 . H43 . 109.6 no H42 . C4 . H43 . 109.9 no N1 . C11 . C111 . 111.7(10) yes N1 . C11 . C112 . 111.7(9) yes C111 . C11 . C112 . 110.4(10) yes N1 . C11 . C113 . 108.8(9) yes C111 . C11 . C113 . 107.6(10) yes C112 . C11 . C113 . 106.4(11) yes N2 . C21 . C211 . 107.5(8) yes N2 . C21 . C212 . 111.5(9) yes C211 . C21 . C212 . 107.9(9) yes N2 . C21 . C213 . 112.0(8) yes C211 . C21 . C213 . 108.7(10) yes C212 . C21 . C213 . 109.2(9) yes Co1 . C31 . Si30 . 128.1(5) yes Co1 . C31 . H311 . 104.4 no Si30 . C31 . H311 . 104.2 no Co1 . C31 . H312 . 104.7 no Si30 . C31 . H312 . 105.2 no H311 . C31 . H312 . 109.5 no Si30 . C32 . H321 . 110.0 no Si30 . C32 . H322 . 109.3 no H321 . C32 . H322 . 109.5 no Si30 . C32 . H323 . 109.1 no H321 . C32 . H323 . 109.5 no H322 . C32 . H323 . 109.5 no Si30 . C33 . H331 . 109.3 no Si30 . C33 . H332 . 109.3 no H331 . C33 . H332 . 110.1 no Si30 . C33 . H333 . 108.8 no H331 . C33 . H333 . 110.0 no H332 . C33 . H333 . 109.4 no Si30 . C34 . H341 . 110.2 no Si30 . C34 . H342 . 109.5 no H341 . C34 . H342 . 109.4 no Si30 . C34 . H343 . 108.1 no H341 . C34 . H343 . 109.4 no H342 . C34 . H343 . 110.2 no Si31 . C35 . H351 . 105.5 no Si31 . C35 . H352 . 111.3 no H351 . C35 . H352 . 109.5 no Si31 . C35 . H353 . 111.6 no H351 . C35 . H353 . 109.5 no H352 . C35 . H353 . 109.5 no Si31 . C36 . H361 . 108.8 no Si31 . C36 . H362 . 111.1 no H361 . C36 . H362 . 109.5 no Si31 . C36 . H363 . 108.0 no H361 . C36 . H363 . 109.7 no H362 . C36 . H363 . 109.7 no Co2 . C41 . Si4 . 125.7(5) yes Co2 . C41 . H411 . 105.3 no Si4 . C41 . H411 . 105.2 no Co2 . C41 . H412 . 105.4 no Si4 . C41 . H412 . 105.2 no H411 . C41 . H412 . 109.5 no Si4 . C42 . H421 . 108.9 no Si4 . C42 . H422 . 109.5 no H421 . C42 . H422 . 109.6 no Si4 . C42 . H423 . 109.6 no H421 . C42 . H423 . 109.8 no H422 . C42 . H423 . 109.5 no Si4 . C43 . H431 . 108.9 no Si4 . C43 . H432 . 109.2 no H431 . C43 . H432 . 109.6 no Si4 . C43 . H433 . 109.7 no H431 . C43 . H433 . 109.6 no H432 . C43 . H433 . 109.8 no Si4 . C44 . H441 . 109.5 no Si4 . C44 . H442 . 109.7 no H441 . C44 . H442 . 109.5 no Si4 . C44 . H443 . 109.2 no H441 . C44 . H443 . 109.5 no H442 . C44 . H443 . 109.5 no C11 . C111 . H1111 . 110.6 no C11 . C111 . H1112 . 108.1 no H1111 . C111 . H1112 . 109.9 no C11 . C111 . H1113 . 108.3 no H1111 . C111 . H1113 . 109.9 no H1112 . C111 . H1113 . 110.0 no C11 . C112 . H1121 . 110.8 no C11 . C112 . H1122 . 108.9 no H1121 . C112 . H1122 . 109.6 no C11 . C112 . H1123 . 108.2 no H1121 . C112 . H1123 . 109.6 no H1122 . C112 . H1123 . 109.7 no C11 . C113 . H1131 . 108.8 no C11 . C113 . H1132 . 110.4 no H1131 . C113 . H1132 . 109.4 no C11 . C113 . H1133 . 109.0 no H1131 . C113 . H1133 . 109.7 no H1132 . C113 . H1133 . 109.5 no C21 . C211 . H2111 . 109.3 no C21 . C211 . H2112 . 110.2 no H2111 . C211 . H2112 . 109.7 no C21 . C211 . H2113 . 108.6 no H2111 . C211 . H2113 . 109.6 no H2112 . C211 . H2113 . 109.4 no C21 . C212 . H2121 . 109.3 no C21 . C212 . H2122 . 110.4 no H2121 . C212 . H2122 . 109.4 no C21 . C212 . H2123 . 108.5 no H2121 . C212 . H2123 . 109.6 no H2122 . C212 . H2123 . 109.7 no C21 . C213 . H2131 . 109.5 no C21 . C213 . H2132 . 110.5 no H2131 . C213 . H2132 . 109.5 no C21 . C213 . H2133 . 108.2 no H2131 . C213 . H2133 . 109.6 no H2132 . C213 . H2133 . 109.6 no