# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Xin-E Duan' _publ_contact_author_email duanxe@sxu.edu.cn loop_ _publ_author_name 'Xin-E Duan' 'Shi-Fang Yuan' 'Hongbo Tong' 'Shengdi Bai' 'Xuehong Wei' ; Diansheng Liu ; data_3 _database_code_depnum_ccdc_archive 'CCDC 858901' #TrackingRef '3-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 423-425 _chemical_formula_moiety 'C22 H40 Br2 Mg2 N6 O Si2' _chemical_formula_sum 'C22 H40 Br2 Mg2 N6 O Si2' _chemical_formula_weight 669.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.527(7) _cell_length_b 14.789(6) _cell_length_c 13.593(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3322(2) _cell_formula_units_Z 4 _cell_measurement_temperature 238(2) _cell_measurement_reflns_used 2773 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 24.01 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 2.574 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5123 _exptl_absorpt_correction_T_max 0.6270 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 238(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD AREA DETECOR' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11457 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.04 _reflns_number_total 2926 _reflns_number_gt 1853 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1435P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0067(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2926 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1123 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.2206 _refine_ls_wR_factor_gt 0.1504 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg Mg 0.41509(10) 0.23714(14) 0.30909(12) 0.0383(6) Uani 1 1 d . . . Br1 Br 0.31033(4) 0.12237(6) 0.36008(6) 0.0656(4) Uani 1 1 d . . . N1 N 0.5104(3) 0.2548(3) 0.0681(3) 0.0411(12) Uani 1 1 d . . . N3 N 0.3419(3) 0.3660(4) 0.3344(3) 0.0491(14) Uani 1 1 d . . . N2 N 0.4065(3) 0.3013(4) 0.1725(3) 0.0395(12) Uani 1 1 d . . . O1 O 0.5000 0.1307(4) 0.2500 0.0521(16) Uani 1 2 d S . . Si1 Si 0.32583(11) 0.37036(14) 0.20418(12) 0.0539(6) Uani 1 1 d . . . C5 C 0.5416(4) 0.2441(5) -0.0239(4) 0.0563(18) Uani 1 1 d . . . H5 H 0.5934 0.2183 -0.0295 0.068 Uiso 1 1 calc R . . C4 C 0.5025(4) 0.2683(6) -0.1089(5) 0.072(2) Uani 1 1 d . . . H4 H 0.5267 0.2610 -0.1710 0.086 Uiso 1 1 calc R . . C3 C 0.4250(4) 0.3043(6) -0.0987(4) 0.066(2) Uani 1 1 d . . . H3 H 0.3956 0.3209 -0.1551 0.079 Uiso 1 1 calc R . . C2 C 0.3914(4) 0.3157(5) -0.0085(4) 0.0558(19) Uani 1 1 d . . . H2 H 0.3392 0.3407 -0.0032 0.067 Uiso 1 1 calc R . . C1 C 0.4345(3) 0.2902(4) 0.0791(4) 0.0409(15) Uani 1 1 d . . . C6 C 0.2250(4) 0.3190(8) 0.1768(6) 0.100(4) Uani 1 1 d . . . H6A H 0.2150 0.3214 0.1066 0.151 Uiso 1 1 calc R . . H6B H 0.1832 0.3523 0.2112 0.151 Uiso 1 1 calc R . . H6C H 0.2246 0.2565 0.1985 0.151 Uiso 1 1 calc R . . C7 C 0.3317(7) 0.4885(7) 0.1541(6) 0.099(3) Uani 1 1 d . . . H7A H 0.3861 0.5117 0.1627 0.149 Uiso 1 1 calc R . . H7B H 0.2938 0.5269 0.1890 0.149 Uiso 1 1 calc R . . H7C H 0.3183 0.4879 0.0846 0.149 Uiso 1 1 calc R . . C8 C 0.2690(5) 0.3632(5) 0.4004(5) 0.068(2) Uani 1 1 d . . . H8A H 0.2857 0.3483 0.4668 0.103 Uiso 1 1 calc R . . H8B H 0.2315 0.3177 0.3767 0.103 Uiso 1 1 calc R . . H8C H 0.2427 0.4219 0.4002 0.103 Uiso 1 1 calc R . . C9 C 0.3983(5) 0.4362(6) 0.3702(5) 0.070(2) Uani 1 1 d . . . H9A H 0.3720 0.4948 0.3675 0.105 Uiso 1 1 calc R . . H9B H 0.4462 0.4369 0.3290 0.105 Uiso 1 1 calc R . . H9C H 0.4136 0.4229 0.4376 0.105 Uiso 1 1 calc R . . C10 C 0.4638(5) 0.0732(6) 0.1727(6) 0.084(3) Uani 1 1 d . . . H10A H 0.4943 0.0780 0.1111 0.101 Uiso 1 1 calc R . . H10B H 0.4074 0.0904 0.1603 0.101 Uiso 1 1 calc R . . C11 C 0.4689(9) -0.0210(8) 0.2143(12) 0.163(7) Uani 1 1 d . . . H11A H 0.4173 -0.0381 0.2444 0.196 Uiso 1 1 calc R . . H11B H 0.4814 -0.0645 0.1619 0.196 Uiso 1 1 calc 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 Mg 0.0282(9) 0.0490(15) 0.0376(9) 0.0006(8) -0.0018(7) -0.0007(8) Br1 0.0428(5) 0.0662(7) 0.0877(6) -0.0076(4) 0.0177(3) -0.0153(3) N1 0.034(2) 0.051(4) 0.038(2) -0.012(2) -0.0036(18) 0.007(2) N3 0.048(3) 0.060(4) 0.039(2) -0.004(2) 0.005(2) 0.008(3) N2 0.037(2) 0.045(3) 0.037(2) -0.003(2) -0.0051(18) 0.010(2) O1 0.043(3) 0.046(4) 0.067(4) 0.000 0.010(3) 0.000 Si1 0.0484(10) 0.0719(16) 0.0415(9) 0.0029(8) -0.0003(7) 0.0256(9) C5 0.045(3) 0.079(5) 0.045(3) -0.010(3) 0.004(3) 0.015(3) C4 0.071(5) 0.102(7) 0.041(3) -0.017(4) 0.002(3) 0.014(5) C3 0.061(4) 0.098(7) 0.038(3) -0.003(3) -0.014(3) 0.009(4) C2 0.046(3) 0.081(6) 0.041(3) -0.006(3) -0.013(3) 0.015(4) C1 0.038(3) 0.048(4) 0.037(3) -0.008(2) -0.007(2) 0.006(3) C6 0.040(4) 0.189(12) 0.072(5) -0.012(6) -0.009(3) 0.021(6) C7 0.153(9) 0.074(7) 0.072(5) 0.025(4) 0.032(5) 0.061(7) C8 0.066(5) 0.080(6) 0.059(4) 0.000(4) 0.022(3) 0.025(4) C9 0.091(6) 0.054(6) 0.064(4) -0.006(4) 0.005(4) 0.003(4) C10 0.075(5) 0.070(7) 0.108(6) -0.041(5) 0.020(5) -0.018(5) C11 0.162(16) 0.066(9) 0.26(2) -0.032(10) 0.038(13) -0.026(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg N2 2.090(5) . ? Mg N1 2.091(4) 3_655 ? Mg O1 2.257(5) . ? Mg N3 2.283(6) . ? Mg Br1 2.522(2) . ? Mg Si1 2.844(3) . ? Mg Mg 3.234(4) 3_655 ? N1 C5 1.362(7) . ? N1 C1 1.368(6) . ? N1 Mg 2.091(4) 3_655 ? N3 C9 1.477(10) . ? N3 C8 1.502(9) . ? N3 Si1 1.791(5) . ? N2 C1 1.361(7) . ? N2 Si1 1.734(5) . ? O1 C10 1.478(8) . ? O1 C10 1.478(8) 3_655 ? O1 Mg 2.257(5) 3_655 ? Si1 C6 1.868(9) . ? Si1 C7 1.878(9) . ? C5 C4 1.372(9) . ? C5 H5 0.9400 . ? C4 C3 1.394(9) . ? C4 H4 0.9400 . ? C3 C2 1.357(8) . ? C3 H3 0.9400 . ? C2 C1 1.438(7) . ? C2 H2 0.9400 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C11 1.507(15) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C11 1.41(3) 3_655 ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Mg N1 133.8(2) . 3_655 ? N2 Mg O1 92.46(15) . . ? N1 Mg O1 90.28(15) 3_655 . ? N2 Mg N3 73.68(19) . . ? N1 Mg N3 95.0(2) 3_655 . ? O1 Mg N3 164.88(18) . . ? N2 Mg Br1 120.22(15) . . ? N1 Mg Br1 105.61(14) 3_655 . ? O1 Mg Br1 93.17(14) . . ? N3 Mg Br1 98.99(16) . . ? N2 Mg Si1 37.34(13) . . ? N1 Mg Si1 128.27(17) 3_655 . ? O1 Mg Si1 128.85(9) . . ? N3 Mg Si1 39.00(13) . . ? Br1 Mg Si1 104.35(8) . . ? N2 Mg Mg 67.52(13) . 3_655 ? N1 Mg Mg 83.41(14) 3_655 3_655 ? O1 Mg Mg 44.24(12) . 3_655 ? N3 Mg Mg 122.34(14) . 3_655 ? Br1 Mg Mg 137.09(5) . 3_655 ? Si1 Mg Mg 101.60(7) . 3_655 ? C5 N1 C1 119.5(4) . . ? C5 N1 Mg 119.7(4) . 3_655 ? C1 N1 Mg 120.1(3) . 3_655 ? C9 N3 C8 109.2(5) . . ? C9 N3 Si1 113.2(4) . . ? C8 N3 Si1 118.2(5) . . ? C9 N3 Mg 107.6(4) . . ? C8 N3 Mg 119.5(4) . . ? Si1 N3 Mg 87.7(2) . . ? C1 N2 Si1 124.3(4) . . ? C1 N2 Mg 138.7(4) . . ? Si1 N2 Mg 95.7(2) . . ? C10 O1 C10 109.9(9) . 3_655 ? C10 O1 Mg 113.7(4) . . ? C10 O1 Mg 113.6(4) 3_655 . ? C10 O1 Mg 113.6(4) . 3_655 ? C10 O1 Mg 113.7(4) 3_655 3_655 ? Mg O1 Mg 91.5(2) . 3_655 ? N2 Si1 N3 96.3(2) . . ? N2 Si1 C6 113.4(4) . . ? N3 Si1 C6 108.3(3) . . ? N2 Si1 C7 114.7(3) . . ? N3 Si1 C7 112.6(4) . . ? C6 Si1 C7 110.6(5) . . ? N2 Si1 Mg 46.99(15) . . ? N3 Si1 Mg 53.33(18) . . ? C6 Si1 Mg 106.3(4) . . ? C7 Si1 Mg 143.1(4) . . ? N1 C5 C4 124.4(6) . . ? N1 C5 H5 117.8 . . ? C4 C5 H5 117.8 . . ? C5 C4 C3 116.7(6) . . ? C5 C4 H4 121.7 . . ? C3 C4 H4 121.7 . . ? C2 C3 C4 120.9(6) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C3 C2 C1 120.9(6) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? N2 C1 N1 117.3(4) . . ? N2 C1 C2 124.9(5) . . ? N1 C1 C2 117.7(5) . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C10 C11 104.0(9) . . ? O1 C10 H10A 111.0 . . ? C11 C10 H10A 111.0 . . ? O1 C10 H10B 111.0 . . ? C11 C10 H10B 111.0 . . ? H10A C10 H10B 109.0 . . ? C11 C11 C10 107.4(7) 3_655 . ? C11 C11 H11A 110.2 3_655 . ? C10 C11 H11A 110.2 . . ? C11 C11 H11B 110.2 3_655 . ? C10 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Mg N3 C9 -96.3(4) . . . . ? N1 Mg N3 C9 38.0(4) 3_655 . . . ? O1 Mg N3 C9 -72.1(8) . . . . ? Br1 Mg N3 C9 144.7(4) . . . . ? Si1 Mg N3 C9 -113.6(5) . . . . ? Mg Mg N3 C9 -47.4(4) 3_655 . . . ? N2 Mg N3 C8 138.6(5) . . . . ? N1 Mg N3 C8 -87.1(5) 3_655 . . . ? O1 Mg N3 C8 162.8(6) . . . . ? Br1 Mg N3 C8 19.6(5) . . . . ? Si1 Mg N3 C8 121.3(6) . . . . ? Mg Mg N3 C8 -172.5(4) 3_655 . . . ? N2 Mg N3 Si1 17.3(2) . . . . ? N1 Mg N3 Si1 151.6(2) 3_655 . . . ? O1 Mg N3 Si1 41.4(8) . . . . ? Br1 Mg N3 Si1 -101.74(19) . . . . ? Mg Mg N3 Si1 66.2(3) 3_655 . . . ? N1 Mg N2 C1 94.8(6) 3_655 . . . ? O1 Mg N2 C1 2.1(6) . . . . ? N3 Mg N2 C1 175.9(6) . . . . ? Br1 Mg N2 C1 -93.0(6) . . . . ? Si1 Mg N2 C1 -166.1(7) . . . . ? Mg Mg N2 C1 39.5(5) 3_655 . . . ? N1 Mg N2 Si1 -99.0(3) 3_655 . . . ? O1 Mg N2 Si1 168.2(2) . . . . ? N3 Mg N2 Si1 -17.9(2) . . . . ? Br1 Mg N2 Si1 73.1(2) . . . . ? Mg Mg N2 Si1 -154.3(2) 3_655 . . . ? N2 Mg O1 C10 -63.0(5) . . . . ? N1 Mg O1 C10 163.1(5) 3_655 . . . ? N3 Mg O1 C10 -86.2(9) . . . . ? Br1 Mg O1 C10 57.5(5) . . . . ? Si1 Mg O1 C10 -53.8(5) . . . . ? Mg Mg O1 C10 -116.6(5) 3_655 . . . ? N2 Mg O1 C10 170.4(5) . . . 3_655 ? N1 Mg O1 C10 36.5(5) 3_655 . . 3_655 ? N3 Mg O1 C10 147.2(7) . . . 3_655 ? Br1 Mg O1 C10 -69.1(5) . . . 3_655 ? Si1 Mg O1 C10 179.6(5) . . . 3_655 ? Mg Mg O1 C10 116.8(5) 3_655 . . 3_655 ? N2 Mg O1 Mg 53.65(14) . . . 3_655 ? N1 Mg O1 Mg -80.24(13) 3_655 . . 3_655 ? N3 Mg O1 Mg 30.5(6) . . . 3_655 ? Br1 Mg O1 Mg 174.11(8) . . . 3_655 ? Si1 Mg O1 Mg 62.80(12) . . . 3_655 ? C1 N2 Si1 N3 -168.8(5) . . . . ? Mg N2 Si1 N3 22.3(3) . . . . ? C1 N2 Si1 C6 78.1(6) . . . . ? Mg N2 Si1 C6 -90.8(4) . . . . ? C1 N2 Si1 C7 -50.3(6) . . . . ? Mg N2 Si1 C7 140.7(4) . . . . ? C1 N2 Si1 Mg 168.9(6) . . . . ? C9 N3 Si1 N2 87.9(5) . . . . ? C8 N3 Si1 N2 -142.7(5) . . . . ? Mg N3 Si1 N2 -20.2(2) . . . . ? C9 N3 Si1 C6 -154.9(6) . . . . ? C8 N3 Si1 C6 -25.5(6) . . . . ? Mg N3 Si1 C6 97.0(4) . . . . ? C9 N3 Si1 C7 -32.2(6) . . . . ? C8 N3 Si1 C7 97.2(6) . . . . ? Mg N3 Si1 C7 -140.3(4) . . . . ? C9 N3 Si1 Mg 108.1(5) . . . . ? C8 N3 Si1 Mg -122.5(5) . . . . ? N1 Mg Si1 N2 114.8(3) 3_655 . . . ? O1 Mg Si1 N2 -15.2(3) . . . . ? N3 Mg Si1 N2 152.0(3) . . . . ? Br1 Mg Si1 N2 -121.4(2) . . . . ? Mg Mg Si1 N2 24.1(2) 3_655 . . . ? N2 Mg Si1 N3 -152.0(3) . . . . ? N1 Mg Si1 N3 -37.2(3) 3_655 . . . ? O1 Mg Si1 N3 -167.2(3) . . . . ? Br1 Mg Si1 N3 86.6(2) . . . . ? Mg Mg Si1 N3 -127.9(2) 3_655 . . . ? N2 Mg Si1 C6 107.0(4) . . . . ? N1 Mg Si1 C6 -138.1(3) 3_655 . . . ? O1 Mg Si1 C6 91.8(3) . . . . ? N3 Mg Si1 C6 -101.0(4) . . . . ? Br1 Mg Si1 C6 -14.4(3) . . . . ? Mg Mg Si1 C6 131.1(3) 3_655 . . . ? N2 Mg Si1 C7 -73.1(5) . . . . ? N1 Mg Si1 C7 41.7(5) 3_655 . . . ? O1 Mg Si1 C7 -88.3(5) . . . . ? N3 Mg Si1 C7 78.9(5) . . . . ? Br1 Mg Si1 C7 165.5(4) . . . . ? Mg Mg Si1 C7 -49.0(4) 3_655 . . . ? C1 N1 C5 C4 1.4(11) . . . . ? Mg N1 C5 C4 -168.7(6) 3_655 . . . ? N1 C5 C4 C3 -1.5(12) . . . . ? C5 C4 C3 C2 1.0(13) . . . . ? C4 C3 C2 C1 -0.6(12) . . . . ? Si1 N2 C1 N1 162.4(4) . . . . ? Mg N2 C1 N1 -34.4(9) . . . . ? Si1 N2 C1 C2 -15.4(9) . . . . ? Mg N2 C1 C2 147.9(6) . . . . ? C5 N1 C1 N2 -178.7(6) . . . . ? Mg N1 C1 N2 -8.7(7) 3_655 . . . ? C5 N1 C1 C2 -0.8(9) . . . . ? Mg N1 C1 C2 169.2(5) 3_655 . . . ? C3 C2 C1 N2 178.2(7) . . . . ? C3 C2 C1 N1 0.4(10) . . . . ? C10 O1 C10 C11 8.1(7) 3_655 . . . ? Mg O1 C10 C11 -120.4(8) . . . . ? Mg O1 C10 C11 136.7(7) 3_655 . . . ? O1 C10 C11 C11 -22.5(19) . . . 3_655 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.089 _refine_diff_density_min -1.295 _refine_diff_density_rms 0.138 #===end data_4 _database_code_depnum_ccdc_archive 'CCDC 858902' #TrackingRef '3-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 403 _chemical_formula_moiety 'C22 H32 Cl4 N4 O3 Ti2' _chemical_formula_sum 'C22 H32 Cl4 N4 O3 Ti2' _chemical_formula_weight 638.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.206(6) _cell_length_b 11.636(4) _cell_length_c 15.911(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.202(5) _cell_angle_gamma 90.00 _cell_volume 2810.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 238(2) _cell_measurement_reflns_used 6973 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 26.92 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.979 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7577 _exptl_absorpt_correction_T_max 0.8282 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 238(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD AREA DETECOR' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29060 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4948 _reflns_number_gt 3999 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+3.5053P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4948 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.77929(3) 0.73008(4) 0.08784(3) 0.02580(14) Uani 1 1 d . . . Ti2 Ti 0.73813(3) 0.75932(5) -0.09790(3) 0.02729(14) Uani 1 1 d . . . Cl1 Cl 0.83886(5) 0.91321(7) 0.10815(5) 0.03709(19) Uani 1 1 d . . . Cl2 Cl 0.72552(6) 0.54204(7) 0.09263(5) 0.0417(2) Uani 1 1 d . . . Cl3 Cl 0.80955(6) 0.70510(8) -0.22372(5) 0.0498(2) Uani 1 1 d . . . Cl4 Cl 0.61803(5) 0.84747(8) -0.18313(5) 0.0475(2) Uani 1 1 d . . . N1 N 0.65382(16) 0.7890(2) 0.13655(15) 0.0351(6) Uani 1 1 d . . . N2 N 0.68299(15) 0.7894(2) 0.00187(14) 0.0296(5) Uani 1 1 d . . . N3 N 0.91438(15) 0.6654(2) 0.08579(15) 0.0319(6) Uani 1 1 d . . . N4 N 0.83131(15) 0.7043(2) -0.02909(14) 0.0295(5) Uani 1 1 d . . . O1 O 0.80992(14) 0.70791(17) 0.22643(12) 0.0340(5) Uani 1 1 d . . . O2 O 0.79880(13) 0.92122(18) -0.10439(13) 0.0347(5) Uani 1 1 d . . . O3 O 0.66762(13) 0.60277(18) -0.11353(13) 0.0365(5) Uani 1 1 d . . . C1 C 0.62157(18) 0.8144(3) 0.05816(18) 0.0299(6) Uani 1 1 d . . . C2 C 0.5373(2) 0.8584(3) 0.0430(2) 0.0433(8) Uani 1 1 d . . . H2 H 0.5153 0.8758 -0.0119 0.052 Uiso 1 1 calc R . . C3 C 0.4877(2) 0.8756(4) 0.1110(3) 0.0576(10) Uani 1 1 d . . . H3 H 0.4305 0.9058 0.1031 0.069 Uiso 1 1 calc R . . C4 C 0.5210(2) 0.8490(4) 0.1914(2) 0.0570(10) Uani 1 1 d . . . H4 H 0.4867 0.8606 0.2380 0.068 Uiso 1 1 calc R . . C5 C 0.6040(2) 0.8057(3) 0.2022(2) 0.0496(9) Uani 1 1 d . . . H5 H 0.6267 0.7872 0.2567 0.059 Uiso 1 1 calc R . . C6 C 0.91383(18) 0.6729(2) 0.00130(18) 0.0290(6) Uani 1 1 d . . . C7 C 0.9897(2) 0.6545(3) -0.0418(2) 0.0385(7) Uani 1 1 d . . . H7 H 0.9893 0.6611 -0.1007 0.046 Uiso 1 1 calc R . . C8 C 1.0651(2) 0.6266(3) 0.0048(2) 0.0461(8) Uani 1 1 d . . . H8 H 1.1172 0.6116 -0.0224 0.055 Uiso 1 1 calc R . . C9 C 1.0651(2) 0.6203(3) 0.0920(2) 0.0464(9) Uani 1 1 d . . . H9 H 1.1172 0.6023 0.1240 0.056 Uiso 1 1 calc R . . C10 C 0.9887(2) 0.6405(3) 0.1308(2) 0.0393(8) Uani 1 1 d . . . H10 H 0.9884 0.6369 0.1898 0.047 Uiso 1 1 calc R . . C11 C 0.8104(3) 0.5980(4) 0.2704(2) 0.0716(14) Uani 1 1 d . . . H11A H 0.8425 0.5400 0.2396 0.086 Uiso 1 1 calc R . . H11B H 0.7502 0.5706 0.2767 0.086 Uiso 1 1 calc R . . C12 C 0.8562(4) 0.6216(4) 0.3553(3) 0.0790(14) Uani 1 1 d . . . H12A H 0.8350 0.5700 0.3985 0.095 Uiso 1 1 calc R . . H12B H 0.9202 0.6134 0.3533 0.095 Uiso 1 1 calc R . . C13 C 0.8323(5) 0.7371(4) 0.3706(2) 0.099(2) Uani 1 1 d . . . H13A H 0.8731 0.7725 0.4130 0.119 Uiso 1 1 calc R . . H13B H 0.7723 0.7417 0.3901 0.119 Uiso 1 1 calc R . . C14 C 0.8381(3) 0.7960(3) 0.2852(2) 0.0643(12) Uani 1 1 d . . . H14A H 0.7991 0.8630 0.2804 0.077 Uiso 1 1 calc R . . H14B H 0.8986 0.8204 0.2762 0.077 Uiso 1 1 calc R . . C15 C 0.8927(2) 0.9414(3) -0.1132(2) 0.0458(8) Uani 1 1 d . . . H15A H 0.9138 0.8988 -0.1612 0.055 Uiso 1 1 calc R . . H15B H 0.9272 0.9184 -0.0621 0.055 Uiso 1 1 calc R . . C16 C 0.8990(3) 1.0689(3) -0.1272(3) 0.0629(11) Uani 1 1 d . . . H16A H 0.8894 1.0879 -0.1870 0.075 Uiso 1 1 calc R . . H16B H 0.9566 1.0984 -0.1067 0.075 Uiso 1 1 calc R . . C17 C 0.8265(3) 1.1172(3) -0.0768(3) 0.0582(10) Uani 1 1 d . . . H17A H 0.8455 1.1241 -0.0171 0.070 Uiso 1 1 calc R . . H17B H 0.8073 1.1927 -0.0981 0.070 Uiso 1 1 calc R . . C18 C 0.7546(2) 1.0296(3) -0.0896(2) 0.0418(8) Uani 1 1 d . . . H18A H 0.7200 1.0245 -0.0396 0.050 Uiso 1 1 calc R . . H18B H 0.7151 1.0501 -0.1381 0.050 Uiso 1 1 calc R . . C19 C 0.7060(2) 0.4905(3) -0.1274(2) 0.0495(9) Uani 1 1 d . . . H19A H 0.7584 0.4786 -0.0896 0.059 Uiso 1 1 calc R . . H19B H 0.7228 0.4828 -0.1857 0.059 Uiso 1 1 calc R . . C20 C 0.6352(3) 0.4057(4) -0.1088(3) 0.0742(13) Uani 1 1 d . . . H20A H 0.6377 0.3380 -0.1452 0.089 Uiso 1 1 calc R . . H20B H 0.6405 0.3811 -0.0498 0.089 Uiso 1 1 calc R . . C21 C 0.5517(3) 0.4716(4) -0.1270(3) 0.0742(13) Uani 1 1 d . . . H21A H 0.5349 0.4716 -0.1874 0.089 Uiso 1 1 calc R . . H21B H 0.5033 0.4397 -0.0962 0.089 Uiso 1 1 calc R . . C22 C 0.5755(2) 0.5892(3) -0.0968(3) 0.0523(9) Uani 1 1 d . . . H22A H 0.5394 0.6471 -0.1273 0.063 Uiso 1 1 calc R . . H22B H 0.5669 0.5966 -0.0365 0.063 Uiso 1 1 calc 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 Ti1 0.0243(3) 0.0333(3) 0.0197(3) 0.0012(2) 0.00025(19) 0.0040(2) Ti2 0.0254(3) 0.0373(3) 0.0189(3) 0.0011(2) -0.0005(2) 0.0024(2) Cl1 0.0426(4) 0.0353(4) 0.0332(4) -0.0004(3) 0.0011(3) -0.0015(3) Cl2 0.0537(5) 0.0383(4) 0.0327(4) 0.0025(3) -0.0026(4) -0.0081(4) Cl3 0.0534(5) 0.0663(6) 0.0312(4) -0.0107(4) 0.0162(4) -0.0074(4) Cl4 0.0411(5) 0.0580(5) 0.0413(5) 0.0091(4) -0.0180(4) 0.0029(4) N1 0.0319(14) 0.0473(16) 0.0264(13) 0.0002(11) 0.0047(11) 0.0026(12) N2 0.0243(12) 0.0386(14) 0.0256(12) 0.0020(10) 0.0002(10) 0.0040(11) N3 0.0278(13) 0.0389(14) 0.0283(13) -0.0023(11) -0.0037(10) 0.0077(11) N4 0.0252(12) 0.0379(14) 0.0255(12) -0.0009(10) 0.0020(10) 0.0053(10) O1 0.0448(12) 0.0340(11) 0.0226(10) 0.0022(8) -0.0030(9) 0.0013(9) O2 0.0286(11) 0.0396(12) 0.0359(12) 0.0027(9) 0.0018(9) -0.0005(9) O3 0.0306(11) 0.0405(12) 0.0385(12) -0.0031(10) 0.0034(9) -0.0018(9) C1 0.0280(15) 0.0335(16) 0.0282(15) -0.0020(12) 0.0017(12) 0.0004(12) C2 0.0298(17) 0.056(2) 0.0432(19) -0.0058(16) -0.0045(14) 0.0106(15) C3 0.0288(18) 0.078(3) 0.066(3) -0.011(2) 0.0082(17) 0.0131(18) C4 0.041(2) 0.082(3) 0.049(2) -0.010(2) 0.0189(17) 0.0045(19) C5 0.046(2) 0.072(3) 0.0316(18) -0.0023(17) 0.0106(15) 0.0005(18) C6 0.0263(15) 0.0300(15) 0.0305(16) -0.0012(12) -0.0005(12) 0.0029(12) C7 0.0364(17) 0.0441(19) 0.0353(17) -0.0016(14) 0.0064(14) 0.0062(15) C8 0.0272(17) 0.053(2) 0.059(2) -0.0045(18) 0.0046(15) 0.0069(15) C9 0.0307(18) 0.052(2) 0.055(2) -0.0075(17) -0.0091(15) 0.0083(15) C10 0.0361(18) 0.0446(19) 0.0357(17) -0.0041(14) -0.0105(14) 0.0088(14) C11 0.116(4) 0.060(3) 0.036(2) 0.0174(18) -0.022(2) -0.029(3) C12 0.115(4) 0.074(3) 0.045(2) 0.014(2) -0.021(2) -0.013(3) C13 0.198(6) 0.073(3) 0.022(2) -0.003(2) -0.022(3) 0.039(4) C14 0.120(4) 0.041(2) 0.0295(19) -0.0041(16) -0.018(2) 0.005(2) C15 0.0328(18) 0.053(2) 0.052(2) 0.0017(17) 0.0080(15) -0.0057(15) C16 0.053(2) 0.059(3) 0.078(3) 0.008(2) 0.008(2) -0.016(2) C17 0.058(2) 0.045(2) 0.071(3) 0.0000(19) -0.005(2) -0.0012(18) C18 0.0450(19) 0.0385(18) 0.0421(19) 0.0047(15) 0.0042(15) 0.0069(15) C19 0.060(2) 0.040(2) 0.048(2) -0.0079(16) 0.0024(17) 0.0059(17) C20 0.110(4) 0.047(2) 0.068(3) -0.014(2) 0.024(3) -0.018(3) C21 0.072(3) 0.080(3) 0.073(3) -0.015(2) 0.021(2) -0.036(3) C22 0.0361(19) 0.060(2) 0.061(2) -0.0010(19) 0.0071(17) -0.0079(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N2 2.066(2) . ? Ti1 N4 2.084(2) . ? Ti1 N3 2.190(2) . ? Ti1 N1 2.208(3) . ? Ti1 O1 2.243(2) . ? Ti1 Cl1 2.3308(12) . ? Ti1 Cl2 2.3385(12) . ? Ti1 Ti2 3.0057(13) . ? Ti2 N4 1.855(2) . ? Ti2 N2 1.869(2) . ? Ti2 O2 2.103(2) . ? Ti2 O3 2.121(2) . ? Ti2 Cl3 2.4141(11) . ? Ti2 Cl4 2.4392(11) . ? N1 C5 1.339(4) . ? N1 C1 1.347(4) . ? N2 C1 1.361(4) . ? N3 C10 1.335(4) . ? N3 C6 1.347(4) . ? N4 C6 1.369(4) . ? O1 C14 1.436(4) . ? O1 C11 1.458(4) . ? O2 C18 1.455(4) . ? O2 C15 1.461(4) . ? O3 C22 1.449(4) . ? O3 C19 1.453(4) . ? C1 C2 1.388(4) . ? C2 C3 1.369(5) . ? C2 H2 0.9400 . ? C3 C4 1.385(6) . ? C3 H3 0.9400 . ? C4 C5 1.360(5) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C6 C7 1.391(4) . ? C7 C8 1.368(5) . ? C7 H7 0.9400 . ? C8 C9 1.390(5) . ? C8 H8 0.9400 . ? C9 C10 1.366(5) . ? C9 H9 0.9400 . ? C10 H10 0.9400 . ? C11 C12 1.510(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.418(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 C14 1.530(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.504(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C17 1.508(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 C18 1.499(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 C20 1.502(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.497(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C22 1.488(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ti1 N4 75.36(9) . . ? N2 Ti1 N3 137.37(9) . . ? N4 Ti1 N3 62.22(9) . . ? N2 Ti1 N1 62.25(9) . . ? N4 Ti1 N1 137.45(9) . . ? N3 Ti1 N1 160.33(9) . . ? N2 Ti1 O1 142.19(9) . . ? N4 Ti1 O1 142.45(9) . . ? N3 Ti1 O1 80.30(8) . . ? N1 Ti1 O1 80.02(9) . . ? N2 Ti1 Cl1 92.41(8) . . ? N4 Ti1 Cl1 95.24(7) . . ? N3 Ti1 Cl1 87.64(7) . . ? N1 Ti1 Cl1 90.26(8) . . ? O1 Ti1 Cl1 84.90(6) . . ? N2 Ti1 Cl2 95.62(7) . . ? N4 Ti1 Cl2 92.59(7) . . ? N3 Ti1 Cl2 90.50(8) . . ? N1 Ti1 Cl2 88.18(8) . . ? O1 Ti1 Cl2 85.08(6) . . ? Cl1 Ti1 Cl2 169.98(3) . . ? N2 Ti1 Ti2 37.83(7) . . ? N4 Ti1 Ti2 37.53(7) . . ? N3 Ti1 Ti2 99.68(7) . . ? N1 Ti1 Ti2 99.99(7) . . ? O1 Ti1 Ti2 179.89(7) . . ? Cl1 Ti1 Ti2 95.21(3) . . ? Cl2 Ti1 Ti2 94.82(3) . . ? N4 Ti2 N2 85.85(10) . . ? N4 Ti2 O2 90.88(10) . . ? N2 Ti2 O2 95.33(10) . . ? N4 Ti2 O3 97.89(10) . . ? N2 Ti2 O3 90.71(10) . . ? O2 Ti2 O3 169.69(8) . . ? N4 Ti2 Cl3 92.01(8) . . ? N2 Ti2 Cl3 175.60(8) . . ? O2 Ti2 Cl3 88.54(6) . . ? O3 Ti2 Cl3 85.77(6) . . ? N4 Ti2 Cl4 175.20(8) . . ? N2 Ti2 Cl4 92.06(8) . . ? O2 Ti2 Cl4 85.00(6) . . ? O3 Ti2 Cl4 86.44(7) . . ? Cl3 Ti2 Cl4 90.36(4) . . ? N4 Ti2 Ti1 43.17(7) . . ? N2 Ti2 Ti1 42.68(7) . . ? O2 Ti2 Ti1 94.70(6) . . ? O3 Ti2 Ti1 95.40(6) . . ? Cl3 Ti2 Ti1 135.01(4) . . ? Cl4 Ti2 Ti1 134.63(3) . . ? C5 N1 C1 119.8(3) . . ? C5 N1 Ti1 149.0(2) . . ? C1 N1 Ti1 91.16(17) . . ? C1 N2 Ti2 162.9(2) . . ? C1 N2 Ti1 97.05(17) . . ? Ti2 N2 Ti1 99.48(11) . . ? C10 N3 C6 120.5(3) . . ? C10 N3 Ti1 146.4(2) . . ? C6 N3 Ti1 92.24(16) . . ? C6 N4 Ti2 162.8(2) . . ? C6 N4 Ti1 96.27(17) . . ? Ti2 N4 Ti1 99.30(10) . . ? C14 O1 C11 108.7(2) . . ? C14 O1 Ti1 126.56(19) . . ? C11 O1 Ti1 124.58(19) . . ? C18 O2 C15 109.8(2) . . ? C18 O2 Ti2 124.13(18) . . ? C15 O2 Ti2 125.64(19) . . ? C22 O3 C19 109.3(3) . . ? C22 O3 Ti2 124.0(2) . . ? C19 O3 Ti2 125.82(19) . . ? N1 C1 N2 109.5(2) . . ? N1 C1 C2 121.8(3) . . ? N2 C1 C2 128.7(3) . . ? C3 C2 C1 117.4(3) . . ? C3 C2 H2 121.3 . . ? C1 C2 H2 121.3 . . ? C2 C3 C4 120.6(3) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 119.2(3) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 121.2(3) . . ? N1 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? N3 C6 N4 108.9(2) . . ? N3 C6 C7 121.5(3) . . ? N4 C6 C7 129.5(3) . . ? C8 C7 C6 117.5(3) . . ? C8 C7 H7 121.2 . . ? C6 C7 H7 121.2 . . ? C7 C8 C9 120.5(3) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 119.2(3) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? N3 C10 C9 120.7(3) . . ? N3 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? O1 C11 C12 105.0(3) . . ? O1 C11 H11A 110.7 . . ? C12 C11 H11A 110.7 . . ? O1 C11 H11B 110.7 . . ? C12 C11 H11B 110.7 . . ? H11A C11 H11B 108.8 . . ? C13 C12 C11 102.5(4) . . ? C13 C12 H12A 111.3 . . ? C11 C12 H12A 111.3 . . ? C13 C12 H12B 111.3 . . ? C11 C12 H12B 111.3 . . ? H12A C12 H12B 109.2 . . ? C12 C13 C14 104.1(4) . . ? C12 C13 H13A 110.9 . . ? C14 C13 H13A 110.9 . . ? C12 C13 H13B 110.9 . . ? C14 C13 H13B 110.9 . . ? H13A C13 H13B 109.0 . . ? O1 C14 C13 103.2(3) . . ? O1 C14 H14A 111.1 . . ? C13 C14 H14A 111.1 . . ? O1 C14 H14B 111.1 . . ? C13 C14 H14B 111.1 . . ? H14A C14 H14B 109.1 . . ? O2 C15 C16 104.1(3) . . ? O2 C15 H15A 110.9 . . ? C16 C15 H15A 110.9 . . ? O2 C15 H15B 110.9 . . ? C16 C15 H15B 110.9 . . ? H15A C15 H15B 109.0 . . ? C15 C16 C17 103.5(3) . . ? C15 C16 H16A 111.1 . . ? C17 C16 H16A 111.1 . . ? C15 C16 H16B 111.1 . . ? C17 C16 H16B 111.1 . . ? H16A C16 H16B 109.0 . . ? C18 C17 C16 102.9(3) . . ? C18 C17 H17A 111.2 . . ? C16 C17 H17A 111.2 . . ? C18 C17 H17B 111.2 . . ? C16 C17 H17B 111.2 . . ? H17A C17 H17B 109.1 . . ? O2 C18 C17 105.7(3) . . ? O2 C18 H18A 110.6 . . ? C17 C18 H18A 110.6 . . ? O2 C18 H18B 110.6 . . ? C17 C18 H18B 110.6 . . ? H18A C18 H18B 108.7 . . ? O3 C19 C20 105.2(3) . . ? O3 C19 H19A 110.7 . . ? C20 C19 H19A 110.7 . . ? O3 C19 H19B 110.7 . . ? C20 C19 H19B 110.7 . . ? H19A C19 H19B 108.8 . . ? C21 C20 C19 103.6(3) . . ? C21 C20 H20A 111.0 . . ? C19 C20 H20A 111.0 . . ? C21 C20 H20B 111.0 . . ? C19 C20 H20B 111.0 . . ? H20A C20 H20B 109.0 . . ? C22 C21 C20 102.7(3) . . ? C22 C21 H21A 111.2 . . ? C20 C21 H21A 111.2 . . ? C22 C21 H21B 111.2 . . ? C20 C21 H21B 111.2 . . ? H21A C21 H21B 109.1 . . ? O3 C22 C21 105.1(3) . . ? O3 C22 H22A 110.7 . . ? C21 C22 H22A 110.7 . . ? O3 C22 H22B 110.7 . . ? C21 C22 H22B 110.7 . . ? H22A C22 H22B 108.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ti1 Ti2 N4 179.05(16) . . . . ? N3 Ti1 Ti2 N4 3.35(13) . . . . ? N1 Ti1 Ti2 N4 -176.99(14) . . . . ? O1 Ti1 Ti2 N4 -81(56) . . . . ? Cl1 Ti1 Ti2 N4 91.83(12) . . . . ? Cl2 Ti1 Ti2 N4 -87.99(12) . . . . ? N4 Ti1 Ti2 N2 -179.05(16) . . . . ? N3 Ti1 Ti2 N2 -175.70(13) . . . . ? N1 Ti1 Ti2 N2 3.96(13) . . . . ? O1 Ti1 Ti2 N2 100(39) . . . . ? Cl1 Ti1 Ti2 N2 -87.22(12) . . . . ? Cl2 Ti1 Ti2 N2 92.96(12) . . . . ? N2 Ti1 Ti2 O2 92.77(13) . . . . ? N4 Ti1 Ti2 O2 -86.27(13) . . . . ? N3 Ti1 Ti2 O2 -82.93(9) . . . . ? N1 Ti1 Ti2 O2 96.74(9) . . . . ? O1 Ti1 Ti2 O2 -167(100) . . . . ? Cl1 Ti1 Ti2 O2 5.56(6) . . . . ? Cl2 Ti1 Ti2 O2 -174.26(6) . . . . ? N2 Ti1 Ti2 O3 -85.18(13) . . . . ? N4 Ti1 Ti2 O3 95.78(13) . . . . ? N3 Ti1 Ti2 O3 99.12(9) . . . . ? N1 Ti1 Ti2 O3 -81.21(9) . . . . ? O1 Ti1 Ti2 O3 15(39) . . . . ? Cl1 Ti1 Ti2 O3 -172.39(6) . . . . ? Cl2 Ti1 Ti2 O3 7.79(6) . . . . ? N2 Ti1 Ti2 Cl3 -174.59(12) . . . . ? N4 Ti1 Ti2 Cl3 6.36(12) . . . . ? N3 Ti1 Ti2 Cl3 9.71(8) . . . . ? N1 Ti1 Ti2 Cl3 -170.62(8) . . . . ? O1 Ti1 Ti2 Cl3 -74(56) . . . . ? Cl1 Ti1 Ti2 Cl3 98.19(5) . . . . ? Cl2 Ti1 Ti2 Cl3 -81.62(5) . . . . ? N2 Ti1 Ti2 Cl4 5.16(12) . . . . ? N4 Ti1 Ti2 Cl4 -173.89(12) . . . . ? N3 Ti1 Ti2 Cl4 -170.54(8) . . . . ? N1 Ti1 Ti2 Cl4 9.12(9) . . . . ? O1 Ti1 Ti2 Cl4 106(39) . . . . ? Cl1 Ti1 Ti2 Cl4 -82.06(5) . . . . ? Cl2 Ti1 Ti2 Cl4 98.12(5) . . . . ? N2 Ti1 N1 C5 178.8(5) . . . . ? N4 Ti1 N1 C5 173.3(4) . . . . ? N3 Ti1 N1 C5 -5.0(7) . . . . ? O1 Ti1 N1 C5 -3.9(5) . . . . ? Cl1 Ti1 N1 C5 -88.6(5) . . . . ? Cl2 Ti1 N1 C5 81.4(5) . . . . ? Ti2 Ti1 N1 C5 176.0(5) . . . . ? N2 Ti1 N1 C1 0.05(17) . . . . ? N4 Ti1 N1 C1 -5.4(3) . . . . ? N3 Ti1 N1 C1 176.3(3) . . . . ? O1 Ti1 N1 C1 177.42(19) . . . . ? Cl1 Ti1 N1 C1 92.64(17) . . . . ? Cl2 Ti1 N1 C1 -97.27(17) . . . . ? Ti2 Ti1 N1 C1 -2.69(18) . . . . ? N4 Ti2 N2 C1 -165.4(7) . . . . ? O2 Ti2 N2 C1 104.1(7) . . . . ? O3 Ti2 N2 C1 -67.6(7) . . . . ? Cl3 Ti2 N2 C1 -104.5(11) . . . . ? Cl4 Ti2 N2 C1 18.9(7) . . . . ? Ti1 Ti2 N2 C1 -164.8(8) . . . . ? N4 Ti2 N2 Ti1 -0.65(11) . . . . ? O2 Ti2 N2 Ti1 -91.16(10) . . . . ? O3 Ti2 N2 Ti1 97.20(10) . . . . ? Cl3 Ti2 N2 Ti1 60.3(10) . . . . ? Cl4 Ti2 N2 Ti1 -176.33(8) . . . . ? N4 Ti1 N2 C1 176.1(2) . . . . ? N3 Ti1 N2 C1 -178.20(17) . . . . ? N1 Ti1 N2 C1 -0.05(17) . . . . ? O1 Ti1 N2 C1 -4.3(3) . . . . ? Cl1 Ti1 N2 C1 -89.07(17) . . . . ? Cl2 Ti1 N2 C1 84.91(17) . . . . ? Ti2 Ti1 N2 C1 175.5(2) . . . . ? N4 Ti1 N2 Ti2 0.60(10) . . . . ? N3 Ti1 N2 Ti2 6.26(19) . . . . ? N1 Ti1 N2 Ti2 -175.59(15) . . . . ? O1 Ti1 N2 Ti2 -179.83(9) . . . . ? Cl1 Ti1 N2 Ti2 95.39(9) . . . . ? Cl2 Ti1 N2 Ti2 -90.62(9) . . . . ? N2 Ti1 N3 C10 165.0(4) . . . . ? N4 Ti1 N3 C10 171.2(4) . . . . ? N1 Ti1 N3 C10 -10.2(6) . . . . ? O1 Ti1 N3 C10 -11.3(4) . . . . ? Cl1 Ti1 N3 C10 74.0(4) . . . . ? Cl2 Ti1 N3 C10 -96.2(4) . . . . ? Ti2 Ti1 N3 C10 168.9(4) . . . . ? N2 Ti1 N3 C6 -2.5(2) . . . . ? N4 Ti1 N3 C6 3.66(17) . . . . ? N1 Ti1 N3 C6 -177.7(3) . . . . ? O1 Ti1 N3 C6 -178.76(18) . . . . ? Cl1 Ti1 N3 C6 -93.53(17) . . . . ? Cl2 Ti1 N3 C6 96.32(17) . . . . ? Ti2 Ti1 N3 C6 1.35(18) . . . . ? N2 Ti2 N4 C6 -153.9(7) . . . . ? O2 Ti2 N4 C6 -58.6(7) . . . . ? O3 Ti2 N4 C6 115.9(7) . . . . ? Cl3 Ti2 N4 C6 29.9(7) . . . . ? Cl4 Ti2 N4 C6 -89.6(12) . . . . ? Ti1 Ti2 N4 C6 -154.6(8) . . . . ? N2 Ti2 N4 Ti1 0.65(11) . . . . ? O2 Ti2 N4 Ti1 95.93(10) . . . . ? O3 Ti2 N4 Ti1 -89.50(10) . . . . ? Cl3 Ti2 N4 Ti1 -175.50(8) . . . . ? Cl4 Ti2 N4 Ti1 64.9(10) . . . . ? N2 Ti1 N4 C6 172.05(19) . . . . ? N3 Ti1 N4 C6 -3.62(16) . . . . ? N1 Ti1 N4 C6 177.04(17) . . . . ? O1 Ti1 N4 C6 -7.5(3) . . . . ? Cl1 Ti1 N4 C6 80.93(17) . . . . ? Cl2 Ti1 N4 C6 -92.82(17) . . . . ? Ti2 Ti1 N4 C6 172.7(2) . . . . ? N2 Ti1 N4 Ti2 -0.60(10) . . . . ? N3 Ti1 N4 Ti2 -176.27(15) . . . . ? N1 Ti1 N4 Ti2 4.4(2) . . . . ? O1 Ti1 N4 Ti2 179.82(10) . . . . ? Cl1 Ti1 N4 Ti2 -91.73(10) . . . . ? Cl2 Ti1 N4 Ti2 94.53(10) . . . . ? N2 Ti1 O1 C14 -77.9(3) . . . . ? N4 Ti1 O1 C14 101.4(3) . . . . ? N3 Ti1 O1 C14 97.9(3) . . . . ? N1 Ti1 O1 C14 -81.7(3) . . . . ? Cl1 Ti1 O1 C14 9.5(3) . . . . ? Cl2 Ti1 O1 C14 -170.7(3) . . . . ? Ti2 Ti1 O1 C14 -178(100) . . . . ? N2 Ti1 O1 C11 106.9(3) . . . . ? N4 Ti1 O1 C11 -73.8(3) . . . . ? N3 Ti1 O1 C11 -77.3(3) . . . . ? N1 Ti1 O1 C11 103.1(3) . . . . ? Cl1 Ti1 O1 C11 -165.8(3) . . . . ? Cl2 Ti1 O1 C11 14.1(3) . . . . ? Ti2 Ti1 O1 C11 7(39) . . . . ? N4 Ti2 O2 C18 -130.7(2) . . . . ? N2 Ti2 O2 C18 -44.8(2) . . . . ? O3 Ti2 O2 C18 80.9(5) . . . . ? Cl3 Ti2 O2 C18 137.3(2) . . . . ? Cl4 Ti2 O2 C18 46.8(2) . . . . ? Ti1 Ti2 O2 C18 -87.7(2) . . . . ? N4 Ti2 O2 C15 40.8(2) . . . . ? N2 Ti2 O2 C15 126.7(2) . . . . ? O3 Ti2 O2 C15 -107.6(5) . . . . ? Cl3 Ti2 O2 C15 -51.2(2) . . . . ? Cl4 Ti2 O2 C15 -141.7(2) . . . . ? Ti1 Ti2 O2 C15 83.9(2) . . . . ? N4 Ti2 O3 C22 126.8(2) . . . . ? N2 Ti2 O3 C22 40.9(2) . . . . ? O2 Ti2 O3 C22 -85.1(5) . . . . ? Cl3 Ti2 O3 C22 -141.8(2) . . . . ? Cl4 Ti2 O3 C22 -51.1(2) . . . . ? Ti1 Ti2 O3 C22 83.4(2) . . . . ? N4 Ti2 O3 C19 -41.5(2) . . . . ? N2 Ti2 O3 C19 -127.4(2) . . . . ? O2 Ti2 O3 C19 106.6(5) . . . . ? Cl3 Ti2 O3 C19 49.9(2) . . . . ? Cl4 Ti2 O3 C19 140.5(2) . . . . ? Ti1 Ti2 O3 C19 -84.9(2) . . . . ? C5 N1 C1 N2 -179.3(3) . . . . ? Ti1 N1 C1 N2 -0.1(2) . . . . ? C5 N1 C1 C2 0.3(5) . . . . ? Ti1 N1 C1 C2 179.5(3) . . . . ? Ti2 N2 C1 N1 165.0(6) . . . . ? Ti1 N2 C1 N1 0.1(3) . . . . ? Ti2 N2 C1 C2 -14.6(10) . . . . ? Ti1 N2 C1 C2 -179.5(3) . . . . ? N1 C1 C2 C3 0.2(5) . . . . ? N2 C1 C2 C3 179.7(3) . . . . ? C1 C2 C3 C4 -0.4(6) . . . . ? C2 C3 C4 C5 0.2(6) . . . . ? C1 N1 C5 C4 -0.5(5) . . . . ? Ti1 N1 C5 C4 -179.0(3) . . . . ? C3 C4 C5 N1 0.3(6) . . . . ? C10 N3 C6 N4 -177.2(3) . . . . ? Ti1 N3 C6 N4 -5.2(2) . . . . ? C10 N3 C6 C7 0.4(5) . . . . ? Ti1 N3 C6 C7 172.4(3) . . . . ? Ti2 N4 C6 N3 160.3(6) . . . . ? Ti1 N4 C6 N3 5.5(2) . . . . ? Ti2 N4 C6 C7 -17.1(10) . . . . ? Ti1 N4 C6 C7 -171.8(3) . . . . ? N3 C6 C7 C8 1.0(5) . . . . ? N4 C6 C7 C8 178.1(3) . . . . ? C6 C7 C8 C9 -1.7(5) . . . . ? C7 C8 C9 C10 1.0(5) . . . . ? C6 N3 C10 C9 -1.1(5) . . . . ? Ti1 N3 C10 C9 -166.6(3) . . . . ? C8 C9 C10 N3 0.4(5) . . . . ? C14 O1 C11 C12 -9.9(5) . . . . ? Ti1 O1 C11 C12 166.0(3) . . . . ? O1 C11 C12 C13 31.9(5) . . . . ? C11 C12 C13 C14 -40.5(6) . . . . ? C11 O1 C14 C13 -14.2(5) . . . . ? Ti1 O1 C14 C13 170.0(3) . . . . ? C12 C13 C14 O1 34.9(6) . . . . ? C18 O2 C15 C16 -15.3(4) . . . . ? Ti2 O2 C15 C16 172.1(2) . . . . ? O2 C15 C16 C17 32.5(4) . . . . ? C15 C16 C17 C18 -37.3(4) . . . . ? C15 O2 C18 C17 -8.1(4) . . . . ? Ti2 O2 C18 C17 164.6(2) . . . . ? C16 C17 C18 O2 28.1(4) . . . . ? C22 O3 C19 C20 -6.1(4) . . . . ? Ti2 O3 C19 C20 163.6(2) . . . . ? O3 C19 C20 C21 26.9(4) . . . . ? C19 C20 C21 C22 -37.1(4) . . . . ? C19 O3 C22 C21 -17.4(4) . . . . ? Ti2 O3 C22 C21 172.7(2) . . . . ? C20 C21 C22 O3 33.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.800 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.063 #===end data_5 _database_code_depnum_ccdc_archive 'CCDC 858903' #TrackingRef '3-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 379-381 _chemical_formula_moiety 'C17 H32 Cl4 Li N3 O2 Si Zr' _chemical_formula_sum 'C17 H32 Cl4 Li N3 O2 Si Zr' _chemical_formula_weight 578.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.139(3) _cell_length_b 16.253(4) _cell_length_c 31.206(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.317(6) _cell_angle_gamma 90.00 _cell_volume 5590(2) _cell_formula_units_Z 8 _cell_measurement_temperature 238(2) _cell_measurement_reflns_used 2877 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 17.62 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7312 _exptl_absorpt_correction_T_max 0.8508 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 238(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD AREA DETECOR' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24474 _diffrn_reflns_av_R_equivalents 0.1231 _diffrn_reflns_av_sigmaI/netI 0.1520 _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 -37 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10216 _reflns_number_gt 4184 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1807P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10216 _refine_ls_number_parameters 531 _refine_ls_number_restraints 521 _refine_ls_R_factor_all 0.2175 _refine_ls_R_factor_gt 0.0912 _refine_ls_wR_factor_ref 0.3333 _refine_ls_wR_factor_gt 0.2584 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr2 Zr -0.02371(11) 0.04974(6) 0.36969(4) 0.0645(4) Uani 1 1 d . . . Cl5 Cl 0.1495(3) 0.0085(2) 0.33365(13) 0.1004(12) Uani 1 1 d . . . Cl6 Cl -0.1951(3) 0.0903(2) 0.40726(12) 0.0944(11) Uani 1 1 d . . . Cl7 Cl 0.1234(4) 0.1118(2) 0.43129(12) 0.1065(13) Uani 1 1 d . . . Cl8 Cl -0.0144(4) 0.1962(2) 0.33918(13) 0.1020(12) Uani 1 1 d . . . N4 N 0.0057(9) -0.0594(6) 0.4194(3) 0.072(3) Uani 1 1 d . . . N5 N -0.1042(9) -0.0680(5) 0.3556(3) 0.068(3) Uani 1 1 d . . . N6 N -0.1678(10) 0.0407(5) 0.2996(3) 0.075(3) Uani 1 1 d . . . Si2 Si -0.2080(4) -0.0627(2) 0.31019(13) 0.0875(12) Uani 1 1 d . . . Li2 Li 0.153(2) 0.2336(18) 0.3909(13) 0.144(14) Uani 1 1 d . . . O1 O 0.2984(12) 0.7316(8) 0.3790(5) 0.151(3) Uani 1 1 d U . . O2 O 0.5033(14) 0.8290(9) 0.4300(5) 0.179(4) Uani 1 1 d DU . . C18 C -0.0693(14) -0.1073(8) 0.3917(5) 0.084(3) Uani 1 1 d U . . C19 C -0.0944(14) -0.1847(8) 0.4068(4) 0.088(3) Uani 1 1 d U . . H19 H -0.1478 -0.2194 0.3890 0.105 Uiso 1 1 calc R . . C20 C -0.0432(13) -0.2120(8) 0.4471(4) 0.092(3) Uani 1 1 d U . . H20 H -0.0579 -0.2656 0.4564 0.110 Uiso 1 1 calc R . . C21 C 0.0291(14) -0.1593(8) 0.4731(5) 0.093(3) Uani 1 1 d U . . H21 H 0.0617 -0.1757 0.5013 0.112 Uiso 1 1 calc R . . C22 C 0.0544(14) -0.0838(8) 0.4589(5) 0.088(3) Uani 1 1 d U . . H22 H 0.1063 -0.0485 0.4769 0.106 Uiso 1 1 calc R . . C23 C -0.3595(16) -0.0691(10) 0.3251(6) 0.129(4) Uani 1 1 d U . . H23A H -0.3666 -0.1191 0.3416 0.193 Uiso 1 1 calc R . . H23B H -0.4190 -0.0698 0.2992 0.193 Uiso 1 1 calc R . . H23C H -0.3737 -0.0218 0.3427 0.193 Uiso 1 1 calc R . . C24 C -0.1820(18) -0.1309(10) 0.2676(5) 0.135(5) Uani 1 1 d U . . H24A H -0.1299 -0.1042 0.2494 0.202 Uiso 1 1 calc R . . H24B H -0.2588 -0.1448 0.2503 0.202 Uiso 1 1 calc R . . H24C H -0.1431 -0.1806 0.2799 0.202 Uiso 1 1 calc R . . C25 C -0.2715(15) 0.0997(9) 0.2936(5) 0.117(4) Uani 1 1 d U . . H25A H -0.2422 0.1539 0.2873 0.175 Uiso 1 1 calc R . . H25B H -0.3083 0.1019 0.3199 0.175 Uiso 1 1 calc R . . H25C H -0.3312 0.0815 0.2698 0.175 Uiso 1 1 calc R . . C26 C -0.1029(16) 0.0508(10) 0.2602(5) 0.115(4) Uani 1 1 d U . . H26A H -0.1282 0.0075 0.2395 0.173 Uiso 1 1 calc R . . H26B H -0.0159 0.0476 0.2691 0.173 Uiso 1 1 calc R . . H26C H -0.1233 0.1039 0.2469 0.173 Uiso 1 1 calc R . . C27 C 0.4044(18) 0.1787(11) 0.3908(6) 0.135(2) Uani 1 1 d U . . H27A H 0.4584 0.2037 0.4149 0.162 Uiso 1 1 calc R . . H27B H 0.3723 0.1269 0.4006 0.162 Uiso 1 1 calc R . . C28 C 0.4650(18) 0.1661(11) 0.3542(6) 0.136(3) Uani 1 1 d U . . H28A H 0.4397 0.1133 0.3407 0.163 Uiso 1 1 calc R . . H28B H 0.5527 0.1638 0.3637 0.163 Uiso 1 1 calc R . . C29 C 0.4368(17) 0.2360(11) 0.3201(6) 0.135(3) Uani 1 1 d U . . H29A H 0.4878 0.2846 0.3272 0.162 Uiso 1 1 calc R . . H29B H 0.4428 0.2174 0.2906 0.162 Uiso 1 1 calc R . . C30 C 0.3198(18) 0.2485(12) 0.3266(7) 0.146(3) Uani 1 1 d U . . H30A H 0.2660 0.2109 0.3083 0.175 Uiso 1 1 calc R . . H30B H 0.2954 0.3050 0.3186 0.175 Uiso 1 1 calc R . . C31 C 0.2444(19) 0.3960(12) 0.4262(7) 0.154(3) Uani 1 1 d DU . . H31A H 0.3232 0.3709 0.4367 0.185 Uiso 1 1 calc R . . H31B H 0.2489 0.4237 0.3985 0.185 Uiso 1 1 calc R . . C32 C 0.2095(17) 0.4504(12) 0.4565(7) 0.162(3) Uani 1 1 d DU . . H32A H 0.2639 0.4444 0.4840 0.194 Uiso 1 1 calc R . . H32B H 0.2163 0.5070 0.4463 0.194 Uiso 1 1 calc R . . C33 C 0.0907(18) 0.4355(13) 0.4632(7) 0.163(3) Uani 1 1 d DU . . H33A H 0.0357 0.4761 0.4477 0.195 Uiso 1 1 calc R . . H33B H 0.0840 0.4387 0.4941 0.195 Uiso 1 1 calc R . . C34 C 0.061(2) 0.3547(13) 0.4471(7) 0.160(3) Uani 1 1 d U . . H34A H 0.0621 0.3158 0.4712 0.192 Uiso 1 1 calc R . . H34B H -0.0205 0.3542 0.4302 0.192 Uiso 1 1 calc R . . Zr1 Zr 0.61926(10) 0.54661(6) 0.37174(3) 0.0586(4) Uani 1 1 d . . . Cl1 Cl 0.8195(3) 0.5903(2) 0.40844(12) 0.0912(11) Uani 1 1 d . . . Cl2 Cl 0.4172(3) 0.5051(2) 0.33602(13) 0.0974(11) Uani 1 1 d . . . Cl3 Cl 0.5208(4) 0.60548(19) 0.43468(11) 0.0939(12) Uani 1 1 d . . . Cl4 Cl 0.5799(4) 0.69278(18) 0.34154(12) 0.0928(11) Uani 1 1 d . . . N1 N 0.6256(8) 0.4367(5) 0.4197(3) 0.056(2) Uani 1 1 d . . . N2 N 0.6930(9) 0.4297(5) 0.3569(3) 0.065(3) Uani 1 1 d . . . N3 N 0.7061(8) 0.5409(5) 0.3011(3) 0.062(2) Uani 1 1 d . . . Si1 Si 0.7611(4) 0.4377(2) 0.31197(12) 0.0791(11) Uani 1 1 d . . . Li1 Li 0.458(2) 0.7299(12) 0.3959(8) 0.091(7) Uani 1 1 d . . . O3 O 0.3087(12) 0.2337(8) 0.3739(4) 0.141(3) Uani 1 1 d U . . O4 O 0.1447(13) 0.3330(8) 0.4217(5) 0.154(3) Uani 1 1 d U . . C1 C 0.6847(14) 0.3888(8) 0.3935(5) 0.094(2) Uani 1 1 d U . . C2 C 0.7264(15) 0.3108(9) 0.4074(5) 0.108(2) Uani 1 1 d U . . H2 H 0.7695 0.2783 0.3899 0.129 Uiso 1 1 calc R . . C3 C 0.7034(14) 0.2818(9) 0.4474(5) 0.105(3) Uani 1 1 d U . . H3 H 0.7305 0.2293 0.4571 0.126 Uiso 1 1 calc R . . C4 C 0.6418(14) 0.3297(9) 0.4722(5) 0.101(3) Uani 1 1 d U . . H4 H 0.6250 0.3100 0.4990 0.121 Uiso 1 1 calc R . . C5 C 0.6034(14) 0.4076(9) 0.4584(5) 0.100(3) Uani 1 1 d U . . H5 H 0.5615 0.4405 0.4761 0.120 Uiso 1 1 calc R . . C7 C 0.9323(15) 0.4354(10) 0.3247(5) 0.120(4) Uani 1 1 d U . . H7A H 0.9613 0.4876 0.3372 0.181 Uiso 1 1 calc R . . H7B H 0.9665 0.4258 0.2982 0.181 Uiso 1 1 calc R . . H7C H 0.9569 0.3914 0.3451 0.181 Uiso 1 1 calc R . . C6 C 0.7224(17) 0.3684(10) 0.2690(5) 0.127(4) Uani 1 1 d U . . H6A H 0.7330 0.3125 0.2798 0.191 Uiso 1 1 calc R . . H6B H 0.7744 0.3777 0.2471 0.191 Uiso 1 1 calc R . . H6C H 0.6384 0.3768 0.2565 0.191 Uiso 1 1 calc R . . C8 C 0.6143(15) 0.5489(9) 0.2633(4) 0.101(4) Uani 1 1 d U . . H8A H 0.5859 0.6054 0.2609 0.151 Uiso 1 1 calc R . . H8B H 0.5469 0.5126 0.2663 0.151 Uiso 1 1 calc R . . H8C H 0.6488 0.5341 0.2376 0.151 Uiso 1 1 calc R . . C9 C 0.8017(14) 0.6043(8) 0.2954(5) 0.108(4) Uani 1 1 d U . . H9A H 0.8185 0.6031 0.2658 0.162 Uiso 1 1 calc R . . H9B H 0.8753 0.5921 0.3150 0.162 Uiso 1 1 calc R . . H9C H 0.7725 0.6585 0.3019 0.162 Uiso 1 1 calc R . . C10 C 0.213(2) 0.6789(14) 0.3931(7) 0.172(3) Uani 1 1 d U . . H10A H 0.1773 0.7041 0.4169 0.207 Uiso 1 1 calc R . . H10B H 0.2508 0.6266 0.4033 0.207 Uiso 1 1 calc R . . C11 C 0.122(2) 0.6657(14) 0.3567(8) 0.174(4) Uani 1 1 d U . . H11A H 0.0419 0.6660 0.3660 0.208 Uiso 1 1 calc R . . H11B H 0.1344 0.6117 0.3440 0.208 Uiso 1 1 calc R . . C12 C 0.128(2) 0.7370(14) 0.3205(8) 0.172(4) Uani 1 1 d U . . H12A H 0.1137 0.7162 0.2907 0.206 Uiso 1 1 calc R . . H12B H 0.0756 0.7840 0.3238 0.206 Uiso 1 1 calc R . . C13 C 0.248(2) 0.7526(13) 0.3346(8) 0.166(3) Uani 1 1 d U . . H13A H 0.2613 0.8115 0.3308 0.199 Uiso 1 1 calc R . . H13B H 0.2955 0.7234 0.3154 0.199 Uiso 1 1 calc R . . C15 C 0.507(2) 0.9345(15) 0.4592(8) 0.212(5) Uani 1 1 d DU . . H15A H 0.4952 0.9216 0.4889 0.255 Uiso 1 1 calc R . . H15B H 0.5072 0.9945 0.4560 0.255 Uiso 1 1 calc R . . C16 C 0.632(2) 0.8991(14) 0.4504(9) 0.211(4) Uani 1 1 d DU . . H16A H 0.6399 0.8990 0.4195 0.253 Uiso 1 1 calc R . . H16B H 0.7011 0.9286 0.4667 0.253 Uiso 1 1 calc R . . C14 C 0.409(2) 0.8990(14) 0.4289(8) 0.192(4) Uani 1 1 d DU . . H14A H 0.3909 0.9277 0.4011 0.230 Uiso 1 1 calc R . . H14B H 0.3357 0.8852 0.4412 0.230 Uiso 1 1 calc R . . C17 C 0.619(2) 0.8178(14) 0.4669(7) 0.202(4) Uani 1 1 d DU . . H17A H 0.6015 0.8145 0.4967 0.243 Uiso 1 1 calc R . . H17B H 0.6795 0.7774 0.4607 0.243 Uiso 1 1 calc 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 Zr2 0.0763(8) 0.0455(6) 0.0726(8) -0.0049(5) 0.0140(6) 0.0006(5) Cl5 0.088(3) 0.106(3) 0.115(3) -0.002(2) 0.037(2) 0.012(2) Cl6 0.099(3) 0.080(2) 0.109(3) -0.0168(19) 0.034(2) 0.0142(19) Cl7 0.129(3) 0.091(3) 0.096(3) -0.015(2) 0.001(2) -0.031(2) Cl8 0.115(3) 0.0583(19) 0.130(3) 0.0127(19) 0.010(3) -0.0150(19) N4 0.086(7) 0.061(6) 0.070(7) 0.002(5) 0.012(6) 0.003(5) N5 0.094(7) 0.039(5) 0.069(7) 0.003(4) 0.008(6) 0.004(5) N6 0.092(7) 0.047(5) 0.086(7) 0.018(5) 0.015(6) 0.007(5) Si2 0.116(3) 0.053(2) 0.087(3) 0.0073(18) -0.007(3) -0.014(2) Li2 0.087(17) 0.11(2) 0.24(4) -0.09(2) 0.04(2) -0.030(16) O1 0.136(7) 0.125(7) 0.192(8) -0.003(7) 0.025(7) -0.012(6) O2 0.162(8) 0.148(8) 0.224(9) -0.039(7) 0.024(7) 0.024(6) C18 0.112(6) 0.062(5) 0.079(6) 0.000(5) 0.021(5) 0.008(5) C19 0.116(6) 0.068(5) 0.082(6) 0.010(5) 0.021(5) 0.001(5) C20 0.119(7) 0.073(5) 0.086(6) 0.013(5) 0.020(6) -0.001(5) C21 0.118(7) 0.075(5) 0.086(6) 0.012(5) 0.013(6) 0.005(5) C22 0.112(6) 0.071(5) 0.083(6) 0.006(5) 0.022(5) 0.006(5) C23 0.135(9) 0.102(8) 0.144(9) 0.021(7) 0.003(8) -0.020(7) C24 0.182(10) 0.102(8) 0.110(9) -0.015(7) -0.011(9) -0.011(8) C25 0.125(10) 0.088(8) 0.131(10) 0.003(8) 0.001(9) -0.004(8) C26 0.138(10) 0.106(9) 0.106(9) 0.009(7) 0.033(8) -0.012(8) C27 0.139(5) 0.123(4) 0.149(5) -0.004(4) 0.037(4) 0.005(4) C28 0.138(6) 0.122(5) 0.151(6) -0.005(5) 0.035(5) 0.009(5) C29 0.137(6) 0.122(5) 0.151(6) -0.007(5) 0.039(5) 0.002(5) C30 0.147(5) 0.133(5) 0.161(5) -0.003(5) 0.036(5) 0.004(5) C31 0.156(5) 0.133(5) 0.178(5) -0.022(4) 0.035(5) -0.014(4) C32 0.164(6) 0.140(5) 0.183(6) -0.030(5) 0.033(5) -0.017(5) C33 0.166(6) 0.143(6) 0.183(6) -0.032(5) 0.037(5) -0.012(5) C34 0.162(6) 0.140(6) 0.182(6) -0.028(5) 0.040(5) -0.017(5) Zr1 0.0722(8) 0.0427(6) 0.0644(8) 0.0020(5) 0.0215(6) 0.0048(5) Cl1 0.089(2) 0.082(2) 0.098(3) -0.0077(18) 0.000(2) -0.0146(18) Cl2 0.077(2) 0.104(3) 0.111(3) 0.006(2) 0.015(2) -0.010(2) Cl3 0.143(3) 0.0690(19) 0.080(2) 0.0026(16) 0.052(2) 0.036(2) Cl4 0.125(3) 0.0510(17) 0.111(3) 0.0175(16) 0.046(2) 0.0199(18) N1 0.061(6) 0.050(5) 0.058(6) 0.000(4) 0.015(5) -0.004(4) N2 0.087(7) 0.052(5) 0.064(6) -0.002(4) 0.032(5) 0.002(5) N3 0.071(6) 0.057(5) 0.059(6) 0.009(4) 0.010(5) -0.002(5) Si1 0.118(3) 0.056(2) 0.073(2) 0.0096(16) 0.046(2) 0.0198(19) Li1 0.104(17) 0.051(11) 0.13(2) -0.012(11) 0.053(15) 0.008(11) O3 0.143(5) 0.127(5) 0.156(5) -0.006(5) 0.035(5) 0.009(4) O4 0.154(6) 0.131(5) 0.181(6) -0.027(5) 0.039(5) -0.018(5) C1 0.108(5) 0.076(5) 0.109(5) 0.002(5) 0.051(5) 0.000(4) C2 0.117(5) 0.091(5) 0.124(5) -0.002(4) 0.046(4) 0.007(4) C3 0.117(5) 0.089(5) 0.119(5) 0.006(5) 0.046(5) 0.008(4) C4 0.119(5) 0.085(5) 0.109(5) 0.008(5) 0.049(5) 0.006(5) C5 0.116(5) 0.083(5) 0.111(5) -0.001(5) 0.050(5) 0.005(5) C7 0.129(8) 0.107(8) 0.136(8) 0.027(7) 0.055(7) 0.008(7) C6 0.168(9) 0.105(8) 0.115(8) 0.006(7) 0.039(8) -0.006(8) C8 0.128(9) 0.091(8) 0.091(8) 0.005(7) 0.042(8) 0.003(7) C9 0.122(9) 0.088(8) 0.129(9) 0.015(7) 0.071(8) -0.004(7) C10 0.156(7) 0.154(6) 0.204(7) -0.016(6) 0.018(6) -0.009(6) C11 0.152(8) 0.156(8) 0.209(9) -0.011(7) 0.012(8) -0.018(7) C12 0.151(8) 0.156(8) 0.203(9) -0.012(7) 0.010(8) -0.011(7) C13 0.148(7) 0.145(6) 0.201(8) -0.004(6) 0.018(7) -0.010(6) C15 0.191(9) 0.181(8) 0.258(10) -0.044(8) 0.008(8) 0.015(8) C16 0.182(8) 0.183(9) 0.260(10) -0.032(8) 0.011(8) 0.012(8) C14 0.172(7) 0.163(7) 0.235(8) -0.032(7) 0.013(7) 0.008(6) C17 0.178(8) 0.173(8) 0.250(9) -0.039(8) 0.011(8) 0.010(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr2 N5 2.133(9) . ? Zr2 N4 2.347(10) . ? Zr2 Cl5 2.463(4) . ? Zr2 Cl6 2.470(4) . ? Zr2 N6 2.522(11) . ? Zr2 Cl7 2.547(4) . ? Zr2 Cl8 2.571(3) . ? Cl7 Li2 2.40(4) . ? Cl8 Li2 2.36(3) . ? N4 C22 1.335(16) . ? N4 C18 1.358(16) . ? N5 C18 1.303(15) . ? N5 Si2 1.697(11) . ? N6 C25 1.492(18) . ? N6 C26 1.524(17) . ? N6 Si2 1.781(9) . ? Si2 C24 1.787(16) . ? Si2 C23 1.818(18) . ? Li2 O3 1.89(3) . ? Li2 O4 1.89(3) . ? O1 C10 1.40(2) . ? O1 C13 1.46(2) . ? O1 Li1 1.78(3) . ? O2 C14 1.54(2) . ? O2 C17 1.609(10) . ? O2 Li1 1.96(3) . ? C18 C19 1.385(17) . ? C19 C20 1.378(17) . ? C19 H19 0.9400 . ? C20 C21 1.361(18) . ? C20 H20 0.9400 . ? C21 C22 1.348(17) . ? C21 H21 0.9400 . ? C22 H22 0.9400 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 C28 1.42(2) . ? C27 O3 1.433(19) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.56(2) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.36(2) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 O3 1.52(2) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 C32 1.391(10) . ? C31 O4 1.50(2) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C32 C33 1.391(10) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C33 C34 1.43(2) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 O4 1.36(2) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? Zr1 N2 2.147(8) . ? Zr1 N1 2.326(8) . ? Zr1 Cl2 2.457(4) . ? Zr1 Cl1 2.460(4) . ? Zr1 N3 2.536(9) . ? Zr1 Cl3 2.569(3) . ? Zr1 Cl4 2.570(3) . ? Cl3 Li1 2.41(2) . ? Cl4 Li1 2.40(2) . ? N1 C5 1.351(16) . ? N1 C1 1.365(15) . ? N2 C1 1.337(15) . ? N2 Si1 1.694(9) . ? N3 C8 1.449(16) . ? N3 C9 1.510(15) . ? N3 Si1 1.801(9) . ? Si1 C6 1.756(16) . ? Si1 C7 1.891(17) . ? C1 C2 1.396(19) . ? C2 C3 1.391(18) . ? C2 H2 0.9400 . ? C3 C4 1.353(18) . ? C3 H3 0.9400 . ? C4 C5 1.384(18) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C11 1.42(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.63(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.36(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C15 C14 1.459(10) . ? C15 C16 1.565(10) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C17 1.434(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Zr2 N4 58.1(4) . . ? N5 Zr2 Cl5 89.8(3) . . ? N4 Zr2 Cl5 93.0(3) . . ? N5 Zr2 Cl6 90.3(3) . . ? N4 Zr2 Cl6 86.1(3) . . ? Cl5 Zr2 Cl6 178.85(14) . . ? N5 Zr2 N6 64.7(3) . . ? N4 Zr2 N6 122.6(3) . . ? Cl5 Zr2 N6 91.7(3) . . ? Cl6 Zr2 N6 89.3(3) . . ? N5 Zr2 Cl7 135.7(3) . . ? N4 Zr2 Cl7 77.7(3) . . ? Cl5 Zr2 Cl7 89.50(15) . . ? Cl6 Zr2 Cl7 89.62(14) . . ? N6 Zr2 Cl7 159.5(2) . . ? N5 Zr2 Cl8 142.5(3) . . ? N4 Zr2 Cl8 159.2(3) . . ? Cl5 Zr2 Cl8 90.37(14) . . ? Cl6 Zr2 Cl8 90.25(13) . . ? N6 Zr2 Cl8 77.8(2) . . ? Cl7 Zr2 Cl8 81.78(13) . . ? Li2 Cl7 Zr2 93.0(7) . . ? Li2 Cl8 Zr2 93.2(9) . . ? C22 N4 C18 123.2(11) . . ? C22 N4 Zr2 146.6(9) . . ? C18 N4 Zr2 89.9(8) . . ? C18 N5 Si2 146.0(10) . . ? C18 N5 Zr2 101.4(8) . . ? Si2 N5 Zr2 109.9(4) . . ? C25 N6 C26 106.2(10) . . ? C25 N6 Si2 114.7(9) . . ? C26 N6 Si2 114.4(8) . . ? C25 N6 Zr2 117.0(9) . . ? C26 N6 Zr2 112.2(8) . . ? Si2 N6 Zr2 92.3(4) . . ? N5 Si2 N6 92.5(5) . . ? N5 Si2 C24 115.2(7) . . ? N6 Si2 C24 112.0(7) . . ? N5 Si2 C23 109.1(7) . . ? N6 Si2 C23 111.7(6) . . ? C24 Si2 C23 114.3(9) . . ? O3 Li2 O4 104.9(13) . . ? O3 Li2 Cl8 118.3(17) . . ? O4 Li2 Cl8 118.4(16) . . ? O3 Li2 Cl7 110.5(16) . . ? O4 Li2 Cl7 114.8(19) . . ? Cl8 Li2 Cl7 89.5(9) . . ? C10 O1 C13 104.8(16) . . ? C10 O1 Li1 126.3(16) . . ? C13 O1 Li1 121.2(15) . . ? C14 O2 C17 124.9(15) . . ? C14 O2 Li1 118.1(14) . . ? C17 O2 Li1 114.5(14) . . ? N5 C18 N4 110.3(12) . . ? N5 C18 C19 133.5(14) . . ? N4 C18 C19 116.2(13) . . ? C20 C19 C18 121.7(14) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C21 C20 C19 118.3(13) . . ? C21 C20 H20 120.9 . . ? C19 C20 H20 120.9 . . ? C22 C21 C20 120.7(14) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? N4 C22 C21 119.9(14) . . ? N4 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si2 C24 H24A 109.5 . . ? Si2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N6 C25 H25A 109.5 . . ? N6 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N6 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N6 C26 H26A 109.5 . . ? N6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 O3 102.0(16) . . ? C28 C27 H27A 111.4 . . ? O3 C27 H27A 111.4 . . ? C28 C27 H27B 111.4 . . ? O3 C27 H27B 111.4 . . ? H27A C27 H27B 109.2 . . ? C27 C28 C29 111.8(16) . . ? C27 C28 H28A 109.3 . . ? C29 C28 H28A 109.3 . . ? C27 C28 H28B 109.3 . . ? C29 C28 H28B 109.3 . . ? H28A C28 H28B 107.9 . . ? C30 C29 C28 96.4(16) . . ? C30 C29 H29A 112.5 . . ? C28 C29 H29A 112.5 . . ? C30 C29 H29B 112.5 . . ? C28 C29 H29B 112.5 . . ? H29A C29 H29B 110.0 . . ? C29 C30 O3 109.6(18) . . ? C29 C30 H30A 109.8 . . ? O3 C30 H30A 109.8 . . ? C29 C30 H30B 109.8 . . ? O3 C30 H30B 109.8 . . ? H30A C30 H30B 108.2 . . ? C32 C31 O4 102.7(16) . . ? C32 C31 H31A 111.2 . . ? O4 C31 H31A 111.2 . . ? C32 C31 H31B 111.2 . . ? O4 C31 H31B 111.2 . . ? H31A C31 H31B 109.1 . . ? C33 C32 C31 111.0(19) . . ? C33 C32 H32A 109.4 . . ? C31 C32 H32A 109.4 . . ? C33 C32 H32B 109.4 . . ? C31 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C32 C33 C34 106.6(18) . . ? C32 C33 H33A 110.4 . . ? C34 C33 H33A 110.4 . . ? C32 C33 H33B 110.4 . . ? C34 C33 H33B 110.4 . . ? H33A C33 H33B 108.6 . . ? O4 C34 C33 107.4(18) . . ? O4 C34 H34A 110.2 . . ? C33 C34 H34A 110.2 . . ? O4 C34 H34B 110.2 . . ? C33 C34 H34B 110.2 . . ? H34A C34 H34B 108.5 . . ? N2 Zr1 N1 58.8(3) . . ? N2 Zr1 Cl2 90.8(3) . . ? N1 Zr1 Cl2 91.2(2) . . ? N2 Zr1 Cl1 90.3(3) . . ? N1 Zr1 Cl1 88.9(2) . . ? Cl2 Zr1 Cl1 178.78(14) . . ? N2 Zr1 N3 64.8(3) . . ? N1 Zr1 N3 123.5(3) . . ? Cl2 Zr1 N3 92.0(2) . . ? Cl1 Zr1 N3 88.9(2) . . ? N2 Zr1 Cl3 135.5(2) . . ? N1 Zr1 Cl3 76.7(2) . . ? Cl2 Zr1 Cl3 89.12(14) . . ? Cl1 Zr1 Cl3 89.73(14) . . ? N3 Zr1 Cl3 159.7(2) . . ? N2 Zr1 Cl4 142.1(2) . . ? N1 Zr1 Cl4 159.1(2) . . ? Cl2 Zr1 Cl4 89.47(14) . . ? Cl1 Zr1 Cl4 89.96(13) . . ? N3 Zr1 Cl4 77.4(2) . . ? Cl3 Zr1 Cl4 82.36(11) . . ? Li1 Cl3 Zr1 93.1(5) . . ? Li1 Cl4 Zr1 93.3(5) . . ? C5 N1 C1 120.0(11) . . ? C5 N1 Zr1 148.4(8) . . ? C1 N1 Zr1 91.4(7) . . ? C1 N2 Si1 147.2(9) . . ? C1 N2 Zr1 100.4(8) . . ? Si1 N2 Zr1 110.0(4) . . ? C8 N3 C9 105.7(10) . . ? C8 N3 Si1 114.7(8) . . ? C9 N3 Si1 115.6(8) . . ? C8 N3 Zr1 113.0(7) . . ? C9 N3 Zr1 116.1(7) . . ? Si1 N3 Zr1 91.8(4) . . ? N2 Si1 C6 119.5(7) . . ? N2 Si1 N3 92.7(4) . . ? C6 Si1 N3 114.4(7) . . ? N2 Si1 C7 112.6(6) . . ? C6 Si1 C7 106.0(8) . . ? N3 Si1 C7 111.3(6) . . ? O1 Li1 O2 108.6(11) . . ? O1 Li1 Cl4 116.0(13) . . ? O2 Li1 Cl4 117.5(11) . . ? O1 Li1 Cl3 111.7(11) . . ? O2 Li1 Cl3 112.5(13) . . ? Cl4 Li1 Cl3 89.4(7) . . ? C27 O3 C30 107.2(14) . . ? C27 O3 Li2 124.2(17) . . ? C30 O3 Li2 118.8(18) . . ? C34 O4 C31 109.4(14) . . ? C34 O4 Li2 127.5(16) . . ? C31 O4 Li2 122.7(14) . . ? N2 C1 N1 109.1(11) . . ? N2 C1 C2 130.9(13) . . ? N1 C1 C2 120.0(13) . . ? C3 C2 C1 119.3(14) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C4 C3 C2 119.4(15) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 120.5(14) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? N1 C5 C4 120.7(13) . . ? N1 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C10 C11 106(2) . . ? O1 C10 H10A 110.5 . . ? C11 C10 H10A 110.5 . . ? O1 C10 H10B 110.5 . . ? C11 C10 H10B 110.5 . . ? H10A C10 H10B 108.7 . . ? C10 C11 C12 110.6(19) . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C13 C12 C11 92.5(19) . . ? C13 C12 H12A 113.2 . . ? C11 C12 H12A 113.2 . . ? C13 C12 H12B 113.2 . . ? C11 C12 H12B 113.2 . . ? H12A C12 H12B 110.6 . . ? C12 C13 O1 119(2) . . ? C12 C13 H13A 107.5 . . ? O1 C13 H13A 107.5 . . ? C12 C13 H13B 107.5 . . ? O1 C13 H13B 107.5 . . ? H13A C13 H13B 107.0 . . ? C14 C15 C16 110(2) . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.2 . . ? C17 C16 C15 98(2) . . ? C17 C16 H16A 112.2 . . ? C15 C16 H16A 112.2 . . ? C17 C16 H16B 112.2 . . ? C15 C16 H16B 112.2 . . ? H16A C16 H16B 109.8 . . ? C15 C14 O2 80.4(15) . . ? C15 C14 H14A 115.2 . . ? O2 C14 H14A 115.2 . . ? C15 C14 H14B 115.2 . . ? O2 C14 H14B 115.2 . . ? H14A C14 H14B 112.2 . . ? C16 C17 O2 75.7(14) . . ? C16 C17 H17A 115.9 . . ? O2 C17 H17A 115.9 . . ? C16 C17 H17B 115.9 . . ? O2 C17 H17B 115.9 . . ? H17A C17 H17B 112.9 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.895 _refine_diff_density_min -1.027 _refine_diff_density_rms 0.126 #===end data_s529b _database_code_depnum_ccdc_archive 'CCDC 859331' #TrackingRef '1-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H40 Cl2 Fe2 N6 O Si2' _chemical_formula_sum 'C22 H40 Cl2 Fe2 N6 O Si2' _chemical_formula_weight 643.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.417(2) _cell_length_b 16.024(2) _cell_length_c 14.649(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.060(3) _cell_angle_gamma 90.00 _cell_volume 3147.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 238(2) _cell_measurement_reflns_used 3773 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 19.76 _exptl_crystal_description block _exptl_crystal_colour black-brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 1.193 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7161 _exptl_absorpt_correction_T_max 0.7964 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 238(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD AREA DETECOR' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13382 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5536 _reflns_number_gt 4195 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+9.4437P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5536 _refine_ls_number_parameters 316 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1720 _refine_ls_wR_factor_gt 0.1599 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.79639(6) -0.07792(5) 0.24377(6) 0.0325(2) Uani 1 1 d . . . Fe2 Fe 0.68150(6) 0.09536(5) 0.23332(6) 0.0318(2) Uani 1 1 d . . . Cl1 Cl 0.84484(14) -0.18144(10) 0.14441(12) 0.0534(4) Uani 1 1 d . . . Cl2 Cl 0.62152(13) 0.18500(10) 0.12102(11) 0.0518(4) Uani 1 1 d . . . N1 N 0.9181(3) 0.0020(3) 0.2528(4) 0.0377(11) Uani 1 1 d . . . N2 N 0.8169(3) 0.1114(3) 0.2965(3) 0.0335(11) Uani 1 1 d . . . N3 N 0.6577(3) 0.1806(3) 0.3618(3) 0.0342(11) Uani 1 1 d . . . N4 N 0.5624(3) 0.0196(3) 0.2634(3) 0.0317(10) Uani 1 1 d . . . N5 N 0.6699(3) -0.0847(3) 0.3168(3) 0.0313(10) Uani 1 1 d . . . N6 N 0.8389(4) -0.1444(3) 0.3823(3) 0.0391(12) Uani 1 1 d . . . O1 O 0.7279(3) -0.0016(3) 0.1251(3) 0.0472(11) Uani 1 1 d . . . Si1 Si 0.78646(13) 0.19897(11) 0.35762(13) 0.0436(4) Uani 1 1 d . . . Si2 Si 0.71017(13) -0.16358(11) 0.38818(13) 0.0417(4) Uani 1 1 d . . . C1 C 0.9095(4) 0.0819(4) 0.2843(4) 0.0366(12) Uani 1 1 d U . . C2 C 0.9978(4) 0.1285(4) 0.3020(4) 0.0419(12) Uani 1 1 d U . . H2A H 0.9931 0.1837 0.3233 0.050 Uiso 1 1 calc R . . C3 C 1.0889(5) 0.0950(4) 0.2889(5) 0.0506(14) Uani 1 1 d U . . H3A H 1.1470 0.1264 0.3012 0.061 Uiso 1 1 calc R . . C4 C 1.0952(5) 0.0138(4) 0.2571(5) 0.0541(14) Uani 1 1 d U . . H4A H 1.1575 -0.0108 0.2475 0.065 Uiso 1 1 calc R . . C5 C 1.0098(5) -0.0292(4) 0.2402(5) 0.0534(15) Uani 1 1 d U . . H5A H 1.0147 -0.0841 0.2183 0.064 Uiso 1 1 calc R . . C6 C 0.8469(6) 0.2031(6) 0.4742(6) 0.085(3) Uani 1 1 d . . . H6A H 0.8748 0.2582 0.4849 0.127 Uiso 1 1 calc R . . H6B H 0.8996 0.1618 0.4789 0.127 Uiso 1 1 calc R . . H6C H 0.7976 0.1915 0.5193 0.127 Uiso 1 1 calc R . . C7 C 0.8070(6) 0.2976(4) 0.2935(7) 0.077(3) Uani 1 1 d . . . H7A H 0.8433 0.3369 0.3325 0.116 Uiso 1 1 calc R . . H7B H 0.7431 0.3214 0.2745 0.116 Uiso 1 1 calc R . . H7C H 0.8453 0.2858 0.2401 0.116 Uiso 1 1 calc R . . C8 C 0.6291(5) 0.1273(4) 0.4375(4) 0.0495(16) Uani 1 1 d . . . H8A H 0.6189 0.1614 0.4911 0.074 Uiso 1 1 calc R . . H8B H 0.6816 0.0870 0.4509 0.074 Uiso 1 1 calc R . . H8C H 0.5678 0.0981 0.4208 0.074 Uiso 1 1 calc R . . C9 C 0.5874(5) 0.2503(4) 0.3521(5) 0.0524(17) Uani 1 1 d . . . H9A H 0.5847 0.2799 0.4097 0.079 Uiso 1 1 calc R . . H9B H 0.5217 0.2290 0.3351 0.079 Uiso 1 1 calc R . . H9C H 0.6094 0.2880 0.3051 0.079 Uiso 1 1 calc R . . C10 C 0.5761(4) -0.0557(3) 0.3063(4) 0.0316(12) Uani 1 1 d U . . C11 C 0.4911(4) -0.0976(4) 0.3371(4) 0.0410(12) Uani 1 1 d U . . H11A H 0.4988 -0.1497 0.3659 0.049 Uiso 1 1 calc R . . C12 C 0.3985(4) -0.0644(4) 0.3260(5) 0.0462(13) Uani 1 1 d U . . H12A H 0.3429 -0.0935 0.3468 0.055 Uiso 1 1 calc R . . C13 C 0.3862(4) 0.0134(4) 0.2834(5) 0.0469(13) Uani 1 1 d U . . H13A H 0.3230 0.0384 0.2764 0.056 Uiso 1 1 calc R . . C14 C 0.4692(4) 0.0513(4) 0.2526(5) 0.0424(13) Uani 1 1 d U . . H14A H 0.4614 0.1026 0.2219 0.051 Uiso 1 1 calc R . . C15 C 0.6663(6) -0.1551(6) 0.5064(5) 0.079(3) Uani 1 1 d . . . H15A H 0.6406 -0.2086 0.5255 0.119 Uiso 1 1 calc R . . H15B H 0.6140 -0.1135 0.5084 0.119 Uiso 1 1 calc R . . H15C H 0.7215 -0.1387 0.5471 0.119 Uiso 1 1 calc R . . C16 C 0.6821(6) -0.2692(4) 0.3403(8) 0.086(3) Uani 1 1 d . . . H16A H 0.6517 -0.3033 0.3864 0.129 Uiso 1 1 calc R . . H16B H 0.7435 -0.2952 0.3219 0.129 Uiso 1 1 calc R . . H16C H 0.6366 -0.2639 0.2877 0.129 Uiso 1 1 calc R . . C17 C 0.9074(5) -0.2155(5) 0.3807(6) 0.063(2) Uani 1 1 d . . . H17A H 0.9185 -0.2367 0.4422 0.094 Uiso 1 1 calc R . . H17B H 0.9704 -0.1978 0.3567 0.094 Uiso 1 1 calc R . . H17C H 0.8787 -0.2591 0.3421 0.094 Uiso 1 1 calc R . . C18 C 0.8782(6) -0.0817(5) 0.4463(5) 0.0597(19) Uani 1 1 d . . . H18A H 0.8963 -0.1082 0.5041 0.090 Uiso 1 1 calc R . . H18B H 0.8277 -0.0396 0.4559 0.090 Uiso 1 1 calc R . . H18C H 0.9367 -0.0557 0.4216 0.090 Uiso 1 1 calc R . . C19 C 0.7977(7) 0.0301(6) 0.0590(5) 0.083(2) Uani 1 1 d U . . H19A H 0.8634 0.0040 0.0680 0.100 Uiso 1 1 calc R . . H19B H 0.8050 0.0908 0.0643 0.100 Uiso 1 1 calc R . . C20 C 0.7516(9) 0.0067(8) -0.0311(6) 0.104(2) Uani 1 1 d U . . H20A H 0.7527 0.0548 -0.0724 0.125 Uiso 1 1 calc R . . H20B H 0.7899 -0.0385 -0.0580 0.125 Uiso 1 1 calc R . . C21 C 0.6556(9) -0.0185(8) -0.0210(6) 0.107(2) Uani 1 1 d U . . H21A H 0.6398 -0.0652 -0.0621 0.128 Uiso 1 1 calc R . . H21B H 0.6095 0.0274 -0.0356 0.128 Uiso 1 1 calc R . . C22 C 0.6463(7) -0.0445(7) 0.0748(5) 0.087(2) Uani 1 1 d U . . H22A H 0.6530 -0.1051 0.0807 0.104 Uiso 1 1 calc R . . H22B H 0.5815 -0.0276 0.0976 0.104 Uiso 1 1 calc 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 0.0295(4) 0.0274(4) 0.0406(5) -0.0026(3) 0.0023(3) -0.0010(3) Fe2 0.0292(4) 0.0273(4) 0.0387(5) 0.0038(3) -0.0009(3) -0.0008(3) Cl1 0.0678(11) 0.0379(9) 0.0541(10) -0.0137(7) -0.0019(8) 0.0105(8) Cl2 0.0687(11) 0.0422(9) 0.0444(9) 0.0116(7) 0.0020(8) 0.0160(8) N1 0.026(3) 0.031(3) 0.056(3) -0.005(2) 0.004(2) 0.0001(19) N2 0.025(2) 0.032(2) 0.044(3) -0.004(2) 0.004(2) -0.0015(19) N3 0.036(3) 0.030(2) 0.036(3) -0.006(2) 0.003(2) 0.003(2) N4 0.026(2) 0.032(2) 0.038(3) 0.003(2) -0.0011(19) -0.0022(19) N5 0.029(2) 0.028(2) 0.037(3) 0.007(2) 0.0008(19) -0.0018(19) N6 0.040(3) 0.038(3) 0.039(3) 0.001(2) -0.006(2) 0.006(2) O1 0.057(3) 0.048(3) 0.036(2) -0.003(2) 0.001(2) 0.011(2) Si1 0.0344(9) 0.0358(9) 0.0604(12) -0.0157(8) 0.0007(8) -0.0014(7) Si2 0.0376(9) 0.0366(9) 0.0509(10) 0.0137(8) 0.0011(8) 0.0038(7) C1 0.028(3) 0.032(3) 0.050(3) -0.001(2) 0.004(2) -0.001(2) C2 0.032(2) 0.036(3) 0.058(3) -0.005(2) 0.004(2) -0.005(2) C3 0.029(3) 0.049(3) 0.073(3) -0.006(3) 0.003(2) -0.006(2) C4 0.030(3) 0.052(3) 0.081(3) -0.010(3) 0.009(3) 0.003(2) C5 0.033(3) 0.046(3) 0.082(4) -0.014(3) 0.009(3) 0.000(3) C6 0.054(5) 0.118(8) 0.081(6) -0.051(6) -0.018(4) 0.015(5) C7 0.063(5) 0.027(4) 0.144(8) -0.007(4) 0.026(5) -0.008(3) C8 0.051(4) 0.056(4) 0.041(4) -0.003(3) 0.006(3) 0.000(3) C9 0.046(4) 0.053(4) 0.058(4) -0.011(3) 0.002(3) 0.015(3) C10 0.023(2) 0.034(3) 0.038(3) 0.000(2) 0.001(2) -0.003(2) C11 0.032(2) 0.042(3) 0.049(3) 0.006(2) -0.001(2) -0.006(2) C12 0.030(2) 0.053(3) 0.055(3) 0.004(3) -0.001(2) -0.008(2) C13 0.027(2) 0.056(3) 0.058(3) 0.001(3) -0.005(2) 0.001(2) C14 0.029(3) 0.043(3) 0.055(3) 0.003(3) -0.006(2) 0.003(2) C15 0.071(5) 0.110(7) 0.058(5) 0.040(5) 0.016(4) 0.022(5) C16 0.054(5) 0.034(4) 0.169(10) 0.013(5) -0.006(5) -0.005(3) C17 0.051(4) 0.060(5) 0.076(5) 0.009(4) -0.005(4) 0.020(4) C18 0.061(5) 0.074(5) 0.043(4) -0.006(4) -0.016(3) 0.000(4) C19 0.118(6) 0.091(5) 0.041(3) 0.008(4) 0.021(4) 0.015(5) C20 0.137(5) 0.121(5) 0.054(3) -0.002(4) 0.007(4) 0.006(4) C21 0.133(5) 0.127(5) 0.059(4) -0.017(4) -0.017(4) 0.007(5) C22 0.107(5) 0.105(5) 0.046(4) -0.021(4) -0.030(4) 0.012(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N5 2.041(5) . ? Fe1 N1 2.076(5) . ? Fe1 O1 2.291(4) . ? Fe1 Cl1 2.3153(17) . ? Fe1 N6 2.344(5) . ? Fe2 N2 2.025(5) . ? Fe2 N4 2.066(4) . ? Fe2 Cl2 2.3070(17) . ? Fe2 O1 2.321(4) . ? Fe2 N3 2.356(5) . ? N1 C5 1.346(7) . ? N1 C1 1.368(7) . ? N2 C1 1.347(7) . ? N2 Si1 1.721(5) . ? N3 C8 1.463(8) . ? N3 C9 1.465(7) . ? N3 Si1 1.756(5) . ? N4 C14 1.355(7) . ? N4 C10 1.370(7) . ? N5 C10 1.345(7) . ? N5 Si2 1.715(5) . ? N6 C18 1.460(8) . ? N6 C17 1.465(8) . ? N6 Si2 1.759(5) . ? O1 C19 1.462(9) . ? O1 C22 1.468(9) . ? Si1 C7 1.864(8) . ? Si1 C6 1.865(8) . ? Si2 C15 1.853(8) . ? Si2 C16 1.865(8) . ? C1 C2 1.417(8) . ? C2 C3 1.355(8) . ? C2 H2A 0.9400 . ? C3 C4 1.385(9) . ? C3 H3A 0.9400 . ? C4 C5 1.353(9) . ? C4 H4A 0.9400 . ? C5 H5A 0.9400 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C11 1.411(8) . ? C11 C12 1.354(8) . ? C11 H11A 0.9400 . ? C12 C13 1.402(9) . ? C12 H12A 0.9400 . ? C13 C14 1.359(9) . ? C13 H13A 0.9400 . ? C14 H14A 0.9400 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C20 1.485(12) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.362(13) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C22 1.473(13) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Fe1 N1 131.77(19) . . ? N5 Fe1 O1 96.19(17) . . ? N1 Fe1 O1 90.73(18) . . ? N5 Fe1 Cl1 123.30(14) . . ? N1 Fe1 Cl1 104.13(14) . . ? O1 Fe1 Cl1 91.11(11) . . ? N5 Fe1 N6 72.72(17) . . ? N1 Fe1 N6 93.34(19) . . ? O1 Fe1 N6 167.97(16) . . ? Cl1 Fe1 N6 98.85(13) . . ? N2 Fe2 N4 131.66(19) . . ? N2 Fe2 Cl2 122.05(15) . . ? N4 Fe2 Cl2 105.40(13) . . ? N2 Fe2 O1 98.00(17) . . ? N4 Fe2 O1 88.90(17) . . ? Cl2 Fe2 O1 91.43(11) . . ? N2 Fe2 N3 72.94(17) . . ? N4 Fe2 N3 92.40(17) . . ? Cl2 Fe2 N3 98.89(12) . . ? O1 Fe2 N3 168.84(16) . . ? C5 N1 C1 118.9(5) . . ? C5 N1 Fe1 118.9(4) . . ? C1 N1 Fe1 121.6(4) . . ? C1 N2 Si1 126.3(4) . . ? C1 N2 Fe2 135.3(4) . . ? Si1 N2 Fe2 96.7(2) . . ? C8 N3 C9 109.5(5) . . ? C8 N3 Si1 114.2(4) . . ? C9 N3 Si1 120.0(4) . . ? C8 N3 Fe2 108.3(4) . . ? C9 N3 Fe2 118.0(4) . . ? Si1 N3 Fe2 84.69(19) . . ? C14 N4 C10 119.5(5) . . ? C14 N4 Fe2 118.2(4) . . ? C10 N4 Fe2 121.6(3) . . ? C10 N5 Si2 126.7(4) . . ? C10 N5 Fe1 135.5(4) . . ? Si2 N5 Fe1 96.3(2) . . ? C18 N6 C17 109.4(5) . . ? C18 N6 Si2 114.9(4) . . ? C17 N6 Si2 118.8(5) . . ? C18 N6 Fe1 108.4(4) . . ? C17 N6 Fe1 118.2(4) . . ? Si2 N6 Fe1 85.03(19) . . ? C19 O1 C22 108.3(6) . . ? C19 O1 Fe1 116.0(4) . . ? C22 O1 Fe1 113.8(5) . . ? C19 O1 Fe2 114.4(5) . . ? C22 O1 Fe2 116.3(5) . . ? Fe1 O1 Fe2 87.07(14) . . ? N2 Si1 N3 97.7(2) . . ? N2 Si1 C7 112.7(3) . . ? N3 Si1 C7 108.8(3) . . ? N2 Si1 C6 113.7(3) . . ? N3 Si1 C6 111.7(3) . . ? C7 Si1 C6 111.3(5) . . ? N5 Si2 N6 97.4(2) . . ? N5 Si2 C15 114.3(3) . . ? N6 Si2 C15 112.2(3) . . ? N5 Si2 C16 112.6(4) . . ? N6 Si2 C16 109.0(3) . . ? C15 Si2 C16 110.6(5) . . ? N2 C1 N1 117.6(5) . . ? N2 C1 C2 124.0(5) . . ? N1 C1 C2 118.4(5) . . ? C3 C2 C1 121.2(6) . . ? C3 C2 H2A 119.4 . . ? C1 C2 H2A 119.4 . . ? C2 C3 C4 119.1(6) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C5 C4 C3 118.6(6) . . ? C5 C4 H4A 120.7 . . ? C3 C4 H4A 120.7 . . ? N1 C5 C4 123.9(6) . . ? N1 C5 H5A 118.0 . . ? C4 C5 H5A 118.0 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N5 C10 N4 117.8(5) . . ? N5 C10 C11 124.3(5) . . ? N4 C10 C11 118.0(5) . . ? C12 C11 C10 121.6(6) . . ? C12 C11 H11A 119.2 . . ? C10 C11 H11A 119.2 . . ? C11 C12 C13 119.7(6) . . ? C11 C12 H12A 120.2 . . ? C13 C12 H12A 120.2 . . ? C14 C13 C12 117.4(6) . . ? C14 C13 H13A 121.3 . . ? C12 C13 H13A 121.3 . . ? N4 C14 C13 123.9(6) . . ? N4 C14 H14A 118.1 . . ? C13 C14 H14A 118.1 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 H17A 109.5 . . ? N6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N6 C18 H18A 109.5 . . ? N6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C19 C20 104.1(8) . . ? O1 C19 H19A 110.9 . . ? C20 C19 H19A 110.9 . . ? O1 C19 H19B 110.9 . . ? C20 C19 H19B 110.9 . . ? H19A C19 H19B 108.9 . . ? C21 C20 C19 110.1(9) . . ? C21 C20 H20A 109.6 . . ? C19 C20 H20A 109.6 . . ? C21 C20 H20B 109.6 . . ? C19 C20 H20B 109.6 . . ? H20A C20 H20B 108.2 . . ? C20 C21 C22 107.5(9) . . ? C20 C21 H21A 110.2 . . ? C22 C21 H21A 110.2 . . ? C20 C21 H21B 110.2 . . ? C22 C21 H21B 110.2 . . ? H21A C21 H21B 108.5 . . ? C21 C22 O1 105.0(8) . . ? C21 C22 H22A 110.8 . . ? O1 C22 H22A 110.8 . . ? C21 C22 H22B 110.8 . . ? O1 C22 H22B 110.8 . . ? H22A C22 H22B 108.8 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.791 _refine_diff_density_min -0.929 _refine_diff_density_rms 0.096 #===end data_s570b _database_code_depnum_ccdc_archive 'CCDC 859332' #TrackingRef '1-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H40 Cl2 Co2 N6 O Si2' _chemical_formula_sum 'C22 H40 Cl2 Co2 N6 O Si2' _chemical_formula_weight 649.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.3409(17) _cell_length_b 15.996(2) _cell_length_c 14.6355(19) _cell_angle_alpha 90.00 _cell_angle_beta 92.207(2) _cell_angle_gamma 90.00 _cell_volume 3120.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 234(2) _cell_measurement_reflns_used 8874 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.23 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 1.336 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6900 _exptl_absorpt_correction_T_max 0.7760 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 234(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD AREA DETECOR' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32362 _diffrn_reflns_av_R_equivalents 0.0774 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5506 _reflns_number_gt 4611 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+3.0342P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5506 _refine_ls_number_parameters 324 _refine_ls_number_restraints 474 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.1011 _refine_ls_wR_factor_gt 0.0937 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.70418(3) 1.07557(3) 0.75334(3) 0.03134(13) Uani 1 1 d . . . Cl1 Cl 0.66146(8) 1.18041(6) 0.85115(7) 0.0520(3) Uani 1 1 d . . . N1 N 0.93589(18) 0.97907(16) 0.73519(17) 0.0301(6) Uani 1 1 d . . . N2 N 0.82878(19) 1.08418(15) 0.68330(18) 0.0307(6) Uani 1 1 d . . . N3 N 0.6585(2) 1.14347(18) 0.61852(19) 0.0386(7) Uani 1 1 d . . . Si1 Si 0.78795(7) 1.16291(6) 0.61104(7) 0.0405(2) Uani 1 1 d . . . C1 C 0.9232(2) 1.0544(2) 0.6940(2) 0.0322(7) Uani 1 1 d U . . C2 C 1.0087(3) 1.0966(2) 0.6640(2) 0.0406(8) Uani 1 1 d U . . H2 H 1.0014 1.1491 0.6355 0.049 Uiso 1 1 calc R . . C3 C 1.1018(3) 1.0626(2) 0.6756(3) 0.0460(8) Uani 1 1 d U . . H3 H 1.1581 1.0914 0.6552 0.055 Uiso 1 1 calc R . . C4 C 1.1136(3) 0.9852(2) 0.7177(3) 0.0448(8) Uani 1 1 d U . . H4 H 1.1772 0.9605 0.7260 0.054 Uiso 1 1 calc R . . C5 C 1.0295(2) 0.9463(2) 0.7466(2) 0.0408(8) Uani 1 1 d U . . H5 H 1.0367 0.8942 0.7759 0.049 Uiso 1 1 calc R . . C6 C 0.8170(3) 1.2681(3) 0.6572(4) 0.0746(14) Uani 1 1 d U . . H6A H 0.8015 1.2700 0.7214 0.112 Uiso 1 1 calc R . . H6B H 0.7771 1.3095 0.6238 0.112 Uiso 1 1 calc R . . H6C H 0.8877 1.2799 0.6508 0.112 Uiso 1 1 calc R . . C7 C 0.8306(4) 1.1536(4) 0.4926(3) 0.0740(13) Uani 1 1 d U . . H7A H 0.8988 1.1742 0.4899 0.111 Uiso 1 1 calc R . . H7B H 0.7870 1.1864 0.4519 0.111 Uiso 1 1 calc R . . H7C H 0.8282 1.0955 0.4739 0.111 Uiso 1 1 calc R . . C8 C 0.6181(3) 1.0799(3) 0.5538(3) 0.0569(10) Uani 1 1 d U . . H8A H 0.5534 1.0607 0.5735 0.085 Uiso 1 1 calc R . . H8B H 0.6640 1.0330 0.5522 0.085 Uiso 1 1 calc R . . H8C H 0.6103 1.1042 0.4932 0.085 Uiso 1 1 calc R . . C9 C 0.5893(3) 1.2152(3) 0.6202(3) 0.0575(11) Uani 1 1 d U . . H9A H 0.5864 1.2420 0.5607 0.086 Uiso 1 1 calc R . . H9B H 0.6131 1.2550 0.6661 0.086 Uiso 1 1 calc R . . H9C H 0.5229 1.1959 0.6348 0.086 Uiso 1 1 calc R . . C10 C 0.4921(3) 1.0299(2) 0.7582(3) 0.0483(9) Uani 1 1 d U . . H10 H 0.4881 1.0853 0.7790 0.058 Uiso 1 1 calc R . . C11 C 0.4055(3) 0.9872(3) 0.7424(3) 0.0537(9) Uani 1 1 d U . . H11 H 0.3431 1.0122 0.7523 0.064 Uiso 1 1 calc R . . C12 C 0.4116(3) 0.9054(2) 0.7112(3) 0.0470(9) Uani 1 1 d U . . H12 H 0.3529 0.8743 0.6987 0.056 Uiso 1 1 calc R . . C13 C 0.5033(2) 0.8706(2) 0.6986(2) 0.0405(8) Uani 1 1 d U . . H13 H 0.5075 0.8150 0.6783 0.049 Uiso 1 1 calc R . . C14 C 0.5924(2) 0.9173(2) 0.7160(2) 0.0326(7) Uani 1 1 d U . . Co2 Co 0.81880(3) 0.90464(3) 0.76355(3) 0.03033(13) Uani 1 1 d . . . Cl2 Cl 0.87337(8) 0.81344(6) 0.87506(6) 0.0498(2) Uani 1 1 d . . . N4 N 0.58433(19) 0.99717(16) 0.74563(19) 0.0355(6) Uani 1 1 d . . . N5 N 0.68532(19) 0.88707(16) 0.70289(19) 0.0329(6) Uani 1 1 d . . . N6 N 0.84530(19) 0.81954(16) 0.63800(18) 0.0331(6) Uani 1 1 d . . . Si2 Si 0.71570(7) 0.80003(6) 0.64096(7) 0.0403(2) Uani 1 1 d . . . O1 O 0.77255(18) 0.99985(15) 0.87138(15) 0.0436(6) Uani 1 1 d . . . C15 C 0.6550(3) 0.7958(3) 0.5251(3) 0.0750(14) Uani 1 1 d U . . H15A H 0.5892 0.7703 0.5285 0.112 Uiso 1 1 calc R . . H15B H 0.6959 0.7628 0.4853 0.112 Uiso 1 1 calc R . . H15C H 0.6480 0.8520 0.5009 0.112 Uiso 1 1 calc R . . C16 C 0.6942(3) 0.7012(2) 0.7043(4) 0.0721(13) Uani 1 1 d U . . H16A H 0.7274 0.7044 0.7644 0.108 Uiso 1 1 calc R . . H16B H 0.7213 0.6546 0.6708 0.108 Uiso 1 1 calc R . . H16C H 0.6228 0.6932 0.7109 0.108 Uiso 1 1 calc R . . C17 C 0.9164(3) 0.7494(2) 0.6476(3) 0.0503(9) Uani 1 1 d U . . H17A H 0.9118 0.7150 0.5931 0.075 Uiso 1 1 calc R . . H17B H 0.9003 0.7160 0.7004 0.075 Uiso 1 1 calc R . . H17C H 0.9841 0.7711 0.6557 0.075 Uiso 1 1 calc R . . C18 C 0.8736(3) 0.8733(2) 0.5619(2) 0.0468(9) Uani 1 1 d U . . H18A H 0.9417 0.8932 0.5728 0.070 Uiso 1 1 calc R . . H18B H 0.8282 0.9206 0.5571 0.070 Uiso 1 1 calc R . . H18C H 0.8696 0.8416 0.5054 0.070 Uiso 1 1 calc R . . C19 C 0.7019(4) 0.9692(3) 0.9378(3) 0.0656(11) Uani 1 1 d U . . H19A H 0.6921 0.9088 0.9315 0.079 Uiso 1 1 calc R . . H19B H 0.6368 0.9971 0.9294 0.079 Uiso 1 1 calc R . . C20 C 0.7491(6) 0.9898(5) 1.0279(4) 0.119(2) Uani 1 1 d U . . H20A H 0.7058 1.0282 1.0606 0.143 Uiso 1 1 calc R . . H20B H 0.7573 0.9387 1.0644 0.143 Uiso 1 1 calc R . . C21 C 0.8387(6) 1.0254(5) 1.0176(4) 0.1213(19) Uani 1 1 d U . . H21A H 0.8915 0.9883 1.0423 0.146 Uiso 1 1 calc R . . H21B H 0.8423 1.0780 1.0519 0.146 Uiso 1 1 calc R . . C22 C 0.8551(4) 1.0418(3) 0.9220(3) 0.0666(11) Uani 1 1 d U . . H22A H 0.9199 1.0193 0.9045 0.080 Uiso 1 1 calc R . . H22B H 0.8540 1.1021 0.9098 0.080 Uiso 1 1 calc 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 0.0286(2) 0.0283(2) 0.0372(3) -0.00391(17) 0.00289(18) -0.00166(17) Cl1 0.0654(6) 0.0395(5) 0.0506(5) -0.0136(4) -0.0022(5) 0.0110(4) N1 0.0247(13) 0.0300(14) 0.0354(14) 0.0022(11) -0.0028(11) 0.0006(11) N2 0.0274(14) 0.0281(14) 0.0365(15) 0.0037(11) 0.0019(11) -0.0005(10) N3 0.0324(15) 0.0418(16) 0.0410(16) 0.0015(13) -0.0047(12) 0.0051(12) Si1 0.0354(5) 0.0368(5) 0.0492(6) 0.0146(4) 0.0019(4) 0.0028(4) C1 0.0297(15) 0.0351(16) 0.0313(15) -0.0006(13) -0.0036(12) -0.0020(13) C2 0.0340(17) 0.0410(18) 0.0466(19) 0.0075(15) -0.0024(15) -0.0077(14) C3 0.0284(17) 0.057(2) 0.053(2) 0.0027(17) 0.0005(15) -0.0095(15) C4 0.0246(16) 0.056(2) 0.053(2) 0.0005(17) -0.0047(14) 0.0019(15) C5 0.0333(17) 0.0419(18) 0.0466(19) 0.0029(15) -0.0050(15) 0.0026(14) C6 0.057(3) 0.037(2) 0.129(4) 0.011(2) -0.005(3) -0.0057(19) C7 0.063(3) 0.102(3) 0.058(3) 0.035(3) 0.013(2) 0.018(3) C8 0.054(2) 0.071(3) 0.045(2) -0.0077(19) -0.0104(18) -0.0012(19) C9 0.045(2) 0.058(2) 0.068(3) 0.007(2) -0.0032(19) 0.0194(19) C10 0.0345(18) 0.0412(19) 0.070(2) -0.0108(17) 0.0118(16) 0.0043(15) C11 0.0286(17) 0.057(2) 0.076(2) -0.0093(19) 0.0136(17) 0.0032(16) C12 0.0269(17) 0.050(2) 0.064(2) -0.0029(17) 0.0069(16) -0.0091(15) C13 0.0306(16) 0.0362(17) 0.055(2) -0.0015(15) 0.0072(15) -0.0073(14) C14 0.0282(15) 0.0328(16) 0.0371(16) 0.0007(13) 0.0057(13) -0.0022(12) Co2 0.0282(2) 0.0288(2) 0.0339(2) 0.00488(17) 0.00022(17) -0.00104(17) Cl2 0.0636(6) 0.0433(5) 0.0427(5) 0.0141(4) 0.0050(4) 0.0155(4) N4 0.0274(14) 0.0305(14) 0.0491(17) -0.0046(12) 0.0068(12) -0.0014(11) N5 0.0272(14) 0.0307(14) 0.0408(16) -0.0027(12) 0.0031(11) -0.0020(11) N6 0.0283(14) 0.0341(14) 0.0369(15) -0.0021(12) 0.0040(11) 0.0024(11) Si2 0.0308(5) 0.0338(5) 0.0564(6) -0.0139(4) 0.0016(4) -0.0018(4) O1 0.0541(16) 0.0457(14) 0.0311(12) 0.0006(10) 0.0025(11) 0.0089(12) C15 0.053(3) 0.095(3) 0.076(3) -0.042(3) -0.017(2) 0.011(2) C16 0.056(3) 0.036(2) 0.125(4) -0.004(2) 0.020(3) -0.0076(19) C17 0.043(2) 0.050(2) 0.058(2) -0.0085(18) 0.0038(17) 0.0129(17) C18 0.049(2) 0.055(2) 0.0369(19) 0.0002(16) 0.0055(16) 0.0002(17) C19 0.081(3) 0.069(2) 0.049(2) 0.0092(19) 0.0218(19) 0.013(2) C20 0.145(5) 0.162(5) 0.050(3) 0.011(3) 0.013(3) 0.000(4) C21 0.138(4) 0.159(4) 0.065(3) -0.025(3) -0.013(3) -0.006(4) C22 0.074(2) 0.077(3) 0.047(2) -0.0152(19) -0.0215(19) 0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 1.991(3) . ? Co1 N4 2.032(3) . ? Co1 O1 2.272(2) . ? Co1 Cl1 2.2911(10) . ? Co1 N3 2.313(3) . ? N1 C1 1.355(4) . ? N1 C5 1.359(4) . ? N1 Co2 2.020(3) . ? N2 C1 1.350(4) . ? N2 Si1 1.720(3) . ? N3 C9 1.473(4) . ? N3 C8 1.477(5) . ? N3 Si1 1.763(3) . ? Si1 C6 1.848(5) . ? Si1 C7 1.851(5) . ? C1 C2 1.411(5) . ? C2 C3 1.360(5) . ? C2 H2 0.9400 . ? C3 C4 1.388(5) . ? C3 H3 0.9400 . ? C4 C5 1.364(5) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C11 1.354(5) . ? C10 N4 1.356(4) . ? C10 H10 0.9400 . ? C11 C12 1.389(5) . ? C11 H11 0.9400 . ? C12 C13 1.363(5) . ? C12 H12 0.9400 . ? C13 C14 1.419(4) . ? C13 H13 0.9400 . ? C14 N5 1.351(4) . ? C14 N4 1.355(4) . ? Co2 N5 1.979(3) . ? Co2 Cl2 2.2868(10) . ? Co2 O1 2.295(2) . ? Co2 N6 2.325(3) . ? N5 Si2 1.718(3) . ? N6 C18 1.468(4) . ? N6 C17 1.473(4) . ? N6 Si2 1.759(3) . ? Si2 C15 1.852(4) . ? Si2 C16 1.860(4) . ? O1 C19 1.464(5) . ? O1 C22 1.466(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C20 1.477(7) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.337(9) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C22 1.449(7) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N4 133.23(11) . . ? N2 Co1 O1 96.29(10) . . ? N4 Co1 O1 90.29(10) . . ? N2 Co1 Cl1 120.25(8) . . ? N4 Co1 Cl1 105.81(8) . . ? O1 Co1 Cl1 90.99(7) . . ? N2 Co1 N3 74.12(10) . . ? N4 Co1 N3 93.52(11) . . ? O1 Co1 N3 169.64(9) . . ? Cl1 Co1 N3 97.21(8) . . ? C1 N1 C5 119.7(3) . . ? C1 N1 Co2 122.1(2) . . ? C5 N1 Co2 117.5(2) . . ? C1 N2 Si1 127.0(2) . . ? C1 N2 Co1 135.2(2) . . ? Si1 N2 Co1 96.67(12) . . ? C9 N3 C8 109.5(3) . . ? C9 N3 Si1 118.6(3) . . ? C8 N3 Si1 114.6(2) . . ? C9 N3 Co1 119.8(2) . . ? C8 N3 Co1 107.5(2) . . ? Si1 N3 Co1 84.78(11) . . ? N2 Si1 N3 96.93(13) . . ? N2 Si1 C6 112.61(19) . . ? N3 Si1 C6 109.27(18) . . ? N2 Si1 C7 114.57(18) . . ? N3 Si1 C7 112.40(19) . . ? C6 Si1 C7 110.4(3) . . ? N2 C1 N1 117.7(3) . . ? N2 C1 C2 123.9(3) . . ? N1 C1 C2 118.4(3) . . ? C3 C2 C1 121.0(3) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 120.0(3) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 117.6(3) . . ? C5 C4 H4 121.2 . . ? C3 C4 H4 121.2 . . ? N1 C5 C4 123.3(3) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 N4 123.7(3) . . ? C11 C10 H10 118.2 . . ? N4 C10 H10 118.2 . . ? C10 C11 C12 118.1(3) . . ? C10 C11 H11 121.0 . . ? C12 C11 H11 121.0 . . ? C13 C12 C11 119.6(3) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C14 120.7(3) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? N5 C14 N4 117.9(3) . . ? N5 C14 C13 123.6(3) . . ? N4 C14 C13 118.5(3) . . ? N5 Co2 N1 132.93(11) . . ? N5 Co2 Cl2 119.06(8) . . ? N1 Co2 Cl2 107.17(8) . . ? N5 Co2 O1 98.14(10) . . ? N1 Co2 O1 88.89(10) . . ? Cl2 Co2 O1 91.10(6) . . ? N5 Co2 N6 73.97(10) . . ? N1 Co2 N6 92.31(10) . . ? Cl2 Co2 N6 97.86(7) . . ? O1 Co2 N6 170.16(9) . . ? C14 N4 C10 119.4(3) . . ? C14 N4 Co1 121.8(2) . . ? C10 N4 Co1 118.1(2) . . ? C14 N5 Si2 127.0(2) . . ? C14 N5 Co2 134.4(2) . . ? Si2 N5 Co2 97.20(12) . . ? C18 N6 C17 109.6(3) . . ? C18 N6 Si2 113.8(2) . . ? C17 N6 Si2 119.5(2) . . ? C18 N6 Co2 108.0(2) . . ? C17 N6 Co2 119.2(2) . . ? Si2 N6 Co2 84.54(10) . . ? N5 Si2 N6 96.96(13) . . ? N5 Si2 C15 114.13(18) . . ? N6 Si2 C15 112.32(19) . . ? N5 Si2 C16 112.41(19) . . ? N6 Si2 C16 109.48(18) . . ? C15 Si2 C16 110.8(3) . . ? C19 O1 C22 108.0(3) . . ? C19 O1 Co1 115.7(2) . . ? C22 O1 Co1 114.3(2) . . ? C19 O1 Co2 115.6(2) . . ? C22 O1 Co2 115.8(2) . . ? Co1 O1 Co2 86.66(8) . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 H17A 109.5 . . ? N6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N6 C18 H18A 109.5 . . ? N6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C19 C20 104.8(4) . . ? O1 C19 H19A 110.8 . . ? C20 C19 H19A 110.8 . . ? O1 C19 H19B 110.8 . . ? C20 C19 H19B 110.8 . . ? H19A C19 H19B 108.9 . . ? C21 C20 C19 110.2(5) . . ? C21 C20 H20A 109.6 . . ? C19 C20 H20A 109.6 . . ? C21 C20 H20B 109.6 . . ? C19 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C20 C21 C22 110.8(5) . . ? C20 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C21 C22 O1 105.4(5) . . ? C21 C22 H22A 110.7 . . ? O1 C22 H22A 110.7 . . ? C21 C22 H22B 110.7 . . ? O1 C22 H22B 110.7 . . ? H22A C22 H22B 108.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.510 _refine_diff_density_min -0.901 _refine_diff_density_rms 0.065