# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2264 data_may497-MFL2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '[{ZrCl2(thf)(C6H4(NSiMe2vinyl)2)}2]' _chemical_formula_moiety 'C36 H60 Cl4 N4 O2 Si4 Zr2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H60 Cl4 N4 O2 Si4 Zr2' _chemical_formula_weight 1017.48 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Zr' 'Zr' -2.9673 0.5597 '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)/n 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 9.836(4) _cell_length_b 13.669(4) _cell_length_c 18.534(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.90(3) _cell_angle_gamma 90.00 _cell_volume 2486.1(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method ? _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.763 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Enraf-Nonius CAD4' _diffrn_measurement_method 'omega-2theta scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3692 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0812 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 22.98 _reflns_number_total 3449 _reflns_number_observed 2212 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+0.8334P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3449 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0946 _refine_ls_R_factor_obs 0.0479 _refine_ls_wR_factor_all 0.1071 _refine_ls_wR_factor_obs 0.0895 _refine_ls_goodness_of_fit_all 1.020 _refine_ls_goodness_of_fit_obs 1.084 _refine_ls_restrained_S_all 1.020 _refine_ls_restrained_S_obs 1.084 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zr Zr 0.03354(6) 0.61414(4) 0.06980(3) 0.0498(2) Uani 1 d . . Cl1 Cl -0.1586(2) 0.69774(13) 0.01127(10) 0.0758(6) Uani 1 d . . Cl2 Cl 0.1019(2) 0.55659(11) -0.06056(8) 0.0570(4) Uani 1 d . . Si1 Si 0.2278(2) 0.82249(14) 0.03573(11) 0.0665(6) Uani 1 d . . Si2 Si -0.1404(2) 0.6248(2) 0.22896(11) 0.0709(6) Uani 1 d . . O1 O 0.2044(4) 0.5104(3) 0.1021(2) 0.0533(11) Uani 1 d . . N1 N 0.1698(5) 0.7268(3) 0.0874(2) 0.0486(13) Uani 1 d . . N2 N 0.0005(5) 0.6354(3) 0.1764(2) 0.0506(13) Uani 1 d . . C1 C 0.2185(6) 0.7127(4) 0.1611(3) 0.0469(15) Uani 1 d . . C2 C 0.1302(6) 0.6661(4) 0.2067(3) 0.049(2) Uani 1 d . . C3 C 0.1763(7) 0.6472(4) 0.2783(3) 0.056(2) Uani 1 d . . H3 H 0.1196(7) 0.6146(4) 0.3085(3) 0.067 Uiso 1 calc R . C4 C 0.3038(7) 0.6759(5) 0.3049(4) 0.066(2) Uani 1 d . . H4 H 0.3317(7) 0.6644(5) 0.3531(4) 0.079 Uiso 1 calc R . C5 C 0.3896(7) 0.7214(5) 0.2607(4) 0.064(2) Uani 1 d . . H5 H 0.4762(7) 0.7404(5) 0.2786(4) 0.077 Uiso 1 calc R . C6 C 0.3474(6) 0.7391(4) 0.1895(3) 0.056(2) Uani 1 d . . H6 H 0.4069(6) 0.7695(4) 0.1597(3) 0.068 Uiso 1 calc R . C7 C 0.3993(9) 0.7911(7) 0.0067(5) 0.112(3) Uani 1 d . . H7 H 0.4103(9) 0.7269(7) -0.0085(5) 0.134 Uiso 1 calc R . C8 C 0.4993(13) 0.8433(9) 0.0050(7) 0.161(5) Uani 1 d . . H8B H 0.4951(13) 0.9083(9) 0.0195(7) 0.193 Uiso 1 calc R . H8A H 0.5799(13) 0.8182(9) -0.0109(7) 0.193 Uiso 1 calc R . C9 C 0.1130(8) 0.8358(5) -0.0470(4) 0.091(3) Uani 1 d . . H9C H 0.1115(8) 0.7757(5) -0.0739(4) 0.137 Uiso 1 calc R . H9B H 0.1453(8) 0.8877(5) -0.0763(4) 0.137 Uiso 1 calc R . H9A H 0.0226(8) 0.8508(5) -0.0339(4) 0.137 Uiso 1 calc R . C10 C 0.2300(10) 0.9386(5) 0.0871(4) 0.109(3) Uani 1 d . . H10C H 0.2893(10) 0.9321(5) 0.1301(4) 0.163 Uiso 1 calc R . H10B H 0.1395(10) 0.9536(5) 0.1001(4) 0.163 Uiso 1 calc R . H10A H 0.2623(10) 0.9904(5) 0.0577(4) 0.163 Uiso 1 calc R . C11 C -0.1306(12) 0.5096(12) 0.2810(9) 0.166(6) Uani 1 d . . H11 H -0.0584(12) 0.4757(12) 0.2628(9) 0.199 Uiso 1 calc R . C12 C -0.1619(20) 0.4678(15) 0.3168(12) 0.292(12) Uani 1 d . . H12B H -0.2350(20) 0.4867(15) 0.3429(12) 0.350 Uiso 1 calc R . H12A H -0.1197(20) 0.4078(15) 0.3259(12) 0.350 Uiso 1 calc R . C13 C -0.1504(7) 0.7337(6) 0.2887(4) 0.099(3) Uani 1 d . . H13C H -0.0691(7) 0.7378(6) 0.3203(4) 0.149 Uiso 1 calc R . H13B H -0.2281(7) 0.7277(6) 0.3170(4) 0.149 Uiso 1 calc R . H13A H -0.1591(7) 0.7918(6) 0.2596(4) 0.149 Uiso 1 calc R . C14 C -0.2972(7) 0.6187(6) 0.1689(4) 0.103(3) Uani 1 d . . H14C H -0.3062(7) 0.6776(6) 0.1407(4) 0.154 Uiso 1 calc R . H14B H -0.3745(7) 0.6119(6) 0.1974(4) 0.154 Uiso 1 calc R . H14A H -0.2926(7) 0.5634(6) 0.1372(4) 0.154 Uiso 1 calc R . C15 C 0.3418(6) 0.5114(5) 0.0770(4) 0.067(2) Uani 1 d . . H15B H 0.3846(6) 0.5745(5) 0.0862(4) 0.081 Uiso 1 calc R . H15A H 0.3396(6) 0.4980(5) 0.0255(4) 0.081 Uiso 1 calc R . C16 C 0.4168(7) 0.4335(5) 0.1186(4) 0.086(2) Uani 1 d . . H16B H 0.5115(7) 0.4517(5) 0.1289(4) 0.103 Uiso 1 calc R . H16A H 0.4132(7) 0.3723(5) 0.0920(4) 0.103 Uiso 1 calc R . C17 C 0.3455(8) 0.4246(6) 0.1864(4) 0.087(2) Uani 1 d . . H17B H 0.3751(8) 0.4749(6) 0.2210(4) 0.105 Uiso 1 calc R . H17A H 0.3603(8) 0.3608(6) 0.2085(4) 0.105 Uiso 1 calc R . C18 C 0.2001(7) 0.4383(5) 0.1603(3) 0.064(2) Uani 1 d . . H18B H 0.1606(7) 0.3773(5) 0.1423(3) 0.076 Uiso 1 calc R . H18A H 0.1470(7) 0.4626(5) 0.1987(3) 0.076 Uiso 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 Zr 0.0506(4) 0.0454(3) 0.0512(4) -0.0089(3) -0.0111(3) 0.0010(4) Cl1 0.0695(12) 0.0715(12) 0.0820(12) -0.0108(10) -0.0273(10) 0.0152(10) Cl2 0.0601(10) 0.0560(10) 0.0541(9) -0.0078(8) -0.0027(8) -0.0078(9) Si1 0.0778(14) 0.0557(12) 0.0648(12) 0.0040(10) -0.0046(11) -0.0078(11) Si2 0.0604(12) 0.0785(15) 0.0742(13) -0.0060(12) 0.0083(10) -0.0092(12) O1 0.054(3) 0.048(2) 0.056(3) 0.001(2) -0.009(2) 0.004(2) N1 0.051(3) 0.054(3) 0.040(3) -0.005(2) -0.006(2) -0.002(3) N2 0.047(3) 0.048(3) 0.056(3) -0.004(2) -0.004(2) -0.003(3) C1 0.045(4) 0.048(4) 0.047(4) -0.008(3) -0.004(3) -0.003(3) C2 0.051(4) 0.042(4) 0.053(4) -0.015(3) -0.005(3) 0.002(3) C3 0.063(4) 0.054(4) 0.049(4) -0.004(3) -0.006(3) 0.000(3) C4 0.069(5) 0.076(5) 0.049(4) -0.008(4) -0.016(4) -0.002(4) C5 0.054(4) 0.069(5) 0.068(5) -0.017(4) -0.015(4) 0.007(4) C6 0.050(4) 0.061(4) 0.058(4) -0.007(3) 0.001(3) -0.011(3) C7 0.099(8) 0.112(8) 0.125(8) 0.042(6) 0.018(6) -0.027(6) C8 0.135(10) 0.160(11) 0.187(12) 0.030(9) 0.018(9) 0.019(9) C9 0.108(6) 0.095(6) 0.070(5) 0.024(4) -0.005(5) -0.013(5) C10 0.165(9) 0.055(5) 0.103(6) -0.003(5) -0.016(6) -0.006(6) C11 0.078(7) 0.198(15) 0.227(16) 0.100(11) 0.054(8) -0.015(8) C12 0.301(26) 0.237(22) 0.350(30) 0.146(19) 0.111(21) 0.046(19) C13 0.079(6) 0.139(7) 0.080(5) -0.039(5) 0.015(5) -0.007(5) C14 0.057(5) 0.135(7) 0.117(7) -0.038(6) 0.011(5) -0.017(5) C15 0.047(4) 0.071(5) 0.084(5) -0.001(4) 0.000(4) 0.003(4) C16 0.056(5) 0.076(5) 0.122(7) 0.001(5) -0.023(5) 0.010(4) C17 0.080(6) 0.078(5) 0.099(6) 0.022(5) -0.033(5) 0.012(5) C18 0.075(5) 0.050(4) 0.065(4) 0.003(4) -0.004(4) 0.001(4) _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 Zr N2 2.044(5) . ? Zr N1 2.053(5) . ? Zr O1 2.249(4) . ? Zr Cl1 2.403(2) . ? Zr Cl2 2.670(2) . ? Zr Cl2 2.687(2) 3_565 ? Zr C2 2.742(6) . ? Zr C1 2.751(6) . ? Cl2 Zr 2.687(2) 3_565 ? Si1 N1 1.740(5) . ? Si1 C9 1.851(7) . ? Si1 C10 1.850(7) . ? Si1 C7 1.855(10) . ? Si2 N2 1.753(5) . ? Si2 C14 1.842(7) . ? Si2 C11 1.846(13) . ? Si2 C13 1.862(7) . ? O1 C15 1.459(7) . ? O1 C18 1.463(7) . ? N1 C1 1.430(6) . ? N2 C2 1.422(7) . ? C1 C6 1.387(7) . ? C1 C2 1.405(8) . ? C2 C3 1.397(8) . ? C3 C4 1.373(8) . ? C4 C5 1.366(9) . ? C5 C6 1.377(8) . ? C7 C8 1.218(12) . ? C11 C12 0.942(15) . ? C15 C16 1.482(8) . ? C16 C17 1.486(10) . ? C17 C18 1.491(9) . ? 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 Zr N1 83.4(2) . . ? N2 Zr O1 89.8(2) . . ? N1 Zr O1 87.9(2) . . ? N2 Zr Cl1 101.35(14) . . ? N1 Zr Cl1 101.53(14) . . ? O1 Zr Cl1 166.05(10) . . ? N2 Zr Cl2 169.29(13) . . ? N1 Zr Cl2 99.37(13) . . ? O1 Zr Cl2 79.96(11) . . ? Cl1 Zr Cl2 88.29(6) . . ? N2 Zr Cl2 94.25(13) . 3_565 ? N1 Zr Cl2 167.72(13) . 3_565 ? O1 Zr Cl2 80.05(11) . 3_565 ? Cl1 Zr Cl2 90.75(6) . 3_565 ? Cl2 Zr Cl2 80.83(6) . 3_565 ? N2 Zr C2 30.3(2) . . ? N1 Zr C2 58.5(2) . . ? O1 Zr C2 73.2(2) . . ? Cl1 Zr C2 120.46(13) . . ? Cl2 Zr C2 145.18(14) . . ? Cl2 Zr C2 115.04(14) 3_565 . ? N2 Zr C1 58.5(2) . . ? N1 Zr C1 30.4(2) . . ? O1 Zr C1 72.2(2) . . ? Cl1 Zr C1 120.76(13) . . ? Cl2 Zr C1 120.28(13) . . ? Cl2 Zr C1 140.25(13) 3_565 . ? C2 Zr C1 29.6(2) . . ? Zr Cl2 Zr 99.17(6) . 3_565 ? N1 Si1 C9 109.0(3) . . ? N1 Si1 C10 110.8(3) . . ? C9 Si1 C10 109.1(4) . . ? N1 Si1 C7 108.9(3) . . ? C9 Si1 C7 107.3(4) . . ? C10 Si1 C7 111.6(5) . . ? N2 Si2 C14 109.2(3) . . ? N2 Si2 C11 110.3(5) . . ? C14 Si2 C11 106.8(5) . . ? N2 Si2 C13 109.9(3) . . ? C14 Si2 C13 108.6(3) . . ? C11 Si2 C13 112.0(6) . . ? C15 O1 C18 108.4(5) . . ? C15 O1 Zr 126.9(4) . . ? C18 O1 Zr 124.2(4) . . ? C1 N1 Si1 121.7(4) . . ? C1 N1 Zr 102.9(3) . . ? Si1 N1 Zr 135.4(2) . . ? C2 N2 Si2 121.7(4) . . ? C2 N2 Zr 103.1(4) . . ? Si2 N2 Zr 135.2(3) . . ? C6 C1 C2 118.4(5) . . ? C6 C1 N1 124.5(6) . . ? C2 C1 N1 117.1(5) . . ? C6 C1 Zr 155.5(4) . . ? C2 C1 Zr 74.8(3) . . ? N1 C1 Zr 46.7(2) . . ? C3 C2 C1 118.8(6) . . ? C3 C2 N2 123.0(6) . . ? C1 C2 N2 118.1(5) . . ? C3 C2 Zr 154.2(4) . . ? C1 C2 Zr 75.5(3) . . ? N2 C2 Zr 46.5(3) . . ? C4 C3 C2 121.1(6) . . ? C5 C4 C3 120.1(6) . . ? C4 C5 C6 119.8(6) . . ? C5 C6 C1 121.7(6) . . ? C8 C7 Si1 128.6(11) . . ? C12 C11 Si2 151.2(24) . . ? O1 C15 C16 105.5(5) . . ? C15 C16 C17 104.6(6) . . ? C16 C17 C18 102.2(6) . . ? O1 C18 C17 104.4(5) . . ? _refine_diff_density_max 0.273 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.064 #===END data_jun397-MFL4 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '[{Zr(C6H4(NSiMe2vinyl)2)(NMe2)2}2]' _chemical_formula_moiety 'C36 H68 N8 Si4 Zr2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H68 N8 Si4 Zr2' _chemical_formula_weight 907.78 _chemical_melting_point ? _chemical_compound_source ? 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' 'Si' 'Si' 0.0817 0.0704 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 18.596(11) _cell_length_b 10.248(4) _cell_length_c 25.869(13) _cell_angle_alpha 90.00 _cell_angle_beta 111.00(4) _cell_angle_gamma 90.00 _cell_volume 4602.5(40) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method ? _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.590 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.35 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Enraf-Nonius CAD4' _diffrn_measurement_method 'omega-2theta scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6614 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 22.99 _reflns_number_total 6398 _reflns_number_observed 5776 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1522P)^2^+5.3904P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6398 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0750 _refine_ls_R_factor_obs 0.0704 _refine_ls_wR_factor_all 0.1995 _refine_ls_wR_factor_obs 0.1918 _refine_ls_goodness_of_fit_all 1.100 _refine_ls_goodness_of_fit_obs 1.116 _refine_ls_restrained_S_all 1.100 _refine_ls_restrained_S_obs 1.116 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zr1 Zr 0.26431(3) 0.16277(4) 0.55509(2) 0.0167(2) Uani 1 d . . Zr2 Zr 0.25288(3) 0.21486(5) 0.41392(2) 0.0163(2) Uani 1 d . . Si1 Si 0.14932(8) -0.0734(2) 0.59405(6) 0.0293(4) Uani 1 d . . Si2 Si 0.42416(9) 0.1907(2) 0.68420(6) 0.0259(4) Uani 1 d . . Si3 Si 0.09498(9) 0.16489(15) 0.28892(6) 0.0261(4) Uani 1 d . . Si4 Si 0.31934(9) 0.53320(14) 0.39942(6) 0.0263(4) Uani 1 d . . N1 N 0.2280(2) -0.0131(4) 0.5807(2) 0.0213(10) Uani 1 d . . N2 N 0.3646(2) 0.1171(4) 0.6238(2) 0.0221(10) Uani 1 d . . N3 N 0.1423(2) 0.2405(4) 0.3521(2) 0.0218(10) Uani 1 d . . N4 N 0.2531(2) 0.4184(4) 0.4039(2) 0.0207(9) Uani 1 d . . N5 N 0.3403(2) 0.2203(4) 0.5067(2) 0.0215(10) Uani 1 d . . N6 N 0.1965(2) 0.1034(4) 0.4648(2) 0.0202(9) Uani 1 d . . N7 N 0.2106(3) 0.3220(4) 0.5700(2) 0.0272(11) Uani 1 d . . N8 N 0.3129(3) 0.1183(4) 0.3743(2) 0.0261(10) Uani 1 d . . C1 C 0.2961(3) -0.0873(5) 0.5943(2) 0.0220(11) Uani 1 d . . C2 C 0.3673(3) -0.0188(5) 0.6172(2) 0.0198(11) Uani 1 d . . C3 C 0.4358(3) -0.0917(6) 0.6306(2) 0.0273(12) Uani 1 d . . H3 H 0.4840(3) -0.0482(6) 0.6455(2) 0.033 Uiso 1 calc R . C4 C 0.4345(4) -0.2245(6) 0.6225(2) 0.0356(15) Uani 1 d . . H4 H 0.4817(4) -0.2711(6) 0.6322(2) 0.043 Uiso 1 calc R . C5 C 0.3655(4) -0.2911(6) 0.6007(2) 0.0333(14) Uani 1 d . . H5 H 0.3652(4) -0.3830(6) 0.5958(2) 0.040 Uiso 1 calc R . C6 C 0.2966(3) -0.2222(5) 0.5859(2) 0.0273(13) Uani 1 d . . H6 H 0.2492(3) -0.2674(5) 0.5698(2) 0.033 Uiso 1 calc R . C7 C 0.1822(4) -0.1554(9) 0.6628(3) 0.063(2) Uani 1 d . . H7A H 0.2166(4) -0.2279(9) 0.6628(3) 0.095 Uiso 1 calc R . H7B H 0.1375(4) -0.1888(9) 0.6702(3) 0.095 Uiso 1 calc R . H7C H 0.2099(4) -0.0925(9) 0.6916(3) 0.095 Uiso 1 calc R . C8 C 0.0837(3) 0.0653(7) 0.5929(3) 0.042(2) Uani 1 d . . H8A H 0.0668(3) 0.1073(7) 0.5565(3) 0.064 Uiso 1 calc R . H8B H 0.1112(3) 0.1289(7) 0.6214(3) 0.064 Uiso 1 calc R . H8C H 0.0388(3) 0.0325(7) 0.6002(3) 0.064 Uiso 1 calc R . C9 C 0.0921(4) -0.1936(7) 0.5399(3) 0.046(2) Uani 1 d . . H9 H 0.0787(4) -0.1660(7) 0.5026(3) 0.055 Uiso 1 calc R . C10 C 0.0686(5) -0.3082(8) 0.5468(4) 0.068(2) Uani 1 d . . H10A H 0.0799(5) -0.3416(8) 0.5831(4) 0.082 Uiso 1 calc R . H10B H 0.0399(5) -0.3593(8) 0.5156(4) 0.082 Uiso 1 calc R . C11 C 0.4172(3) 0.0988(7) 0.7444(2) 0.040(2) Uani 1 d . . H11A H 0.4340(3) 0.0085(7) 0.7432(2) 0.060 Uiso 1 calc R . H11B H 0.3637(3) 0.0994(7) 0.7427(2) 0.060 Uiso 1 calc R . H11C H 0.4502(3) 0.1402(7) 0.7789(2) 0.060 Uiso 1 calc R . C12 C 0.3926(4) 0.3619(7) 0.6859(3) 0.055(2) Uani 1 d . . H12A H 0.3964(4) 0.4096(7) 0.6542(3) 0.082 Uiso 1 calc R . H12B H 0.4256(4) 0.4036(7) 0.7203(3) 0.082 Uiso 1 calc R . H12C H 0.3391(4) 0.3628(7) 0.6842(3) 0.082 Uiso 1 calc R . C13 C 0.5273(3) 0.1985(6) 0.6897(2) 0.0357(14) Uani 1 d . . H13 H 0.5367(3) 0.2131(6) 0.6565(2) 0.043 Uiso 1 calc R . C14 C 0.5872(4) 0.1859(7) 0.7349(3) 0.045(2) Uani 1 d . . H14A H 0.5807(4) 0.1712(7) 0.7692(3) 0.054 Uiso 1 calc R . H14B H 0.6376(4) 0.1914(7) 0.7336(3) 0.054 Uiso 1 calc R . C15 C 0.1173(3) 0.3603(5) 0.3660(2) 0.0227(12) Uani 1 d . . C16 C 0.1751(3) 0.4556(5) 0.3924(2) 0.0231(12) Uani 1 d . . C17 C 0.1524(3) 0.5773(5) 0.4068(2) 0.0290(13) Uani 1 d . . H17 H 0.1904(3) 0.6415(5) 0.4239(2) 0.035 Uiso 1 calc R . C18 C 0.0761(4) 0.6044(6) 0.3964(2) 0.0362(14) Uani 1 d . . H18 H 0.0618(4) 0.6874(6) 0.4059(2) 0.043 Uiso 1 calc R . C19 C 0.0205(4) 0.5123(6) 0.3723(3) 0.040(2) Uani 1 d . . H19 H -0.0320(4) 0.5320(6) 0.3654(3) 0.048 Uiso 1 calc R . C20 C 0.0404(3) 0.3909(6) 0.3580(2) 0.0297(13) Uani 1 d . . H20 H 0.0014(3) 0.3273(6) 0.3425(2) 0.036 Uiso 1 calc R . C21 C 0.1050(4) 0.2676(7) 0.2324(2) 0.044(2) Uani 1 d . . H21A H 0.0808(4) 0.3527(7) 0.2321(2) 0.066 Uiso 1 calc R . H21B H 0.0798(4) 0.2242(7) 0.1967(2) 0.066 Uiso 1 calc R . H21C H 0.1597(4) 0.2800(7) 0.2387(2) 0.066 Uiso 1 calc R . C22 C -0.0102(4) 0.1318(8) 0.2725(3) 0.055(2) Uani 1 d . . H22A H -0.0166(4) 0.0778(8) 0.3018(3) 0.082 Uiso 1 calc R . H22B H -0.0312(4) 0.0858(8) 0.2370(3) 0.082 Uiso 1 calc R . H22C H -0.0375(4) 0.2146(8) 0.2701(3) 0.082 Uiso 1 calc R . C23 C 0.1410(4) 0.0028(6) 0.2896(2) 0.041(2) Uani 1 d . . H23 H 0.1457(4) -0.0538(6) 0.3198(2) 0.049 Uiso 1 calc R . C24 C 0.1674(5) -0.0394(10) 0.2519(4) 0.081(3) Uani 1 d . . H24A H 0.1638(5) 0.0142(10) 0.2211(4) 0.098 Uiso 1 calc R . H24B H 0.1901(5) -0.1235(10) 0.2554(4) 0.098 Uiso 1 calc R . C25 C 0.2771(4) 0.6290(7) 0.3348(3) 0.051(2) Uani 1 d . . H25A H 0.2303(4) 0.6730(7) 0.3348(3) 0.076 Uiso 1 calc R . H25B H 0.2642(4) 0.5704(7) 0.3028(3) 0.076 Uiso 1 calc R . H25C H 0.3145(4) 0.6942(7) 0.3326(3) 0.076 Uiso 1 calc R . C26 C 0.4079(3) 0.4493(7) 0.3999(3) 0.042(2) Uani 1 d . . H26A H 0.4300(3) 0.3988(7) 0.4341(3) 0.062 Uiso 1 calc R . H26B H 0.4455(3) 0.5143(7) 0.3978(3) 0.062 Uiso 1 calc R . H26C H 0.3952(3) 0.3905(7) 0.3680(3) 0.062 Uiso 1 calc R . C27 C 0.3490(3) 0.6478(6) 0.4604(2) 0.0332(14) Uani 1 d . . H27 H 0.3163(3) 0.6529(6) 0.4814(2) 0.040 Uiso 1 calc R . C28 C 0.4094(4) 0.7195(7) 0.4759(3) 0.046(2) Uani 1 d . . H28A H 0.4437(4) 0.7174(7) 0.4561(3) 0.055 Uiso 1 calc R . H28B H 0.4200(4) 0.7747(7) 0.5073(3) 0.055 Uiso 1 calc R . C29 C 0.4030(3) 0.1264(6) 0.5122(2) 0.0299(13) Uani 1 d . . H29A H 0.3807(3) 0.0413(6) 0.4976(2) 0.045 Uiso 1 calc R . H29B H 0.4355(3) 0.1175(6) 0.5513(2) 0.045 Uiso 1 calc R . H29C H 0.4341(3) 0.1580(6) 0.4912(2) 0.045 Uiso 1 calc R . C30 C 0.3773(3) 0.3461(6) 0.5292(2) 0.0312(14) Uani 1 d . . H30A H 0.3375(3) 0.4114(6) 0.5264(2) 0.047 Uiso 1 calc R . H30B H 0.4087(3) 0.3755(6) 0.5081(2) 0.047 Uiso 1 calc R . H30C H 0.4101(3) 0.3349(6) 0.5682(2) 0.047 Uiso 1 calc R . C31 C 0.2094(4) -0.0335(6) 0.4525(2) 0.0344(14) Uani 1 d . . H31A H 0.2643(4) -0.0475(6) 0.4601(2) 0.052 Uiso 1 calc R . H31B H 0.1801(4) -0.0520(6) 0.4134(2) 0.052 Uiso 1 calc R . H31C H 0.1922(4) -0.0918(6) 0.4758(2) 0.052 Uiso 1 calc R . C32 C 0.1135(3) 0.1196(6) 0.4527(2) 0.0299(13) Uani 1 d . . H32A H 0.1030(3) 0.2098(6) 0.4605(2) 0.045 Uiso 1 calc R . H32B H 0.0970(3) 0.0600(6) 0.4759(2) 0.045 Uiso 1 calc R . H32C H 0.0850(3) 0.0999(6) 0.4136(2) 0.045 Uiso 1 calc R . C33 C 0.1888(4) 0.3555(7) 0.6172(3) 0.044(2) Uani 1 d . . H33A H 0.2072(4) 0.2875(7) 0.6456(3) 0.065 Uiso 1 calc R . H33B H 0.1326(4) 0.3620(7) 0.6051(3) 0.065 Uiso 1 calc R . H33C H 0.2120(4) 0.4393(7) 0.6326(3) 0.065 Uiso 1 calc R . C34 C 0.1845(4) 0.4204(6) 0.5271(3) 0.043(2) Uani 1 d . . H34A H 0.1999(4) 0.3955(6) 0.4959(3) 0.064 Uiso 1 calc R . H34B H 0.2077(4) 0.5046(6) 0.5419(3) 0.064 Uiso 1 calc R . H34C H 0.1283(4) 0.4274(6) 0.5143(3) 0.064 Uiso 1 calc R . C35 C 0.3203(4) 0.1820(6) 0.3254(2) 0.0342(14) Uani 1 d . . H35A H 0.2969(4) 0.2689(6) 0.3207(2) 0.051 Uiso 1 calc R . H35B H 0.2940(4) 0.1293(6) 0.2923(2) 0.051 Uiso 1 calc R . H35C H 0.3750(4) 0.1901(6) 0.3305(2) 0.051 Uiso 1 calc R . C36 C 0.3477(4) -0.0109(6) 0.3811(3) 0.041(2) Uani 1 d . . H36A H 0.3428(4) -0.0534(6) 0.4136(3) 0.061 Uiso 1 calc R . H36B H 0.4024(4) -0.0027(6) 0.3862(3) 0.061 Uiso 1 calc R . H36C H 0.3215(4) -0.0635(6) 0.3481(3) 0.061 Uiso 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 Zr1 0.0240(3) 0.0043(3) 0.0178(3) 0.0008(2) 0.0027(2) 0.0013(2) Zr2 0.0254(3) 0.0024(3) 0.0188(3) 0.0003(2) 0.0049(2) -0.0001(2) Si1 0.0313(8) 0.0245(9) 0.0299(8) 0.0090(7) 0.0083(7) -0.0042(7) Si2 0.0333(9) 0.0139(8) 0.0230(8) -0.0043(6) 0.0008(7) -0.0031(6) Si3 0.0352(9) 0.0162(9) 0.0212(8) -0.0033(6) 0.0034(7) -0.0057(6) Si4 0.0398(9) 0.0075(8) 0.0298(8) -0.0014(6) 0.0102(7) -0.0070(6) N1 0.025(2) 0.016(3) 0.019(2) 0.000(2) 0.005(2) 0.000(2) N2 0.028(2) 0.012(2) 0.021(2) 0.003(2) 0.003(2) 0.000(2) N3 0.029(2) 0.014(2) 0.017(2) 0.000(2) 0.002(2) -0.002(2) N4 0.029(2) 0.004(2) 0.026(2) 0.001(2) 0.004(2) -0.004(2) N5 0.026(2) 0.013(3) 0.022(2) 0.001(2) 0.005(2) -0.003(2) N6 0.026(2) 0.013(2) 0.018(2) 0.000(2) 0.004(2) -0.007(2) N7 0.040(3) 0.009(2) 0.030(2) 0.003(2) 0.008(2) 0.004(2) N8 0.040(3) 0.012(2) 0.030(2) -0.003(2) 0.017(2) 0.001(2) C1 0.036(3) 0.009(3) 0.016(2) 0.004(2) 0.003(2) 0.001(2) C2 0.028(3) 0.010(3) 0.016(2) 0.003(2) 0.001(2) 0.000(2) C3 0.028(3) 0.020(3) 0.025(3) 0.003(2) -0.002(2) 0.004(2) C4 0.047(4) 0.026(4) 0.029(3) 0.003(3) 0.009(3) 0.019(3) C5 0.056(4) 0.008(3) 0.029(3) -0.001(2) 0.007(3) 0.006(3) C6 0.040(3) 0.014(3) 0.024(3) -0.001(2) 0.007(2) -0.005(2) C7 0.056(4) 0.084(7) 0.051(4) 0.038(4) 0.021(4) 0.007(4) C8 0.031(3) 0.050(4) 0.048(4) -0.004(3) 0.015(3) -0.007(3) C9 0.041(4) 0.031(4) 0.061(4) 0.001(3) 0.013(3) -0.011(3) C10 0.076(5) 0.033(5) 0.105(7) -0.008(4) 0.044(5) -0.013(4) C11 0.042(3) 0.047(4) 0.028(3) -0.010(3) 0.010(3) -0.008(3) C12 0.058(4) 0.024(4) 0.061(4) -0.020(3) -0.003(4) -0.001(3) C13 0.039(3) 0.033(4) 0.031(3) -0.001(3) 0.008(3) -0.010(3) C14 0.042(4) 0.045(4) 0.045(4) -0.002(3) 0.011(3) -0.010(3) C15 0.037(3) 0.008(3) 0.020(2) 0.003(2) 0.005(2) 0.005(2) C16 0.034(3) 0.009(3) 0.022(2) 0.003(2) 0.005(2) 0.001(2) C17 0.044(3) 0.009(3) 0.030(3) 0.002(2) 0.008(2) 0.004(2) C18 0.055(4) 0.012(3) 0.039(3) 0.005(3) 0.014(3) 0.015(3) C19 0.039(3) 0.035(4) 0.044(3) 0.008(3) 0.014(3) 0.017(3) C20 0.031(3) 0.023(3) 0.032(3) -0.001(2) 0.007(2) 0.001(2) C21 0.074(5) 0.026(4) 0.029(3) 0.003(3) 0.013(3) -0.001(3) C22 0.047(4) 0.064(5) 0.052(4) -0.029(4) 0.016(3) -0.026(4) C23 0.065(4) 0.023(3) 0.026(3) -0.006(3) 0.007(3) -0.003(3) C24 0.094(6) 0.062(6) 0.064(5) -0.008(5) -0.001(5) 0.010(5) C25 0.080(5) 0.027(4) 0.039(3) 0.011(3) 0.015(3) -0.009(4) C26 0.043(3) 0.037(4) 0.047(4) -0.017(3) 0.019(3) -0.013(3) C27 0.044(3) 0.015(3) 0.037(3) -0.005(2) 0.011(3) -0.004(3) C28 0.051(4) 0.039(4) 0.039(4) -0.012(3) 0.006(3) -0.012(3) C29 0.028(3) 0.024(3) 0.036(3) 0.003(3) 0.009(2) 0.001(2) C30 0.035(3) 0.025(3) 0.026(3) -0.002(2) 0.001(2) -0.014(2) C31 0.048(3) 0.023(3) 0.030(3) -0.005(2) 0.010(3) -0.010(3) C32 0.029(3) 0.030(3) 0.027(3) 0.007(2) 0.006(2) -0.007(2) C33 0.064(4) 0.035(4) 0.040(3) -0.010(3) 0.029(3) 0.010(3) C34 0.058(4) 0.019(3) 0.047(4) 0.006(3) 0.012(3) 0.009(3) C35 0.051(4) 0.021(3) 0.039(3) -0.005(3) 0.026(3) -0.003(3) C36 0.055(4) 0.020(3) 0.057(4) 0.000(3) 0.032(3) 0.011(3) _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 Zr1 N7 2.021(5) . ? Zr1 N1 2.112(4) . ? Zr1 N2 2.116(4) . ? Zr1 N5 2.276(4) . ? Zr1 N6 2.304(4) . ? Zr1 C2 2.739(5) . ? Zr1 C1 2.742(5) . ? Zr1 Zr2 3.621(2) . ? Zr2 N8 2.024(4) . ? Zr2 N4 2.102(4) . ? Zr2 N3 2.120(4) . ? Zr2 N6 2.263(4) . ? Zr2 N5 2.369(4) . ? Zr2 C15 2.806(5) . ? Zr2 C16 2.813(5) . ? Si1 N1 1.734(4) . ? Si1 C7 1.862(7) . ? Si1 C8 1.867(7) . ? Si1 C9 1.882(7) . ? Si2 N2 1.732(4) . ? Si2 C12 1.856(7) . ? Si2 C11 1.864(6) . ? Si2 C13 1.873(6) . ? Si3 N3 1.737(4) . ? Si3 C21 1.864(6) . ? Si3 C23 1.865(7) . ? Si3 C22 1.877(7) . ? Si4 N4 1.736(4) . ? Si4 C25 1.853(6) . ? Si4 C26 1.855(6) . ? Si4 C27 1.884(6) . ? N1 C1 1.409(7) . ? N2 C2 1.405(7) . ? N3 C15 1.404(7) . ? N4 C16 1.425(7) . ? N5 C29 1.478(7) . ? N5 C30 1.479(7) . ? N6 C32 1.472(7) . ? N6 C31 1.477(7) . ? N7 C34 1.449(7) . ? N7 C33 1.458(7) . ? N8 C36 1.456(7) . ? N8 C35 1.474(7) . ? C1 C6 1.400(8) . ? C1 C2 1.426(7) . ? C2 C3 1.409(7) . ? C3 C4 1.376(9) . ? C4 C5 1.382(9) . ? C5 C6 1.391(8) . ? C9 C10 1.288(10) . ? C13 C14 1.300(9) . ? C15 C20 1.405(8) . ? C15 C16 1.432(8) . ? C16 C17 1.408(8) . ? C17 C18 1.374(8) . ? C18 C19 1.374(9) . ? C19 C20 1.386(9) . ? C23 C24 1.314(11) . ? C27 C28 1.281(9) . ? 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 N7 Zr1 N1 113.2(2) . . ? N7 Zr1 N2 111.4(2) . . ? N1 Zr1 N2 80.4(2) . . ? N7 Zr1 N5 110.0(2) . . ? N1 Zr1 N5 136.4(2) . . ? N2 Zr1 N5 89.1(2) . . ? N7 Zr1 N6 106.2(2) . . ? N1 Zr1 N6 88.41(15) . . ? N2 Zr1 N6 142.2(2) . . ? N5 Zr1 N6 74.49(15) . . ? N7 Zr1 C2 136.5(2) . . ? N1 Zr1 C2 58.1(2) . . ? N2 Zr1 C2 30.3(2) . . ? N5 Zr1 C2 93.3(2) . . ? N6 Zr1 C2 115.4(2) . . ? N7 Zr1 C1 137.7(2) . . ? N1 Zr1 C1 30.4(2) . . ? N2 Zr1 C1 58.3(2) . . ? N5 Zr1 C1 110.6(2) . . ? N6 Zr1 C1 95.48(15) . . ? C2 Zr1 C1 30.2(2) . . ? N7 Zr1 Zr2 102.68(13) . . ? N1 Zr1 Zr2 122.12(11) . . ? N2 Zr1 Zr2 126.49(12) . . ? N5 Zr1 Zr2 39.71(10) . . ? N6 Zr1 Zr2 37.15(10) . . ? C2 Zr1 Zr2 117.88(11) . . ? C1 Zr1 Zr2 115.97(10) . . ? N8 Zr2 N4 113.4(2) . . ? N8 Zr2 N3 103.9(2) . . ? N4 Zr2 N3 80.1(2) . . ? N8 Zr2 N6 120.1(2) . . ? N4 Zr2 N6 126.5(2) . . ? N3 Zr2 N6 88.6(2) . . ? N8 Zr2 N5 102.8(2) . . ? N4 Zr2 N5 94.05(15) . . ? N3 Zr2 N5 152.8(2) . . ? N6 Zr2 N5 73.49(15) . . ? N8 Zr2 C15 127.3(2) . . ? N4 Zr2 C15 57.3(2) . . ? N3 Zr2 C15 29.1(2) . . ? N6 Zr2 C15 89.7(2) . . ? N5 Zr2 C15 128.1(2) . . ? N8 Zr2 C16 131.8(2) . . ? N4 Zr2 C16 29.4(2) . . ? N3 Zr2 C16 56.7(2) . . ? N6 Zr2 C16 104.2(2) . . ? N5 Zr2 C16 107.28(15) . . ? C15 Zr2 C16 29.5(2) . . ? N8 Zr2 Zr1 126.52(13) . . ? N4 Zr2 Zr1 105.61(11) . . ? N3 Zr2 Zr1 117.99(12) . . ? N6 Zr2 Zr1 37.95(10) . . ? N5 Zr2 Zr1 37.87(11) . . ? C15 Zr2 Zr1 104.07(11) . . ? C16 Zr2 Zr1 99.71(10) . . ? N1 Si1 C7 109.9(3) . . ? N1 Si1 C8 108.6(3) . . ? C7 Si1 C8 110.4(3) . . ? N1 Si1 C9 112.2(3) . . ? C7 Si1 C9 108.7(4) . . ? C8 Si1 C9 107.1(3) . . ? N2 Si2 C12 109.1(3) . . ? N2 Si2 C11 108.7(3) . . ? C12 Si2 C11 109.9(4) . . ? N2 Si2 C13 113.2(2) . . ? C12 Si2 C13 106.4(3) . . ? C11 Si2 C13 109.5(3) . . ? N3 Si3 C21 109.1(3) . . ? N3 Si3 C23 108.2(2) . . ? C21 Si3 C23 109.7(3) . . ? N3 Si3 C22 115.4(3) . . ? C21 Si3 C22 108.2(3) . . ? C23 Si3 C22 106.2(3) . . ? N4 Si4 C25 109.7(3) . . ? N4 Si4 C26 109.6(3) . . ? C25 Si4 C26 109.8(3) . . ? N4 Si4 C27 111.6(2) . . ? C25 Si4 C27 109.1(3) . . ? C26 Si4 C27 106.9(3) . . ? C1 N1 Si1 120.3(4) . . ? C1 N1 Zr1 100.4(3) . . ? Si1 N1 Zr1 138.9(2) . . ? C2 N2 Si2 120.1(3) . . ? C2 N2 Zr1 100.2(3) . . ? Si2 N2 Zr1 138.4(3) . . ? C15 N3 Si3 121.8(3) . . ? C15 N3 Zr2 103.7(3) . . ? Si3 N3 Zr2 133.0(3) . . ? C16 N4 Si4 119.9(3) . . ? C16 N4 Zr2 104.1(3) . . ? Si4 N4 Zr2 135.5(2) . . ? C29 N5 C30 106.9(4) . . ? C29 N5 Zr1 113.7(3) . . ? C30 N5 Zr1 107.6(3) . . ? C29 N5 Zr2 108.2(3) . . ? C30 N5 Zr2 118.2(3) . . ? Zr1 N5 Zr2 102.4(2) . . ? C32 N6 C31 107.5(4) . . ? C32 N6 Zr2 119.3(3) . . ? C31 N6 Zr2 102.1(3) . . ? C32 N6 Zr1 109.7(3) . . ? C31 N6 Zr1 113.4(3) . . ? Zr2 N6 Zr1 104.9(2) . . ? C34 N7 C33 111.2(5) . . ? C34 N7 Zr1 117.9(4) . . ? C33 N7 Zr1 130.9(4) . . ? C36 N8 C35 109.4(4) . . ? C36 N8 Zr2 133.3(4) . . ? C35 N8 Zr2 117.2(4) . . ? C6 C1 N1 123.4(5) . . ? C6 C1 C2 119.6(5) . . ? N1 C1 C2 117.1(5) . . ? C6 C1 Zr1 151.4(3) . . ? N1 C1 Zr1 49.3(2) . . ? C2 C1 Zr1 74.8(3) . . ? N2 C2 C3 124.3(5) . . ? N2 C2 C1 118.1(4) . . ? C3 C2 C1 117.6(5) . . ? N2 C2 Zr1 49.5(2) . . ? C3 C2 Zr1 152.2(4) . . ? C1 C2 Zr1 75.0(3) . . ? C4 C3 C2 121.5(5) . . ? C3 C4 C5 120.9(5) . . ? C4 C5 C6 119.4(5) . . ? C5 C6 C1 121.0(5) . . ? C10 C9 Si1 128.5(7) . . ? C14 C13 Si2 126.1(5) . . ? C20 C15 N3 124.8(5) . . ? C20 C15 C16 117.9(5) . . ? N3 C15 C16 117.3(5) . . ? C20 C15 Zr2 152.8(4) . . ? N3 C15 Zr2 47.2(2) . . ? C16 C15 Zr2 75.5(3) . . ? C17 C16 N4 124.1(5) . . ? C17 C16 C15 119.1(5) . . ? N4 C16 C15 116.8(5) . . ? C17 C16 Zr2 155.0(4) . . ? N4 C16 Zr2 46.5(2) . . ? C15 C16 Zr2 75.0(3) . . ? C18 C17 C16 120.8(5) . . ? C17 C18 C19 120.4(5) . . ? C18 C19 C20 120.5(6) . . ? C19 C20 C15 121.1(5) . . ? C24 C23 Si3 125.3(6) . . ? C28 C27 Si4 125.5(5) . . ? _refine_diff_density_max 3.147 _refine_diff_density_min -2.101 _refine_diff_density_rms 0.203 #===END data_jan499-MFL6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[{C6H4(NSiMe3)2}ZrCl2(Me2NCH2CH2NMe2)]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H38 Cl2 N4 Si2 Zr' _chemical_formula_weight 528.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 30.39(2) _cell_length_b 18.203(5) _cell_length_c 14.315(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.52(4) _cell_angle_gamma 90.00 _cell_volume 7731(6) _cell_formula_units_Z 12 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description block _exptl_crystal_colour ? _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 1.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3312 _exptl_absorpt_coefficient_mu 0.738 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5487 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 23.00 _reflns_number_total 5487 _reflns_number_gt 4994 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; There are three independent molecules. I have run TRACER to try to find any higher symmetry centred cell (e.g.R3c) but it does not give anything. I have looked at packing diagrams and also can not see any higher symmetry. 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^)+(0.0126P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(4) _refine_ls_number_reflns 5487 _refine_ls_number_parameters 730 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0715 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Zr Zr 0.40713(2) 0.08805(4) 0.90038(4) 0.01953(18) Uani 1 1 d . . . Cl1 Cl 0.47689(7) 0.06819(11) 0.83322(14) 0.0314(5) Uani 1 1 d . . . Cl2 Cl 0.36537(7) 0.03009(11) 0.75487(13) 0.0314(5) Uani 1 1 d . . . Si1 Si 0.29159(7) 0.09908(12) 0.93611(15) 0.0257(5) Uani 1 1 d . . . Si2 Si 0.42062(7) 0.25633(11) 0.78741(15) 0.0226(5) Uani 1 1 d . . . N1 N 0.34925(19) 0.1182(3) 0.9514(4) 0.0196(14) Uani 1 1 d . . . N2 N 0.4093(2) 0.1989(3) 0.8767(4) 0.0195(14) Uani 1 1 d . . . N3 N 0.4170(2) -0.0380(3) 0.9707(4) 0.0261(15) Uani 1 1 d . . . N4 N 0.4625(2) 0.0949(3) 1.0538(4) 0.0243(15) Uani 1 1 d . . . C1 C 0.3635(2) 0.1879(4) 0.9950(5) 0.0230(18) Uani 1 1 d . . . C2 C 0.3949(2) 0.2292(4) 0.9571(5) 0.0193(17) Uani 1 1 d . . . C3 C 0.4120(2) 0.2945(4) 1.0011(5) 0.0218(17) Uani 1 1 d . . . H3 H 0.4345 0.3207 0.9781 0.026 Uiso 1 1 calc R . . C4 C 0.3963(3) 0.3216(4) 1.0781(5) 0.0290(19) Uani 1 1 d . . . H4 H 0.4072 0.3673 1.1059 0.035 Uiso 1 1 calc R . . C5 C 0.3646(3) 0.2827(5) 1.1150(5) 0.032(2) Uani 1 1 d . . . H5 H 0.3538 0.3016 1.1677 0.038 Uiso 1 1 calc R . . C6 C 0.3489(3) 0.2156(4) 1.0742(5) 0.0266(19) Uani 1 1 d . . . H6 H 0.3279 0.1883 1.1006 0.032 Uiso 1 1 calc R . . C7 C 0.2709(3) 0.0349(5) 0.8346(6) 0.043(2) Uani 1 1 d . . . H7A H 0.2873 -0.0117 0.8466 0.064 Uiso 1 1 calc R . . H7B H 0.2758 0.0567 0.7752 0.064 Uiso 1 1 calc R . . H7C H 0.2386 0.0259 0.8288 0.064 Uiso 1 1 calc R . . C8 C 0.2763(3) 0.0583(5) 1.0447(7) 0.048(3) Uani 1 1 d . . . H8A H 0.2935 0.0129 1.0621 0.073 Uiso 1 1 calc R . . H8B H 0.2440 0.0473 1.0310 0.073 Uiso 1 1 calc R . . H8C H 0.2835 0.0933 1.0978 0.073 Uiso 1 1 calc R . . C9 C 0.2589(3) 0.1856(4) 0.9054(6) 0.038(2) Uani 1 1 d . . . H9A H 0.2684 0.2216 0.9566 0.057 Uiso 1 1 calc R . . H9B H 0.2267 0.1753 0.8981 0.057 Uiso 1 1 calc R . . H9C H 0.2644 0.2053 0.8452 0.057 Uiso 1 1 calc R . . C10 C 0.3826(3) 0.3379(4) 0.7763(5) 0.032(2) Uani 1 1 d . . . H10A H 0.3892 0.3659 0.8362 0.049 Uiso 1 1 calc R . . H10B H 0.3511 0.3214 0.7633 0.049 Uiso 1 1 calc R . . H10C H 0.3874 0.3691 0.7237 0.049 Uiso 1 1 calc R . . C11 C 0.4806(3) 0.2839(4) 0.8125(6) 0.034(2) Uani 1 1 d . . . H11A H 0.4880 0.3108 0.8732 0.051 Uiso 1 1 calc R . . H11B H 0.4861 0.3154 0.7608 0.051 Uiso 1 1 calc R . . H11C H 0.4996 0.2400 0.8170 0.051 Uiso 1 1 calc R . . C12 C 0.4065(3) 0.2060(5) 0.6728(6) 0.041(2) Uani 1 1 d . . . H12A H 0.3748 0.1915 0.6597 0.061 Uiso 1 1 calc R . . H12B H 0.4255 0.1621 0.6768 0.061 Uiso 1 1 calc R . . H12C H 0.4119 0.2378 0.6212 0.061 Uiso 1 1 calc R . . C13 C 0.4482(3) -0.0376(4) 1.0667(5) 0.0288(19) Uani 1 1 d . . . H13A H 0.4630 -0.0861 1.0793 0.035 Uiso 1 1 calc R . . H13B H 0.4309 -0.0285 1.1167 0.035 Uiso 1 1 calc R . . C14 C 0.4834(3) 0.0212(4) 1.0709(6) 0.032(2) Uani 1 1 d . . . H14A H 0.5042 0.0204 1.1346 0.039 Uiso 1 1 calc R . . H14B H 0.5012 0.0111 1.0221 0.039 Uiso 1 1 calc R . . C15 C 0.4353(3) -0.0896(4) 0.9094(6) 0.036(2) Uani 1 1 d . . . H15A H 0.4648 -0.0722 0.9016 0.053 Uiso 1 1 calc R . . H15B H 0.4147 -0.0927 0.8466 0.053 Uiso 1 1 calc R . . H15C H 0.4386 -0.1383 0.9393 0.053 Uiso 1 1 calc R . . C16 C 0.3728(3) -0.0671(4) 0.9813(6) 0.0300(19) Uani 1 1 d . . . H16A H 0.3518 -0.0673 0.9189 0.045 Uiso 1 1 calc R . . H16B H 0.3607 -0.0360 1.0257 0.045 Uiso 1 1 calc R . . H16C H 0.3766 -0.1174 1.0065 0.045 Uiso 1 1 calc R . . C17 C 0.4427(3) 0.1144(5) 1.1391(5) 0.035(2) Uani 1 1 d . . . H17A H 0.4282 0.1627 1.1288 0.053 Uiso 1 1 calc R . . H17B H 0.4667 0.1158 1.1971 0.053 Uiso 1 1 calc R . . H17C H 0.4203 0.0774 1.1465 0.053 Uiso 1 1 calc R . . C18 C 0.4991(3) 0.1502(5) 1.0518(6) 0.037(2) Uani 1 1 d . . . H18A H 0.4858 0.1993 1.0404 0.055 Uiso 1 1 calc R . . H18B H 0.5145 0.1377 1.0004 0.055 Uiso 1 1 calc R . . H18C H 0.5209 0.1497 1.1133 0.055 Uiso 1 1 calc R . . Zr1B Zr 0.04760(2) 0.18064(4) 0.94946(5) 0.01854(17) Uani 1 1 d . . . Cl1B Cl -0.01197(7) 0.20711(12) 1.04235(14) 0.0350(5) Uani 1 1 d . . . Cl2B Cl 0.01627(7) 0.28078(10) 0.84365(14) 0.0299(5) Uani 1 1 d . . . Si1B Si 0.09689(7) 0.17926(12) 0.74677(15) 0.0235(5) Uani 1 1 d . . . Si2B Si -0.03728(7) 0.05312(12) 0.86070(15) 0.0238(5) Uani 1 1 d . . . N1B N 0.09260(19) 0.1514(3) 0.8627(4) 0.0198(14) Uani 1 1 d . . . N2B N 0.0184(2) 0.0825(3) 0.8979(4) 0.0187(13) Uani 1 1 d . . . N3B N 0.0948(2) 0.2771(3) 1.0489(4) 0.0241(15) Uani 1 1 d . . . N4B N 0.0857(2) 0.1232(3) 1.1018(4) 0.0211(14) Uani 1 1 d . . . C1B C 0.0951(3) 0.0734(4) 0.8777(5) 0.0230(18) Uani 1 1 d . . . C2B C 0.0560(3) 0.0377(4) 0.8947(5) 0.0236(18) Uani 1 1 d . . . C3B C 0.0585(3) -0.0374(4) 0.9131(5) 0.0276(19) Uani 1 1 d . . . H3B H 0.0326 -0.0622 0.9242 0.033 Uiso 1 1 calc R . . C4B C 0.0975(3) -0.0767(4) 0.9157(5) 0.031(2) Uani 1 1 d . . . H4B H 0.0983 -0.1281 0.9276 0.037 Uiso 1 1 calc R . . C5B C 0.1352(3) -0.0410(5) 0.9011(5) 0.032(2) Uani 1 1 d . . . H5B H 0.1623 -0.0678 0.9035 0.039 Uiso 1 1 calc R . . C6B C 0.1342(3) 0.0329(4) 0.8830(5) 0.0291(19) Uani 1 1 d . . . H6B H 0.1607 0.0568 0.8739 0.035 Uiso 1 1 calc R . . C7B C 0.1122(3) 0.2782(4) 0.7445(5) 0.030(2) Uani 1 1 d . . . H7B1 H 0.0902 0.3078 0.7687 0.045 Uiso 1 1 calc R . . H7B2 H 0.1123 0.2928 0.6786 0.045 Uiso 1 1 calc R . . H7B3 H 0.1423 0.2859 0.7849 0.045 Uiso 1 1 calc R . . C8B C 0.0427(3) 0.1602(5) 0.6608(5) 0.035(2) Uani 1 1 d . . . H8B1 H 0.0181 0.1857 0.6817 0.052 Uiso 1 1 calc R . . H8B2 H 0.0369 0.1072 0.6584 0.052 Uiso 1 1 calc R . . H8B3 H 0.0446 0.1777 0.5970 0.052 Uiso 1 1 calc R . . C9B C 0.1408(3) 0.1275(4) 0.7004(5) 0.034(2) Uani 1 1 d . . . H9B1 H 0.1343 0.0748 0.7003 0.051 Uiso 1 1 calc R . . H9B2 H 0.1705 0.1370 0.7416 0.051 Uiso 1 1 calc R . . H9B3 H 0.1407 0.1436 0.6350 0.051 Uiso 1 1 calc R . . C10B C -0.0421(3) -0.0028(4) 0.7498(6) 0.039(2) Uani 1 1 d . . . H10D H -0.0227 -0.0463 0.7638 0.059 Uiso 1 1 calc R . . H10E H -0.0326 0.0267 0.7004 0.059 Uiso 1 1 calc R . . H10F H -0.0734 -0.0183 0.7268 0.059 Uiso 1 1 calc R . . C11B C -0.0551(3) -0.0014(5) 0.9566(6) 0.038(2) Uani 1 1 d . . . H11D H -0.0355 -0.0445 0.9721 0.057 Uiso 1 1 calc R . . H11E H -0.0864 -0.0174 0.9342 0.057 Uiso 1 1 calc R . . H11F H -0.0527 0.0292 1.0139 0.057 Uiso 1 1 calc R . . C12B C -0.0742(2) 0.1339(4) 0.8318(5) 0.0281(19) Uani 1 1 d . . . H12D H -0.0650 0.1625 0.7813 0.042 Uiso 1 1 calc R . . H12E H -0.0717 0.1645 0.8891 0.042 Uiso 1 1 calc R . . H12F H -0.1054 0.1177 0.8097 0.042 Uiso 1 1 calc R . . C13B C 0.1216(3) 0.2428(4) 1.1363(5) 0.0261(18) Uani 1 1 d . . . H13C H 0.1302 0.2807 1.1864 0.031 Uiso 1 1 calc R . . H13D H 0.1496 0.2222 1.1222 0.031 Uiso 1 1 calc R . . C14B C 0.0964(3) 0.1833(4) 1.1729(5) 0.0261(18) Uani 1 1 d . . . H14C H 0.1147 0.1638 1.2335 0.031 Uiso 1 1 calc R . . H14D H 0.0681 0.2034 1.1862 0.031 Uiso 1 1 calc R . . C15B C 0.0665(3) 0.3375(4) 1.0770(6) 0.041(2) Uani 1 1 d . . . H15D H 0.0485 0.3605 1.0192 0.062 Uiso 1 1 calc R . . H15E H 0.0861 0.3744 1.1146 0.062 Uiso 1 1 calc R . . H15F H 0.0464 0.3169 1.1153 0.062 Uiso 1 1 calc R . . C16B C 0.1252(3) 0.3128(4) 0.9947(6) 0.038(2) Uani 1 1 d . . . H16D H 0.1073 0.3353 0.9365 0.057 Uiso 1 1 calc R . . H16E H 0.1455 0.2759 0.9772 0.057 Uiso 1 1 calc R . . H16F H 0.1430 0.3508 1.0344 0.057 Uiso 1 1 calc R . . C17B C 0.1278(3) 0.0822(4) 1.0993(6) 0.036(2) Uani 1 1 d . . . H17D H 0.1488 0.1146 1.0760 0.054 Uiso 1 1 calc R . . H17E H 0.1205 0.0399 1.0563 0.054 Uiso 1 1 calc R . . H17F H 0.1416 0.0651 1.1638 0.054 Uiso 1 1 calc R . . C18B C 0.0556(3) 0.0706(4) 1.1376(6) 0.033(2) Uani 1 1 d . . . H18D H 0.0272 0.0951 1.1403 0.049 Uiso 1 1 calc R . . H18E H 0.0703 0.0537 1.2017 0.049 Uiso 1 1 calc R . . H18F H 0.0494 0.0284 1.0941 0.049 Uiso 1 1 calc R . . Zr1C Zr -0.25910(2) 0.07740(4) 0.85978(4) 0.01771(17) Uani 1 1 d . . . Cl1C Cl -0.19393(6) 0.06541(11) 0.77556(13) 0.0264(5) Uani 1 1 d . . . Cl2C Cl -0.30564(7) 0.04379(11) 0.70480(13) 0.0313(5) Uani 1 1 d . . . Si1C Si -0.37231(7) 0.08510(13) 0.90826(16) 0.0276(5) Uani 1 1 d . . . Si2C Si -0.23797(7) 0.25709(12) 0.79024(15) 0.0231(5) Uani 1 1 d . . . N1C N -0.3138(2) 0.0978(3) 0.9229(4) 0.0215(15) Uani 1 1 d . . . N2C N -0.2535(2) 0.1898(3) 0.8642(4) 0.0194(14) Uani 1 1 d . . . N3C N -0.2521(2) -0.0561(3) 0.8990(4) 0.0239(15) Uani 1 1 d . . . N4C N -0.1984(2) 0.0627(3) 1.0031(4) 0.0222(14) Uani 1 1 d . . . C1C C -0.2955(2) 0.1592(4) 0.9834(5) 0.0233(18) Uani 1 1 d . . . C2C C -0.2647(3) 0.2062(4) 0.9523(5) 0.0241(18) Uani 1 1 d . . . C3C C -0.2444(3) 0.2625(4) 1.0137(6) 0.032(2) Uani 1 1 d . . . H3C H -0.2227 0.2932 0.9946 0.039 Uiso 1 1 calc R . . C4C C -0.2553(3) 0.2745(5) 1.1012(6) 0.040(2) Uani 1 1 d . . . H4C H -0.2417 0.3138 1.1408 0.047 Uiso 1 1 calc R . . C5C C -0.2862(3) 0.2291(5) 1.1309(6) 0.039(2) Uani 1 1 d . . . H5C H -0.2940 0.2374 1.1908 0.047 Uiso 1 1 calc R . . C6C C -0.3055(3) 0.1718(4) 1.0734(5) 0.029(2) Uani 1 1 d . . . H6C H -0.3261 0.1403 1.0950 0.035 Uiso 1 1 calc R . . C7C C -0.3969(3) 0.0256(5) 0.8047(6) 0.040(2) Uani 1 1 d . . . H7C1 H -0.3825 -0.0229 0.8134 0.060 Uiso 1 1 calc R . . H7C2 H -0.3917 0.0479 0.7457 0.060 Uiso 1 1 calc R . . H7C3 H -0.4293 0.0203 0.8003 0.060 Uiso 1 1 calc R . . C8C C -0.3895(3) 0.0391(5) 1.0118(6) 0.038(2) Uani 1 1 d . . . H8C1 H -0.3780 0.0672 1.0704 0.057 Uiso 1 1 calc R . . H8C2 H -0.3771 -0.0108 1.0193 0.057 Uiso 1 1 calc R . . H8C3 H -0.4225 0.0366 1.0000 0.057 Uiso 1 1 calc R . . C9C C -0.4002(3) 0.1765(5) 0.8895(7) 0.050(3) Uani 1 1 d . . . H9C1 H -0.3878 0.2086 0.9439 0.075 Uiso 1 1 calc R . . H9C2 H -0.4327 0.1706 0.8841 0.075 Uiso 1 1 calc R . . H9C3 H -0.3947 0.1985 0.8306 0.075 Uiso 1 1 calc R . . C10C C -0.2722(3) 0.3416(4) 0.7969(6) 0.038(2) Uani 1 1 d . . . H10G H -0.3043 0.3297 0.7774 0.056 Uiso 1 1 calc R . . H10H H -0.2645 0.3793 0.7541 0.056 Uiso 1 1 calc R . . H10I H -0.2656 0.3602 0.8627 0.056 Uiso 1 1 calc R . . C11C C -0.1766(3) 0.2787(5) 0.8267(6) 0.035(2) Uani 1 1 d . . . H11G H -0.1697 0.2967 0.8928 0.053 Uiso 1 1 calc R . . H11H H -0.1689 0.3165 0.7842 0.053 Uiso 1 1 calc R . . H11I H -0.1590 0.2342 0.8222 0.053 Uiso 1 1 calc R . . C12C C -0.2515(3) 0.2228(4) 0.6641(5) 0.0292(19) Uani 1 1 d . . . H12G H -0.2837 0.2117 0.6451 0.044 Uiso 1 1 calc R . . H12H H -0.2341 0.1782 0.6594 0.044 Uiso 1 1 calc R . . H12I H -0.2437 0.2606 0.6216 0.044 Uiso 1 1 calc R . . C13C C -0.2195(3) -0.0682(4) 0.9925(5) 0.0306(19) Uani 1 1 d . . . H13E H -0.2075 -0.1188 0.9951 0.037 Uiso 1 1 calc R . . H13F H -0.2351 -0.0619 1.0459 0.037 Uiso 1 1 calc R . . C14C C -0.1814(3) -0.0138(4) 1.0027(6) 0.0303(19) Uani 1 1 d . . . H14E H -0.1592 -0.0234 1.0630 0.036 Uiso 1 1 calc R . . H14F H -0.1660 -0.0200 0.9489 0.036 Uiso 1 1 calc R . . C15C C -0.2363(3) -0.0983(4) 0.8237(6) 0.034(2) Uani 1 1 d . . . H15G H -0.2074 -0.0783 0.8155 0.051 Uiso 1 1 calc R . . H15H H -0.2586 -0.0945 0.7632 0.051 Uiso 1 1 calc R . . H15I H -0.2324 -0.1500 0.8428 0.051 Uiso 1 1 calc R . . C16C C -0.2955(3) -0.0891(5) 0.9067(7) 0.039(2) Uani 1 1 d . . . H16G H -0.3175 -0.0822 0.8464 0.059 Uiso 1 1 calc R . . H16H H -0.3064 -0.0653 0.9587 0.059 Uiso 1 1 calc R . . H16I H -0.2913 -0.1417 0.9203 0.059 Uiso 1 1 calc R . . C17C C -0.2127(3) 0.0747(4) 1.0964(5) 0.0289(19) Uani 1 1 d . . . H17G H -0.2382 0.0426 1.0992 0.043 Uiso 1 1 calc R . . H17H H -0.2216 0.1261 1.1008 0.043 Uiso 1 1 calc R . . H17I H -0.1875 0.0633 1.1498 0.043 Uiso 1 1 calc R . . C18C C -0.1598(2) 0.1135(4) 1.0035(5) 0.0286(19) Uani 1 1 d . . . H18G H -0.1701 0.1645 1.0038 0.043 Uiso 1 1 calc R . . H18H H -0.1478 0.1049 0.9462 0.043 Uiso 1 1 calc R . . H18I H -0.1361 0.1044 1.0607 0.043 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 Zr 0.0211(4) 0.0201(4) 0.0180(4) 0.0009(3) 0.0058(3) -0.0014(3) Cl1 0.0278(12) 0.0378(12) 0.0322(12) 0.0002(9) 0.0144(9) 0.0034(9) Cl2 0.0356(12) 0.0338(12) 0.0240(11) -0.0070(9) 0.0050(9) -0.0053(10) Si1 0.0196(12) 0.0257(12) 0.0326(13) 0.0013(10) 0.0079(10) -0.0036(10) Si2 0.0264(12) 0.0226(12) 0.0207(12) 0.0008(9) 0.0094(9) -0.0013(10) N1 0.023(4) 0.026(4) 0.010(3) 0.005(3) 0.006(3) -0.004(3) N2 0.021(4) 0.020(3) 0.019(4) -0.008(3) 0.009(3) -0.003(3) N3 0.030(4) 0.025(4) 0.025(4) -0.001(3) 0.008(3) 0.001(3) N4 0.022(4) 0.032(4) 0.017(3) 0.004(3) 0.000(3) -0.007(3) C1 0.013(4) 0.029(4) 0.025(4) 0.002(4) 0.000(3) -0.004(3) C2 0.013(4) 0.023(4) 0.018(4) 0.005(3) -0.006(3) 0.002(3) C3 0.027(4) 0.018(4) 0.020(4) -0.001(3) 0.006(3) -0.010(3) C4 0.036(5) 0.028(4) 0.022(4) -0.010(4) 0.007(4) -0.005(4) C5 0.031(5) 0.047(5) 0.021(4) -0.005(4) 0.013(4) 0.001(4) C6 0.025(4) 0.039(5) 0.017(4) -0.004(4) 0.008(4) -0.007(4) C7 0.030(5) 0.039(5) 0.058(6) -0.009(5) 0.006(5) -0.007(4) C8 0.029(5) 0.054(6) 0.070(7) 0.015(5) 0.026(5) 0.003(4) C9 0.030(5) 0.038(5) 0.044(5) 0.000(4) 0.004(4) 0.001(4) C10 0.038(5) 0.038(5) 0.019(4) 0.001(4) 0.001(4) 0.000(4) C11 0.032(5) 0.029(5) 0.047(5) 0.009(4) 0.022(4) 0.002(4) C12 0.053(6) 0.042(5) 0.028(5) -0.003(4) 0.011(4) -0.010(5) C13 0.040(5) 0.024(4) 0.022(4) 0.010(3) 0.006(4) 0.006(4) C14 0.022(5) 0.035(5) 0.038(5) 0.009(4) 0.002(4) 0.009(4) C15 0.059(6) 0.021(4) 0.027(5) 0.005(4) 0.011(4) 0.006(4) C16 0.033(5) 0.027(5) 0.030(5) 0.007(4) 0.007(4) -0.011(4) C17 0.037(5) 0.046(5) 0.017(4) 0.001(4) -0.007(4) 0.004(4) C18 0.025(5) 0.042(5) 0.037(5) -0.001(4) -0.004(4) -0.008(4) Zr1B 0.0186(4) 0.0202(4) 0.0174(4) -0.0011(3) 0.0055(3) -0.0010(3) Cl1B 0.0282(12) 0.0499(13) 0.0305(12) -0.0059(10) 0.0145(9) 0.0005(10) Cl2B 0.0324(12) 0.0273(11) 0.0306(11) 0.0056(9) 0.0081(9) 0.0092(9) Si1B 0.0224(12) 0.0285(12) 0.0216(11) -0.0023(10) 0.0091(9) -0.0049(10) Si2B 0.0181(11) 0.0303(12) 0.0226(12) 0.0002(10) 0.0035(9) -0.0057(10) N1B 0.020(3) 0.022(4) 0.018(3) -0.004(3) 0.004(3) 0.003(3) N2B 0.012(3) 0.024(3) 0.020(3) -0.003(3) 0.005(2) 0.003(3) N3B 0.027(4) 0.025(4) 0.023(4) -0.003(3) 0.011(3) -0.004(3) N4B 0.024(4) 0.020(3) 0.019(3) 0.002(3) 0.006(3) -0.001(3) C1B 0.021(4) 0.033(5) 0.015(4) -0.002(3) 0.004(3) 0.001(4) C2B 0.027(5) 0.028(5) 0.015(4) 0.003(3) 0.004(3) -0.004(4) C3B 0.032(5) 0.020(4) 0.029(5) -0.001(3) 0.003(4) -0.002(4) C4B 0.051(6) 0.021(4) 0.022(4) 0.000(3) 0.008(4) 0.010(4) C5B 0.026(5) 0.046(6) 0.024(5) -0.002(4) 0.003(4) 0.015(4) C6B 0.021(5) 0.038(5) 0.029(5) -0.002(4) 0.006(4) 0.005(4) C7B 0.046(5) 0.028(5) 0.018(4) -0.002(3) 0.013(4) -0.011(4) C8B 0.038(5) 0.043(5) 0.020(4) 0.000(4) -0.002(4) -0.003(4) C9B 0.039(5) 0.039(5) 0.025(5) -0.006(4) 0.012(4) -0.004(4) C10B 0.035(5) 0.039(5) 0.042(5) 0.007(4) 0.003(4) -0.005(4) C11B 0.032(5) 0.042(5) 0.041(5) 0.009(4) 0.010(4) -0.006(4) C12B 0.020(4) 0.040(5) 0.021(4) 0.002(4) -0.003(3) 0.000(4) C13B 0.027(5) 0.028(4) 0.021(4) -0.005(3) 0.000(4) -0.008(4) C14B 0.027(4) 0.036(5) 0.013(4) 0.001(4) 0.000(3) -0.004(4) C15B 0.058(6) 0.029(5) 0.037(5) -0.004(4) 0.008(5) 0.003(4) C16B 0.051(6) 0.038(5) 0.031(5) -0.007(4) 0.019(4) -0.015(4) C17B 0.035(5) 0.037(5) 0.034(5) 0.001(4) 0.002(4) 0.001(4) C18B 0.032(5) 0.035(5) 0.031(5) 0.006(4) 0.005(4) -0.005(4) Zr1C 0.0157(4) 0.0200(4) 0.0175(4) -0.0004(3) 0.0039(3) -0.0013(3) Cl1C 0.0222(10) 0.0351(11) 0.0249(11) -0.0036(9) 0.0115(8) -0.0030(9) Cl2C 0.0258(11) 0.0430(13) 0.0221(10) -0.0056(9) -0.0016(9) -0.0072(10) Si1C 0.0165(11) 0.0352(13) 0.0323(13) 0.0112(10) 0.0078(10) 0.0037(10) Si2C 0.0246(12) 0.0234(12) 0.0223(12) -0.0026(9) 0.0074(9) -0.0040(10) N1C 0.019(4) 0.026(4) 0.024(4) 0.005(3) 0.014(3) 0.001(3) N2C 0.024(4) 0.025(3) 0.013(3) -0.008(3) 0.013(3) -0.003(3) N3C 0.027(4) 0.024(3) 0.023(3) -0.004(3) 0.009(3) 0.003(3) N4C 0.022(4) 0.026(4) 0.019(3) 0.000(3) 0.007(3) -0.004(3) C1C 0.017(4) 0.027(4) 0.028(5) 0.002(4) 0.008(4) 0.008(4) C2C 0.023(4) 0.025(4) 0.025(4) 0.005(3) 0.008(4) 0.006(4) C3C 0.043(5) 0.021(4) 0.035(5) -0.017(4) 0.016(4) -0.006(4) C4C 0.052(6) 0.038(5) 0.031(5) -0.014(4) 0.017(4) -0.003(5) C5C 0.045(6) 0.046(6) 0.030(5) -0.013(4) 0.018(4) 0.004(5) C6C 0.027(5) 0.040(5) 0.026(4) -0.001(4) 0.019(4) 0.008(4) C7C 0.012(4) 0.066(6) 0.042(5) 0.007(5) 0.006(4) -0.003(4) C8C 0.015(4) 0.049(5) 0.050(6) 0.018(4) 0.006(4) 0.002(4) C9C 0.033(6) 0.058(6) 0.060(7) 0.016(5) 0.015(5) 0.015(5) C10C 0.038(5) 0.030(5) 0.044(6) 0.008(4) 0.006(4) -0.002(4) C11C 0.033(5) 0.044(5) 0.034(5) -0.001(4) 0.019(4) -0.014(4) C12C 0.030(5) 0.035(5) 0.023(4) -0.001(4) 0.008(4) -0.005(4) C13C 0.040(5) 0.021(4) 0.031(5) 0.003(3) 0.007(4) 0.003(4) C14C 0.022(4) 0.038(5) 0.025(4) 0.003(4) -0.008(3) 0.003(4) C15C 0.046(6) 0.026(5) 0.035(5) -0.003(4) 0.020(4) 0.001(4) C16C 0.022(5) 0.037(5) 0.061(6) 0.001(5) 0.012(4) -0.012(4) C17C 0.028(5) 0.042(5) 0.018(4) 0.007(4) 0.008(3) 0.005(4) C18C 0.018(4) 0.044(5) 0.022(4) -0.002(4) 0.001(3) -0.014(4) _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 Zr N2 2.050(6) . ? Zr N1 2.118(6) . ? Zr Cl2 2.432(2) . ? Zr N4 2.464(6) . ? Zr N3 2.497(6) . ? Zr Cl1 2.537(2) . ? Zr C2 2.744(7) . ? Zr C1 2.769(8) . ? Si1 N1 1.753(6) . ? Si1 C9 1.863(8) . ? Si1 C7 1.865(8) . ? Si1 C8 1.869(8) . ? Si2 N2 1.742(6) . ? Si2 C12 1.846(8) . ? Si2 C11 1.850(8) . ? Si2 C10 1.867(8) . ? N1 C1 1.438(9) . ? N2 C2 1.428(9) . ? N3 C15 1.476(9) . ? N3 C16 1.484(9) . ? N3 C13 1.491(9) . ? N4 C14 1.481(9) . ? N4 C18 1.504(9) . ? N4 C17 1.517(9) . ? C1 C6 1.399(10) . ? C1 C2 1.412(10) . ? C2 C3 1.392(10) . ? C3 C4 1.383(10) . ? C4 C5 1.388(11) . ? C5 C6 1.392(10) . ? C13 C14 1.506(10) . ? Zr1B N2B 2.059(6) . ? Zr1B N1B 2.106(6) . ? Zr1B Cl2B 2.429(2) . ? Zr1B N4B 2.469(6) . ? Zr1B N3B 2.506(6) . ? Zr1B Cl1B 2.514(2) . ? Zr1B C2B 2.745(8) . ? Zr1B C1B 2.755(7) . ? Si1B N1B 1.767(6) . ? Si1B C7B 1.861(7) . ? Si1B C8B 1.862(8) . ? Si1B C9B 1.870(8) . ? Si2B N2B 1.745(6) . ? Si2B C12B 1.841(8) . ? Si2B C10B 1.865(8) . ? Si2B C11B 1.866(8) . ? N1B C1B 1.434(9) . ? N2B C2B 1.412(9) . ? N3B C13B 1.477(9) . ? N3B C16B 1.480(9) . ? N3B C15B 1.503(9) . ? N4B C14B 1.480(9) . ? N4B C17B 1.487(10) . ? N4B C18B 1.490(9) . ? C1B C6B 1.388(10) . ? C1B C2B 1.421(10) . ? C2B C3B 1.391(10) . ? C3B C4B 1.380(11) . ? C4B C5B 1.373(11) . ? C5B C6B 1.369(11) . ? C13B C14B 1.485(10) . ? Zr1C N2C 2.053(6) . ? Zr1C N1C 2.089(6) . ? Zr1C Cl2C 2.437(2) . ? Zr1C N4C 2.459(6) . ? Zr1C N3C 2.493(6) . ? Zr1C Cl1C 2.541(2) . ? Zr1C C2C 2.716(8) . ? Zr1C C1C 2.723(7) . ? Si1C N1C 1.761(6) . ? Si1C C7C 1.857(9) . ? Si1C C9C 1.860(8) . ? Si1C C8C 1.874(8) . ? Si2C N2C 1.749(6) . ? Si2C C11C 1.866(8) . ? Si2C C12C 1.870(7) . ? Si2C C10C 1.871(8) . ? N1C C1C 1.448(10) . ? N2C C2C 1.408(9) . ? N3C C16C 1.474(9) . ? N3C C15C 1.486(9) . ? N3C C13C 1.499(9) . ? N4C C14C 1.486(9) . ? N4C C18C 1.493(9) . ? N4C C17C 1.507(9) . ? C1C C6C 1.406(10) . ? C1C C2C 1.409(11) . ? C2C C3C 1.403(10) . ? C3C C4C 1.380(10) . ? C4C C5C 1.384(11) . ? C5C C6C 1.379(11) . ? C13C C14C 1.506(11) . ? 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 Zr N1 82.0(2) . . ? N2 Zr Cl2 108.37(17) . . ? N1 Zr Cl2 95.13(17) . . ? N2 Zr N4 93.3(2) . . ? N1 Zr N4 97.9(2) . . ? Cl2 Zr N4 156.09(15) . . ? N2 Zr N3 165.0(2) . . ? N1 Zr N3 97.8(2) . . ? Cl2 Zr N3 86.65(15) . . ? N4 Zr N3 71.8(2) . . ? N2 Zr Cl1 91.03(16) . . ? N1 Zr Cl1 173.01(16) . . ? Cl2 Zr Cl1 86.41(8) . . ? N4 Zr Cl1 83.06(15) . . ? N3 Zr Cl1 89.11(15) . . ? N2 Zr C2 30.5(2) . . ? N1 Zr C2 58.6(2) . . ? Cl2 Zr C2 125.50(15) . . ? N4 Zr C2 78.4(2) . . ? N3 Zr C2 138.9(2) . . ? Cl1 Zr C2 115.06(16) . . ? N2 Zr C1 58.1(2) . . ? N1 Zr C1 30.7(2) . . ? Cl2 Zr C1 119.16(16) . . ? N4 Zr C1 80.7(2) . . ? N3 Zr C1 115.7(2) . . ? Cl1 Zr C1 143.78(16) . . ? C2 Zr C1 29.7(2) . . ? N1 Si1 C9 109.2(3) . . ? N1 Si1 C7 112.4(3) . . ? C9 Si1 C7 105.9(4) . . ? N1 Si1 C8 113.4(4) . . ? C9 Si1 C8 108.4(4) . . ? C7 Si1 C8 107.2(4) . . ? N2 Si2 C12 108.1(3) . . ? N2 Si2 C11 111.3(3) . . ? C12 Si2 C11 109.6(4) . . ? N2 Si2 C10 108.8(3) . . ? C12 Si2 C10 107.4(4) . . ? C11 Si2 C10 111.5(4) . . ? C1 N1 Si1 115.4(5) . . ? C1 N1 Zr 100.6(4) . . ? Si1 N1 Zr 142.0(3) . . ? C2 N2 Si2 120.3(5) . . ? C2 N2 Zr 102.7(4) . . ? Si2 N2 Zr 136.9(3) . . ? C15 N3 C16 107.5(6) . . ? C15 N3 C13 107.8(6) . . ? C16 N3 C13 108.4(6) . . ? C15 N3 Zr 111.9(4) . . ? C16 N3 Zr 109.7(4) . . ? C13 N3 Zr 111.4(4) . . ? C14 N4 C18 108.5(6) . . ? C14 N4 C17 108.1(6) . . ? C18 N4 C17 106.5(6) . . ? C14 N4 Zr 106.7(4) . . ? C18 N4 Zr 112.4(4) . . ? C17 N4 Zr 114.5(4) . . ? C6 C1 C2 118.6(7) . . ? C6 C1 N1 123.5(7) . . ? C2 C1 N1 117.9(7) . . ? C6 C1 Zr 154.6(5) . . ? C2 C1 Zr 74.2(4) . . ? N1 C1 Zr 48.7(3) . . ? C3 C2 C1 119.9(7) . . ? C3 C2 N2 123.0(6) . . ? C1 C2 N2 117.0(6) . . ? C3 C2 Zr 150.8(5) . . ? C1 C2 Zr 76.1(4) . . ? N2 C2 Zr 46.8(3) . . ? C4 C3 C2 120.4(7) . . ? C3 C4 C5 120.5(7) . . ? C4 C5 C6 119.5(7) . . ? C5 C6 C1 121.0(7) . . ? N3 C13 C14 110.1(6) . . ? N4 C14 C13 111.3(6) . . ? N2B Zr1B N1B 81.6(2) . . ? N2B Zr1B Cl2B 110.34(18) . . ? N1B Zr1B Cl2B 92.24(17) . . ? N2B Zr1B N4B 91.9(2) . . ? N1B Zr1B N4B 100.0(2) . . ? Cl2B Zr1B N4B 156.07(15) . . ? N2B Zr1B N3B 163.9(2) . . ? N1B Zr1B N3B 98.5(2) . . ? Cl2B Zr1B N3B 85.80(15) . . ? N4B Zr1B N3B 72.2(2) . . ? N2B Zr1B Cl1B 93.00(17) . . ? N1B Zr1B Cl1B 174.10(17) . . ? Cl2B Zr1B Cl1B 87.49(7) . . ? N4B Zr1B Cl1B 82.39(15) . . ? N3B Zr1B Cl1B 87.38(15) . . ? N2B Zr1B C2B 30.1(2) . . ? N1B Zr1B C2B 58.6(2) . . ? Cl2B Zr1B C2B 125.54(16) . . ? N4B Zr1B C2B 78.3(2) . . ? N3B Zr1B C2B 138.5(2) . . ? Cl1B Zr1B C2B 117.06(16) . . ? N2B Zr1B C1B 58.1(2) . . ? N1B Zr1B C1B 30.8(2) . . ? Cl2B Zr1B C1B 117.74(16) . . ? N4B Zr1B C1B 81.1(2) . . ? N3B Zr1B C1B 115.3(2) . . ? Cl1B Zr1B C1B 145.94(17) . . ? C2B Zr1B C1B 29.9(2) . . ? N1B Si1B C7B 111.4(3) . . ? N1B Si1B C8B 109.4(3) . . ? C7B Si1B C8B 110.9(4) . . ? N1B Si1B C9B 113.1(3) . . ? C7B Si1B C9B 106.3(4) . . ? C8B Si1B C9B 105.6(4) . . ? N2B Si2B C12B 109.1(3) . . ? N2B Si2B C10B 108.6(3) . . ? C12B Si2B C10B 108.3(4) . . ? N2B Si2B C11B 110.8(3) . . ? C12B Si2B C11B 109.3(4) . . ? C10B Si2B C11B 110.8(4) . . ? C1B N1B Si1B 114.4(4) . . ? C1B N1B Zr1B 100.5(4) . . ? Si1B N1B Zr1B 132.1(3) . . ? C2B N2B Si2B 123.4(5) . . ? C2B N2B Zr1B 103.0(5) . . ? Si2B N2B Zr1B 133.6(3) . . ? C13B N3B C16B 109.7(6) . . ? C13B N3B C15B 109.1(6) . . ? C16B N3B C15B 106.2(6) . . ? C13B N3B Zr1B 109.1(4) . . ? C16B N3B Zr1B 110.8(4) . . ? C15B N3B Zr1B 112.0(5) . . ? C14B N4B C17B 109.0(6) . . ? C14B N4B C18B 107.4(6) . . ? C17B N4B C18B 106.3(6) . . ? C14B N4B Zr1B 106.6(4) . . ? C17B N4B Zr1B 115.6(4) . . ? C18B N4B Zr1B 111.7(4) . . ? C6B C1B C2B 119.1(7) . . ? C6B C1B N1B 123.4(7) . . ? C2B C1B N1B 117.3(7) . . ? C6B C1B Zr1B 150.3(6) . . ? C2B C1B Zr1B 74.6(4) . . ? N1B C1B Zr1B 48.7(3) . . ? C3B C2B N2B 124.9(7) . . ? C3B C2B C1B 118.0(7) . . ? N2B C2B C1B 117.0(7) . . ? C3B C2B Zr1B 151.8(5) . . ? N2B C2B Zr1B 46.9(3) . . ? C1B C2B Zr1B 75.4(4) . . ? C4B C3B C2B 121.7(8) . . ? C5B C4B C3B 119.5(7) . . ? C6B C5B C4B 120.6(7) . . ? C5B C6B C1B 121.1(8) . . ? N3B C13B C14B 112.0(6) . . ? N4B C14B C13B 110.4(6) . . ? N2C Zr1C N1C 83.0(2) . . ? N2C Zr1C Cl2C 107.85(18) . . ? N1C Zr1C Cl2C 94.55(18) . . ? N2C Zr1C N4C 92.3(2) . . ? N1C Zr1C N4C 100.5(2) . . ? Cl2C Zr1C N4C 156.21(15) . . ? N2C Zr1C N3C 164.2(2) . . ? N1C Zr1C N3C 96.5(2) . . ? Cl2C Zr1C N3C 87.96(15) . . ? N4C Zr1C N3C 72.19(19) . . ? N2C Zr1C Cl1C 91.82(16) . . ? N1C Zr1C Cl1C 174.20(17) . . ? Cl2C Zr1C Cl1C 84.53(8) . . ? N4C Zr1C Cl1C 82.26(15) . . ? N3C Zr1C Cl1C 89.19(14) . . ? N2C Zr1C C2C 30.5(2) . . ? N1C Zr1C C2C 59.7(2) . . ? Cl2C Zr1C C2C 125.13(17) . . ? N4C Zr1C C2C 78.6(2) . . ? N3C Zr1C C2C 138.0(2) . . ? Cl1C Zr1C C2C 116.31(17) . . ? N2C Zr1C C1C 58.6(2) . . ? N1C Zr1C C1C 31.7(2) . . ? Cl2C Zr1C C1C 119.45(17) . . ? N4C Zr1C C1C 81.6(2) . . ? N3C Zr1C C1C 114.4(2) . . ? Cl1C Zr1C C1C 145.39(17) . . ? C2C Zr1C C1C 30.0(2) . . ? N1C Si1C C7C 113.1(3) . . ? N1C Si1C C9C 108.4(4) . . ? C7C Si1C C9C 108.4(4) . . ? N1C Si1C C8C 114.4(3) . . ? C7C Si1C C8C 103.8(4) . . ? C9C Si1C C8C 108.5(4) . . ? N2C Si2C C11C 111.2(3) . . ? N2C Si2C C12C 108.6(3) . . ? C11C Si2C C12C 109.7(4) . . ? N2C Si2C C10C 108.6(3) . . ? C11C Si2C C10C 110.2(4) . . ? C12C Si2C C10C 108.4(4) . . ? C1C N1C Si1C 114.8(5) . . ? C1C N1C Zr1C 99.1(4) . . ? Si1C N1C Zr1C 143.4(4) . . ? C2C N2C Si2C 123.0(5) . . ? C2C N2C Zr1C 101.7(4) . . ? Si2C N2C Zr1C 135.3(3) . . ? C16C N3C C15C 106.2(6) . . ? C16C N3C C13C 107.6(6) . . ? C15C N3C C13C 108.5(6) . . ? C16C N3C Zr1C 112.3(5) . . ? C15C N3C Zr1C 111.5(4) . . ? C13C N3C Zr1C 110.6(4) . . ? C14C N4C C18C 107.9(6) . . ? C14C N4C C17C 107.9(6) . . ? C18C N4C C17C 106.5(5) . . ? C14C N4C Zr1C 107.3(4) . . ? C18C N4C Zr1C 112.5(4) . . ? C17C N4C Zr1C 114.5(4) . . ? C6C C1C C2C 118.7(7) . . ? C6C C1C N1C 122.9(7) . . ? C2C C1C N1C 118.3(6) . . ? C6C C1C Zr1C 152.2(5) . . ? C2C C1C Zr1C 74.7(4) . . ? N1C C1C Zr1C 49.2(3) . . ? C3C C2C N2C 123.8(7) . . ? C3C C2C C1C 118.5(7) . . ? N2C C2C C1C 117.5(7) . . ? C3C C2C Zr1C 150.6(6) . . ? N2C C2C Zr1C 47.8(3) . . ? C1C C2C Zr1C 75.3(4) . . ? C4C C3C C2C 121.7(8) . . ? C3C C4C C5C 119.7(8) . . ? C6C C5C C4C 119.9(7) . . ? C5C C6C C1C 121.5(8) . . ? N3C C13C C14C 109.6(6) . . ? N4C C14C C13C 110.9(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.384 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.070 #===END data_oct2999-MFL7 _audit_creation_date 1999-10-27T09:52:42-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[{Zr(NMe2)2(C6H4(NSiMe3)2)}2]' _chemical_formula_moiety 'C32 H68 N8 Si4 Zr2' _chemical_formula_structural 'C32 H68 N8 Si4 Zr2' _chemical_formula_sum 'C32 H68 N8 Si4 Zr2' _chemical_formula_weight 859.74 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.7431(4) _cell_length_b 10.1941(2) _cell_length_c 18.7501(4) _cell_angle_alpha 90 _cell_angle_beta 116.8770(10) _cell_angle_gamma 90 _cell_volume 4389.02(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12797 _cell_measurement_theta_min 4.246 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.615 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8325 _exptl_absorpt_correction_T_max 0.9039 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 23086 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.32 _diffrn_reflns_theta_max 27.87 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 5216 _reflns_number_gt 4722 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0307P)^2^+4.9560P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00096(13) _refine_ls_number_reflns 5216 _refine_ls_number_parameters 219 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0691 _refine_ls_wR_factor_gt 0.0664 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.469 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.058 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Zr Zr 0.069185(6) 0.043630(15) 0.002093(8) 0.02139(7) Uani 1 1 d . . . Si1 Si 0.20318(2) -0.01358(5) 0.17415(3) 0.02768(11) Uani 1 1 d . . . Si2 Si 0.10846(2) 0.34337(5) -0.06718(3) 0.02901(11) Uani 1 1 d . . . N1 N 0.13486(6) 0.05639(13) 0.11818(8) 0.0240(3) Uani 1 1 d . . . N2 N 0.09763(6) 0.24016(14) -0.00147(8) 0.0239(3) Uani 1 1 d . . . N3 N -0.02304(6) 0.11634(15) -0.04430(9) 0.0294(3) Uani 1 1 d . . . N4 N 0.08870(8) -0.06357(17) -0.07431(10) 0.0409(4) Uani 1 1 d . . . C1 C 0.12342(6) 0.18508(17) 0.13627(9) 0.0239(3) Uani 1 1 d . . . C2 C 0.10599(6) 0.28185(16) 0.07457(9) 0.0239(3) Uani 1 1 d . . . C3 C 0.09594(8) 0.41017(18) 0.09293(11) 0.0310(4) Uani 1 1 d . . . H3 H 0.0848 0.476 0.0529 0.037 Uiso 1 1 calc R . . C4 C 0.10190(8) 0.4428(2) 0.16769(12) 0.0370(4) Uani 1 1 d . . . H4 H 0.0961 0.5309 0.179 0.044 Uiso 1 1 calc R . . C5 C 0.11643(8) 0.3471(2) 0.22661(11) 0.0385(4) Uani 1 1 d . . . H5 H 0.1194 0.3691 0.2776 0.046 Uiso 1 1 calc R . . C6 C 0.12643(8) 0.2202(2) 0.21051(10) 0.0323(4) Uani 1 1 d . . . H6 H 0.1356 0.1549 0.2506 0.039 Uiso 1 1 calc R . . C7 C 0.25832(8) 0.0922(2) 0.16321(13) 0.0424(5) Uani 1 1 d . . . H7A H 0.2493 0.0979 0.1066 0.064 Uiso 1 1 calc R . . H7B H 0.2972 0.0541 0.1936 0.064 Uiso 1 1 calc R . . H7C H 0.2575 0.1803 0.1836 0.064 Uiso 1 1 calc R . . C8 C 0.22468(9) -0.0303(2) 0.28332(11) 0.0396(5) Uani 1 1 d . . . H8A H 0.2292 0.057 0.3073 0.059 Uiso 1 1 calc R . . H8B H 0.2616 -0.078 0.3095 0.059 Uiso 1 1 calc R . . H8C H 0.1944 -0.0788 0.2904 0.059 Uiso 1 1 calc R . . C9 C 0.20236(9) -0.1827(2) 0.13578(13) 0.0454(5) Uani 1 1 d . . . H9A H 0.1816 -0.2415 0.1555 0.068 Uiso 1 1 calc R . . H9B H 0.2424 -0.2137 0.1545 0.068 Uiso 1 1 calc R . . H9C H 0.1826 -0.1818 0.0772 0.068 Uiso 1 1 calc R . . C10 C 0.17673(11) 0.4402(3) -0.01333(15) 0.0584(7) Uani 1 1 d . . . H10A H 0.1742 0.4924 0.0288 0.088 Uiso 1 1 calc R . . H10B H 0.1819 0.4986 -0.0511 0.088 Uiso 1 1 calc R . . H10C H 0.21 0.3803 0.0106 0.088 Uiso 1 1 calc R . . C11 C 0.11257(11) 0.2429(2) -0.14702(13) 0.0503(6) Uani 1 1 d . . . H11A H 0.149 0.1929 -0.1246 0.075 Uiso 1 1 calc R . . H11B H 0.1114 0.3005 -0.1896 0.075 Uiso 1 1 calc R . . H11C H 0.0795 0.1822 -0.1691 0.075 Uiso 1 1 calc R . . C12 C 0.04693(12) 0.4611(2) -0.12211(16) 0.0553(6) Uani 1 1 d . . . H12A H 0.0115 0.4118 -0.1555 0.083 Uiso 1 1 calc R . . H12B H 0.0569 0.5185 -0.156 0.083 Uiso 1 1 calc R . . H12C H 0.0403 0.5143 -0.0835 0.083 Uiso 1 1 calc R . . C13 C -0.03302(8) 0.24884(19) -0.02014(16) 0.0479(5) Uani 1 1 d . . . H13A H -0.0153 0.3149 -0.0403 0.072 Uiso 1 1 calc R . . H13B H -0.0154 0.254 0.0383 0.072 Uiso 1 1 calc R . . H13C H -0.075 0.2651 -0.0425 0.072 Uiso 1 1 calc R . . C14 C -0.04206(9) 0.1189(3) -0.13113(12) 0.0517(6) Uani 1 1 d . . . H14A H -0.0827 0.1477 -0.1589 0.077 Uiso 1 1 calc R . . H14B H -0.0386 0.0308 -0.1494 0.077 Uiso 1 1 calc R . . H14C H -0.0175 0.18 -0.1428 0.077 Uiso 1 1 calc R . . C15 C 0.14893(12) -0.0666(3) -0.06183(16) 0.0610(7) Uani 1 1 d . . . H15A H 0.1637 -0.1567 -0.0503 0.091 Uiso 1 1 calc R . . H15B H 0.1729 -0.0098 -0.0166 0.091 Uiso 1 1 calc R . . H15C H 0.1506 -0.0353 -0.1101 0.091 Uiso 1 1 calc R . . C16 C 0.05193(16) -0.1393(3) -0.14459(17) 0.0834(10) Uani 1 1 d . . . H16A H 0.0516 -0.0984 -0.1921 0.125 Uiso 1 1 calc R . . H16B H 0.0122 -0.1418 -0.1503 0.125 Uiso 1 1 calc R . . H16C H 0.0671 -0.2289 -0.1389 0.125 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 Zr 0.02222(9) 0.02288(10) 0.01838(9) -0.00076(5) 0.00856(6) -0.00197(5) Si1 0.0216(2) 0.0277(2) 0.0283(2) 0.00436(19) 0.00651(18) 0.00067(18) Si2 0.0319(2) 0.0310(3) 0.0279(2) 0.00153(19) 0.01685(19) -0.00542(19) N1 0.0211(6) 0.0259(7) 0.0214(6) 0.0011(5) 0.0065(5) -0.0004(5) N2 0.0251(6) 0.0253(7) 0.0223(6) 0.0000(5) 0.0116(5) -0.0018(5) N3 0.0246(7) 0.0282(8) 0.0305(7) 0.0076(6) 0.0083(6) -0.0019(6) N4 0.0616(11) 0.0352(9) 0.0327(8) -0.0070(7) 0.0273(8) 0.0001(8) C1 0.0179(7) 0.0296(8) 0.0235(7) -0.0013(6) 0.0086(6) -0.0015(6) C2 0.0194(7) 0.0284(8) 0.0238(7) -0.0016(6) 0.0097(6) -0.0013(6) C3 0.0315(9) 0.0282(9) 0.0327(9) -0.0007(7) 0.0138(7) 0.0025(7) C4 0.0351(10) 0.0361(10) 0.0403(10) -0.0104(8) 0.0174(8) 0.0026(8) C5 0.0367(9) 0.0517(12) 0.0300(9) -0.0117(8) 0.0177(8) -0.0007(9) C6 0.0315(8) 0.0418(10) 0.0246(8) -0.0002(7) 0.0134(7) -0.0013(7) C7 0.0295(9) 0.0452(12) 0.0542(12) 0.0050(10) 0.0206(9) -0.0020(8) C8 0.0361(10) 0.0426(11) 0.0283(9) 0.0088(8) 0.0041(8) -0.0003(8) C9 0.0421(11) 0.0336(11) 0.0484(12) 0.0009(9) 0.0099(9) 0.0084(9) C10 0.0561(14) 0.0768(18) 0.0467(12) -0.0091(12) 0.0272(11) -0.0355(13) C11 0.0775(16) 0.0477(13) 0.0395(11) -0.0030(10) 0.0386(11) -0.0101(12) C12 0.0640(15) 0.0515(14) 0.0576(14) 0.0264(11) 0.0339(13) 0.0139(11) C13 0.0288(9) 0.0273(10) 0.0862(17) 0.0090(10) 0.0248(10) 0.0032(8) C14 0.0353(10) 0.0792(17) 0.0317(10) 0.0208(10) 0.0074(8) -0.0157(11) C15 0.0799(18) 0.0640(16) 0.0631(15) 0.0102(13) 0.0535(15) 0.0241(14) C16 0.124(3) 0.075(2) 0.0511(15) -0.0305(14) 0.0389(17) -0.0189(19) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Zr N4 2.0370(16) . ? Zr N1 2.0702(13) . ? Zr N2 2.1444(14) . ? Zr N3 2.2528(14) . ? Zr N3 2.3551(14) 5 ? Zr C1 2.6799(16) . ? Zr C2 2.7345(16) . ? Zr Zr 3.6377(3) 5 ? Si1 N1 1.7419(14) . ? Si1 C9 1.864(2) . ? Si1 C7 1.867(2) . ? Si1 C8 1.871(2) . ? Si2 N2 1.7358(14) . ? Si2 C11 1.856(2) . ? Si2 C10 1.865(2) . ? Si2 C12 1.880(2) . ? N1 C1 1.419(2) . ? N2 C2 1.4080(19) . ? N3 C14 1.473(2) . ? N3 C13 1.484(3) . ? N3 Zr 2.3551(14) 5 ? N4 C16 1.449(3) . ? N4 C15 1.460(3) . ? C1 C6 1.405(2) . ? C1 C2 1.430(2) . ? C2 C3 1.406(2) . ? C3 C4 1.380(3) . ? C4 C5 1.393(3) . ? C5 C6 1.379(3) . ? 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 N4 Zr N1 115.42(7) . . ? N4 Zr N2 106.44(6) . . ? N1 Zr N2 81.14(5) . . ? N4 Zr N3 117.18(7) . . ? N1 Zr N3 127.05(5) . . ? N2 Zr N3 89.75(5) . . ? N4 Zr N3 100.78(6) . 5 ? N1 Zr N3 89.22(5) . 5 ? N2 Zr N3 152.69(5) . 5 ? N3 Zr N3 75.76(6) . 5 ? N4 Zr C1 139.41(6) . . ? N1 Zr C1 31.56(5) . . ? N2 Zr C1 59.09(5) . . ? N3 Zr C1 101.32(5) . . ? N3 Zr C1 100.66(5) 5 . ? N4 Zr C2 133.29(6) . . ? N1 Zr C2 59.13(5) . . ? N2 Zr C2 30.61(5) . . ? N3 Zr C2 88.14(5) . . ? N3 Zr C2 124.19(5) 5 . ? C1 Zr C2 30.60(5) . . ? N4 Zr Zr 113.83(5) . 5 ? N1 Zr Zr 111.37(4) . 5 ? N2 Zr Zr 124.93(4) . 5 ? N3 Zr Zr 38.87(4) . 5 ? N3 Zr Zr 36.89(3) 5 5 ? C1 Zr Zr 103.96(3) . 5 ? C2 Zr Zr 110.11(3) . 5 ? N1 Si1 C9 108.29(8) . . ? N1 Si1 C7 107.95(8) . . ? C9 Si1 C7 111.62(11) . . ? N1 Si1 C8 114.52(8) . . ? C9 Si1 C8 106.49(10) . . ? C7 Si1 C8 108.03(10) . . ? N2 Si2 C11 108.90(8) . . ? N2 Si2 C10 110.55(9) . . ? C11 Si2 C10 110.20(12) . . ? N2 Si2 C12 114.19(9) . . ? C11 Si2 C12 104.56(12) . . ? C10 Si2 C12 108.27(13) . . ? C1 N1 Si1 119.79(11) . . ? C1 N1 Zr 98.64(9) . . ? Si1 N1 Zr 136.88(8) . . ? C2 N2 Si2 122.39(11) . . ? C2 N2 Zr 98.54(10) . . ? Si2 N2 Zr 139.03(7) . . ? C14 N3 C13 107.70(18) . . ? C14 N3 Zr 101.44(12) . . ? C13 N3 Zr 118.65(11) . . ? C14 N3 Zr 114.69(12) . 5 ? C13 N3 Zr 110.16(11) . 5 ? Zr N3 Zr 104.24(6) . 5 ? C16 N4 C15 110.1(2) . . ? C16 N4 Zr 131.13(19) . . ? C15 N4 Zr 118.71(15) . . ? C6 C1 N1 123.23(15) . . ? C6 C1 C2 118.84(16) . . ? N1 C1 C2 117.89(14) . . ? C6 C1 Zr 147.05(12) . . ? N1 C1 Zr 49.79(7) . . ? C2 C1 Zr 76.81(9) . . ? C3 C2 N2 124.60(15) . . ? C3 C2 C1 117.97(15) . . ? N2 C2 C1 117.36(14) . . ? C3 C2 Zr 152.51(12) . . ? N2 C2 Zr 50.85(8) . . ? C1 C2 Zr 72.59(9) . . ? C4 C3 C2 121.65(17) . . ? C3 C4 C5 120.23(18) . . ? C6 C5 C4 119.57(17) . . ? C5 C6 C1 121.60(17) . . ? #===END