Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Martyn Coles' _publ_contact_author_address ; The Chemical Laboratories University of Sussex Chichester Building Falmer Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.P.COLES@SUSSEX.AC.UK _publ_section_title ; Titanium and zirconium complexes incorporating 1,3-bis(furyl)-1,1,3,3-tetramethyldisilazides : ligand transfer as a likely deactivation pathway in ethylene polymerization catalysis, deduced from stoichiometric alkylation studies ; _publ_requested_category FM loop_ _publ_author_name 'Martyn Coles' F.Cloke 'LLoyd T. J. Evans' P.B.Hitchcock # Attachment 'Combined_cif.cif' data_(1a)-apr806 _database_code_depnum_ccdc_archive 'CCDC 630138' _audit_creation_date 2006-04-06T16:15:45-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C12 H18 Cl3 N O2 Si2 Ti' _chemical_formula_sum 'C12 H18 Cl3 N O2 Si2 Ti' _chemical_formula_weight 418.7 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.8208(2) _cell_length_b 9.3822(3) _cell_length_c 15.0516(6) _cell_angle_alpha 97.848(2) _cell_angle_beta 90.932(2) _cell_angle_gamma 96.928(2) _cell_volume 946.70(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9672 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 428 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.003 _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 0.7198 _exptl_absorpt_correction_T_max 0.7905 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _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_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.146541 _diffrn_orient_matrix_ub_12 0.270447E-1 _diffrn_orient_matrix_ub_13 0.4599E-2 _diffrn_orient_matrix_ub_21 -0.37628E-2 _diffrn_orient_matrix_ub_22 0.55456E-2 _diffrn_orient_matrix_ub_23 0.667613E-1 _diffrn_orient_matrix_ub_31 0.186458E-1 _diffrn_orient_matrix_ub_32 -0.104856 _diffrn_orient_matrix_ub_33 -0.49665E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_unetI/netI 0.0375 _diffrn_reflns_number 13530 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 25.96 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 3688 _reflns_number_gt 3295 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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 icluding possible twinning by 180 degrees rotation about [001]with matrix (-1 0 0 0 -1 0 0.146 0.450 1) gave BASF 0.019 with a small reduction in residuals. 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^)+(0.0736P)^2^+16.7351P] 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_number_reflns 3688 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0848 _refine_ls_wR_factor_ref 0.2547 _refine_ls_wR_factor_gt 0.2494 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.34 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.155 #----------------------------------------------------------------------------# # 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' 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' O O 0.0106 0.006 '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' Ti Ti 0.2776 0.4457 '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 Ti Ti 0.3381(2) 0.89373(15) 0.25690(10) 0.0257(4) Uani 1 1 d . . . Cl1 Cl 0.6476(3) 0.8577(3) 0.22768(18) 0.0434(6) Uani 1 1 d . . . Cl2 Cl 0.2107(4) 1.0547(2) 0.18436(16) 0.0421(6) Uani 1 1 d . . . Cl3 Cl 0.3688(4) 1.0142(3) 0.39347(16) 0.0463(6) Uani 1 1 d . . . Si1 Si 0.1135(3) 0.6614(2) 0.37194(14) 0.0239(5) Uani 1 1 d . . . Si2 Si 0.1562(3) 0.6070(2) 0.16309(14) 0.0228(5) Uani 1 1 d . . . O1 O -0.2310(9) 0.4648(7) 0.3318(4) 0.0350(14) Uani 1 1 d . . . O2 O 0.0811(11) 0.7845(8) 0.0370(4) 0.0424(16) Uani 1 1 d . . . N N 0.1859(10) 0.7225(7) 0.2677(4) 0.0232(13) Uani 1 1 d . . . C1 C -0.2946(16) 0.3200(11) 0.3162(7) 0.044(2) Uani 1 1 d . . . H1 H -0.4285 0.2809 0.3029 0.052 Uiso 1 1 calc R . . C2 C -0.1504(16) 0.2406(10) 0.3215(7) 0.045(2) Uani 1 1 d . . . H2 H -0.1603 0.1377 0.3134 0.053 Uiso 1 1 calc R . . C3 C 0.0264(15) 0.3416(10) 0.3421(6) 0.036(2) Uani 1 1 d . . . H3 H 0.1563 0.3179 0.3507 0.044 Uiso 1 1 calc R . . C4 C -0.0284(12) 0.4775(9) 0.3469(5) 0.0273(17) Uani 1 1 d . . . C5 C 0.3397(14) 0.6400(11) 0.4370(6) 0.037(2) Uani 1 1 d . . . H5A H 0.4199 0.7345 0.4519 0.056 Uiso 1 1 calc R . . H5B H 0.4165 0.5729 0.4009 0.056 Uiso 1 1 calc R . . H5C H 0.3019 0.6013 0.4924 0.056 Uiso 1 1 calc R . . C6 C -0.0550(14) 0.7817(10) 0.4306(6) 0.036(2) Uani 1 1 d . . . H6A H 0.0144 0.8802 0.445 0.055 Uiso 1 1 calc R . . H6B H -0.0972 0.7452 0.4861 0.055 Uiso 1 1 calc R . . H6C H -0.171 0.7833 0.3916 0.055 Uiso 1 1 calc R . . C7 C -0.1019(14) 0.5322(11) 0.1349(6) 0.039(2) Uani 1 1 d . . . H7A H -0.1837 0.6116 0.1373 0.058 Uiso 1 1 calc R . . H7B H -0.1486 0.4674 0.178 0.058 Uiso 1 1 calc R . . H7C H -0.1111 0.4778 0.0743 0.058 Uiso 1 1 calc R . . C8 C 0.3269(14) 0.4678(10) 0.1600(7) 0.037(2) Uani 1 1 d . . . H8A H 0.4617 0.515 0.1751 0.055 Uiso 1 1 calc R . . H8B H 0.3224 0.4125 0.0997 0.055 Uiso 1 1 calc R . . H8C H 0.2871 0.4021 0.2036 0.055 Uiso 1 1 calc R . . C9 C 0.2335(13) 0.7279(9) 0.0780(5) 0.0284(17) Uani 1 1 d . . . C10 C 0.4010(15) 0.7568(9) 0.0332(6) 0.035(2) Uani 1 1 d . . . H10 H 0.526 0.7278 0.0461 0.042 Uiso 1 1 calc R . . C11 C 0.358(2) 0.8385(12) -0.0366(6) 0.054(3) Uani 1 1 d . . . H11 H 0.4463 0.8743 -0.0788 0.064 Uiso 1 1 calc R . . C12 C 0.165(2) 0.8537(12) -0.0298(7) 0.052(3) Uani 1 1 d . . . H12 H 0.0958 0.9063 -0.0669 0.062 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 Ti 0.0288(8) 0.0179(7) 0.0287(8) 0.0022(5) 0.0004(6) -0.0021(5) Cl1 0.0273(11) 0.0419(13) 0.0561(15) -0.0067(11) -0.0019(10) -0.0001(9) Cl2 0.0614(15) 0.0254(11) 0.0407(12) 0.0021(9) -0.0068(11) 0.0143(10) Cl3 0.0650(16) 0.0332(12) 0.0329(12) -0.0067(9) -0.0013(11) -0.0131(11) Si1 0.0282(11) 0.0194(10) 0.0230(11) 0.0012(8) 0.0019(8) 0.0006(8) Si2 0.0243(11) 0.0189(10) 0.0228(10) -0.0027(8) 0.0014(8) -0.0003(8) O1 0.029(3) 0.034(3) 0.040(3) 0.008(3) 0.004(3) -0.006(3) O2 0.051(4) 0.046(4) 0.033(3) 0.002(3) -0.011(3) 0.018(3) N 0.030(3) 0.017(3) 0.020(3) -0.002(2) 0.001(3) -0.001(3) C1 0.047(6) 0.036(5) 0.042(5) 0.003(4) 0.003(4) -0.016(4) C2 0.054(6) 0.023(4) 0.052(6) -0.001(4) 0.010(5) -0.009(4) C3 0.045(5) 0.027(4) 0.035(5) 0.002(4) 0.007(4) 0.003(4) C4 0.026(4) 0.027(4) 0.027(4) 0.002(3) 0.005(3) 0.002(3) C5 0.034(5) 0.041(5) 0.036(5) 0.007(4) -0.003(4) 0.001(4) C6 0.038(5) 0.032(5) 0.039(5) -0.002(4) 0.008(4) 0.007(4) C7 0.035(5) 0.043(5) 0.032(5) -0.011(4) 0.001(4) -0.005(4) C8 0.036(5) 0.032(5) 0.045(5) 0.012(4) 0.013(4) 0.009(4) C9 0.036(4) 0.024(4) 0.024(4) -0.002(3) -0.002(3) 0.005(3) C10 0.048(5) 0.028(4) 0.028(4) 0.004(3) 0.009(4) -0.001(4) C11 0.097(10) 0.040(6) 0.022(5) 0.009(4) 0.006(5) -0.005(6) C12 0.089(9) 0.039(6) 0.030(5) 0.010(4) -0.010(5) 0.016(6) #----------------------------------------------------------------------------# # 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 Ti N 1.833(6) . ? Ti Cl3 2.200(3) . ? Ti Cl1 2.219(3) . ? Ti Cl2 2.228(3) . ? Si1 N 1.799(7) . ? Si1 C6 1.857(9) . ? Si1 C5 1.860(9) . ? Si1 C4 1.861(9) . ? Si2 N 1.779(6) . ? Si2 C7 1.835(9) . ? Si2 C8 1.848(9) . ? Si2 C9 1.866(9) . ? O1 C1 1.362(11) . ? O1 C4 1.385(10) . ? O2 C12 1.367(13) . ? O2 C9 1.395(10) . ? C1 C2 1.311(15) . ? C1 H1 0.95 . ? C2 C3 1.442(13) . ? C2 H2 0.95 . ? C3 C4 1.365(12) . ? C3 H3 0.95 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 C10 1.354(13) . ? C10 C11 1.430(14) . ? C10 H10 0.95 . ? C11 C12 1.342(18) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? 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 N Ti Cl3 105.2(2) . . ? N Ti Cl1 111.0(2) . . ? Cl3 Ti Cl1 102.19(12) . . ? N Ti Cl2 118.8(2) . . ? Cl3 Ti Cl2 100.12(11) . . ? Cl1 Ti Cl2 116.60(12) . . ? N Si1 C6 110.3(4) . . ? N Si1 C5 108.7(4) . . ? C6 Si1 C5 115.8(4) . . ? N Si1 C4 108.6(3) . . ? C6 Si1 C4 106.9(4) . . ? C5 Si1 C4 106.3(4) . . ? N Si2 C7 113.0(4) . . ? N Si2 C8 109.8(4) . . ? C7 Si2 C8 113.7(5) . . ? N Si2 C9 104.7(3) . . ? C7 Si2 C9 106.7(4) . . ? C8 Si2 C9 108.3(4) . . ? C1 O1 C4 106.3(7) . . ? C12 O2 C9 106.1(8) . . ? Si2 N Si1 122.7(4) . . ? Si2 N Ti 111.1(3) . . ? Si1 N Ti 125.3(4) . . ? C2 C1 O1 112.5(9) . . ? C2 C1 H1 123.7 . . ? O1 C1 H1 123.7 . . ? C1 C2 C3 105.8(8) . . ? C1 C2 H2 127.1 . . ? C3 C2 H2 127.1 . . ? C4 C3 C2 107.0(9) . . ? C4 C3 H3 126.5 . . ? C2 C3 H3 126.5 . . ? C3 C4 O1 108.4(8) . . ? C3 C4 Si1 132.4(7) . . ? O1 C4 Si1 119.2(6) . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 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 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 O2 108.4(8) . . ? C10 C9 Si2 134.8(7) . . ? O2 C9 Si2 115.6(6) . . ? C9 C10 C11 108.3(10) . . ? C9 C10 H10 125.8 . . ? C11 C10 H10 125.8 . . ? C12 C11 C10 105.2(9) . . ? C12 C11 H11 127.4 . . ? C10 C11 H11 127.4 . . ? C11 C12 O2 111.8(9) . . ? C11 C12 H12 124.1 . . ? O2 C12 H12 124.1 . . ? #===END data_(1b)-mar2206 _database_code_depnum_ccdc_archive 'CCDC 630139' _audit_creation_date 2006-03-31T11:17:55-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C14 H22 Cl3 N O2 Si2 Ti' _chemical_formula_sum 'C14 H22 Cl3 N O2 Si2 Ti' _chemical_formula_weight 446.76 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 27.1916(4) _cell_length_b 11.2759(2) _cell_length_c 29.9679(4) _cell_angle_alpha 90 _cell_angle_beta 110.992(1) _cell_angle_gamma 90 _cell_volume 8578.6(2) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 54214 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3680 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.89 _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 0.7847 _exptl_absorpt_correction_T_max 0.8571 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.344663E-1 _diffrn_orient_matrix_ub_12 0.66662E-2 _diffrn_orient_matrix_ub_13 0.4756E-2 _diffrn_orient_matrix_ub_21 -0.190198E-1 _diffrn_orient_matrix_ub_22 -0.56583E-2 _diffrn_orient_matrix_ub_23 -0.353259E-1 _diffrn_orient_matrix_ub_31 -0.1384E-2 _diffrn_orient_matrix_ub_32 -0.882526E-1 _diffrn_orient_matrix_ub_33 0.26242E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_unetI/netI 0.0412 _diffrn_reflns_number 58579 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 8426 _reflns_number_gt 6156 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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^)+(0.0351P)^2^+12.9275P] 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_number_reflns 8426 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0673 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0917 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.382 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.059 #----------------------------------------------------------------------------# # 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' 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' O O 0.0106 0.006 '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' Ti Ti 0.2776 0.4457 '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 Ti Ti 0.118116(19) 0.54340(4) 0.201665(16) 0.02917(12) Uani 1 1 d . . . Cl1 Cl 0.17747(3) 0.66116(6) 0.25397(3) 0.04096(18) Uani 1 1 d . . . Cl2 Cl 0.12529(3) 0.61776(6) 0.13596(3) 0.0500(2) Uani 1 1 d . . . Cl3 Cl 0.03283(3) 0.57414(7) 0.18714(3) 0.04610(19) Uani 1 1 d . . . Si1 Si 0.13823(3) 0.31107(6) 0.25151(3) 0.03119(18) Uani 1 1 d . . . Si2 Si 0.13296(3) 0.30876(6) 0.14525(2) 0.02700(17) Uani 1 1 d . . . O1 O 0.17780(7) 0.47484(16) 0.32561(6) 0.0342(4) Uani 1 1 d . . . O2 O 0.08035(7) 0.09645(15) 0.14076(6) 0.0344(4) Uani 1 1 d . . . N N 0.13163(8) 0.38477(17) 0.19726(7) 0.0277(5) Uani 1 1 d . . . C1 C 0.20769(13) 0.6108(3) 0.39233(10) 0.0526(8) Uani 1 1 d . . . H1A H 0.1938 0.6748 0.4065 0.079 Uiso 1 1 calc R . . H1B H 0.2333 0.6434 0.3795 0.079 Uiso 1 1 calc R . . H1C H 0.2249 0.5514 0.4168 0.079 Uiso 1 1 calc R . . C2 C 0.16391(12) 0.5547(2) 0.35320(9) 0.0365(7) Uani 1 1 d . . . C3 C 0.11118(12) 0.5633(2) 0.33845(10) 0.0398(7) Uani 1 1 d . . . H3 H 0.0916 0.6118 0.352 0.048 Uiso 1 1 calc R . . C4 C 0.09054(11) 0.4862(2) 0.29888(9) 0.0355(6) Uani 1 1 d . . . H4 H 0.0543 0.473 0.281 0.043 Uiso 1 1 calc R . . C5 C 0.13181(10) 0.4339(2) 0.29079(9) 0.0305(6) Uani 1 1 d . . . C6 C 0.20463(13) 0.2462(3) 0.28026(11) 0.0538(9) Uani 1 1 d . . . H6A H 0.2313 0.3072 0.2834 0.081 Uiso 1 1 calc R . . H6B H 0.2093 0.1809 0.2606 0.081 Uiso 1 1 calc R . . H6C H 0.2084 0.2163 0.312 0.081 Uiso 1 1 calc R . . C7 C 0.08293(13) 0.2077(3) 0.24284(10) 0.0503(8) Uani 1 1 d . . . H7A H 0.0853 0.142 0.2223 0.075 Uiso 1 1 calc R . . H7B H 0.0495 0.2498 0.2277 0.075 Uiso 1 1 calc R . . H7C H 0.0847 0.1765 0.2739 0.075 Uiso 1 1 calc R . . C8 C 0.19690(11) 0.3423(3) 0.13920(10) 0.0412(7) Uani 1 1 d . . . H8A H 0.2257 0.3202 0.1687 0.062 Uiso 1 1 calc R . . H8B H 0.1989 0.4273 0.1333 0.062 Uiso 1 1 calc R . . H8C H 0.2 0.297 0.1124 0.062 Uiso 1 1 calc R . . C9 C 0.07367(10) 0.3445(3) 0.09289(9) 0.0378(7) Uani 1 1 d . . . H9A H 0.0421 0.3236 0.0997 0.057 Uiso 1 1 calc R . . H9B H 0.0742 0.2994 0.0651 0.057 Uiso 1 1 calc R . . H9C H 0.0732 0.4296 0.086 0.057 Uiso 1 1 calc R . . C10 C 0.13060(10) 0.1465(2) 0.15546(9) 0.0303(6) Uani 1 1 d . . . C11 C 0.16577(12) 0.0589(2) 0.17381(10) 0.0387(7) Uani 1 1 d . . . H11 H 0.203 0.0673 0.1863 0.046 Uiso 1 1 calc R . . C12 C 0.13739(13) -0.0485(2) 0.17124(10) 0.0445(8) Uani 1 1 d . . . H12 H 0.1521 -0.1245 0.1818 0.053 Uiso 1 1 calc R . . C13 C 0.08615(12) -0.0222(2) 0.15121(10) 0.0394(7) Uani 1 1 d . . . C14 C 0.03603(13) -0.0909(3) 0.13771(12) 0.0521(8) Uani 1 1 d . . . H14A H 0.044 -0.1749 0.1452 0.078 Uiso 1 1 calc R . . H14B H 0.0164 -0.082 0.1034 0.078 Uiso 1 1 calc R . . H14C H 0.0148 -0.0609 0.1556 0.078 Uiso 1 1 calc R . . Ti1B Ti 0.145419(19) 1.05463(4) 0.963889(17) 0.03092(13) Uani 1 1 d . A 1 Cl1B Cl 0.09668(3) 1.18135(6) 0.90941(3) 0.04193(18) Uani 1 1 d . A 1 Cl2B Cl 0.13402(4) 1.12955(6) 1.02762(3) 0.0530(2) Uani 1 1 d . A 1 Cl3B Cl 0.23147(3) 1.06978(8) 0.98124(3) 0.0535(2) Uani 1 1 d . A 1 Si1B Si 0.12442(3) 0.82311(6) 0.91120(2) 0.03077(18) Uani 1 1 d . A 1 Si2B Si 0.11600(3) 0.82299(6) 1.01265(3) 0.02971(17) Uani 1 1 d . A 1 O1B O 0.09183(7) 0.99081(16) 0.83733(6) 0.0330(4) Uani 1 1 d . A 1 O2B O 0.06597(7) 0.60431(15) 0.97823(6) 0.0326(4) Uani 1 1 d . A 1 N1B N 0.12541(8) 0.89844(18) 0.96353(7) 0.0287(5) Uani 1 1 d . A 1 C1B C 0.06923(12) 1.1328(3) 0.77263(11) 0.0538(8) Uani 1 1 d . A 1 H1B1 H 0.0863 1.1873 0.7572 0.081 Uiso 1 1 calc R A 1 H1B2 H 0.0466 1.1779 0.7856 0.081 Uiso 1 1 calc R A 1 H1B3 H 0.0479 1.0754 0.7491 0.081 Uiso 1 1 calc R A 1 C2B C 0.10991(11) 1.0692(2) 0.81189(9) 0.0365(7) Uani 1 1 d . A 1 C3B C 0.16272(11) 1.0693(3) 0.82866(10) 0.0420(7) Uani 1 1 d . A 1 H3B H 0.1848 1.115 0.8169 0.05 Uiso 1 1 calc R A 1 C4B C 0.17920(11) 0.9888(3) 0.86700(10) 0.0377(7) Uani 1 1 d . A 1 H4B H 0.2147 0.9701 0.8857 0.045 Uiso 1 1 calc R A 1 C5B C 0.13569(10) 0.9423(2) 0.87269(9) 0.0315(6) Uani 1 1 d . A 1 C6B C 0.05966(12) 0.7550(3) 0.87925(10) 0.0482(8) Uani 1 1 d . A 1 H6B1 H 0.032 0.8151 0.8735 0.072 Uiso 1 1 calc R A 1 H6B2 H 0.0536 0.6907 0.8987 0.072 Uiso 1 1 calc R A 1 H6B3 H 0.059 0.723 0.8486 0.072 Uiso 1 1 calc R A 1 C7B C 0.18118(13) 0.7217(3) 0.92490(11) 0.0520(8) Uani 1 1 d . A 1 H7B1 H 0.2137 0.7653 0.9418 0.078 Uiso 1 1 calc R A 1 H7B2 H 0.1827 0.6893 0.8951 0.078 Uiso 1 1 calc R A 1 H7B3 H 0.1772 0.6567 0.9451 0.078 Uiso 1 1 calc R A 1 C8B C 0.05201(12) 0.8686(3) 1.01577(12) 0.0481(8) Uani 1 1 d . A 1 H8B1 H 0.0521 0.9544 1.021 0.072 Uiso 1 1 calc R A 1 H8B2 H 0.0463 0.8273 1.0423 0.072 Uiso 1 1 calc R A 1 H8B3 H 0.0237 0.8483 0.9857 0.072 Uiso 1 1 calc R A 1 C9B C 0.17427(12) 0.8483(3) 1.06776(10) 0.0445(7) Uani 1 1 d . A 1 H9B1 H 0.1777 0.9333 1.0751 0.067 Uiso 1 1 calc R A 1 H9B2 H 0.206 0.82 1.0628 0.067 Uiso 1 1 calc R A 1 H9B3 H 0.1698 0.805 1.0944 0.067 Uiso 1 1 calc R A 1 C10B C 0.11386(10) 0.6604(2) 1.00272(9) 0.0319(6) Uani 1 1 d . A 1 C11B C 0.15117(12) 0.5747(2) 1.01709(11) 0.0423(7) Uani 1 1 d . A 1 H11B H 0.1875 0.5869 1.0349 0.051 Uiso 1 1 calc R A 1 C12B C 0.12683(12) 0.4643(2) 1.00115(11) 0.0417(7) Uani 1 1 d . A 1 H12B H 0.1438 0.3892 1.006 0.05 Uiso 1 1 calc R A 1 C13B C 0.07564(11) 0.4845(2) 0.97811(9) 0.0331(6) Uani 1 1 d . A 1 C14B C 0.02943(12) 0.4078(2) 0.95499(11) 0.0450(7) Uani 1 1 d . A 1 H14D H 0.0407 0.3248 0.9576 0.068 Uiso 1 1 calc R A 1 H14E H 0.0131 0.4296 0.9212 0.068 Uiso 1 1 calc R A 1 H14F H 0.0039 0.4184 0.9709 0.068 Uiso 1 1 calc R A 1 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 Ti 0.0368(3) 0.0219(2) 0.0327(3) -0.0011(2) 0.0172(2) -0.0018(2) Cl1 0.0459(4) 0.0325(4) 0.0444(4) -0.0032(3) 0.0161(3) -0.0105(3) Cl2 0.0837(6) 0.0319(4) 0.0474(4) 0.0054(3) 0.0391(4) -0.0048(4) Cl3 0.0367(4) 0.0573(5) 0.0432(4) 0.0082(4) 0.0130(3) 0.0065(3) Si1 0.0449(5) 0.0252(4) 0.0272(4) 0.0004(3) 0.0175(3) 0.0002(3) Si2 0.0323(4) 0.0250(4) 0.0275(4) -0.0018(3) 0.0154(3) -0.0003(3) O1 0.0374(11) 0.0340(10) 0.0288(10) -0.0017(8) 0.0092(8) 0.0004(9) O2 0.0409(11) 0.0284(10) 0.0357(10) -0.0036(8) 0.0161(9) -0.0028(9) N 0.0373(12) 0.0224(11) 0.0281(11) -0.0006(9) 0.0172(10) -0.0009(9) C1 0.063(2) 0.0491(19) 0.0354(17) -0.0090(15) 0.0053(15) -0.0036(17) C2 0.054(2) 0.0299(15) 0.0254(14) -0.0027(12) 0.0140(13) -0.0008(13) C3 0.0517(19) 0.0369(16) 0.0358(16) -0.0067(13) 0.0216(14) 0.0052(14) C4 0.0373(16) 0.0400(16) 0.0316(15) -0.0027(13) 0.0151(13) -0.0008(13) C5 0.0355(15) 0.0294(14) 0.0272(14) -0.0031(12) 0.0120(12) -0.0050(12) C6 0.065(2) 0.052(2) 0.0409(17) 0.0006(16) 0.0152(16) 0.0212(17) C7 0.082(2) 0.0394(17) 0.0414(17) -0.0056(14) 0.0359(17) -0.0206(17) C8 0.0405(17) 0.0421(17) 0.0486(18) -0.0030(14) 0.0252(14) -0.0011(14) C9 0.0394(16) 0.0402(16) 0.0333(15) 0.0017(13) 0.0124(13) 0.0037(13) C10 0.0362(15) 0.0292(14) 0.0288(14) -0.0053(12) 0.0156(12) -0.0033(12) C11 0.0415(17) 0.0330(16) 0.0412(16) -0.0035(13) 0.0146(13) 0.0039(13) C12 0.064(2) 0.0236(15) 0.0491(18) -0.0026(13) 0.0243(16) 0.0026(14) C13 0.058(2) 0.0267(15) 0.0384(16) -0.0073(13) 0.0231(15) -0.0071(14) C14 0.066(2) 0.0382(17) 0.057(2) -0.0102(16) 0.0284(17) -0.0195(16) Ti1B 0.0417(3) 0.0214(2) 0.0320(3) -0.0010(2) 0.0160(2) -0.0010(2) Cl1B 0.0555(5) 0.0289(4) 0.0432(4) 0.0050(3) 0.0198(3) 0.0080(3) Cl2B 0.0942(6) 0.0294(4) 0.0467(4) -0.0083(3) 0.0391(4) 0.0007(4) Cl3B 0.0403(4) 0.0707(6) 0.0438(4) -0.0128(4) 0.0083(3) -0.0102(4) Si1B 0.0452(5) 0.0240(4) 0.0282(4) -0.0024(3) 0.0192(3) 0.0002(3) Si2B 0.0412(4) 0.0237(4) 0.0309(4) 0.0002(3) 0.0210(3) 0.0003(3) O1B 0.0336(10) 0.0355(10) 0.0305(10) 0.0021(8) 0.0123(8) -0.0041(8) O2B 0.0410(11) 0.0225(9) 0.0381(10) 0.0027(8) 0.0188(9) 0.0037(8) N1B 0.0398(13) 0.0216(11) 0.0289(11) -0.0011(9) 0.0174(10) 0.0015(9) C1B 0.052(2) 0.060(2) 0.0420(18) 0.0151(16) 0.0077(15) -0.0029(17) C2B 0.0422(18) 0.0378(16) 0.0296(15) 0.0044(13) 0.0129(13) -0.0060(13) C3B 0.0413(18) 0.0482(18) 0.0391(16) 0.0081(14) 0.0178(14) -0.0095(14) C4B 0.0317(16) 0.0472(17) 0.0353(15) 0.0028(14) 0.0133(12) -0.0004(13) C5B 0.0376(16) 0.0305(14) 0.0275(14) -0.0014(12) 0.0130(12) -0.0003(12) C6B 0.067(2) 0.0462(18) 0.0351(16) -0.0069(14) 0.0233(15) -0.0203(16) C7B 0.077(2) 0.0424(18) 0.0490(19) 0.0040(15) 0.0378(17) 0.0217(17) C8B 0.055(2) 0.0358(17) 0.070(2) -0.0062(16) 0.0421(17) -0.0011(15) C9B 0.063(2) 0.0398(17) 0.0338(16) 0.0030(14) 0.0205(15) -0.0049(15) C10B 0.0400(16) 0.0276(14) 0.0333(15) 0.0010(12) 0.0193(13) -0.0021(12) C11B 0.0387(17) 0.0309(16) 0.0563(19) 0.0079(14) 0.0156(14) 0.0049(13) C12B 0.0475(19) 0.0259(15) 0.0562(19) 0.0073(14) 0.0240(15) 0.0076(13) C13B 0.0484(18) 0.0214(13) 0.0356(15) 0.0021(12) 0.0225(14) 0.0033(12) C14B 0.0550(19) 0.0291(15) 0.0522(19) -0.0050(14) 0.0207(16) -0.0011(14) #----------------------------------------------------------------------------# # 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 Ti N 1.840(2) . ? Ti Cl2 2.2121(8) . ? Ti Cl3 2.2280(8) . ? Ti Cl1 2.2388(8) . ? Si1 N 1.777(2) . ? Si1 C7 1.846(3) . ? Si1 C6 1.850(3) . ? Si1 C5 1.866(3) . ? Si2 N 1.790(2) . ? Si2 C9 1.847(3) . ? Si2 C8 1.851(3) . ? Si2 C10 1.860(3) . ? O1 C2 1.364(3) . ? O1 C5 1.390(3) . ? O2 C13 1.370(3) . ? O2 C10 1.396(3) . ? C1 C2 1.481(4) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 C3 1.344(4) . ? C3 C4 1.415(4) . ? C3 H3 0.95 . ? C4 C5 1.364(4) . ? C4 H4 0.95 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 C11 1.348(4) . ? C11 C12 1.423(4) . ? C11 H11 0.95 . ? C12 C13 1.338(4) . ? C12 H12 0.95 . ? C13 C14 1.492(4) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? Ti1B N1B 1.842(2) . ? Ti1B Cl2B 2.2095(8) . ? Ti1B Cl3B 2.2143(9) . ? Ti1B Cl1B 2.2166(8) . ? Si1B N1B 1.775(2) . ? Si1B C6B 1.844(3) . ? Si1B C7B 1.845(3) . ? Si1B C5B 1.867(3) . ? Si2B N1B 1.796(2) . ? Si2B C8B 1.849(3) . ? Si2B C10B 1.855(3) . ? Si2B C9B 1.856(3) . ? O1B C2B 1.368(3) . ? O1B C5B 1.393(3) . ? O2B C13B 1.377(3) . ? O2B C10B 1.396(3) . ? C1B C2B 1.480(4) . ? C1B H1B1 0.98 . ? C1B H1B2 0.98 . ? C1B H1B3 0.98 . ? C2B C3B 1.341(4) . ? C3B C4B 1.405(4) . ? C3B H3B 0.95 . ? C4B C5B 1.360(4) . ? C4B H4B 0.95 . ? C6B H6B1 0.98 . ? C6B H6B2 0.98 . ? C6B H6B3 0.98 . ? C7B H7B1 0.98 . ? C7B H7B2 0.98 . ? C7B H7B3 0.98 . ? C8B H8B1 0.98 . ? C8B H8B2 0.98 . ? C8B H8B3 0.98 . ? C9B H9B1 0.98 . ? C9B H9B2 0.98 . ? C9B H9B3 0.98 . ? C10B C11B 1.354(4) . ? C11B C12B 1.411(4) . ? C11B H11B 0.95 . ? C12B C13B 1.333(4) . ? C12B H12B 0.95 . ? C13B C14B 1.477(4) . ? C14B H14D 0.98 . ? C14B H14E 0.98 . ? C14B H14F 0.98 . ? 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 N Ti Cl2 102.77(6) . . ? N Ti Cl3 110.97(7) . . ? Cl2 Ti Cl3 100.64(3) . . ? N Ti Cl1 120.95(7) . . ? Cl2 Ti Cl1 97.30(3) . . ? Cl3 Ti Cl1 118.90(3) . . ? N Si1 C7 110.87(12) . . ? N Si1 C6 111.88(13) . . ? C7 Si1 C6 115.22(16) . . ? N Si1 C5 103.21(11) . . ? C7 Si1 C5 107.57(13) . . ? C6 Si1 C5 107.21(13) . . ? N Si2 C9 110.57(11) . . ? N Si2 C8 107.47(12) . . ? C9 Si2 C8 115.91(13) . . ? N Si2 C10 108.36(10) . . ? C9 Si2 C10 106.47(12) . . ? C8 Si2 C10 107.82(12) . . ? C2 O1 C5 107.7(2) . . ? C13 O2 C10 107.7(2) . . ? Si1 N Si2 123.08(11) . . ? Si1 N Ti 110.25(10) . . ? Si2 N Ti 126.48(11) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 110.1(2) . . ? C3 C2 C1 133.6(3) . . ? O1 C2 C1 116.3(3) . . ? C2 C3 C4 106.7(2) . . ? C2 C3 H3 126.7 . . ? C4 C3 H3 126.7 . . ? C5 C4 C3 108.1(2) . . ? C5 C4 H4 126 . . ? C3 C4 H4 126 . . ? C4 C5 O1 107.4(2) . . ? C4 C5 Si1 134.6(2) . . ? O1 C5 Si1 117.25(18) . . ? 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 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 O2 107.6(2) . . ? C11 C10 Si2 136.7(2) . . ? O2 C10 Si2 115.70(18) . . ? C10 C11 C12 108.1(3) . . ? C10 C11 H11 126 . . ? C12 C11 H11 126 . . ? C13 C12 C11 107.1(3) . . ? C13 C12 H12 126.5 . . ? C11 C12 H12 126.5 . . ? C12 C13 O2 109.6(2) . . ? C12 C13 C14 135.2(3) . . ? O2 C13 C14 115.2(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1B Ti1B Cl2B 103.76(7) . . ? N1B Ti1B Cl3B 111.11(7) . . ? Cl2B Ti1B Cl3B 103.37(4) . . ? N1B Ti1B Cl1B 120.96(7) . . ? Cl2B Ti1B Cl1B 99.10(3) . . ? Cl3B Ti1B Cl1B 115.21(4) . . ? N1B Si1B C6B 111.56(12) . . ? N1B Si1B C7B 110.68(12) . . ? C6B Si1B C7B 115.13(16) . . ? N1B Si1B C5B 104.35(11) . . ? C6B Si1B C5B 108.46(13) . . ? C7B Si1B C5B 105.90(13) . . ? N1B Si2B C8B 108.82(12) . . ? N1B Si2B C10B 110.01(10) . . ? C8B Si2B C10B 107.88(13) . . ? N1B Si2B C9B 109.25(12) . . ? C8B Si2B C9B 115.54(14) . . ? C10B Si2B C9B 105.22(13) . . ? C2B O1B C5B 107.3(2) . . ? C13B O2B C10B 107.6(2) . . ? Si1B N1B Si2B 122.40(12) . . ? Si1B N1B Ti1B 111.94(11) . . ? Si2B N1B Ti1B 125.21(11) . . ? C3B C2B O1B 110.0(2) . . ? C3B C2B C1B 133.8(3) . . ? O1B C2B C1B 116.2(2) . . ? C2B C3B C4B 106.9(2) . . ? C2B C3B H3B 126.6 . . ? C4B C3B H3B 126.6 . . ? C5B C4B C3B 108.4(2) . . ? C5B C4B H4B 125.8 . . ? C3B C4B H4B 125.8 . . ? C4B C5B O1B 107.4(2) . . ? C4B C5B Si1B 134.3(2) . . ? O1B C5B Si1B 117.88(18) . . ? Si1B C6B H6B1 109.5 . . ? Si1B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? Si1B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? Si1B C7B H7B1 109.5 . . ? Si1B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? Si1B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? Si2B C8B H8B1 109.5 . . ? Si2B C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? Si2B C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? Si2B C9B H9B1 109.5 . . ? Si2B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? Si2B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C11B C10B O2B 107.2(2) . . ? C11B C10B Si2B 132.6(2) . . ? O2B C10B Si2B 120.10(18) . . ? C10B C11B C12B 108.3(3) . . ? C10B C11B H11B 125.8 . . ? C12B C11B H11B 125.8 . . ? C13B C12B C11B 107.5(3) . . ? C13B C12B H12B 126.3 . . ? C11B C12B H12B 126.3 . . ? C12B C13B O2B 109.4(2) . . ? C12B C13B C14B 134.2(3) . . ? O2B C13B C14B 116.4(2) . . ? #===END data_(3a)-sep1006 _database_code_depnum_ccdc_archive 'CCDC 630140' _audit_creation_date 2006-09-14T13:43:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H36 Cl6 N2 O4 Si4 Zr2' _chemical_formula_sum 'C24 H36 Cl6 N2 O4 Si4 Zr2' _chemical_formula_weight 924.05 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 15.7737(13) _cell_length_b 8.0018(8) _cell_length_c 16.6741(14) _cell_angle_alpha 90 _cell_angle_beta 113.423(5) _cell_angle_gamma 90 _cell_volume 1931.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19207 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_special_details ; Higher anglediffraction was very weak . ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.11 _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 0.5970 _exptl_absorpt_correction_T_max 0.8982 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _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_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.374402E-1 _diffrn_orient_matrix_ub_12 -0.10398 _diffrn_orient_matrix_ub_13 0.69655E-2 _diffrn_orient_matrix_ub_21 -0.578741E-1 _diffrn_orient_matrix_ub_22 -0.682565E-1 _diffrn_orient_matrix_ub_23 -0.215104E-1 _diffrn_orient_matrix_ub_31 -0.47191E-2 _diffrn_orient_matrix_ub_32 0.121314E-1 _diffrn_orient_matrix_ub_33 -0.613239E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_av_unetI/netI 0.0568 _diffrn_reflns_number 8301 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 23.06 _diffrn_reflns_theta_full 23.06 _diffrn_measured_fraction_theta_full 0.971 _diffrn_measured_fraction_theta_max 0.971 _reflns_number_total 2641 _reflns_number_gt 2145 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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 ; There is unresolved disorder between the two orientations of the O2..C9 > C12 ring related by 180 degree rotation i.e. interchangind O2 and C10. 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^)+(0.0344P)^2^+4.2210P] 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_number_reflns 2641 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.044 _refine_ls_wR_factor_ref 0.1065 _refine_ls_wR_factor_gt 0.0971 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.438 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.082 #----------------------------------------------------------------------------# # 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' 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' O O 0.0106 0.006 '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 0.63817(3) 0.43687(7) 0.54529(3) 0.0353(2) Uani 1 1 d . . . Cl1 Cl 0.69292(10) 0.1962(2) 0.49526(9) 0.0521(4) Uani 1 1 d . . . Cl2 Cl 0.52804(9) 0.64036(18) 0.57693(8) 0.0408(4) Uani 1 1 d . . . Cl3 Cl 0.66277(11) 0.6301(2) 0.45034(9) 0.0536(4) Uani 1 1 d . . . Si1 Si 0.73515(10) 0.4168(2) 0.75690(9) 0.0379(4) Uani 1 1 d . . . Si2 Si 0.82476(11) 0.6532(2) 0.67259(10) 0.0430(4) Uani 1 1 d . . . O1 O 0.5882(2) 0.2523(4) 0.6239(2) 0.0397(9) Uani 1 1 d . . . N1 N 0.7414(3) 0.4947(6) 0.6604(3) 0.0356(10) Uani 1 1 d . A . C1 C 0.5262(4) 0.1206(7) 0.6076(4) 0.0442(15) Uani 1 1 d . . . H1 H 0.4815 0.0901 0.5517 0.053 Uiso 1 1 calc R . . C2 C 0.5387(4) 0.0448(7) 0.6814(4) 0.0468(15) Uani 1 1 d . . . H2 H 0.5057 -0.0496 0.6884 0.056 Uiso 1 1 calc R . . C3 C 0.6114(4) 0.1313(8) 0.7493(4) 0.0509(16) Uani 1 1 d . . . H3 H 0.6347 0.1037 0.8096 0.061 Uiso 1 1 calc R . . C4 C 0.6409(4) 0.2543(7) 0.7156(3) 0.0372(13) Uani 1 1 d . . . C5 C 0.6995(4) 0.5828(8) 0.8146(4) 0.0531(16) Uani 1 1 d . . . H5A H 0.6453 0.6412 0.773 0.08 Uiso 1 1 calc R . . H5B H 0.7503 0.6626 0.8407 0.08 Uiso 1 1 calc R . . H5C H 0.6842 0.5325 0.8608 0.08 Uiso 1 1 calc R . . C6 C 0.8379(4) 0.2993(8) 0.8302(4) 0.0591(18) Uani 1 1 d . . . H6A H 0.8537 0.2134 0.7966 0.089 Uiso 1 1 calc R . . H6B H 0.8243 0.246 0.8767 0.089 Uiso 1 1 calc R . . H6C H 0.8901 0.3763 0.8561 0.089 Uiso 1 1 calc R . . C7 C 0.7672(4) 0.8596(8) 0.6564(4) 0.0574(17) Uani 1 1 d . A . H7A H 0.7177 0.8648 0.5978 0.086 Uiso 1 1 calc R . . H7B H 0.8125 0.9479 0.6628 0.086 Uiso 1 1 calc R . . H7C H 0.741 0.8752 0.7002 0.086 Uiso 1 1 calc R . . C8 C 0.8882(5) 0.6098(10) 0.6020(5) 0.069(2) Uani 1 1 d . A . H8A H 0.8445 0.6071 0.5407 0.104 Uiso 1 1 calc R . . H8B H 0.9196 0.5016 0.618 0.104 Uiso 1 1 calc R . . H8C H 0.934 0.6979 0.6101 0.104 Uiso 1 1 calc R . . O2 O 0.9098(3) 0.7376(8) 0.8531(3) 0.073(2) Uani 0.75(3) 1 d P A 1 C9 C 0.9168(4) 0.6552(9) 0.7849(4) 0.0579(18) Uani 0.75(3) 1 d P A 1 C10 C 0.9988(4) 0.5781(8) 0.8169(4) 0.067(2) Uani 0.75(3) 1 d P A 1 H10 H 1.022 0.5081 0.7843 0.081 Uiso 0.75(3) 1 calc PR A 1 C11 C 1.0448(5) 0.6156(11) 0.9046(5) 0.076(2) Uani 0.75(3) 1 d P A 1 H11 H 1.1042 0.5765 0.9423 0.091 Uiso 0.75(3) 1 calc PR A 1 C12 C 0.9904(5) 0.7165(11) 0.9261(5) 0.075(2) Uani 0.75(3) 1 d P A 1 H12 H 1.0046 0.7655 0.9818 0.09 Uiso 0.75(3) 1 calc PR A 1 C2A C 0.9098(3) 0.7376(8) 0.8531(3) 0.073(2) Uani 0.25(3) 1 d P A 2 H2A H 0.8576 0.7999 0.8508 0.087 Uiso 0.25(3) 1 calc PR A 2 C9A C 0.9168(4) 0.6552(9) 0.7849(4) 0.0579(18) Uani 0.25(3) 1 d P A 2 O10A O 0.9988(4) 0.5781(8) 0.8169(4) 0.067(2) Uani 0.25(3) 1 d P A 2 C11A C 1.0448(5) 0.6156(11) 0.9046(5) 0.076(2) Uani 0.25(3) 1 d P A 2 H11A H 1.1042 0.5765 0.9423 0.091 Uiso 0.25(3) 1 calc PR A 2 C12A C 0.9904(5) 0.7165(11) 0.9261(5) 0.075(2) Uani 0.25(3) 1 d P A 2 H12A H 1.0046 0.7655 0.9818 0.09 Uiso 0.25(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.0385(3) 0.0398(4) 0.0245(3) 0.0011(2) 0.0092(2) 0.0019(3) Cl1 0.0575(9) 0.0548(10) 0.0415(8) -0.0043(7) 0.0173(7) 0.0134(8) Cl2 0.0413(8) 0.0440(8) 0.0289(7) -0.0059(6) 0.0054(6) 0.0034(7) Cl3 0.0679(10) 0.0567(10) 0.0381(8) 0.0079(7) 0.0232(7) -0.0034(8) Si1 0.0394(8) 0.0448(10) 0.0254(7) -0.0001(7) 0.0084(6) -0.0028(7) Si2 0.0390(9) 0.0491(10) 0.0395(8) 0.0001(8) 0.0140(7) -0.0048(8) O1 0.045(2) 0.041(2) 0.0259(18) 0.0035(17) 0.0057(16) -0.0060(19) N1 0.035(2) 0.041(3) 0.030(2) 0.001(2) 0.0123(19) 0.003(2) C1 0.038(3) 0.040(3) 0.047(3) -0.004(3) 0.008(3) -0.003(3) C2 0.049(3) 0.036(3) 0.056(4) 0.008(3) 0.022(3) -0.001(3) C3 0.058(4) 0.060(4) 0.032(3) 0.008(3) 0.015(3) -0.006(3) C4 0.039(3) 0.041(3) 0.027(3) 0.005(3) 0.009(2) 0.000(3) C5 0.050(4) 0.072(5) 0.043(3) -0.011(3) 0.024(3) -0.013(3) C6 0.051(4) 0.063(4) 0.043(3) 0.012(3) -0.004(3) -0.009(3) C7 0.065(4) 0.045(4) 0.053(4) 0.007(3) 0.014(3) -0.007(3) C8 0.063(4) 0.088(5) 0.073(4) -0.010(4) 0.043(4) -0.019(4) O2 0.049(3) 0.108(5) 0.054(3) 0.001(3) 0.013(3) 0.000(3) C9 0.045(4) 0.064(4) 0.054(4) 0.005(4) 0.007(3) -0.015(3) C10 0.045(4) 0.073(5) 0.064(4) -0.005(3) 0.000(3) 0.005(3) C11 0.048(4) 0.096(6) 0.057(4) 0.008(4) -0.007(4) -0.005(4) C12 0.059(5) 0.102(6) 0.051(4) -0.003(4) 0.008(4) -0.007(5) C2A 0.049(3) 0.108(5) 0.054(3) 0.001(3) 0.013(3) 0.000(3) C9A 0.045(4) 0.064(4) 0.054(4) 0.005(4) 0.007(3) -0.015(3) O10A 0.045(4) 0.073(5) 0.064(4) -0.005(3) 0.000(3) 0.005(3) C11A 0.048(4) 0.096(6) 0.057(4) 0.008(4) -0.007(4) -0.005(4) C12A 0.059(5) 0.102(6) 0.051(4) -0.003(4) 0.008(4) -0.007(5) #----------------------------------------------------------------------------# # 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 N1 2.016(4) . ? Zr O1 2.311(3) . ? Zr Cl3 2.3529(16) . ? Zr Cl1 2.3925(15) . ? Zr Cl2 2.5838(15) . ? Zr Cl2 2.6759(13) 3_666 ? Cl2 Zr 2.6759(13) 3_666 ? Si1 N1 1.764(4) . ? Si1 C6 1.852(6) . ? Si1 C5 1.854(6) . ? Si1 C4 1.887(6) . ? Si2 N1 1.780(5) . ? Si2 C7 1.852(6) . ? Si2 C8 1.855(7) . ? Si2 C9 1.858(6) . ? O1 C1 1.390(6) . ? O1 C4 1.421(6) . ? C1 C2 1.315(8) . ? C1 H1 0.95 . ? C2 C3 1.429(8) . ? C2 H2 0.95 . ? C3 C4 1.307(8) . ? C3 H3 0.95 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? O2 C9 1.357(8) . ? O2 C12 1.378(8) . ? C9 C10 1.339(8) . ? C10 C11 1.382(9) . ? C10 H10 0.95 . ? C11 C12 1.327(11) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? 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 N1 Zr O1 86.27(15) . . ? N1 Zr Cl3 101.71(13) . . ? O1 Zr Cl3 170.47(10) . . ? N1 Zr Cl1 104.46(13) . . ? O1 Zr Cl1 86.28(10) . . ? Cl3 Zr Cl1 96.63(6) . . ? N1 Zr Cl2 90.86(13) . . ? O1 Zr Cl2 83.02(10) . . ? Cl3 Zr Cl2 91.57(5) . . ? Cl1 Zr Cl2 160.68(5) . . ? N1 Zr Cl2 162.55(13) . 3_666 ? O1 Zr Cl2 80.37(9) . 3_666 ? Cl3 Zr Cl2 90.75(5) . 3_666 ? Cl1 Zr Cl2 85.91(5) . 3_666 ? Cl2 Zr Cl2 76.49(5) . 3_666 ? Zr Cl2 Zr 103.51(5) . 3_666 ? N1 Si1 C6 115.4(3) . . ? N1 Si1 C5 111.0(3) . . ? C6 Si1 C5 112.8(3) . . ? N1 Si1 C4 103.4(2) . . ? C6 Si1 C4 104.3(3) . . ? C5 Si1 C4 109.0(3) . . ? N1 Si2 C7 108.8(3) . . ? N1 Si2 C8 110.8(3) . . ? C7 Si2 C8 115.5(3) . . ? N1 Si2 C9 111.5(2) . . ? C7 Si2 C9 106.3(3) . . ? C8 Si2 C9 103.8(3) . . ? C1 O1 C4 106.5(4) . . ? C1 O1 Zr 138.3(3) . . ? C4 O1 Zr 114.7(3) . . ? Si1 N1 Si2 117.0(2) . . ? Si1 N1 Zr 118.1(2) . . ? Si2 N1 Zr 123.6(2) . . ? C2 C1 O1 109.5(5) . . ? C2 C1 H1 125.2 . . ? O1 C1 H1 125.2 . . ? C1 C2 C3 107.0(5) . . ? C1 C2 H2 126.5 . . ? C3 C2 H2 126.5 . . ? C4 C3 C2 109.6(5) . . ? C4 C3 H3 125.2 . . ? C2 C3 H3 125.2 . . ? C3 C4 O1 107.3(5) . . ? C3 C4 Si1 136.5(4) . . ? O1 C4 Si1 116.1(4) . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 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 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C9 O2 C12 109.1(6) . . ? C10 C9 O2 106.1(5) . . ? C10 C9 Si2 130.0(6) . . ? O2 C9 Si2 123.9(5) . . ? C9 C10 C11 109.9(7) . . ? C9 C10 H10 125.1 . . ? C11 C10 H10 125.1 . . ? C12 C11 C10 107.1(6) . . ? C12 C11 H11 126.5 . . ? C10 C11 H11 126.5 . . ? C11 C12 O2 107.8(6) . . ? C11 C12 H12 126.1 . . ? O2 C12 H12 126.1 . . ? #===END data_(3b)-may1906 _database_code_depnum_ccdc_archive 'CCDC 630141' _audit_creation_date 2006-05-15T15:56:27-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H44 Cl6 N2 O4 Si4 Zr2, C7 H8' _chemical_formula_sum 'C35 H52 Cl6 N2 O4 Si4 Zr2' _chemical_formula_weight 1072.29 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7913(3) _cell_length_b 10.3992(4) _cell_length_c 14.8782(7) _cell_angle_alpha 102.020(2) _cell_angle_beta 97.133(3) _cell_angle_gamma 109.483(2) _cell_volume 1226.24(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10909 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 546 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.885 _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 0.7744 _exptl_absorpt_correction_T_max 0.8482 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _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_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.52561E-2 _diffrn_orient_matrix_ub_12 0.516823E-1 _diffrn_orient_matrix_ub_13 -0.49246E-1 _diffrn_orient_matrix_ub_21 0.12133 _diffrn_orient_matrix_ub_22 0.554613E-1 _diffrn_orient_matrix_ub_23 0.211062E-1 _diffrn_orient_matrix_ub_31 0.219404E-1 _diffrn_orient_matrix_ub_32 -0.738603E-1 _diffrn_orient_matrix_ub_33 -0.45492E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_unetI/netI 0.0496 _diffrn_reflns_number 14725 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 26 _diffrn_reflns_theta_full 26 _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.978 _reflns_number_total 4708 _reflns_number_gt 3836 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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 ; The toluene solvate molecule is disordered about an inversion centre and was refined with H atoms omitted. 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^)+(0.0258P)^2^+1.4432P] 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_number_reflns 4708 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0789 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.56 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.084 #----------------------------------------------------------------------------# # 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' 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' O O 0.0106 0.006 '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 0.15145(3) 0.14138(3) 0.12358(2) 0.01875(9) Uani 1 1 d . . . Cl1 Cl 0.27954(9) 0.07558(8) 0.24809(5) 0.02856(18) Uani 1 1 d . . . Cl2 Cl 0.37746(9) 0.19968(8) 0.04885(6) 0.03065(19) Uani 1 1 d . . . Cl3 Cl 0.05335(9) -0.12737(7) 0.02153(5) 0.02493(17) Uani 1 1 d . . . Si1 Si -0.01856(10) 0.35674(9) 0.20890(6) 0.02267(19) Uani 1 1 d . . . Si2 Si 0.34623(10) 0.49123(8) 0.20850(6) 0.02106(19) Uani 1 1 d . . . O1 O -0.0866(2) 0.0650(2) 0.18448(14) 0.0228(5) Uani 1 1 d . . . O2 O 0.3682(3) 0.6472(2) 0.38922(14) 0.0285(5) Uani 1 1 d . . . N N 0.1656(3) 0.3379(2) 0.18745(16) 0.0184(5) Uani 1 1 d . . . C1 C -0.1546(4) -0.1832(3) 0.1944(3) 0.0380(9) Uani 1 1 d . . . H1A H -0.2322 -0.2493 0.2209 0.057 Uiso 1 1 calc R . . H1B H -0.0433 -0.1501 0.2331 0.057 Uiso 1 1 calc R . . H1C H -0.1554 -0.2312 0.1302 0.057 Uiso 1 1 calc R . . C2 C -0.2045(4) -0.0602(3) 0.1931(2) 0.0270(7) Uani 1 1 d . . . C3 C -0.3422(4) -0.0367(3) 0.2024(2) 0.0329(8) Uani 1 1 d . . . H3 H -0.4418 -0.1035 0.209 0.04 Uiso 1 1 calc R . . C4 C -0.3147(4) 0.1057(3) 0.2010(2) 0.0335(8) Uani 1 1 d . . . H4 H -0.3938 0.1492 0.206 0.04 Uiso 1 1 calc R . . C5 C -0.1600(4) 0.1687(3) 0.1915(2) 0.0235(7) Uani 1 1 d . . . C6 C -0.1029(4) 0.4368(4) 0.1240(2) 0.0349(8) Uani 1 1 d . . . H6A H -0.1034 0.3883 0.06 0.052 Uiso 1 1 calc R . . H6B H -0.0338 0.5374 0.1377 0.052 Uiso 1 1 calc R . . H6C H -0.2158 0.427 0.1296 0.052 Uiso 1 1 calc R . . C7 C -0.0167(4) 0.4468(4) 0.3307(2) 0.0352(8) Uani 1 1 d . . . H7A H 0.028 0.4037 0.3748 0.053 Uiso 1 1 calc R . . H7B H -0.1295 0.437 0.3368 0.053 Uiso 1 1 calc R . . H7C H 0.0525 0.5475 0.345 0.053 Uiso 1 1 calc R . . C8 C 0.3660(4) 0.5468(4) 0.0981(2) 0.0354(8) Uani 1 1 d . . . H8A H 0.3755 0.4711 0.0502 0.053 Uiso 1 1 calc R . . H8B H 0.4647 0.6327 0.1103 0.053 Uiso 1 1 calc R . . H8C H 0.2682 0.566 0.0757 0.053 Uiso 1 1 calc R . . C9 C 0.5288(4) 0.4618(3) 0.2651(2) 0.0311(8) Uani 1 1 d . . . H9A H 0.5447 0.3835 0.223 0.047 Uiso 1 1 calc R . . H9B H 0.5104 0.4385 0.3244 0.047 Uiso 1 1 calc R . . H9C H 0.6274 0.548 0.2777 0.047 Uiso 1 1 calc R . . C10 C 0.3293(4) 0.6406(3) 0.2943(2) 0.0249(7) Uani 1 1 d . . . C11 C 0.2840(4) 0.7517(3) 0.2882(2) 0.0301(7) Uani 1 1 d . . . H11 H 0.2518 0.7741 0.2319 0.036 Uiso 1 1 calc R . . C12 C 0.2930(4) 0.8285(3) 0.3809(2) 0.0349(8) Uani 1 1 d . . . H12 H 0.268 0.9112 0.398 0.042 Uiso 1 1 calc R . . C13 C 0.3439(4) 0.7620(3) 0.4397(2) 0.0323(8) Uani 1 1 d . . . C14 C 0.3796(5) 0.7876(4) 0.5437(2) 0.0508(10) Uani 1 1 d . . . H14A H 0.3814 0.8817 0.5735 0.076 Uiso 1 1 calc R . . H14B H 0.4871 0.7823 0.5644 0.076 Uiso 1 1 calc R . . H14C H 0.2936 0.7156 0.5618 0.076 Uiso 1 1 calc R . . C1S C -0.0544(10) 0.0585(10) 0.4333(4) 0.107(3) Uani 1 1 d . . 1 C2S C -0.1586(11) -0.0683(10) 0.4385(4) 0.115(3) Uani 1 1 d . A 1 C3S C -0.1086(11) -0.1351(9) 0.5065(4) 0.111(3) Uani 1 1 d . . 1 C4S C -0.1964(14) -0.2567(13) 0.5098(8) 0.074(3) Uani 0.5 1 d P B 1 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 0.01550(15) 0.01704(15) 0.02190(16) 0.00390(11) 0.00252(11) 0.00504(11) Cl1 0.0269(4) 0.0293(4) 0.0305(4) 0.0103(3) 0.0007(3) 0.0121(3) Cl2 0.0232(4) 0.0347(4) 0.0325(4) 0.0066(4) 0.0112(3) 0.0084(3) Cl3 0.0276(4) 0.0197(4) 0.0256(4) 0.0033(3) -0.0013(3) 0.0105(3) Si1 0.0192(4) 0.0207(4) 0.0302(5) 0.0080(4) 0.0075(3) 0.0085(3) Si2 0.0178(4) 0.0176(4) 0.0256(5) 0.0058(3) 0.0042(3) 0.0039(3) O1 0.0168(10) 0.0198(11) 0.0320(12) 0.0079(9) 0.0094(9) 0.0050(9) O2 0.0322(12) 0.0253(11) 0.0249(12) 0.0036(9) 0.0009(9) 0.0103(10) N 0.0171(12) 0.0172(12) 0.0216(13) 0.0051(10) 0.0044(10) 0.0072(10) C1 0.040(2) 0.0252(18) 0.052(2) 0.0173(17) 0.0182(17) 0.0084(16) C2 0.0244(17) 0.0205(16) 0.0293(18) 0.0073(13) 0.0070(13) -0.0010(13) C3 0.0205(17) 0.0305(18) 0.042(2) 0.0092(16) 0.0103(14) 0.0009(14) C4 0.0179(17) 0.0330(19) 0.049(2) 0.0099(16) 0.0060(14) 0.0093(14) C5 0.0209(16) 0.0234(16) 0.0282(17) 0.0068(13) 0.0070(12) 0.0102(13) C6 0.0305(19) 0.0317(18) 0.047(2) 0.0129(16) 0.0053(15) 0.0164(15) C7 0.0323(19) 0.0323(19) 0.040(2) 0.0072(16) 0.0179(15) 0.0091(15) C8 0.039(2) 0.0305(19) 0.033(2) 0.0114(16) 0.0110(15) 0.0056(16) C9 0.0190(16) 0.0283(18) 0.041(2) 0.0064(15) 0.0005(14) 0.0060(14) C10 0.0233(16) 0.0215(16) 0.0262(17) 0.0064(13) 0.0047(13) 0.0038(13) C11 0.0390(19) 0.0230(16) 0.0304(18) 0.0097(14) 0.0110(15) 0.0110(15) C12 0.043(2) 0.0231(17) 0.041(2) 0.0074(15) 0.0141(16) 0.0130(15) C13 0.0307(18) 0.0256(17) 0.0329(19) -0.0013(15) 0.0071(14) 0.0059(15) C14 0.065(3) 0.055(3) 0.030(2) 0.0030(18) 0.0059(18) 0.026(2) C1S 0.142(7) 0.178(8) 0.039(3) 0.007(4) 0.014(4) 0.124(6) C2S 0.176(8) 0.179(8) 0.050(4) 0.023(5) 0.028(4) 0.142(7) C3S 0.175(8) 0.165(7) 0.047(3) 0.011(4) 0.037(4) 0.138(7) C4S 0.076(7) 0.072(7) 0.066(7) -0.005(6) 0.003(5) 0.035(6) #----------------------------------------------------------------------------# # 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 N 2.021(2) . ? Zr O1 2.3438(19) . ? Zr Cl2 2.3616(8) . ? Zr Cl1 2.3859(8) . ? Zr Cl3 2.5793(7) 2 ? Zr Cl3 2.6757(8) . ? Cl3 Zr 2.5793(7) 2 ? Si1 N 1.754(2) . ? Si1 C7 1.855(3) . ? Si1 C6 1.859(3) . ? Si1 C5 1.878(3) . ? Si2 N 1.773(2) . ? Si2 C10 1.855(3) . ? Si2 C8 1.860(3) . ? Si2 C9 1.865(3) . ? O1 C2 1.410(3) . ? O1 C5 1.422(3) . ? O2 C13 1.368(4) . ? O2 C10 1.393(3) . ? C1 C2 1.487(4) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 C3 1.330(4) . ? C3 C4 1.423(5) . ? C3 H3 0.95 . ? C4 C5 1.338(4) . ? C4 H4 0.95 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 C11 1.358(4) . ? C11 C12 1.421(5) . ? C11 H11 0.95 . ? C12 C13 1.345(5) . ? C12 H12 0.95 . ? C13 C14 1.488(5) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C1S C2S 1.356(10) . ? C1S C3S 1.454(10) 2_556 ? C2S C3S 1.443(9) . ? C3S C4S 1.258(12) . ? C3S C1S 1.454(10) 2_556 ? 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 N Zr O1 84.64(8) . . ? N Zr Cl2 99.82(7) . . ? O1 Zr Cl2 174.36(5) . . ? N Zr Cl1 102.59(7) . . ? O1 Zr Cl1 85.12(5) . . ? Cl2 Zr Cl1 97.19(3) . . ? N Zr Cl3 91.61(7) . 2 ? O1 Zr Cl3 83.72(5) . 2 ? Cl2 Zr Cl3 92.65(3) . 2 ? Cl1 Zr Cl3 161.02(3) . 2 ? N Zr Cl3 165.34(7) . . ? O1 Zr Cl3 85.91(5) . . ? Cl2 Zr Cl3 89.03(3) . . ? Cl1 Zr Cl3 87.72(3) . . ? Cl3 Zr Cl3 76.22(2) 2 . ? Zr Cl3 Zr 103.78(2) 2 . ? N Si1 C7 116.83(14) . . ? N Si1 C6 112.18(14) . . ? C7 Si1 C6 110.24(16) . . ? N Si1 C5 102.44(12) . . ? C7 Si1 C5 104.20(14) . . ? C6 Si1 C5 110.23(14) . . ? N Si2 C10 110.01(13) . . ? N Si2 C8 109.67(13) . . ? C10 Si2 C8 106.25(15) . . ? N Si2 C9 110.26(13) . . ? C10 Si2 C9 105.35(14) . . ? C8 Si2 C9 115.08(16) . . ? C2 O1 C5 107.6(2) . . ? C2 O1 Zr 140.56(18) . . ? C5 O1 Zr 108.98(16) . . ? C13 O2 C10 107.8(2) . . ? Si1 N Si2 119.27(13) . . ? Si1 N Zr 117.01(12) . . ? Si2 N Zr 123.23(13) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 108.0(3) . . ? C3 C2 C1 133.5(3) . . ? O1 C2 C1 118.4(3) . . ? C2 C3 C4 108.3(3) . . ? C2 C3 H3 125.8 . . ? C4 C3 H3 125.8 . . ? C5 C4 C3 109.3(3) . . ? C5 C4 H4 125.3 . . ? C3 C4 H4 125.3 . . ? C4 C5 O1 106.7(3) . . ? C4 C5 Si1 135.0(3) . . ? O1 C5 Si1 116.96(19) . . ? 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 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 O2 107.6(3) . . ? C11 C10 Si2 135.1(2) . . ? O2 C10 Si2 117.2(2) . . ? C10 C11 C12 107.9(3) . . ? C10 C11 H11 126 . . ? C12 C11 H11 126 . . ? C13 C12 C11 107.0(3) . . ? C13 C12 H12 126.5 . . ? C11 C12 H12 126.5 . . ? C12 C13 O2 109.6(3) . . ? C12 C13 C14 134.3(3) . . ? O2 C13 C14 116.0(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C2S C1S C3S 123.9(7) . 2_556 ? C1S C2S C3S 119.8(8) . . ? C4S C3S C2S 122.0(10) . . ? C4S C3S C1S 121.5(8) . 2_556 ? C2S C3S C1S 116.3(8) . 2_556 ? #===END data_(4b)-mar1005 _database_code_depnum_ccdc_archive 'CCDC 630142' _audit_creation_date 2005-03-10T17:22:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H44 Cl2 N2 O4 Si4 Ti, 0.5(C5 H12)' _chemical_formula_sum 'C30.5 H50 Cl2 N2 O4 Si4 Ti' _chemical_formula_weight 739.89 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4136(8) _cell_length_b 12.1506(8) _cell_length_c 15.1760(13) _cell_angle_alpha 89.866(4) _cell_angle_beta 69.510(4) _cell_angle_gamma 84.790(5) _cell_volume 1962.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 41265 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 782 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.51 _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 0.8718 _exptl_absorpt_correction_T_max 0.9765 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _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_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.663409E-1 _diffrn_orient_matrix_ub_12 -0.546773E-1 _diffrn_orient_matrix_ub_13 -0.42546E-1 _diffrn_orient_matrix_ub_21 0.68044E-2 _diffrn_orient_matrix_ub_22 -0.397545E-1 _diffrn_orient_matrix_ub_23 0.560343E-1 _diffrn_orient_matrix_ub_31 -0.661989E-1 _diffrn_orient_matrix_ub_32 -0.476073E-1 _diffrn_orient_matrix_ub_33 -0.17849E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0827 _diffrn_reflns_av_unetI/netI 0.0679 _diffrn_reflns_number 21736 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 23.01 _diffrn_reflns_theta_full 23.01 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 5439 _reflns_number_gt 3902 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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 ; Diffraction was weak and essentially unobservable at higher angle. The pentane solvate molecule is disordered across an inversion centre and was included with H atoms omitted. 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^)+(0.0274P)^2^+8.5313P] 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_number_reflns 5439 _refine_ls_number_parameters 401 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1134 _refine_ls_R_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.1741 _refine_ls_wR_factor_gt 0.1587 _refine_ls_goodness_of_fit_ref 1.203 _refine_ls_restrained_S_all 1.203 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.418 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.083 #----------------------------------------------------------------------------# # 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' 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' O O 0.0106 0.006 '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' Ti Ti 0.2776 0.4457 '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 Ti Ti 0.66857(11) 0.82148(10) 0.19810(9) 0.0363(3) Uani 1 1 d . . . Cl1 Cl 0.73661(17) 0.90097(15) 0.05609(13) 0.0486(5) Uani 1 1 d . . . Cl2 Cl 0.72049(17) 0.94155(16) 0.28824(14) 0.0510(5) Uani 1 1 d . . . Si1 Si 0.40621(18) 0.96999(16) 0.30178(15) 0.0420(5) Uani 1 1 d . . . Si2 Si 0.43679(18) 0.78535(16) 0.15475(14) 0.0373(5) Uani 1 1 d . . . Si3 Si 0.86987(17) 0.63245(15) 0.19053(14) 0.0351(5) Uani 1 1 d . . . Si4 Si 0.61991(18) 0.62547(16) 0.35043(14) 0.0389(5) Uani 1 1 d . . . O1 O 0.1616(4) 0.9093(4) 0.3842(3) 0.0426(12) Uani 1 1 d . . . O2 O 0.5460(4) 0.5652(4) 0.1251(3) 0.0450(12) Uani 1 1 d . . . O3 O 0.9629(5) 0.7243(4) 0.0106(3) 0.0511(14) Uani 1 1 d . . . O4 O 0.7544(4) 0.4265(4) 0.3782(3) 0.0439(12) Uani 1 1 d . . . N1 N 0.4946(5) 0.8523(4) 0.2332(4) 0.0359(14) Uani 1 1 d . . . N2 N 0.7105(5) 0.6826(4) 0.2430(4) 0.0352(13) Uani 1 1 d . . . C1 C 0.4063(7) 0.9658(7) 0.4233(5) 0.059(2) Uani 1 1 d . . . H1A H 0.4927 0.9653 0.4222 0.088 Uiso 1 1 calc R . . H1B H 0.3706 0.8988 0.4529 0.088 Uiso 1 1 calc R . . H1C H 0.3557 1.0311 0.4594 0.088 Uiso 1 1 calc R . . C2 C 0.4619(7) 1.0988(6) 0.2401(6) 0.061(2) Uani 1 1 d . . . H2A H 0.4594 1.0955 0.1763 0.092 Uiso 1 1 calc R . . H2B H 0.5483 1.1054 0.2367 0.092 Uiso 1 1 calc R . . H2C H 0.4073 1.1631 0.2749 0.092 Uiso 1 1 calc R . . C3 C 0.2377(7) 0.9708(6) 0.3136(5) 0.0425(18) Uani 1 1 d . . . C4 C 0.1654(7) 1.0213(6) 0.2688(5) 0.0470(19) Uani 1 1 d . . . H4 H 0.1927 1.0689 0.2173 0.056 Uiso 1 1 calc R . . C5 C 0.0421(7) 0.9910(6) 0.3118(6) 0.051(2) Uani 1 1 d . . . H5 H -0.0284 1.0148 0.2948 0.061 Uiso 1 1 calc R . . C6 C 0.0427(6) 0.9232(6) 0.3805(5) 0.0434(19) Uani 1 1 d . . . C7 C -0.0535(7) 0.8659(6) 0.4522(6) 0.054(2) Uani 1 1 d . . . H7A H -0.134 0.8796 0.4424 0.08 Uiso 1 1 calc R . . H7B H -0.0626 0.8937 0.515 0.08 Uiso 1 1 calc R . . H7C H -0.0279 0.7862 0.4467 0.08 Uiso 1 1 calc R . . C8 C 0.4175(7) 0.8828(6) 0.0650(5) 0.0463(19) Uani 1 1 d . . . H8A H 0.354 0.9437 0.0961 0.069 Uiso 1 1 calc R . . H8B H 0.3906 0.8437 0.0201 0.069 Uiso 1 1 calc R . . H8C H 0.4978 0.9124 0.0315 0.069 Uiso 1 1 calc R . . C9 C 0.2882(6) 0.7202(6) 0.2136(5) 0.0444(18) Uani 1 1 d . . . H9A H 0.2216 0.7772 0.2484 0.067 Uiso 1 1 calc R . . H9B H 0.3013 0.6652 0.2574 0.067 Uiso 1 1 calc R . . H9C H 0.2635 0.6841 0.166 0.067 Uiso 1 1 calc R . . C10 C 0.5587(6) 0.6719(6) 0.0902(5) 0.0403(17) Uani 1 1 d . . . C11 C 0.6462(7) 0.6621(6) 0.0016(5) 0.050(2) Uani 1 1 d . . . H11 H 0.6746 0.7208 -0.0396 0.06 Uiso 1 1 calc R . . C12 C 0.6870(8) 0.5483(7) -0.0177(6) 0.059(2) Uani 1 1 d . . . H12 H 0.7477 0.5169 -0.0745 0.071 Uiso 1 1 calc R . . C13 C 0.6257(7) 0.4933(6) 0.0573(6) 0.050(2) Uani 1 1 d . . . C14 C 0.6278(8) 0.3742(6) 0.0809(6) 0.067(3) Uani 1 1 d . . . H14A H 0.686 0.3301 0.0266 0.101 Uiso 1 1 calc R . . H14B H 0.5433 0.3505 0.0968 0.101 Uiso 1 1 calc R . . H14C H 0.6557 0.3637 0.1348 0.101 Uiso 1 1 calc R . . C15 C 0.8896(7) 0.4964(6) 0.1298(5) 0.0482(19) Uani 1 1 d . . . H15A H 0.8477 0.4424 0.1754 0.072 Uiso 1 1 calc R . . H15B H 0.9793 0.4717 0.1012 0.072 Uiso 1 1 calc R . . H15C H 0.8522 0.503 0.0807 0.072 Uiso 1 1 calc R . . C16 C 0.9503(6) 0.6275(7) 0.2775(5) 0.051(2) Uani 1 1 d . . . H16A H 0.9135 0.5744 0.3257 0.076 Uiso 1 1 calc R . . H16B H 0.9401 0.701 0.3072 0.076 Uiso 1 1 calc R . . H16C H 1.0399 0.6046 0.2456 0.076 Uiso 1 1 calc R . . C17 C 0.9489(6) 0.7349(6) 0.1053(5) 0.0421(18) Uani 1 1 d . . . C18 C 1.0130(7) 0.8215(6) 0.1153(6) 0.056(2) Uani 1 1 d . . . H18 H 1.0203 0.8465 0.1723 0.067 Uiso 1 1 calc R . . C19 C 1.0661(7) 0.8668(7) 0.0259(7) 0.065(3) Uani 1 1 d . . . H19 H 1.1159 0.9274 0.0112 0.077 Uiso 1 1 calc R . . C20 C 1.0327(8) 0.8079(7) -0.0339(6) 0.062(2) Uani 1 1 d . . . C21 C 1.0519(11) 0.8157(8) -0.1367(7) 0.107(4) Uani 1 1 d . . . H21A H 0.97 0.827 -0.1446 0.16 Uiso 1 1 calc R . . H21B H 1.0975 0.747 -0.17 0.16 Uiso 1 1 calc R . . H21C H 1.1006 0.878 -0.1626 0.16 Uiso 1 1 calc R . . C22 C 0.6512(7) 0.6899(6) 0.4486(5) 0.050(2) Uani 1 1 d . . . H22A H 0.6311 0.7701 0.4495 0.075 Uiso 1 1 calc R . . H22B H 0.7402 0.6736 0.4405 0.075 Uiso 1 1 calc R . . H22C H 0.5991 0.6603 0.5082 0.075 Uiso 1 1 calc R . . C23 C 0.4492(6) 0.6388(6) 0.3723(5) 0.0471(19) Uani 1 1 d . . . H23A H 0.4339 0.6044 0.3195 0.071 Uiso 1 1 calc R . . H23B H 0.4179 0.7173 0.3784 0.071 Uiso 1 1 calc R . . H23C H 0.4055 0.6019 0.4304 0.071 Uiso 1 1 calc R . . C24 C 0.6579(6) 0.4730(6) 0.3486(5) 0.0379(17) Uani 1 1 d . . . C25 C 0.6002(7) 0.3879(6) 0.3306(5) 0.0479(19) Uani 1 1 d . . . H25 H 0.5302 0.3947 0.3103 0.058 Uiso 1 1 calc R . . C26 C 0.6606(7) 0.2872(6) 0.3470(5) 0.052(2) Uani 1 1 d . . . H26 H 0.64 0.2148 0.3388 0.063 Uiso 1 1 calc R . . C27 C 0.7526(7) 0.3143(6) 0.3763(5) 0.0461(19) Uani 1 1 d . . . C28 C 0.8451(8) 0.2475(7) 0.4083(6) 0.069(3) Uani 1 1 d . . . H28A H 0.8297 0.1694 0.409 0.103 Uiso 1 1 calc R . . H28B H 0.8362 0.2728 0.4718 0.103 Uiso 1 1 calc R . . H28C H 0.9304 0.2563 0.3651 0.103 Uiso 1 1 calc R . . C1S C 1.0391(14) 0.4576(11) 0.4600(10) 0.133(7) Uani 1 1 d . . . C2S C 1.1701(16) 0.4715(17) 0.3860(16) 0.189(10) Uani 1 1 d . . . C3S C 1.234(2) 0.3968(19) 0.3120(19) 0.093(8) Uani 0.5 1 d P . . 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 Ti 0.0323(7) 0.0354(7) 0.0407(8) 0.0039(6) -0.0123(6) -0.0030(6) Cl1 0.0412(11) 0.0522(12) 0.0525(12) 0.0156(9) -0.0148(9) -0.0114(9) Cl2 0.0405(11) 0.0497(11) 0.0659(14) -0.0085(10) -0.0225(10) -0.0043(9) Si1 0.0358(11) 0.0395(12) 0.0527(14) -0.0070(10) -0.0189(10) 0.0007(9) Si2 0.0369(11) 0.0375(11) 0.0410(12) 0.0035(9) -0.0175(9) -0.0058(9) Si3 0.0314(11) 0.0352(11) 0.0373(12) 0.0031(9) -0.0104(9) -0.0022(8) Si4 0.0336(11) 0.0420(12) 0.0380(12) 0.0044(9) -0.0091(9) -0.0026(9) O1 0.036(3) 0.046(3) 0.046(3) -0.003(2) -0.016(2) 0.003(2) O2 0.047(3) 0.043(3) 0.045(3) -0.005(3) -0.017(3) -0.002(2) O3 0.061(3) 0.040(3) 0.038(3) 0.004(2) -0.002(3) 0.004(3) O4 0.045(3) 0.042(3) 0.044(3) 0.005(2) -0.016(2) 0.001(2) N1 0.033(3) 0.038(3) 0.040(4) 0.002(3) -0.016(3) -0.004(3) N2 0.027(3) 0.040(3) 0.035(3) 0.003(3) -0.008(3) 0.001(3) C1 0.047(5) 0.073(6) 0.057(5) -0.024(4) -0.022(4) 0.011(4) C2 0.053(5) 0.036(4) 0.094(7) -0.005(4) -0.025(5) -0.004(4) C3 0.039(4) 0.042(4) 0.048(5) -0.003(4) -0.018(4) -0.001(4) C4 0.044(5) 0.045(5) 0.054(5) 0.003(4) -0.021(4) 0.001(4) C5 0.039(5) 0.047(5) 0.072(6) 0.000(4) -0.028(4) 0.004(4) C6 0.035(4) 0.041(4) 0.055(5) -0.010(4) -0.020(4) 0.005(3) C7 0.048(5) 0.056(5) 0.061(6) -0.008(4) -0.022(4) -0.009(4) C8 0.049(5) 0.046(5) 0.050(5) 0.012(4) -0.025(4) -0.007(4) C9 0.044(4) 0.044(4) 0.052(5) 0.004(4) -0.024(4) -0.009(3) C10 0.041(4) 0.042(4) 0.039(5) 0.002(3) -0.016(4) -0.004(3) C11 0.051(5) 0.052(5) 0.045(5) 0.000(4) -0.015(4) 0.001(4) C12 0.060(5) 0.066(6) 0.045(5) -0.015(5) -0.014(4) 0.008(5) C13 0.049(5) 0.050(5) 0.054(6) -0.013(4) -0.025(4) -0.002(4) C14 0.076(6) 0.049(5) 0.082(7) -0.012(5) -0.039(5) 0.007(4) C15 0.037(4) 0.046(5) 0.054(5) 0.002(4) -0.005(4) -0.010(3) C16 0.034(4) 0.069(5) 0.051(5) 0.012(4) -0.017(4) -0.008(4) C17 0.041(4) 0.040(4) 0.043(5) 0.000(3) -0.012(4) -0.002(3) C18 0.045(5) 0.046(5) 0.075(6) 0.012(4) -0.019(5) -0.008(4) C19 0.041(5) 0.045(5) 0.095(8) 0.019(5) -0.007(5) -0.009(4) C20 0.057(5) 0.045(5) 0.058(6) 0.021(5) 0.010(5) 0.011(4) C21 0.131(10) 0.082(7) 0.058(7) 0.030(6) 0.017(6) 0.033(7) C22 0.047(5) 0.060(5) 0.038(5) 0.004(4) -0.009(4) -0.005(4) C23 0.038(4) 0.054(5) 0.045(5) 0.015(4) -0.010(4) -0.005(4) C24 0.037(4) 0.044(4) 0.032(4) 0.009(3) -0.011(3) -0.004(3) C25 0.046(5) 0.052(5) 0.046(5) 0.010(4) -0.016(4) -0.008(4) C26 0.058(5) 0.042(5) 0.052(5) -0.003(4) -0.012(4) -0.011(4) C27 0.050(5) 0.034(4) 0.041(5) 0.003(3) -0.002(4) 0.002(4) C28 0.067(6) 0.057(6) 0.072(6) 0.014(5) -0.017(5) 0.012(5) C1S 0.155(16) 0.129(14) 0.178(18) 0.096(11) -0.127(15) -0.063(11) C2S 0.127(13) 0.24(2) 0.29(2) 0.209(19) -0.155(16) -0.126(14) C3S 0.071(15) 0.074(15) 0.11(2) 0.002(13) -0.014(13) 0.013(12) #----------------------------------------------------------------------------# # 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 Ti N1 1.869(5) . ? Ti N2 1.903(5) . ? Ti Cl2 2.255(2) . ? Ti Cl1 2.266(2) . ? Si1 N1 1.776(6) . ? Si1 C1 1.846(8) . ? Si1 C3 1.867(7) . ? Si1 C2 1.868(8) . ? Si2 N1 1.780(5) . ? Si2 C8 1.860(7) . ? Si2 C9 1.866(7) . ? Si2 C10 1.871(7) . ? Si3 N2 1.761(5) . ? Si3 C17 1.848(7) . ? Si3 C16 1.851(7) . ? Si3 C15 1.852(7) . ? Si4 N2 1.775(6) . ? Si4 C22 1.842(7) . ? Si4 C23 1.850(7) . ? Si4 C24 1.862(7) . ? O1 C6 1.373(8) . ? O1 C3 1.386(8) . ? O2 C13 1.361(8) . ? O2 C10 1.400(8) . ? O3 C20 1.375(9) . ? O3 C17 1.393(8) . ? O4 C27 1.366(8) . ? O4 C24 1.402(8) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 C4 1.349(10) . ? C4 C5 1.411(10) . ? C4 H4 0.95 . ? C5 C6 1.329(10) . ? C5 H5 0.95 . ? C6 C7 1.474(10) . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 C11 1.364(10) . ? C11 C12 1.416(11) . ? C11 H11 0.95 . ? C12 C13 1.326(11) . ? C12 H12 0.95 . ? C13 C14 1.490(11) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 C18 1.373(10) . ? C18 C19 1.411(11) . ? C18 H18 0.95 . ? C19 C20 1.332(12) . ? C19 H19 0.95 . ? C20 C21 1.502(13) . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 C25 1.352(10) . ? C25 C26 1.413(10) . ? C25 H25 0.95 . ? C26 C27 1.342(10) . ? C26 H26 0.95 . ? C27 C28 1.486(11) . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C1S C2S 1.55(2) . ? C1S C1S 1.55(3) 2_766 ? C2S C3S 1.39(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 N1 Ti N2 111.2(2) . . ? N1 Ti Cl2 103.46(17) . . ? N2 Ti Cl2 102.18(18) . . ? N1 Ti Cl1 101.37(18) . . ? N2 Ti Cl1 133.56(17) . . ? Cl2 Ti Cl1 101.33(9) . . ? N1 Si1 C1 111.6(3) . . ? N1 Si1 C3 109.9(3) . . ? C1 Si1 C3 105.2(4) . . ? N1 Si1 C2 109.8(3) . . ? C1 Si1 C2 113.8(4) . . ? C3 Si1 C2 106.3(4) . . ? N1 Si2 C8 110.4(3) . . ? N1 Si2 C9 114.4(3) . . ? C8 Si2 C9 110.3(3) . . ? N1 Si2 C10 107.5(3) . . ? C8 Si2 C10 106.9(3) . . ? C9 Si2 C10 106.9(3) . . ? N2 Si3 C17 107.8(3) . . ? N2 Si3 C16 111.2(3) . . ? C17 Si3 C16 104.4(3) . . ? N2 Si3 C15 112.0(3) . . ? C17 Si3 C15 109.9(3) . . ? C16 Si3 C15 111.3(4) . . ? N2 Si4 C22 109.4(3) . . ? N2 Si4 C23 113.7(3) . . ? C22 Si4 C23 110.3(3) . . ? N2 Si4 C24 111.1(3) . . ? C22 Si4 C24 109.6(3) . . ? C23 Si4 C24 102.6(3) . . ? C6 O1 C3 107.7(6) . . ? C13 O2 C10 107.8(6) . . ? C20 O3 C17 106.1(6) . . ? C27 O4 C24 107.7(5) . . ? Si1 N1 Si2 119.8(3) . . ? Si1 N1 Ti 124.8(3) . . ? Si2 N1 Ti 111.1(3) . . ? Si3 N2 Si4 118.5(3) . . ? Si3 N2 Ti 113.8(3) . . ? Si4 N2 Ti 124.9(3) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 O1 107.5(6) . . ? C4 C3 Si1 134.6(6) . . ? O1 C3 Si1 117.9(5) . . ? C3 C4 C5 108.0(7) . . ? C3 C4 H4 126 . . ? C5 C4 H4 126 . . ? C6 C5 C4 107.5(7) . . ? C6 C5 H5 126.2 . . ? C4 C5 H5 126.2 . . ? C5 C6 O1 109.2(7) . . ? C5 C6 C7 134.8(7) . . ? O1 C6 C7 115.9(7) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 O2 107.1(6) . . ? C11 C10 Si2 133.0(6) . . ? O2 C10 Si2 118.0(5) . . ? C10 C11 C12 107.4(7) . . ? C10 C11 H11 126.3 . . ? C12 C11 H11 126.3 . . ? C13 C12 C11 107.9(7) . . ? C13 C12 H12 126 . . ? C11 C12 H12 126 . . ? C12 C13 O2 109.8(7) . . ? C12 C13 C14 133.7(8) . . ? O2 C13 C14 116.5(7) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si3 C15 H15A 109.5 . . ? Si3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si3 C16 H16A 109.5 . . ? Si3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 O3 108.1(7) . . ? C18 C17 Si3 130.7(6) . . ? O3 C17 Si3 120.8(5) . . ? C17 C18 C19 107.8(8) . . ? C17 C18 H18 126.1 . . ? C19 C18 H18 126.1 . . ? C20 C19 C18 106.6(8) . . ? C20 C19 H19 126.7 . . ? C18 C19 H19 126.7 . . ? C19 C20 O3 111.4(8) . . ? C19 C20 C21 133.9(9) . . ? O3 C20 C21 114.6(9) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si4 C22 H22A 109.5 . . ? Si4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si4 C23 H23A 109.5 . . ? Si4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 O4 106.7(6) . . ? C25 C24 Si4 131.7(6) . . ? O4 C24 Si4 121.4(5) . . ? C24 C25 C26 109.2(7) . . ? C24 C25 H25 125.4 . . ? C26 C25 H25 125.4 . . ? C27 C26 C25 106.3(7) . . ? C27 C26 H26 126.8 . . ? C25 C26 H26 126.8 . . ? C26 C27 O4 110.1(7) . . ? C26 C27 C28 132.8(7) . . ? O4 C27 C28 117.1(7) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C2S C1S C1S 126.0(18) . 2_766 ? C3S C2S C1S 124.5(19) . . ? #===END data_(5b)-dec1904 _database_code_depnum_ccdc_archive 'CCDC 630143' _audit_creation_date 2004-12-10T14:27:28-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H44 Cl2 N2 O4 Si4 Zr' _chemical_formula_sum 'C28 H44 Cl2 N2 O4 Si4 Zr' _chemical_formula_weight 747.13 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 20.2313(8) _cell_length_b 10.0263(4) _cell_length_c 19.8693(5) _cell_angle_alpha 90 _cell_angle_beta 115.341(2) _cell_angle_gamma 90 _cell_volume 3642.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20826 _cell_measurement_theta_min 0.783 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.613 _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 0.8187 _exptl_absorpt_correction_T_max 0.9485 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _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_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.60319E-2 _diffrn_orient_matrix_ub_12 0.899478E-1 _diffrn_orient_matrix_ub_13 0.232096E-1 _diffrn_orient_matrix_ub_21 0.406167E-1 _diffrn_orient_matrix_ub_22 0.213232E-1 _diffrn_orient_matrix_ub_23 -0.150482E-1 _diffrn_orient_matrix_ub_31 -0.376163E-1 _diffrn_orient_matrix_ub_32 0.374475E-1 _diffrn_orient_matrix_ub_33 -0.471802E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0716 _diffrn_reflns_av_unetI/netI 0.0667 _diffrn_reflns_number 32034 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 26.04 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 7173 _reflns_number_gt 4906 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _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^)+(0.0356P)^2^+3.8852P] 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_number_reflns 7173 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1027 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.486 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.078 #----------------------------------------------------------------------------# # 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' 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' O O 0.0106 0.006 '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 0.244862(17) 0.26008(3) 0.243317(16) 0.02466(10) Uani 1 1 d . . . Cl1 Cl 0.27148(5) 0.37966(9) 0.15077(5) 0.0358(2) Uani 1 1 d . . . Cl2 Cl 0.25338(5) 0.44994(10) 0.31959(5) 0.0401(2) Uani 1 1 d . . . Si1 Si 0.06670(6) 0.36036(12) 0.18593(6) 0.0402(3) Uani 1 1 d . . . Si2 Si 0.11867(5) 0.13183(11) 0.11706(5) 0.0324(3) Uani 1 1 d . . . Si3 Si 0.38353(5) 0.14020(10) 0.37216(5) 0.0266(2) Uani 1 1 d . . . Si4 Si 0.24579(5) 0.05371(11) 0.38193(5) 0.0346(3) Uani 1 1 d . . . O1 O -0.06526(14) 0.2194(3) 0.11697(15) 0.0515(8) Uani 1 1 d . . . O2 O 0.21838(14) -0.0717(3) 0.18886(13) 0.0399(6) Uani 1 1 d . . . O3 O 0.41803(13) 0.1789(2) 0.25103(12) 0.0348(6) Uani 1 1 d . . . O4 O 0.32318(13) -0.1900(3) 0.43216(13) 0.0377(6) Uani 1 1 d . . . N2 N 0.13420(14) 0.2475(3) 0.18806(14) 0.0279(6) Uani 1 1 d . . . N5 N 0.28927(14) 0.1249(3) 0.33072(14) 0.0249(6) Uani 1 1 d . . . C1 C 0.0568(2) 0.3531(5) 0.2741(2) 0.0606(14) Uani 1 1 d . . . H1A H 0.0461 0.2613 0.2832 0.091 Uiso 1 1 calc R . . H1B H 0.0166 0.4116 0.2707 0.091 Uiso 1 1 calc R . . H1C H 0.1023 0.3827 0.3153 0.091 Uiso 1 1 calc R . . C2 C 0.0863(2) 0.5316(4) 0.1640(3) 0.0619(13) Uani 1 1 d . . . H2A H 0.0911 0.5306 0.117 0.093 Uiso 1 1 calc R . . H2B H 0.132 0.5634 0.204 0.093 Uiso 1 1 calc R . . H2C H 0.0462 0.5911 0.1594 0.093 Uiso 1 1 calc R . . C3 C -0.0244(2) 0.3211(5) 0.1073(2) 0.0482(11) Uani 1 1 d . . . C4 C -0.0648(2) 0.3763(6) 0.0424(2) 0.0705(16) Uani 1 1 d . . . H4 H -0.05 0.45 0.0221 0.085 Uiso 1 1 calc R . . C5 C -0.1333(3) 0.3114(6) 0.0070(3) 0.0696(15) Uani 1 1 d . . . H5 H -0.1719 0.331 -0.0403 0.084 Uiso 1 1 calc R . . C6 C -0.1315(2) 0.2175(5) 0.0543(2) 0.0513(12) Uani 1 1 d . . . C7 C -0.1848(2) 0.1163(5) 0.0546(3) 0.0704(14) Uani 1 1 d . . . H7A H -0.2305 0.1254 0.0093 0.106 Uiso 1 1 calc R . . H7B H -0.1946 0.1297 0.0984 0.106 Uiso 1 1 calc R . . H7C H -0.1646 0.0268 0.0564 0.106 Uiso 1 1 calc R . . C8 C 0.0535(2) -0.0040(4) 0.1083(2) 0.0461(11) Uani 1 1 d . . . H8A H 0.0664 -0.0442 0.1573 0.069 Uiso 1 1 calc R . . H8B H 0.0557 -0.072 0.074 0.069 Uiso 1 1 calc R . . H8C H 0.0038 0.0325 0.0891 0.069 Uiso 1 1 calc R . . C9 C 0.0974(2) 0.2135(4) 0.02627(19) 0.0439(10) Uani 1 1 d . . . H9A H 0.133 0.2846 0.0332 0.066 Uiso 1 1 calc R . . H9B H 0.0481 0.2515 0.0065 0.066 Uiso 1 1 calc R . . H9C H 0.1 0.1474 -0.0089 0.066 Uiso 1 1 calc R . . C10 C 0.21123(19) 0.0477(4) 0.14958(18) 0.0319(8) Uani 1 1 d . . . C11 C 0.2690(2) 0.0519(4) 0.1310(2) 0.0374(9) Uani 1 1 d . . . H11 H 0.2783 0.1207 0.1033 0.045 Uiso 1 1 calc R . . C12 C 0.3120(2) -0.0620(4) 0.1596(2) 0.0475(11) Uani 1 1 d . . . H12 H 0.3559 -0.0836 0.1556 0.057 Uiso 1 1 calc R . . C13 C 0.2795(2) -0.1352(4) 0.1938(2) 0.0431(10) Uani 1 1 d . . . C14 C 0.2969(3) -0.2651(4) 0.2336(3) 0.0661(14) Uani 1 1 d . . . H14A H 0.2569 -0.3281 0.2079 0.099 Uiso 1 1 calc R . . H14B H 0.3029 -0.2522 0.2848 0.099 Uiso 1 1 calc R . . H14C H 0.3423 -0.3006 0.2344 0.099 Uiso 1 1 calc R . . C15 C 0.4189(2) 0.2337(4) 0.46138(18) 0.0390(9) Uani 1 1 d . . . H15A H 0.3911 0.3167 0.4546 0.059 Uiso 1 1 calc R . . H15B H 0.4707 0.2547 0.477 0.059 Uiso 1 1 calc R . . H15C H 0.4135 0.1791 0.4996 0.059 Uiso 1 1 calc R . . C16 C 0.43411(19) -0.0177(4) 0.3822(2) 0.0377(9) Uani 1 1 d . . . H16A H 0.4144 -0.0651 0.3344 0.056 Uiso 1 1 calc R . . H16B H 0.4287 -0.0735 0.42 0.056 Uiso 1 1 calc R . . H16C H 0.486 0.0017 0.3974 0.056 Uiso 1 1 calc R . . C17 C 0.40711(18) 0.2462(4) 0.30684(17) 0.0304(8) Uani 1 1 d . . . C18 C 0.4325(2) 0.3716(4) 0.3097(2) 0.0377(9) Uani 1 1 d . . . H18 H 0.4328 0.4397 0.343 0.045 Uiso 1 1 calc R . . C19 C 0.4588(2) 0.3844(4) 0.2542(2) 0.0415(10) Uani 1 1 d . . . H19 H 0.4796 0.4619 0.2435 0.05 Uiso 1 1 calc R . . C20 C 0.4487(2) 0.2664(4) 0.2199(2) 0.0386(9) Uani 1 1 d . . . C21 C 0.4602(3) 0.2144(5) 0.1558(2) 0.0557(12) Uani 1 1 d . . . H21A H 0.4814 0.2846 0.1368 0.084 Uiso 1 1 calc R . . H21B H 0.4133 0.1861 0.1164 0.084 Uiso 1 1 calc R . . H21C H 0.4937 0.1381 0.172 0.084 Uiso 1 1 calc R . . C22 C 0.1610(2) -0.0351(5) 0.3210(2) 0.0544(12) Uani 1 1 d . . . H22A H 0.1282 0.0264 0.283 0.082 Uiso 1 1 calc R . . H22B H 0.1367 -0.0687 0.351 0.082 Uiso 1 1 calc R . . H22C H 0.1731 -0.11 0.2967 0.082 Uiso 1 1 calc R . . C23 C 0.2271(2) 0.1841(5) 0.4386(2) 0.0582(13) Uani 1 1 d . . . H23A H 0.1948 0.2522 0.4055 0.087 Uiso 1 1 calc R . . H23B H 0.2733 0.2255 0.4725 0.087 Uiso 1 1 calc R . . H23C H 0.2036 0.143 0.4675 0.087 Uiso 1 1 calc R . . C24 C 0.30793(19) -0.0659(4) 0.45392(19) 0.0336(9) Uani 1 1 d . . . C25 C 0.3434(2) -0.0580(4) 0.52875(19) 0.0381(9) Uani 1 1 d . . . H25 H 0.3424 0.0154 0.5585 0.046 Uiso 1 1 calc R . . C26 C 0.3827(2) -0.1798(4) 0.5553(2) 0.0414(10) Uani 1 1 d . . . H26 H 0.413 -0.2019 0.6057 0.05 Uiso 1 1 calc R . . C27 C 0.3688(2) -0.2562(4) 0.4959(2) 0.0398(9) Uani 1 1 d . . . C28 C 0.3905(2) -0.3928(4) 0.4858(3) 0.0627(13) Uani 1 1 d . . . H28A H 0.4262 -0.4274 0.5338 0.094 Uiso 1 1 calc R . . H28B H 0.4125 -0.3911 0.4504 0.094 Uiso 1 1 calc R . . H28C H 0.3473 -0.4506 0.4665 0.094 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 0.02451(18) 0.0269(2) 0.02223(18) 0.00124(15) 0.00972(13) -0.00058(15) Cl1 0.0406(5) 0.0368(6) 0.0306(5) 0.0045(4) 0.0157(4) -0.0062(4) Cl2 0.0480(6) 0.0347(6) 0.0334(5) -0.0065(4) 0.0134(4) 0.0037(4) Si1 0.0282(6) 0.0505(8) 0.0386(6) -0.0022(5) 0.0113(5) 0.0078(5) Si2 0.0286(5) 0.0393(7) 0.0283(5) -0.0031(5) 0.0113(4) -0.0058(5) Si3 0.0268(5) 0.0275(6) 0.0256(5) 0.0026(4) 0.0112(4) 0.0005(4) Si4 0.0309(6) 0.0460(7) 0.0317(6) 0.0121(5) 0.0181(4) 0.0063(5) O1 0.0379(16) 0.062(2) 0.0517(17) 0.0005(15) 0.0163(13) 0.0111(15) O2 0.0456(16) 0.0317(17) 0.0453(16) -0.0014(12) 0.0222(13) -0.0048(13) O3 0.0423(15) 0.0336(16) 0.0339(14) 0.0023(11) 0.0213(12) -0.0038(12) O4 0.0388(15) 0.0329(16) 0.0366(15) 0.0021(12) 0.0116(12) -0.0031(12) N2 0.0271(15) 0.0312(18) 0.0251(15) -0.0001(13) 0.0108(11) -0.0008(13) N5 0.0265(15) 0.0260(17) 0.0235(15) 0.0032(12) 0.0119(12) 0.0036(13) C1 0.045(3) 0.091(4) 0.052(3) 0.000(3) 0.027(2) 0.017(3) C2 0.059(3) 0.049(3) 0.067(3) 0.005(2) 0.018(2) 0.013(2) C3 0.038(2) 0.061(3) 0.053(3) 0.006(2) 0.026(2) 0.003(2) C4 0.033(3) 0.123(5) 0.047(3) 0.008(3) 0.010(2) -0.006(3) C5 0.051(3) 0.109(5) 0.048(3) 0.008(3) 0.021(2) 0.005(3) C6 0.023(2) 0.074(4) 0.049(3) -0.019(2) 0.0088(18) 0.005(2) C7 0.051(3) 0.079(4) 0.079(4) -0.010(3) 0.026(3) -0.002(3) C8 0.040(2) 0.054(3) 0.044(2) -0.007(2) 0.0175(19) -0.015(2) C9 0.040(2) 0.058(3) 0.031(2) -0.0031(18) 0.0128(17) -0.008(2) C10 0.036(2) 0.031(2) 0.030(2) -0.0027(16) 0.0155(16) -0.0084(17) C11 0.042(2) 0.034(2) 0.040(2) -0.0037(18) 0.0219(18) -0.0044(19) C12 0.043(2) 0.042(3) 0.063(3) -0.011(2) 0.028(2) -0.002(2) C13 0.046(3) 0.027(2) 0.049(2) -0.0122(19) 0.0128(19) -0.0023(19) C14 0.078(3) 0.030(3) 0.080(3) -0.004(2) 0.024(3) 0.000(2) C15 0.040(2) 0.042(3) 0.029(2) 0.0028(17) 0.0093(16) -0.0003(19) C16 0.030(2) 0.037(2) 0.048(2) 0.0059(18) 0.0191(17) 0.0044(17) C17 0.0315(19) 0.035(2) 0.0253(18) 0.0010(17) 0.0122(14) -0.0017(17) C18 0.039(2) 0.035(3) 0.037(2) -0.0029(17) 0.0139(17) -0.0061(18) C19 0.040(2) 0.043(3) 0.044(2) 0.006(2) 0.0199(18) -0.0104(19) C20 0.038(2) 0.044(3) 0.036(2) 0.0079(19) 0.0182(17) -0.0066(19) C21 0.076(3) 0.058(3) 0.049(3) 0.009(2) 0.042(2) -0.002(2) C22 0.036(2) 0.078(4) 0.049(3) 0.024(2) 0.0185(19) -0.010(2) C23 0.069(3) 0.074(3) 0.051(3) 0.023(2) 0.044(2) 0.032(3) C24 0.035(2) 0.036(2) 0.037(2) 0.0035(17) 0.0225(17) -0.0025(17) C25 0.043(2) 0.040(3) 0.033(2) 0.0085(18) 0.0191(18) 0.0021(19) C26 0.039(2) 0.039(3) 0.036(2) 0.0097(19) 0.0060(17) -0.0077(19) C27 0.034(2) 0.033(2) 0.046(2) 0.008(2) 0.0103(17) -0.0006(19) C28 0.055(3) 0.035(3) 0.071(3) -0.002(2) 0.001(2) -0.001(2) #----------------------------------------------------------------------------# # 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 N2 2.032(3) . ? Zr N5 2.079(3) . ? Zr Cl2 2.3930(10) . ? Zr Cl1 2.4406(9) . ? Si1 N2 1.760(3) . ? Si1 C1 1.849(4) . ? Si1 C2 1.855(5) . ? Si1 C3 1.878(4) . ? Si2 N2 1.748(3) . ? Si2 C8 1.852(4) . ? Si2 C9 1.856(4) . ? Si2 C10 1.897(4) . ? Si3 N5 1.730(3) . ? Si3 C16 1.849(4) . ? Si3 C15 1.857(4) . ? Si3 C17 1.890(3) . ? Si4 N5 1.757(3) . ? Si4 C22 1.850(4) . ? Si4 C23 1.866(4) . ? Si4 C24 1.878(4) . ? O1 C3 1.378(5) . ? O1 C6 1.385(4) . ? O2 C13 1.357(4) . ? O2 C10 1.402(4) . ? O3 C20 1.366(4) . ? O3 C17 1.394(4) . ? O4 C27 1.377(4) . ? O4 C24 1.394(4) . ? C3 C4 1.316(6) . ? C4 C5 1.416(6) . ? C5 C6 1.321(6) . ? C6 C7 1.482(6) . ? C10 C11 1.368(5) . ? C11 C12 1.401(5) . ? C12 C13 1.347(6) . ? C13 C14 1.485(6) . ? C17 C18 1.351(5) . ? C18 C19 1.420(5) . ? C19 C20 1.335(5) . ? C20 C21 1.484(5) . ? C24 C25 1.349(5) . ? C25 C26 1.429(5) . ? C26 C27 1.332(5) . ? C27 C28 1.478(6) . ? 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 N5 113.14(11) . . ? N2 Zr Cl2 98.95(8) . . ? N5 Zr Cl2 95.81(8) . . ? N2 Zr Cl1 99.83(8) . . ? N5 Zr Cl1 142.52(7) . . ? Cl2 Zr Cl1 96.15(3) . . ? N2 Si1 C1 110.49(17) . . ? N2 Si1 C2 111.04(18) . . ? C1 Si1 C2 112.3(2) . . ? N2 Si1 C3 111.08(17) . . ? C1 Si1 C3 108.35(19) . . ? C2 Si1 C3 103.3(2) . . ? N2 Si2 C8 115.98(16) . . ? N2 Si2 C9 112.26(17) . . ? C8 Si2 C9 111.96(17) . . ? N2 Si2 C10 102.12(14) . . ? C8 Si2 C10 105.35(18) . . ? C9 Si2 C10 108.15(17) . . ? N5 Si3 C16 114.95(16) . . ? N5 Si3 C15 113.24(15) . . ? C16 Si3 C15 111.11(17) . . ? N5 Si3 C17 105.88(14) . . ? C16 Si3 C17 105.36(16) . . ? C15 Si3 C17 105.34(17) . . ? N5 Si4 C22 111.74(15) . . ? N5 Si4 C23 110.19(17) . . ? C22 Si4 C23 111.2(2) . . ? N5 Si4 C24 111.28(14) . . ? C22 Si4 C24 108.80(18) . . ? C23 Si4 C24 103.31(17) . . ? C3 O1 C6 107.0(3) . . ? C13 O2 C10 108.3(3) . . ? C20 O3 C17 107.9(3) . . ? C27 O4 C24 107.2(3) . . ? Si2 N2 Si1 122.53(15) . . ? Si2 N2 Zr 104.66(13) . . ? Si1 N2 Zr 129.58(16) . . ? Si3 N5 Si4 118.91(14) . . ? Si3 N5 Zr 109.51(13) . . ? Si4 N5 Zr 127.18(14) . . ? C4 C3 O1 106.8(4) . . ? C4 C3 Si1 134.7(4) . . ? O1 C3 Si1 118.2(3) . . ? C3 C4 C5 111.1(5) . . ? C6 C5 C4 104.5(4) . . ? C5 C6 O1 110.6(4) . . ? C5 C6 C7 133.8(4) . . ? O1 C6 C7 115.6(4) . . ? C11 C10 O2 106.3(3) . . ? C11 C10 Si2 136.6(3) . . ? O2 C10 Si2 114.9(2) . . ? C10 C11 C12 108.6(4) . . ? C13 C12 C11 107.3(4) . . ? C12 C13 O2 109.5(4) . . ? C12 C13 C14 133.7(4) . . ? O2 C13 C14 116.7(4) . . ? C18 C17 O3 107.2(3) . . ? C18 C17 Si3 134.3(3) . . ? O3 C17 Si3 116.6(3) . . ? C17 C18 C19 108.3(3) . . ? C20 C19 C18 106.8(3) . . ? C19 C20 O3 109.8(3) . . ? C19 C20 C21 134.6(4) . . ? O3 C20 C21 115.5(4) . . ? C25 C24 O4 108.1(3) . . ? C25 C24 Si4 132.0(3) . . ? O4 C24 Si4 119.9(2) . . ? C24 C25 C26 107.8(4) . . ? C27 C26 C25 107.0(3) . . ? C26 C27 O4 109.9(4) . . ? C26 C27 C28 133.7(4) . . ? O4 C27 C28 116.3(3) . . ? #===END data_(6b)-nov2005 _database_code_depnum_ccdc_archive 'CCDC 630144' _audit_creation_date 2005-11-23T15:48:16-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H44 Cl N2 O4 Si4 Ti' _chemical_formula_sum 'C28 H44 Cl N2 O4 Si4 Ti' _chemical_formula_weight 668.36 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 13.5158(8) _cell_length_b 14.9602(8) _cell_length_c 17.5348(7) _cell_angle_alpha 90 _cell_angle_beta 99.427(3) _cell_angle_gamma 90 _cell_volume 3497.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 87673 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _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 0.15 _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.491 _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 0.7549 _exptl_absorpt_correction_T_max 0.9512 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _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_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.277707E-1 _diffrn_orient_matrix_ub_12 0.62087E-1 _diffrn_orient_matrix_ub_13 -0.42364E-2 _diffrn_orient_matrix_ub_21 0.571044E-1 _diffrn_orient_matrix_ub_22 0.197569E-1 _diffrn_orient_matrix_ub_23 -0.256965E-1 _diffrn_orient_matrix_ub_31 -0.399116E-1 _diffrn_orient_matrix_ub_32 -0.149329E-1 _diffrn_orient_matrix_ub_33 -0.516116E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0707 _diffrn_reflns_av_unetI/netI 0.049 _diffrn_reflns_number 39196 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 26.12 _diffrn_reflns_theta_full 26.12 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _reflns_number_total 6799 _reflns_number_gt 5012 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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^)+(0.0401P)^2^+3.1677P] 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_number_reflns 6799 _refine_ls_number_parameters 365 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.312 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.06 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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' Ti Ti 0.2776 0.4457 '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' 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 Ti Ti 0.25921(4) 0.30148(3) 0.02786(2) 0.02451(13) Uani 1 1 d . . . Cl Cl 0.25839(6) 0.45698(5) 0.02006(4) 0.04090(19) Uani 1 1 d . . . Si1 Si 0.09567(6) 0.27144(5) 0.12980(4) 0.03159(19) Uani 1 1 d . . . Si2 Si 0.27129(6) 0.14917(5) 0.16972(4) 0.03190(19) Uani 1 1 d . . . Si3 Si 0.42074(6) 0.24980(5) -0.06805(4) 0.03048(19) Uani 1 1 d . . . Si4 Si 0.24682(6) 0.12283(5) -0.09030(4) 0.03133(19) Uani 1 1 d . . . O1 O 0.10224(13) 0.31550(12) -0.02342(9) 0.0278(4) Uani 1 1 d . . . O2 O 0.31287(14) 0.24190(12) 0.31124(10) 0.0342(5) Uani 1 1 d . . . O3 O 0.41873(13) 0.31985(12) 0.07888(10) 0.0289(4) Uani 1 1 d . . . O4 O 0.21692(15) 0.19679(13) -0.23908(10) 0.0384(5) Uani 1 1 d . . . N1 N 0.21236(16) 0.23548(14) 0.11420(11) 0.0276(5) Uani 1 1 d . . . N2 N 0.30491(16) 0.21744(14) -0.04751(11) 0.0267(5) Uani 1 1 d . . . C1 C 0.1061(3) 0.3631(2) -0.15669(16) 0.0480(8) Uani 1 1 d . . . H1A H 0.0684 0.4006 -0.1972 0.072 Uiso 1 1 calc R . . H1B H 0.1084 0.3016 -0.1756 0.072 Uiso 1 1 calc R . . H1C H 0.1745 0.3862 -0.143 0.072 Uiso 1 1 calc R . . C2 C 0.0561(2) 0.36450(18) -0.08759(15) 0.0319(6) Uani 1 1 d . . . C3 C -0.0251(2) 0.40427(19) -0.07026(17) 0.0376(7) Uani 1 1 d . . . H3 H -0.0706 0.4404 -0.104 0.045 Uiso 1 1 calc R . . C4 C -0.0318(2) 0.38313(19) 0.00797(17) 0.0373(7) Uani 1 1 d . . . H4 H -0.0825 0.4037 0.0353 0.045 Uiso 1 1 calc R . . C5 C 0.0447(2) 0.32979(18) 0.03674(15) 0.0289(6) Uani 1 1 d . . . C6 C 0.0044(2) 0.1820(2) 0.14370(17) 0.0468(8) Uani 1 1 d . . . H6A H 0.0281 0.1501 0.1921 0.07 Uiso 1 1 calc R . . H6B H -0.0017 0.1399 0.1003 0.07 Uiso 1 1 calc R . . H6C H -0.0611 0.2088 0.146 0.07 Uiso 1 1 calc R . . C7 C 0.0994(3) 0.3548(2) 0.20908(17) 0.0491(8) Uani 1 1 d . . . H7A H 0.1253 0.3263 0.2587 0.074 Uiso 1 1 calc R . . H7B H 0.0316 0.3774 0.2101 0.074 Uiso 1 1 calc R . . H7C H 0.1433 0.4046 0.2002 0.074 Uiso 1 1 calc R . . C8 C 0.2077(3) 0.03937(19) 0.14690(17) 0.0463(8) Uani 1 1 d . . . H8A H 0.2083 0.0244 0.0926 0.069 Uiso 1 1 calc R . . H8B H 0.1383 0.0432 0.1561 0.069 Uiso 1 1 calc R . . H8C H 0.2433 -0.0071 0.1801 0.069 Uiso 1 1 calc R . . C9 C 0.4048(2) 0.1342(2) 0.15831(17) 0.0412(7) Uani 1 1 d . . . H9A H 0.4088 0.1243 0.1037 0.062 Uiso 1 1 calc R . . H9B H 0.433 0.0826 0.1887 0.062 Uiso 1 1 calc R . . H9C H 0.4429 0.188 0.1765 0.062 Uiso 1 1 calc R . . C10 C 0.2634(2) 0.16817(18) 0.27370(15) 0.0332(7) Uani 1 1 d . . . C11 C 0.2130(2) 0.12676(19) 0.32486(16) 0.0374(7) Uani 1 1 d . . . H11 H 0.1732 0.0743 0.3153 0.045 Uiso 1 1 calc R . . C12 C 0.2304(2) 0.1759(2) 0.39505(16) 0.0373(7) Uani 1 1 d . . . H12 H 0.2042 0.1626 0.4408 0.045 Uiso 1 1 calc R . . C13 C 0.2903(2) 0.24429(19) 0.38487(15) 0.0336(7) Uani 1 1 d . . . C14 C 0.3391(3) 0.3163(2) 0.43549(16) 0.0444(8) Uani 1 1 d . . . H14A H 0.3035 0.3244 0.4794 0.067 Uiso 1 1 calc R . . H14B H 0.337 0.3722 0.406 0.067 Uiso 1 1 calc R . . H14C H 0.409 0.3001 0.4545 0.067 Uiso 1 1 calc R . . C15 C 0.4229(3) 0.3858(2) 0.20766(16) 0.0453(8) Uani 1 1 d . . . H15A H 0.4551 0.4348 0.2395 0.068 Uiso 1 1 calc R . . H15B H 0.4375 0.329 0.2351 0.068 Uiso 1 1 calc R . . H15C H 0.3502 0.3954 0.1974 0.068 Uiso 1 1 calc R . . C16 C 0.4618(2) 0.38289(18) 0.13379(15) 0.0326(6) Uani 1 1 d . . . C17 C 0.5326(2) 0.42799(19) 0.10446(16) 0.0372(7) Uani 1 1 d . . . H17 H 0.5741 0.4738 0.13 0.045 Uiso 1 1 calc R . . C18 C 0.5347(2) 0.39545(19) 0.02849(17) 0.0360(7) Uani 1 1 d . . . H18 H 0.5773 0.4168 -0.0055 0.043 Uiso 1 1 calc R . . C19 C 0.4666(2) 0.32952(18) 0.01265(15) 0.0306(6) Uani 1 1 d . . . C20 C 0.5146(2) 0.1576(2) -0.06573(19) 0.0465(8) Uani 1 1 d . . . H20A H 0.4923 0.1156 -0.1079 0.07 Uiso 1 1 calc R . . H20B H 0.521 0.1263 -0.0161 0.07 Uiso 1 1 calc R . . H20C H 0.5798 0.1828 -0.072 0.07 Uiso 1 1 calc R . . C21 C 0.4175(2) 0.3131(2) -0.15978(16) 0.0452(8) Uani 1 1 d . . . H21A H 0.3939 0.2738 -0.2037 0.068 Uiso 1 1 calc R . . H21B H 0.4851 0.3346 -0.1634 0.068 Uiso 1 1 calc R . . H21C H 0.3719 0.3641 -0.1605 0.068 Uiso 1 1 calc R . . C22 C 0.3091(3) 0.0164(2) -0.05299(18) 0.0491(8) Uani 1 1 d . . . H22A H 0.3074 0.0112 0.0025 0.074 Uiso 1 1 calc R . . H22B H 0.3789 0.0165 -0.0617 0.074 Uiso 1 1 calc R . . H22C H 0.2735 -0.0344 -0.0802 0.074 Uiso 1 1 calc R . . C23 C 0.1120(2) 0.1159(2) -0.08050(17) 0.0410(7) Uani 1 1 d . . . H23A H 0.1059 0.1149 -0.0256 0.062 Uiso 1 1 calc R . . H23B H 0.0829 0.0612 -0.1055 0.062 Uiso 1 1 calc R . . H23C H 0.0763 0.168 -0.1053 0.062 Uiso 1 1 calc R . . C24 C 0.2565(2) 0.12340(19) -0.19563(15) 0.0346(7) Uani 1 1 d . . . C25 C 0.2993(2) 0.0695(2) -0.24265(17) 0.0472(8) Uani 1 1 d . . . H25 H 0.3316 0.0141 -0.2285 0.057 Uiso 1 1 calc R . . C26 C 0.2878(3) 0.1099(2) -0.31702(18) 0.0520(9) Uani 1 1 d . . . H26 H 0.3108 0.0868 -0.3615 0.062 Uiso 1 1 calc R . . C27 C 0.2383(2) 0.1867(2) -0.31241(16) 0.0443(8) Uani 1 1 d . . . C28 C 0.2025(3) 0.2598(3) -0.36707(18) 0.0609(10) Uani 1 1 d . . . H28A H 0.2191 0.2457 -0.4181 0.091 Uiso 1 1 calc R . . H28B H 0.2351 0.3159 -0.3483 0.091 Uiso 1 1 calc R . . H28C H 0.1297 0.266 -0.371 0.091 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 Ti 0.0285(3) 0.0228(3) 0.0219(2) 0.00028(18) 0.00329(19) 0.0005(2) Cl 0.0372(4) 0.0243(4) 0.0601(5) 0.0010(3) 0.0049(3) 0.0001(3) Si1 0.0322(5) 0.0398(5) 0.0233(4) -0.0008(3) 0.0063(3) -0.0016(3) Si2 0.0430(5) 0.0291(4) 0.0226(4) 0.0034(3) 0.0024(3) -0.0005(3) Si3 0.0320(5) 0.0335(4) 0.0270(4) -0.0014(3) 0.0080(3) 0.0012(3) Si4 0.0414(5) 0.0271(4) 0.0258(4) -0.0035(3) 0.0067(3) -0.0010(3) O1 0.0290(10) 0.0325(10) 0.0213(9) 0.0012(7) 0.0022(7) 0.0036(8) O2 0.0449(13) 0.0333(11) 0.0236(10) 0.0043(8) 0.0038(8) -0.0045(9) O3 0.0304(11) 0.0302(10) 0.0253(9) -0.0019(7) 0.0019(8) -0.0022(8) O4 0.0489(13) 0.0407(12) 0.0258(10) -0.0030(8) 0.0065(9) -0.0025(10) N1 0.0321(13) 0.0298(12) 0.0203(11) -0.0013(9) 0.0025(9) -0.0014(10) N2 0.0307(13) 0.0267(12) 0.0231(11) 0.0002(9) 0.0054(9) 0.0013(10) C1 0.060(2) 0.054(2) 0.0283(16) 0.0100(14) 0.0020(14) 0.0089(17) C2 0.0353(17) 0.0306(15) 0.0266(14) 0.0040(11) -0.0039(12) -0.0011(13) C3 0.0320(18) 0.0335(16) 0.0435(18) 0.0061(13) -0.0051(13) 0.0013(13) C4 0.0276(17) 0.0393(17) 0.0455(18) -0.0008(13) 0.0080(13) 0.0036(13) C5 0.0288(16) 0.0299(15) 0.0287(14) -0.0048(11) 0.0064(11) -0.0019(12) C6 0.041(2) 0.061(2) 0.0393(18) 0.0134(15) 0.0090(14) -0.0088(16) C7 0.047(2) 0.066(2) 0.0343(17) -0.0111(15) 0.0070(14) 0.0094(17) C8 0.070(2) 0.0322(17) 0.0351(17) 0.0034(13) 0.0053(15) -0.0051(16) C9 0.050(2) 0.0390(17) 0.0335(16) 0.0071(13) 0.0031(14) 0.0112(15) C10 0.0436(18) 0.0273(15) 0.0261(14) 0.0038(11) -0.0018(12) -0.0003(12) C11 0.0428(19) 0.0354(16) 0.0332(16) 0.0041(12) 0.0042(13) -0.0066(14) C12 0.0417(19) 0.0427(18) 0.0288(15) 0.0038(12) 0.0094(13) -0.0002(14) C13 0.0402(18) 0.0360(17) 0.0238(14) 0.0036(11) 0.0027(12) 0.0068(13) C14 0.063(2) 0.0360(17) 0.0324(16) 0.0001(13) 0.0037(14) 0.0010(15) C15 0.059(2) 0.0432(18) 0.0322(16) -0.0083(13) 0.0043(14) -0.0061(16) C16 0.0332(17) 0.0305(15) 0.0309(15) -0.0030(11) -0.0044(12) -0.0002(13) C17 0.0328(17) 0.0295(16) 0.0463(18) -0.0060(13) -0.0026(13) -0.0023(13) C18 0.0289(17) 0.0350(17) 0.0450(18) 0.0016(13) 0.0084(13) -0.0025(13) C19 0.0293(16) 0.0352(16) 0.0278(14) 0.0046(11) 0.0063(12) 0.0042(12) C20 0.0360(19) 0.0468(19) 0.058(2) -0.0110(15) 0.0102(15) 0.0061(15) C21 0.048(2) 0.054(2) 0.0346(17) 0.0028(14) 0.0113(14) -0.0137(16) C22 0.069(2) 0.0320(17) 0.0467(19) -0.0002(14) 0.0096(16) 0.0031(16) C23 0.048(2) 0.0397(17) 0.0361(16) -0.0081(13) 0.0099(14) -0.0116(15) C24 0.0396(18) 0.0340(16) 0.0303(15) -0.0072(12) 0.0062(12) -0.0026(13) C25 0.054(2) 0.049(2) 0.0399(18) -0.0100(15) 0.0101(15) 0.0061(16) C26 0.050(2) 0.077(3) 0.0325(18) -0.0139(16) 0.0160(15) -0.0043(19) C27 0.044(2) 0.064(2) 0.0246(15) -0.0044(14) 0.0049(13) -0.0164(17) C28 0.072(3) 0.078(3) 0.0316(18) 0.0068(17) 0.0034(16) -0.018(2) #----------------------------------------------------------------------------# # 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 Ti N2 1.994(2) . ? Ti N1 1.995(2) . ? Ti O1 2.1746(18) . ? Ti O3 2.2119(18) . ? Ti Cl 2.3304(8) . ? Si1 N1 1.730(2) . ? Si1 C7 1.862(3) . ? Si1 C6 1.863(3) . ? Si1 C5 1.879(3) . ? Si2 N1 1.731(2) . ? Si2 C9 1.861(3) . ? Si2 C10 1.865(3) . ? Si2 C8 1.866(3) . ? Si3 N2 1.732(2) . ? Si3 C21 1.861(3) . ? Si3 C20 1.870(3) . ? Si3 C19 1.876(3) . ? Si4 N2 1.729(2) . ? Si4 C23 1.861(3) . ? Si4 C22 1.869(3) . ? Si4 C24 1.873(3) . ? O1 C2 1.401(3) . ? O1 C5 1.426(3) . ? O2 C13 1.375(3) . ? O2 C10 1.397(3) . ? O3 C16 1.404(3) . ? O3 C19 1.426(3) . ? O4 C27 1.372(3) . ? O4 C24 1.392(3) . ? C1 C2 1.480(4) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 C3 1.327(4) . ? C3 C4 1.425(4) . ? C3 H3 0.95 . ? C4 C5 1.337(4) . ? C4 H4 0.95 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 C11 1.361(4) . ? C11 C12 1.420(4) . ? C11 H11 0.95 . ? C12 C13 1.334(4) . ? C12 H12 0.95 . ? C13 C14 1.481(4) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C16 1.476(4) . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 C17 1.340(4) . ? C17 C18 1.423(4) . ? C17 H17 0.95 . ? C18 C19 1.347(4) . ? C18 H18 0.95 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 C25 1.350(4) . ? C25 C26 1.423(4) . ? C25 H25 0.95 . ? C26 C27 1.339(5) . ? C26 H26 0.95 . ? C27 C28 1.481(5) . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? 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 Ti N1 111.23(9) . . ? N2 Ti O1 100.02(8) . . ? N1 Ti O1 87.26(8) . . ? N2 Ti O3 87.66(8) . . ? N1 Ti O3 99.44(8) . . ? O1 Ti O3 167.32(7) . . ? N2 Ti Cl 126.12(7) . . ? N1 Ti Cl 122.65(7) . . ? O1 Ti Cl 83.37(5) . . ? O3 Ti Cl 83.95(5) . . ? N1 Si1 C7 114.35(13) . . ? N1 Si1 C6 115.94(14) . . ? C7 Si1 C6 108.74(15) . . ? N1 Si1 C5 102.80(11) . . ? C7 Si1 C5 107.35(14) . . ? C6 Si1 C5 106.90(13) . . ? N1 Si2 C9 113.20(12) . . ? N1 Si2 C10 109.97(11) . . ? C9 Si2 C10 109.56(13) . . ? N1 Si2 C8 112.50(13) . . ? C9 Si2 C8 106.95(15) . . ? C10 Si2 C8 104.23(13) . . ? N2 Si3 C21 115.35(13) . . ? N2 Si3 C20 115.01(13) . . ? C21 Si3 C20 108.27(15) . . ? N2 Si3 C19 102.64(11) . . ? C21 Si3 C19 106.65(13) . . ? C20 Si3 C19 108.25(13) . . ? N2 Si4 C23 112.79(12) . . ? N2 Si4 C22 113.54(13) . . ? C23 Si4 C22 108.16(15) . . ? N2 Si4 C24 108.91(12) . . ? C23 Si4 C24 108.59(13) . . ? C22 Si4 C24 104.42(14) . . ? C2 O1 C5 106.9(2) . . ? C2 O1 Ti 131.16(16) . . ? C5 O1 Ti 108.80(14) . . ? C13 O2 C10 107.5(2) . . ? C16 O3 C19 107.4(2) . . ? C16 O3 Ti 128.87(16) . . ? C19 O3 Ti 103.02(14) . . ? C27 O4 C24 107.8(2) . . ? Si1 N1 Si2 119.37(12) . . ? Si1 N1 Ti 112.14(11) . . ? Si2 N1 Ti 128.46(13) . . ? Si4 N2 Si3 120.01(12) . . ? Si4 N2 Ti 129.48(12) . . ? Si3 N2 Ti 110.51(11) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 109.1(2) . . ? C3 C2 C1 134.3(3) . . ? O1 C2 C1 116.6(2) . . ? C2 C3 C4 107.8(2) . . ? C2 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? C5 C4 C3 109.2(3) . . ? C5 C4 H4 125.4 . . ? C3 C4 H4 125.4 . . ? C4 C5 O1 107.0(2) . . ? C4 C5 Si1 139.1(2) . . ? O1 C5 Si1 113.93(18) . . ? 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 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 O2 107.5(2) . . ? C11 C10 Si2 133.6(2) . . ? O2 C10 Si2 118.77(19) . . ? C10 C11 C12 107.8(3) . . ? C10 C11 H11 126.1 . . ? C12 C11 H11 126.1 . . ? C13 C12 C11 107.4(2) . . ? C13 C12 H12 126.3 . . ? C11 C12 H12 126.3 . . ? C12 C13 O2 109.8(2) . . ? C12 C13 C14 134.3(3) . . ? O2 C13 C14 115.9(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 O3 108.4(2) . . ? C17 C16 C15 134.5(3) . . ? O3 C16 C15 117.0(2) . . ? C16 C17 C18 108.2(2) . . ? C16 C17 H17 125.9 . . ? C18 C17 H17 125.9 . . ? C19 C18 C17 109.0(3) . . ? C19 C18 H18 125.5 . . ? C17 C18 H18 125.5 . . ? C18 C19 O3 107.0(2) . . ? C18 C19 Si3 138.7(2) . . ? O3 C19 Si3 114.32(18) . . ? Si3 C20 H20A 109.5 . . ? Si3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si3 C21 H21A 109.5 . . ? Si3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si4 C22 H22A 109.5 . . ? Si4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si4 C23 H23A 109.5 . . ? Si4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 O4 107.6(2) . . ? C25 C24 Si4 134.9(2) . . ? O4 C24 Si4 117.43(19) . . ? C24 C25 C26 108.2(3) . . ? C24 C25 H25 125.9 . . ? C26 C25 H25 125.9 . . ? C27 C26 C25 106.9(3) . . ? C27 C26 H26 126.6 . . ? C25 C26 H26 126.6 . . ? C26 C27 O4 109.6(3) . . ? C26 C27 C28 135.0(3) . . ? O4 C27 C28 115.4(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? #===END