Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FM loop_ _publ_author_name M.F.Lappert C.F.Caro P.B.Hitchcock Z.Li X.-H.Wei _publ_contact_author_name 'Prof Michael F. Lappert' _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_section_title ; Synthetic and structural experiments on yttrium, cerium and magnesium trimethylsilylmethyls and their reaction products with nitriles; with a note on two cerium beta diketiminates ; data_(1)-dec101 _database_code_depnum_ccdc_archive 'CCDC 229450' _audit_creation_date 2001-12-03T16:00:34-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common "[Y{CH(SiMe3)2}3]'" _chemical_formula_moiety 'C21 H57 Si6 Y1' _chemical_formula_sum 'C21 H57 Si6 Y' _chemical_formula_weight 567.12 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P31c _symmetry_Int_Tables_number 159 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' 'y, x, z+1/2' '-x+y, -x, z' '-x, -x+y, z+1/2' 'x-y, -y, z+1/2' _cell_length_a 16.2345(10) _cell_length_b 16.2345(10) _cell_length_c 8.6294(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1969.65(18) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6016 _cell_measurement_theta_min 4.076 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 0.956 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.669 _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 0.712 _exptl_absorpt_correction_T_max 0.835 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 9004 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_unetI/netI 0.0532 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 4.35 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 2180 _reflns_number_gt 1927 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+2.0790P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 2180 _refine_ls_number_parameters 85 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1193 _refine_ls_wR_factor_gt 0.1144 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(11) _refine_diff_density_max 0.814 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.071 #----------------------------------------------------------------------------# # 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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 Y Y 0.3333 0.6667 0.67374(12) 0.0325(2) Uani 1 3 d S . . Si1 Si 0.55009(11) 0.71103(12) 0.59937(16) 0.0422(4) Uani 1 1 d . . . Si2 Si 0.55429(12) 0.83092(11) 0.89685(16) 0.0443(4) Uani 1 1 d . . . C1 C 0.4889(4) 0.7264(4) 0.7683(6) 0.0368(13) Uani 1 1 d . . . H1 H 0.4809 0.6734 0.8373 0.044 Uiso 1 1 calc R . . C2 C 0.4524(4) 0.6307(5) 0.4547(6) 0.0494(15) Uani 1 1 d . . . H2A H 0.4817 0.6209 0.3626 0.074 Uiso 1 1 calc R . . H2B H 0.4158 0.6612 0.4244 0.074 Uiso 1 1 calc R . . H2C H 0.4099 0.5692 0.5034 0.074 Uiso 1 1 calc R . . C3 C 0.6196(5) 0.6500(6) 0.6398(9) 0.067(2) Uani 1 1 d . . . H3A H 0.6493 0.6455 0.5438 0.1 Uiso 1 1 calc R . . H3B H 0.5769 0.586 0.68 0.1 Uiso 1 1 calc R . . H3C H 0.669 0.6866 0.7167 0.1 Uiso 1 1 calc R . . C4 C 0.6294(5) 0.8235(5) 0.4925(7) 0.0624(19) Uani 1 1 d . . . H4A H 0.6589 0.8096 0.4048 0.094 Uiso 1 1 calc R . . H4B H 0.6792 0.8685 0.5625 0.094 Uiso 1 1 calc R . . H4C H 0.5919 0.8514 0.4543 0.094 Uiso 1 1 calc R . . C5 C 0.6790(5) 0.8612(6) 0.9491(10) 0.078(2) Uani 1 1 d . . . H5A H 0.7076 0.9173 1.0165 0.117 Uiso 1 1 calc R . . H5B H 0.717 0.8746 0.8545 0.117 Uiso 1 1 calc R . . H5C H 0.6772 0.8073 1.0036 0.117 Uiso 1 1 calc R . . C6 C 0.5646(5) 0.9415(5) 0.8096(8) 0.0636(19) Uani 1 1 d . . . H6A H 0.5995 0.9951 0.8807 0.095 Uiso 1 1 calc R . . H6B H 0.5009 0.9322 0.7918 0.095 Uiso 1 1 calc R . . H6C H 0.5987 0.9551 0.7109 0.095 Uiso 1 1 calc R . . C7 C 0.4875(6) 0.8071(6) 1.0846(7) 0.072(2) Uani 1 1 d . . . H7A H 0.5213 0.862 1.1535 0.109 Uiso 1 1 calc R . . H7B H 0.483 0.7506 1.134 0.109 Uiso 1 1 calc R . . H7C H 0.4234 0.7962 1.0642 0.109 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 Y 0.0353(3) 0.0353(3) 0.0270(4) 0 0 0.01765(15) Si1 0.0399(9) 0.0513(10) 0.0375(9) 0.0046(7) 0.0038(7) 0.0244(8) Si2 0.0453(10) 0.0381(9) 0.0410(9) -0.0010(7) -0.0097(7) 0.0145(8) C1 0.039(3) 0.037(3) 0.033(3) 0.004(2) 0.000(2) 0.018(3) C2 0.056(4) 0.056(4) 0.038(3) -0.007(3) 0.003(3) 0.029(3) C3 0.058(4) 0.093(6) 0.071(5) 0.014(4) 0.007(3) 0.054(4) C4 0.054(4) 0.072(5) 0.050(4) 0.013(3) 0.012(3) 0.023(4) C5 0.052(5) 0.058(5) 0.111(6) -0.004(4) -0.029(4) 0.017(4) C6 0.072(5) 0.039(4) 0.074(5) 0.000(3) -0.021(4) 0.023(4) C7 0.087(6) 0.071(5) 0.041(4) -0.013(3) 0.001(3) 0.026(4) #----------------------------------------------------------------------------# # 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 Y C1 2.353(5) 2_665 ? Y C1 2.353(5) 4_565 ? Y C1 2.353(5) . ? Si1 C1 1.850(5) . ? Si1 C3 1.869(7) . ? Si1 C4 1.869(7) . ? Si1 C2 1.925(6) . ? Si2 C1 1.853(6) . ? Si2 C6 1.876(6) . ? Si2 C7 1.879(7) . ? Si2 C5 1.884(7) . ? 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 C1 Y C1 108.63(13) 2_665 4_565 ? C1 Y C1 108.63(13) 2_665 . ? C1 Y C1 108.63(13) 4_565 . ? C1 Si1 C3 115.6(3) . . ? C1 Si1 C4 114.3(3) . . ? C3 Si1 C4 107.8(3) . . ? C1 Si1 C2 106.6(3) . . ? C3 Si1 C2 105.9(3) . . ? C4 Si1 C2 105.9(3) . . ? C1 Si2 C6 111.9(3) . . ? C1 Si2 C7 108.7(3) . . ? C6 Si2 C7 108.0(4) . . ? C1 Si2 C5 115.5(3) . . ? C6 Si2 C5 106.1(4) . . ? C7 Si2 C5 106.3(4) . . ? Si1 C1 Si2 119.7(3) . . ? Si1 C1 Y 102.1(2) . . ? Si2 C1 Y 126.2(3) . . ? #===END data_(2)-aug601 _database_code_depnum_ccdc_archive 'CCDC 229451' _audit_creation_date 2001-08-06T16:54:53-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[Ce{CH(SiMe3)2}3]' _chemical_formula_moiety 'C21 H57 Ce1 Si6' _chemical_formula_sum 'C21 H57 Ce Si6' _chemical_formula_weight 618.33 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P31c _symmetry_Int_Tables_number 159 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' 'y, x, z+1/2' '-x+y, -x, z' '-x, -x+y, z+1/2' 'x-y, -y, z+1/2' _cell_length_a 16.3636(8) _cell_length_b 16.3636(8) _cell_length_c 8.5950(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1993.12(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5203 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.03 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 650 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.328 _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 0.789 _exptl_absorpt_correction_T_max 0.852 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _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_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 9233 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_unetI/netI 0.0489 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 2213 _reflns_number_gt 2004 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The final difference map showed electron density along the 3-fold axis which could not be successfully refined . This is probably very disordered hexane solvate. 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^)+(0.0781P)^2^+0.6696P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2213 _refine_ls_number_parameters 95 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1185 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(3) _refine_diff_density_max 2.027 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.117 #----------------------------------------------------------------------------# # 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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 Ce Ce 0.3333 0.6667 0.42089(12) 0.0314(2) Uani 1 3 d S . . Si1 Si 0.55660(14) 0.84012(14) 0.3435(2) 0.0398(5) Uani 1 1 d . . . Si2 Si 0.55619(15) 0.72266(15) 0.6434(2) 0.0414(5) Uani 1 1 d . . . C1 C 0.4971(5) 0.7677(6) 0.5140(8) 0.0375(16) Uani 1 1 d . . . H1 H 0.480(5) 0.793(5) 0.569(8) 0.021(18) Uiso 1 1 d . . . C2 C 0.4619(6) 0.8233(6) 0.1938(9) 0.0500(19) Uani 1 1 d . . . H2A H 0.4142 0.8337 0.2443 0.075 Uiso 1 1 calc R . . H2B H 0.4319 0.7589 0.1521 0.075 Uiso 1 1 calc R . . H2C H 0.4914 0.8686 0.1087 0.075 Uiso 1 1 calc R . . C3 C 0.6267(7) 0.9712(6) 0.3785(12) 0.063(3) Uani 1 1 d . . . H3A H 0.6791 0.9855 0.4494 0.094 Uiso 1 1 calc R . . H3B H 0.5858 0.9924 0.4249 0.094 Uiso 1 1 calc R . . H3C H 0.6517 1.0039 0.2794 0.094 Uiso 1 1 calc R . . C4 C 0.6355(7) 0.8045(7) 0.2392(10) 0.065(3) Uani 1 1 d . . . H4A H 0.5973 0.7403 0.1982 0.097 Uiso 1 1 calc R . . H4B H 0.6824 0.8063 0.3122 0.097 Uiso 1 1 calc R . . H4C H 0.6677 0.8483 0.1532 0.097 Uiso 1 1 calc R . . C5 C 0.4857(8) 0.6791(7) 0.8289(10) 0.065(3) Uani 1 1 d . . . H5A H 0.429 0.6179 0.8099 0.097 Uiso 1 1 calc R . . H5B H 0.4672 0.7246 0.8637 0.097 Uiso 1 1 calc R . . H5C H 0.5241 0.6721 0.9094 0.097 Uiso 1 1 calc R . . C6 C 0.5615(7) 0.6211(7) 0.5519(11) 0.057(2) Uani 1 1 d . . . H6A H 0.5887 0.6391 0.4474 0.085 Uiso 1 1 calc R . . H6B H 0.4977 0.5665 0.5448 0.085 Uiso 1 1 calc R . . H6C H 0.6009 0.6049 0.6159 0.085 Uiso 1 1 calc R . . C7 C 0.6820(7) 0.8119(7) 0.7006(15) 0.080(4) Uani 1 1 d . . . H7A H 0.6815 0.8581 0.7726 0.12 Uiso 1 1 calc R . . H7B H 0.7181 0.8445 0.6073 0.12 Uiso 1 1 calc R . . H7C H 0.7113 0.7793 0.7513 0.12 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 Ce 0.0322(2) 0.0322(2) 0.0296(3) 0 0 0.01612(11) Si1 0.0346(11) 0.0401(11) 0.0372(11) -0.0005(8) 0.0060(8) 0.0130(9) Si2 0.0417(12) 0.0485(13) 0.0418(12) -0.0082(9) -0.0092(8) 0.0283(10) C1 0.045(4) 0.049(4) 0.027(4) -0.007(3) -0.001(3) 0.030(4) C2 0.055(5) 0.052(5) 0.040(4) 0.007(3) 0.005(3) 0.025(4) C3 0.048(5) 0.048(5) 0.068(6) -0.006(4) 0.009(4) 0.006(4) C4 0.060(6) 0.077(7) 0.056(6) -0.004(5) 0.016(4) 0.033(5) C5 0.086(7) 0.089(7) 0.043(5) 0.012(4) 0.000(4) 0.061(6) C6 0.061(6) 0.056(5) 0.065(5) -0.013(4) -0.015(4) 0.038(5) C7 0.062(6) 0.062(6) 0.120(9) -0.035(6) -0.049(6) 0.035(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 Ce C1 2.475(7) 2_665 ? Ce C1 2.475(7) . ? Ce C1 2.475(7) 4_565 ? Si1 C1 1.829(8) . ? Si1 C3 1.883(9) . ? Si1 C4 1.888(9) . ? Si1 C2 1.925(8) . ? Si2 C1 1.852(7) . ? Si2 C6 1.879(9) . ? Si2 C5 1.886(10) . ? Si2 C7 1.899(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ce C1 110.08(16) 2_665 . ? C1 Ce C1 110.08(16) 2_665 4_565 ? C1 Ce C1 110.08(16) . 4_565 ? C1 Si1 C3 115.7(4) . . ? C1 Si1 C4 113.9(4) . . ? C3 Si1 C4 107.9(4) . . ? C1 Si1 C2 108.2(4) . . ? C3 Si1 C2 105.0(5) . . ? C4 Si1 C2 105.3(4) . . ? C1 Si2 C6 111.4(4) . . ? C1 Si2 C5 108.4(4) . . ? C6 Si2 C5 108.0(4) . . ? C1 Si2 C7 115.5(5) . . ? C6 Si2 C7 106.1(5) . . ? C5 Si2 C7 107.2(5) . . ? Si1 C1 Si2 121.6(4) . . ? Si1 C1 Ce 102.8(3) . . ? Si2 C1 Ce 122.3(4) . . ? #===END data_(3)-jun1002 _database_code_depnum_ccdc_archive 'CCDC 229452' _audit_creation_date 2002-06-12T12:08:52-00:00 _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_name_common '[Y{CH(SiMe3)(SiMe2OMe)}3].Et2O' _chemical_formula_moiety '(C21 H57 O3 Si6 Y1)(C4 H10 O1)' _chemical_formula_sum 'C25 H67 O4 Si6 Y1' _chemical_formula_weight 689.24 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _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 11.8736(2) _cell_length_b 18.9420(3) _cell_length_c 19.0835(3) _cell_angle_alpha 90 _cell_angle_beta 106.618(1) _cell_angle_gamma 90 _cell_volume 4112.8(1) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16707 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 24.713 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.113 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.616 _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 0.7398 _exptl_absorpt_correction_T_max 0.8573 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.073 _diffrn_reflns_av_unetI/netI 0.0545 _diffrn_reflns_number 34012 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.7 _diffrn_reflns_theta_max 24.7 _diffrn_reflns_theta_full 24.7 _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.978 _reflns_number_total 6852 _reflns_number_gt 5362 _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 ; Hydrogens on C1 ,C8, and C15 were refined; others were in riding mode. 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^)+(0.0205P)^2^+5.2241P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6852 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 1.03 _refine_ls_restrained_S_all 1.03 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.339 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.061 #----------------------------------------------------------------------------# # 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' 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' Y Y -2.7962 3.5667 '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 Y Y 0.04158(3) 0.297225(15) 0.203571(16) 0.02225(9) Uani 1 1 d . . . Si1 Si 0.31018(8) 0.29825(5) 0.21447(5) 0.0328(2) Uani 1 1 d . . . Si2 Si 0.18946(9) 0.36708(5) 0.05847(5) 0.0346(2) Uani 1 1 d . . . Si3 Si -0.04467(9) 0.44764(5) 0.23651(5) 0.0331(2) Uani 1 1 d . . . Si4 Si -0.25412(8) 0.38306(5) 0.10987(5) 0.0355(2) Uani 1 1 d . . . Si5 Si -0.06704(8) 0.16466(5) 0.26128(5) 0.0311(2) Uani 1 1 d . . . Si6 Si -0.02131(9) 0.11386(5) 0.11318(5) 0.0335(2) Uani 1 1 d . . . O1 O 0.23536(18) 0.27044(12) 0.27436(11) 0.0328(5) Uani 1 1 d . . . O2 O 0.07343(19) 0.39687(11) 0.28267(11) 0.0332(5) Uani 1 1 d . . . O3 O -0.01593(19) 0.24428(11) 0.30053(11) 0.0311(5) Uani 1 1 d . . . O4 O -0.1236(3) 0.35215(16) 0.48320(16) 0.0664(8) Uani 1 1 d . . . C1 C 0.1875(3) 0.30747(17) 0.13380(18) 0.0283(8) Uani 1 1 d . . . H1 H 0.169(3) 0.2662(17) 0.1166(17) 0.031(9) Uiso 1 1 d . . . C2 C 0.3842(3) 0.38274(19) 0.2508(2) 0.0511(10) Uani 1 1 d . . . H2C H 0.4147 0.4051 0.2136 0.077 Uiso 1 1 calc R . . H2B H 0.4494 0.3732 0.2947 0.077 Uiso 1 1 calc R . . H2A H 0.3276 0.4144 0.2634 0.077 Uiso 1 1 calc R . . C3 C 0.4243(3) 0.2300(2) 0.2188(2) 0.0528(11) Uani 1 1 d . . . H3C H 0.3879 0.1831 0.2132 0.079 Uiso 1 1 calc R . . H3B H 0.4845 0.2328 0.2662 0.079 Uiso 1 1 calc R . . H3A H 0.4606 0.238 0.1794 0.079 Uiso 1 1 calc R . . C4 C 0.2916(3) 0.2398(2) 0.3447(2) 0.0540(11) Uani 1 1 d . . . H4C H 0.3338 0.197 0.3382 0.081 Uiso 1 1 calc R . . H4B H 0.232 0.2278 0.3692 0.081 Uiso 1 1 calc R . . H4A H 0.3472 0.2738 0.3746 0.081 Uiso 1 1 calc R . . C5 C 0.0575(4) 0.3515(2) -0.0214(2) 0.0553(11) Uani 1 1 d . . . H5C H 0.058 0.3027 -0.0382 0.083 Uiso 1 1 calc R . . H5B H 0.0593 0.3839 -0.0611 0.083 Uiso 1 1 calc R . . H5A H -0.014 0.3599 -0.0066 0.083 Uiso 1 1 calc R . . C6 C 0.1879(4) 0.46236(19) 0.0837(2) 0.0560(11) Uani 1 1 d . . . H6C H 0.1165 0.4725 0.0979 0.084 Uiso 1 1 calc R . . H6B H 0.1894 0.4917 0.0417 0.084 Uiso 1 1 calc R . . H6A H 0.2571 0.4728 0.1248 0.084 Uiso 1 1 calc R . . C7 C 0.3230(3) 0.3537(2) 0.0254(2) 0.0524(11) Uani 1 1 d . . . H7C H 0.3942 0.3618 0.0659 0.079 Uiso 1 1 calc R . . H7B H 0.321 0.387 -0.0142 0.079 Uiso 1 1 calc R . . H7A H 0.3235 0.3053 0.0074 0.079 Uiso 1 1 calc R . . C8 C -0.0976(3) 0.39439(16) 0.15582(18) 0.0265(7) Uani 1 1 d . . . H8 H -0.064(3) 0.4088(16) 0.1217(17) 0.029(9) Uiso 1 1 d . . . C9 C -0.1407(4) 0.4532(2) 0.2982(2) 0.0550(11) Uani 1 1 d . . . H9C H -0.2165 0.4739 0.2716 0.083 Uiso 1 1 calc R . . H9B H -0.1029 0.4829 0.3404 0.083 Uiso 1 1 calc R . . H9A H -0.1533 0.4057 0.315 0.083 Uiso 1 1 calc R . . C10 C 0.0149(4) 0.53718(17) 0.2281(2) 0.0520(11) Uani 1 1 d . . . H10C H 0.0813 0.5332 0.2076 0.078 Uiso 1 1 calc R . . H10B H 0.0413 0.5592 0.2766 0.078 Uiso 1 1 calc R . . H10A H -0.0467 0.5663 0.1959 0.078 Uiso 1 1 calc R . . C11 C 0.1552(3) 0.4173(2) 0.3512(2) 0.0512(11) Uani 1 1 d . . . H11C H 0.193 0.4619 0.3449 0.077 Uiso 1 1 calc R . . H11B H 0.2151 0.3805 0.3672 0.077 Uiso 1 1 calc R . . H11A H 0.113 0.4234 0.3881 0.077 Uiso 1 1 calc R . . C12 C -0.3289(3) 0.3288(2) 0.1656(2) 0.0620(12) Uani 1 1 d . . . H12C H -0.2924 0.282 0.1743 0.093 Uiso 1 1 calc R . . H12B H -0.4124 0.3239 0.1392 0.093 Uiso 1 1 calc R . . H12A H -0.3209 0.3522 0.2126 0.093 Uiso 1 1 calc R . . C13 C -0.3384(4) 0.4679(2) 0.0879(3) 0.0645(13) Uani 1 1 d . . . H13C H -0.3309 0.4944 0.1331 0.097 Uiso 1 1 calc R . . H13B H -0.4214 0.4575 0.0642 0.097 Uiso 1 1 calc R . . H13A H -0.3068 0.4961 0.0548 0.097 Uiso 1 1 calc R . . C14 C -0.2741(4) 0.3361(2) 0.0209(2) 0.0621(12) Uani 1 1 d . . . H14C H -0.239 0.3642 -0.0106 0.093 Uiso 1 1 calc R . . H14B H -0.3581 0.3297 -0.0033 0.093 Uiso 1 1 calc R . . H14A H -0.2355 0.2899 0.0299 0.093 Uiso 1 1 calc R . . C15 C -0.0596(3) 0.18206(16) 0.16983(18) 0.0272(8) Uani 1 1 d . . . H15 H -0.124(3) 0.1993(16) 0.1467(16) 0.024(9) Uiso 1 1 d . . . C16 C 0.0356(4) 0.09631(19) 0.3131(2) 0.0492(10) Uani 1 1 d . . . H16C H 0.0194 0.0512 0.2869 0.074 Uiso 1 1 calc R . . H16B H 0.0247 0.0909 0.3618 0.074 Uiso 1 1 calc R . . H16A H 0.1167 0.1107 0.3178 0.074 Uiso 1 1 calc R . . C17 C -0.2132(3) 0.1506(2) 0.2767(2) 0.0477(10) Uani 1 1 d . . . H17C H -0.2616 0.193 0.2618 0.072 Uiso 1 1 calc R . . H17B H -0.2028 0.1414 0.3287 0.072 Uiso 1 1 calc R . . H17A H -0.2521 0.1102 0.2477 0.072 Uiso 1 1 calc R . . C18 C -0.0191(4) 0.2646(2) 0.37261(18) 0.0459(10) Uani 1 1 d . . . H18C H -0.1008 0.2652 0.3744 0.069 Uiso 1 1 calc R . . H18B H 0.0151 0.3118 0.384 0.069 Uiso 1 1 calc R . . H18A H 0.0262 0.2307 0.4085 0.069 Uiso 1 1 calc R . . C19 C 0.1384(3) 0.0898(2) 0.1452(2) 0.0490(10) Uani 1 1 d . . . H19C H 0.1861 0.1316 0.1435 0.073 Uiso 1 1 calc R . . H19B H 0.1548 0.053 0.1133 0.073 Uiso 1 1 calc R . . H19A H 0.1576 0.072 0.1955 0.073 Uiso 1 1 calc R . . C20 C -0.1023(4) 0.0278(2) 0.1096(3) 0.0620(12) Uani 1 1 d . . . H20C H -0.086 0.0083 0.1591 0.093 Uiso 1 1 calc R . . H20B H -0.0761 -0.0056 0.0783 0.093 Uiso 1 1 calc R . . H20A H -0.1869 0.036 0.0896 0.093 Uiso 1 1 calc R . . C21 C -0.0560(4) 0.1456(2) 0.01605(19) 0.0524(11) Uani 1 1 d . . . H21C H -0.1402 0.156 -0.0025 0.079 Uiso 1 1 calc R . . H21B H -0.0351 0.1089 -0.0142 0.079 Uiso 1 1 calc R . . H21A H -0.0108 0.1885 0.0142 0.079 Uiso 1 1 calc R . . C22 C -0.0520(7) 0.3821(3) 0.5462(3) 0.105(2) Uani 1 1 d . . . H22B H -0.0703 0.3611 0.5892 0.126 Uiso 1 1 calc R . . H22A H -0.0682 0.4334 0.5461 0.126 Uiso 1 1 calc R . . C23 C 0.0732(6) 0.3713(4) 0.5529(3) 0.117(2) Uani 1 1 d . . . H23C H 0.0899 0.3206 0.5538 0.175 Uiso 1 1 calc R . . H23B H 0.1209 0.393 0.5983 0.175 Uiso 1 1 calc R . . H23A H 0.0921 0.393 0.5111 0.175 Uiso 1 1 calc R . . C24 C -0.2463(5) 0.3538(3) 0.4764(3) 0.0853(17) Uani 1 1 d . . . H24B H -0.271 0.4031 0.4807 0.102 Uiso 1 1 calc R . . H24A H -0.262 0.3261 0.5166 0.102 Uiso 1 1 calc R . . C25 C -0.3147(4) 0.3247(3) 0.4064(3) 0.0879(17) Uani 1 1 d . . . H25C H -0.2993 0.3521 0.3665 0.132 Uiso 1 1 calc R . . H25B H -0.3986 0.3272 0.4029 0.132 Uiso 1 1 calc R . . H25A H -0.2921 0.2754 0.4027 0.132 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 Y 0.02299(17) 0.01886(16) 0.02411(17) -0.00036(13) 0.00547(12) -0.00069(14) Si1 0.0234(5) 0.0283(5) 0.0456(6) 0.0036(4) 0.0081(4) -0.0007(4) Si2 0.0370(6) 0.0315(5) 0.0392(6) 0.0064(4) 0.0169(5) -0.0010(4) Si3 0.0401(6) 0.0213(5) 0.0398(6) -0.0033(4) 0.0145(5) 0.0020(4) Si4 0.0268(5) 0.0304(5) 0.0465(6) 0.0078(4) 0.0060(4) 0.0029(4) Si5 0.0367(6) 0.0233(5) 0.0343(5) 0.0042(4) 0.0118(4) -0.0022(4) Si6 0.0367(6) 0.0229(5) 0.0414(6) -0.0061(4) 0.0121(5) -0.0019(4) O1 0.0269(12) 0.0394(14) 0.0279(13) 0.0086(10) 0.0008(10) 0.0029(10) O2 0.0353(13) 0.0287(12) 0.0307(13) -0.0091(10) 0.0014(10) -0.0031(10) O3 0.0385(14) 0.0307(12) 0.0257(12) -0.0021(10) 0.0116(10) -0.0026(10) O4 0.080(2) 0.075(2) 0.0547(19) -0.0038(16) 0.0362(17) 0.0117(18) C1 0.0300(19) 0.0218(19) 0.034(2) -0.0020(15) 0.0104(15) -0.0042(15) C2 0.039(2) 0.043(2) 0.063(3) -0.003(2) 0.002(2) -0.0105(19) C3 0.035(2) 0.043(2) 0.084(3) 0.011(2) 0.022(2) 0.0064(18) C4 0.048(2) 0.065(3) 0.039(2) 0.016(2) -0.0032(19) 0.006(2) C5 0.058(3) 0.065(3) 0.041(2) 0.013(2) 0.011(2) 0.003(2) C6 0.072(3) 0.034(2) 0.069(3) 0.013(2) 0.031(2) -0.002(2) C7 0.055(3) 0.052(3) 0.062(3) 0.010(2) 0.036(2) -0.002(2) C8 0.0277(19) 0.0243(17) 0.0294(19) 0.0044(14) 0.0114(16) 0.0032(14) C9 0.065(3) 0.051(3) 0.057(3) -0.003(2) 0.030(2) 0.014(2) C10 0.077(3) 0.0216(19) 0.059(3) -0.0068(18) 0.022(2) -0.0062(19) C11 0.054(3) 0.049(2) 0.040(2) -0.0179(19) -0.0047(19) -0.009(2) C12 0.036(2) 0.062(3) 0.090(3) 0.025(2) 0.021(2) 0.002(2) C13 0.045(3) 0.049(3) 0.095(4) 0.019(2) 0.012(2) 0.016(2) C14 0.050(3) 0.068(3) 0.053(3) -0.008(2) -0.011(2) -0.005(2) C15 0.025(2) 0.0229(18) 0.031(2) 0.0022(14) 0.0045(16) 0.0021(15) C16 0.063(3) 0.036(2) 0.046(2) 0.0088(18) 0.011(2) 0.005(2) C17 0.049(2) 0.045(2) 0.053(2) 0.0077(19) 0.021(2) -0.0109(19) C18 0.065(3) 0.049(2) 0.029(2) -0.0028(17) 0.0206(19) -0.001(2) C19 0.049(2) 0.039(2) 0.065(3) 0.0057(19) 0.026(2) 0.0133(19) C20 0.068(3) 0.034(2) 0.091(3) -0.023(2) 0.034(3) -0.013(2) C21 0.064(3) 0.056(3) 0.038(2) -0.0097(19) 0.014(2) 0.005(2) C22 0.159(7) 0.099(5) 0.057(4) -0.011(3) 0.034(4) 0.022(4) C23 0.117(6) 0.150(6) 0.077(4) -0.043(4) 0.019(4) -0.033(5) C24 0.101(4) 0.089(4) 0.084(4) 0.030(3) 0.056(4) 0.050(3) C25 0.059(3) 0.123(5) 0.091(4) 0.037(4) 0.036(3) 0.014(3) #----------------------------------------------------------------------------# # 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 Y O1 2.366(2) . ? Y O3 2.370(2) . ? Y O2 2.379(2) . ? Y C8 2.468(3) . ? Y C1 2.476(3) . ? Y C15 2.485(3) . ? Si1 O1 1.719(2) . ? Si1 C1 1.800(3) . ? Si1 C3 1.858(4) . ? Si1 C2 1.862(4) . ? Si2 C1 1.833(3) . ? Si2 C6 1.869(4) . ? Si2 C5 1.870(4) . ? Si2 C7 1.884(4) . ? Si3 O2 1.721(2) . ? Si3 C8 1.797(3) . ? Si3 C9 1.861(4) . ? Si3 C10 1.862(3) . ? Si4 C8 1.826(3) . ? Si4 C14 1.871(4) . ? Si4 C12 1.875(4) . ? Si4 C13 1.876(4) . ? Si5 O3 1.716(2) . ? Si5 C15 1.803(3) . ? Si5 C16 1.857(4) . ? Si5 C17 1.860(4) . ? Si6 C15 1.824(3) . ? Si6 C19 1.874(4) . ? Si6 C21 1.879(4) . ? Si6 C20 1.884(4) . ? O1 C4 1.439(4) . ? O2 C11 1.440(4) . ? O3 C18 1.439(4) . ? O4 C22 1.381(6) . ? O4 C24 1.426(6) . ? C22 C23 1.469(8) . ? C24 C25 1.458(7) . ? 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 O1 Y O3 85.06(7) . . ? O1 Y O2 81.70(8) . . ? O3 Y O2 82.50(7) . . ? O1 Y C8 144.11(9) . . ? O3 Y C8 106.96(9) . . ? O2 Y C8 67.08(9) . . ? O1 Y C1 66.92(9) . . ? O3 Y C1 148.75(9) . . ? O2 Y C1 105.68(10) . . ? C8 Y C1 103.94(11) . . ? O1 Y C15 106.19(10) . . ? O3 Y C15 66.73(9) . . ? O2 Y C15 146.98(9) . . ? C8 Y C15 109.63(11) . . ? C1 Y C15 106.88(11) . . ? O1 Si1 C1 98.79(13) . . ? O1 Si1 C3 105.41(15) . . ? C1 Si1 C3 120.48(18) . . ? O1 Si1 C2 107.12(16) . . ? C1 Si1 C2 114.57(17) . . ? C3 Si1 C2 108.73(18) . . ? C1 Si2 C6 112.91(17) . . ? C1 Si2 C5 110.25(17) . . ? C6 Si2 C5 107.1(2) . . ? C1 Si2 C7 112.34(16) . . ? C6 Si2 C7 106.70(18) . . ? C5 Si2 C7 107.20(19) . . ? O2 Si3 C8 99.16(13) . . ? O2 Si3 C9 105.36(15) . . ? C8 Si3 C9 116.48(18) . . ? O2 Si3 C10 106.22(16) . . ? C8 Si3 C10 119.09(17) . . ? C9 Si3 C10 108.61(18) . . ? C8 Si4 C14 109.82(17) . . ? C8 Si4 C12 111.94(17) . . ? C14 Si4 C12 107.3(2) . . ? C8 Si4 C13 114.26(17) . . ? C14 Si4 C13 106.4(2) . . ? C12 Si4 C13 106.73(19) . . ? O3 Si5 C15 98.79(13) . . ? O3 Si5 C16 106.51(15) . . ? C15 Si5 C16 115.86(17) . . ? O3 Si5 C17 106.62(15) . . ? C15 Si5 C17 119.03(17) . . ? C16 Si5 C17 108.42(18) . . ? C15 Si6 C19 112.32(17) . . ? C15 Si6 C21 109.68(17) . . ? C19 Si6 C21 108.38(18) . . ? C15 Si6 C20 115.04(17) . . ? C19 Si6 C20 105.02(19) . . ? C21 Si6 C20 106.0(2) . . ? C4 O1 Si1 123.6(2) . . ? C4 O1 Y 137.3(2) . . ? Si1 O1 Y 99.08(9) . . ? C11 O2 Si3 123.6(2) . . ? C11 O2 Y 137.1(2) . . ? Si3 O2 Y 99.22(9) . . ? C18 O3 Si5 123.4(2) . . ? C18 O3 Y 136.5(2) . . ? Si5 O3 Y 100.14(9) . . ? C22 O4 C24 115.4(4) . . ? Si1 C1 Si2 122.81(18) . . ? Si1 C1 Y 92.98(13) . . ? Si2 C1 Y 129.61(16) . . ? Si3 C8 Si4 122.42(18) . . ? Si3 C8 Y 93.95(13) . . ? Si4 C8 Y 124.87(16) . . ? Si5 C15 Si6 122.27(18) . . ? Si5 C15 Y 93.64(13) . . ? Si6 C15 Y 126.27(16) . . ? O4 C22 C23 112.0(5) . . ? O4 C24 C25 111.2(4) . . ? #===END data_(4)-nov702 _database_code_depnum_ccdc_archive 'CCDC 229453' _audit_creation_date 2002-11-05T14:26:39-00:00 _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_name_common '[Ce{CH(SiMe3)(SiMe2OMe)}3]' _chemical_formula_moiety 'C21 H57 Ce1 O3 Si6' _chemical_formula_sum 'C21 H57 Ce O3 Si6' _chemical_formula_weight 666.33 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonalh _symmetry_space_group_name_H-M P31c _symmetry_Int_Tables_number 159 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' 'y, x, z+1/2' '-x+y, -x, z' '-x, -x+y, z+1/2' 'x-y, -y, z+1/2' _cell_length_a 15.9563(3) _cell_length_b 15.9563(3) _cell_length_c 9.6101(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 2118.96(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10889 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.044 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 698 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.259 _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 0.7406 _exptl_absorpt_correction_T_max 0.8436 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _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_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_unetI/netI 0.0265 _diffrn_reflns_number 16092 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.9 _diffrn_reflns_theta_max 27.88 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 3227 _reflns_number_gt 3003 _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^)+(0.0569P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'H on C1 refined; others riding' _refine_ls_extinction_method none _refine_ls_number_reflns 3227 _refine_ls_number_parameters 98 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0885 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.011(17) _refine_diff_density_max 1.32 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.087 #----------------------------------------------------------------------------# # 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' Ce Ce -0.2486 2.6331 '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' 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 Ce Ce 0.3333 0.6667 0.32368(3) 0.04068(10) Uani 1 3 d S . . Si1 Si 0.29510(10) 0.84592(9) 0.40085(14) 0.0621(3) Uani 1 1 d . . . Si2 Si 0.17157(8) 0.74431(11) 0.12659(14) 0.0676(3) Uani 1 1 d . . . O O 0.3488(2) 0.7936(2) 0.4941(3) 0.0615(7) Uani 1 1 d . . . C1 C 0.2787(3) 0.7860(3) 0.2364(4) 0.0536(8) Uani 1 1 d . . . H1 H 0.334(3) 0.827(5) 0.178(7) 0.077(18) Uiso 1 1 d . . . C2 C 0.3882(5) 0.8218(4) 0.6326(5) 0.0888(17) Uani 1 1 d . . . H2C H 0.4396 0.8898 0.632 0.133 Uiso 1 1 calc R . . H2B H 0.4148 0.7812 0.663 0.133 Uiso 1 1 calc R . . H2A H 0.3368 0.8136 0.6967 0.133 Uiso 1 1 calc R . . C3 C 0.1839(6) 0.8187(6) 0.4995(7) 0.104(2) Uani 1 1 d . . . H3C H 0.1443 0.8373 0.4437 0.156 Uiso 1 1 calc R . . H3B H 0.2021 0.8553 0.5869 0.156 Uiso 1 1 calc R . . H3A H 0.1466 0.7493 0.5199 0.156 Uiso 1 1 calc R . . C4 C 0.3849(6) 0.9809(4) 0.4090(8) 0.103(2) Uani 1 1 d . . . H4C H 0.4494 0.9928 0.3827 0.155 Uiso 1 1 calc R . . H4B H 0.387 1.0043 0.5038 0.155 Uiso 1 1 calc R . . H4A H 0.3648 1.0151 0.3445 0.155 Uiso 1 1 calc R . . C5 C 0.0587(4) 0.6457(5) 0.2116(8) 0.101(2) Uani 1 1 d . . . H5C H 0.0672 0.5901 0.2314 0.151 Uiso 1 1 calc R . . H5B H 0.0035 0.6256 0.1488 0.151 Uiso 1 1 calc R . . H5A H 0.0468 0.6699 0.2986 0.151 Uiso 1 1 calc R . . C6 C 0.1916(5) 0.6981(8) -0.0405(7) 0.126(3) Uani 1 1 d . . . H6C H 0.2479 0.7501 -0.0881 0.189 Uiso 1 1 calc R . . H6B H 0.1342 0.6754 -0.0997 0.189 Uiso 1 1 calc R . . H6A H 0.2032 0.6443 -0.0218 0.189 Uiso 1 1 calc R . . C7 C 0.1401(6) 0.8376(7) 0.0789(12) 0.139(4) Uani 1 1 d . . . H7C H 0.1276 0.8638 0.1636 0.209 Uiso 1 1 calc R . . H7B H 0.082 0.8084 0.0204 0.209 Uiso 1 1 calc R . . H7A H 0.1939 0.8898 0.0275 0.209 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 Ce 0.04394(11) 0.04394(11) 0.03418(14) 0 0 0.02197(6) Si1 0.0712(7) 0.0554(6) 0.0655(7) -0.0004(5) 0.0135(6) 0.0360(6) Si2 0.0533(6) 0.0774(8) 0.0748(8) 0.0194(6) -0.0016(5) 0.0347(6) O 0.0788(19) 0.0610(16) 0.0451(15) -0.0138(13) -0.0068(12) 0.0353(14) C1 0.050(2) 0.062(2) 0.051(2) 0.0096(16) 0.0049(15) 0.0298(17) C2 0.102(4) 0.096(4) 0.057(3) -0.034(2) -0.012(3) 0.040(3) C3 0.105(5) 0.133(6) 0.092(5) 0.005(4) 0.035(4) 0.073(4) C4 0.127(6) 0.054(3) 0.118(5) -0.009(3) 0.027(4) 0.038(3) C5 0.057(3) 0.100(4) 0.120(6) 0.023(4) 0.004(3) 0.020(3) C6 0.088(4) 0.210(8) 0.059(4) -0.019(5) -0.022(3) 0.059(5) C7 0.097(5) 0.126(6) 0.212(10) 0.074(7) -0.002(6) 0.069(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 Ce O 2.519(3) . ? Ce C1 2.598(4) . ? Si1 O 1.718(4) . ? Si1 C1 1.798(4) . ? Si1 C3 1.862(6) . ? Si1 C4 1.900(6) . ? Si2 C1 1.828(4) . ? Si2 C7 1.850(7) . ? Si2 C6 1.860(8) . ? Si2 C5 1.884(6) . ? O C2 1.444(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 O Ce O 82.28(12) . 2_665 ? O Ce C1 63.57(12) . . ? O Ce C1 106.34(11) 2_665 . ? O Ce C1 142.56(12) 4_565 . ? C1 Ce C1 110.09(9) . 2_665 ? O Si1 C1 100.10(16) . . ? O Si1 C3 105.7(3) . . ? C1 Si1 C3 117.1(3) . . ? O Si1 C4 104.6(3) . . ? C1 Si1 C4 117.8(2) . . ? C3 Si1 C4 109.5(3) . . ? C1 Si2 C7 115.5(4) . . ? C1 Si2 C6 109.1(3) . . ? C7 Si2 C6 105.9(5) . . ? C1 Si2 C5 112.5(3) . . ? C7 Si2 C5 104.4(4) . . ? C6 Si2 C5 108.9(4) . . ? C2 O Si1 125.0(3) . . ? C2 O Ce 134.7(3) . . ? Si1 O Ce 100.33(13) . . ? Si1 C1 Si2 124.2(2) . . ? Si1 C1 Ce 95.33(15) . . ? Si2 C1 Ce 121.0(2) . . ? data_feb1202 _database_code_depnum_ccdc_archive 'CCDC 229454' _audit_creation_date 2004-02-16T09:35:21-00:00 _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_name_common '(Y(CH(SiMe3)2)3(NCtBu)2). 1/2(cyclohexane)' _chemical_formula_moiety '(C31 H75 N2 Si6 Y1), 0.5(C6 H12)' _chemical_formula_sum 'C34 H81 N2 Si6 Y' _chemical_formula_weight 775.46 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M R-3c _symmetry_Int_Tables_number 167 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-y, -x, z+1/2' '-x+y, -x, z' 'x, x-y, z+1/2' '-x+y, y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, -x+1/3, z+1/3' 'x+2/3, x-y+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, -x+2/3, z+2/3' 'x+1/3, x-y+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'y, x, -z-1/2' 'x-y, x, -z' '-x, -x+y, -z-1/2' 'x-y, -y, -z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'y+2/3, x+1/3, -z-1/6' 'x-y+2/3, x+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z-1/6' 'x-y+2/3, -y+1/3, -z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'y+1/3, x+2/3, -z+1/6' 'x-y+1/3, x+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+1/6' 'x-y+1/3, -y+2/3, -z+1/6' _cell_length_a 12.4967(4) _cell_length_b 12.4967(4) _cell_length_c 108.85(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 14722(5) _cell_formula_units_Z 12 _cell_measurement_temperature 173(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.05 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5064 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.356 _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 0.578 _exptl_absorpt_correction_T_max 0.628 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_unetI/netI 0.0533 _diffrn_reflns_number 21353 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -99 _diffrn_reflns_limit_l_max 99 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 22.98 _diffrn_reflns_theta_full 22.98 _diffrn_measured_fraction_theta_full 0.954 _diffrn_measured_fraction_theta_max 0.954 _reflns_number_total 2187 _reflns_number_gt 1684 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # 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^)+(0.0330P)^2^+47.3809P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 2187 _refine_ls_number_parameters 130 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.319 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.053 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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 Y Y 0 0 0.128053(6) 0.0259(2) Uani 1 3 d S . . Si1 Si -0.23924(10) -0.30161(10) 0.117472(10) 0.0364(3) Uani 1 1 d . . . Si2 Si -0.33300(10) -0.19191(10) 0.137902(10) 0.0378(3) Uani 1 1 d . . . N1 N 0 0 0.15056(6) 0.0336(13) Uani 1 3 d S . . N2 N 0 0 0.10556(6) 0.0385(14) Uani 1 3 d S . . C1 C 0 0 0.16093(7) 0.0316(16) Uani 1 3 d S . . C2 C 0 0 0.17458(6) 0.0361(16) Uani 1 3 d S . . C3 C -0.1093(4) -0.1226(4) 0.17892(4) 0.0559(13) Uani 1 1 d . . . H3C H -0.1188 -0.1199 0.1878 0.084 Uiso 1 1 calc R . . H3B H -0.0942 -0.1903 0.1769 0.084 Uiso 1 1 calc R . . H3A H -0.1849 -0.1362 0.1748 0.084 Uiso 1 1 calc R . . C4 C 0 0 0.09510(8) 0.0364(17) Uani 1 3 d S . . C5 C 0 0 0.08136(6) 0.0408(17) Uani 1 3 d S . . C6 C -0.0197(4) -0.1256(4) 0.07710(4) 0.0526(12) Uani 1 1 d . . . H6C H 0.0467 -0.1376 0.0803 0.079 Uiso 1 1 calc R . . H6B H -0.0189 -0.1279 0.0681 0.079 Uiso 1 1 calc R . . H6A H -0.0995 -0.1915 0.0801 0.079 Uiso 1 1 calc R . . C7 C -0.1994(3) -0.1862(3) 0.12992(3) 0.0321(9) Uani 1 1 d . . . H7 H -0.1767 -0.2284 0.1364 0.039 Uiso 1 1 calc R . . C8 C -0.0992(4) -0.3113(4) 0.11285(4) 0.0526(12) Uani 1 1 d . . . H8C H -0.123 -0.377 0.1067 0.079 Uiso 1 1 calc R . . H8B H -0.0647 -0.3299 0.1201 0.079 Uiso 1 1 calc R . . H8A H -0.0371 -0.2322 0.1093 0.079 Uiso 1 1 calc R . . C9 C -0.3003(4) -0.2640(4) 0.10329(4) 0.0471(11) Uani 1 1 d . . . H9C H -0.3731 -0.2577 0.1054 0.071 Uiso 1 1 calc R . . H9B H -0.3233 -0.3296 0.0972 0.071 Uiso 1 1 calc R . . H9A H -0.2363 -0.1852 0.0999 0.071 Uiso 1 1 calc R . . C10 C -0.3581(4) -0.4648(4) 0.12159(4) 0.0613(13) Uani 1 1 d . . . H10C H -0.4372 -0.4693 0.1233 0.092 Uiso 1 1 calc R . . H10B H -0.331 -0.4904 0.1289 0.092 Uiso 1 1 calc R . . H10A H -0.3679 -0.5198 0.1147 0.092 Uiso 1 1 calc R . . C11 C -0.4597(4) -0.2151(4) 0.12714(4) 0.0536(12) Uani 1 1 d . . . H11C H -0.5325 -0.2297 0.1319 0.08 Uiso 1 1 calc R . . H11B H -0.4812 -0.2865 0.1219 0.08 Uiso 1 1 calc R . . H11A H -0.4318 -0.1411 0.122 0.08 Uiso 1 1 calc R . . C12 C -0.4024(4) -0.3193(4) 0.14963(4) 0.0652(14) Uani 1 1 d . . . H12C H -0.3437 -0.3007 0.1564 0.098 Uiso 1 1 calc R . . H12B H -0.4209 -0.3976 0.1458 0.098 Uiso 1 1 calc R . . H12A H -0.4788 -0.3262 0.1529 0.098 Uiso 1 1 calc R . . C13 C -0.2969(4) -0.0483(4) 0.14674(4) 0.0510(12) Uani 1 1 d . . . H13C H -0.2683 0.0215 0.1411 0.077 Uiso 1 1 calc R . . H13B H -0.2322 -0.0309 0.1528 0.077 Uiso 1 1 calc R . . H13A H -0.3716 -0.0608 0.151 0.077 Uiso 1 1 calc R . . C1B C -0.7286(6) -0.2615(7) -0.08192(10) 0.173(4) Uani 1 1 d . . . H1B1 H -0.7688 -0.223 -0.0865 0.207 Uiso 1 1 calc R . . H1B2 H -0.7376 -0.2499 -0.0731 0.207 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 Y 0.0252(2) 0.0252(2) 0.0272(4) 0 0 0.01262(12) Si1 0.0340(7) 0.0303(6) 0.0412(7) -0.0035(5) -0.0079(6) 0.0133(5) Si2 0.0300(6) 0.0351(7) 0.0466(8) 0.0073(5) 0.0052(5) 0.0149(5) N1 0.037(2) 0.037(2) 0.027(4) 0 0 0.0185(11) N2 0.041(2) 0.041(2) 0.034(4) 0 0 0.0204(12) C1 0.027(2) 0.027(2) 0.040(5) 0 0 0.0137(12) C2 0.042(3) 0.042(3) 0.024(5) 0 0 0.0210(13) C3 0.058(3) 0.057(3) 0.045(3) 0.012(2) 0.011(2) 0.023(3) C4 0.028(3) 0.028(3) 0.053(6) 0 0 0.0141(13) C5 0.048(3) 0.048(3) 0.027(5) 0 0 0.0238(14) C6 0.059(3) 0.057(3) 0.042(3) -0.011(2) -0.002(2) 0.029(3) C7 0.028(2) 0.031(2) 0.034(2) 0.0041(18) 0.0001(18) 0.0129(18) C8 0.054(3) 0.053(3) 0.056(3) -0.013(2) -0.012(2) 0.031(2) C9 0.040(3) 0.050(3) 0.044(3) -0.002(2) -0.010(2) 0.016(2) C10 0.068(3) 0.035(3) 0.064(3) 0.000(2) -0.007(3) 0.013(2) C11 0.031(2) 0.048(3) 0.076(3) 0.005(2) 0.000(2) 0.015(2) C12 0.070(3) 0.059(3) 0.063(3) 0.022(3) 0.023(3) 0.030(3) C13 0.036(2) 0.061(3) 0.058(3) -0.001(2) 0.008(2) 0.026(2) C1B 0.161(8) 0.215(10) 0.132(6) 0.003(10) 0.006(9) 0.087(7) #----------------------------------------------------------------------------# # 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 Y C7 2.422(3) 4 ? Y C7 2.422(4) . ? Y C7 2.422(3) 2 ? Y N2 2.449(7) . ? Y N1 2.450(6) . ? Si1 C7 1.856(4) . ? Si1 C10 1.881(4) . ? Si1 C8 1.882(4) . ? Si1 C9 1.883(4) . ? Si2 C7 1.851(4) . ? Si2 C11 1.872(4) . ? Si2 C12 1.880(4) . ? Si2 C13 1.881(4) . ? N1 C1 1.129(8) . ? N2 C4 1.138(8) . ? C1 C2 1.485(10) . ? C2 C3 1.531(4) . ? C4 C5 1.496(11) . ? C5 C6 1.533(4) . ? C1B C1B 1.375(14) 29_345 ? C1B C1B 1.584(16) 30_445 ? 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 C7 Y C7 119.31(3) 4 . ? C7 Y N2 94.81(9) . . ? C7 Y N1 85.19(9) . . ? N2 Y N1 180 . . ? C7 Si1 C10 115.38(19) . . ? C7 Si1 C8 110.41(17) . . ? C10 Si1 C8 104.4(2) . . ? C7 Si1 C9 112.89(18) . . ? C10 Si1 C9 105.5(2) . . ? C8 Si1 C9 107.61(19) . . ? C7 Si2 C11 112.88(19) . . ? C7 Si2 C12 112.11(19) . . ? C11 Si2 C12 107.3(2) . . ? C7 Si2 C13 114.94(17) . . ? C11 Si2 C13 104.36(19) . . ? C12 Si2 C13 104.5(2) . . ? C1 N1 Y 180 . . ? C4 N2 Y 180 . . ? N1 C1 C2 180 . . ? C1 C2 C3 108.0(3) . . ? C3 C2 C3 110.9(3) 4 . ? N2 C4 C5 180 . . ? C4 C5 C6 107.6(3) . . ? C6 C5 C6 111.3(3) 4 . ? Si2 C7 Si1 115.23(19) . . ? Si2 C7 Y 123.47(17) . . ? Si1 C7 Y 115.63(17) . . ? C1B C1B C1B 115.8(6) 29_345 30_445 ? #===END #===END data_(6)-oct1701 _database_code_depnum_ccdc_archive 'CCDC 229455' _audit_creation_date 2001-10-23T09:19:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[Ce{CH(SiMe3)2}3(NCPh)]' _chemical_formula_moiety 'C28 H62 Ce1 N1 Si6' _chemical_formula_sum 'C28 H62 Ce N Si6' _chemical_formula_weight 721.45 _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 12.1618(4) _cell_length_b 12.8020(4) _cell_length_c 27.1173(9) _cell_angle_alpha 79.606(2) _cell_angle_beta 84.609(2) _cell_angle_gamma 80.598(2) _cell_volume 4087.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 89039 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1516 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.305 _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 0.586 _exptl_absorpt_correction_T_max 0.656 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 26858 _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_unetI/netI 0.087 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 27.93 _diffrn_reflns_theta_full 27.93 _diffrn_measured_fraction_theta_full 0.939 _diffrn_measured_fraction_theta_max 0.939 _reflns_number_total 18393 _reflns_number_gt 13040 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The phenyl groups were included as rigid bodies of idealised geometry. 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^)+(0.0568P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 18393 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1283 _refine_ls_wR_factor_gt 0.1141 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.953 _refine_diff_density_min -0.958 _refine_diff_density_rms 0.109 #----------------------------------------------------------------------------# # 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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 Ce Ce 0.021348(19) 0.746946(18) 0.344438(9) 0.03274(7) Uani 1 1 d . A 1 Si1 Si -0.23621(10) 0.61153(10) 0.36476(5) 0.0405(3) Uani 1 1 d . A 1 Si2 Si -0.00111(11) 0.47582(10) 0.34518(5) 0.0402(3) Uani 1 1 d . A 1 Si3 Si 0.24905(12) 0.64578(12) 0.44227(6) 0.0546(4) Uani 1 1 d . A 1 Si4 Si 0.28833(11) 0.81143(11) 0.34209(5) 0.0453(3) Uani 1 1 d . A 1 Si5 Si -0.10968(12) 0.93834(10) 0.42354(5) 0.0452(3) Uani 1 1 d . A 1 Si6 Si -0.16587(11) 1.01537(10) 0.31020(5) 0.0417(3) Uani 1 1 d . A 1 N N 0.0412(4) 0.7359(3) 0.24888(15) 0.0550(11) Uani 1 1 d . A 1 C1 C -0.0841(3) 0.5920(3) 0.37028(16) 0.0363(9) Uani 1 1 d . A 1 H1 H -0.0763 0.5727 0.4073 0.044 Uiso 1 1 calc R A 1 C2 C 0.1915(4) 0.7442(4) 0.38906(16) 0.0430(11) Uani 1 1 d . A 1 H2 H 0.1634 0.8053 0.4075 0.052 Uiso 1 1 calc R A 1 C3 C -0.1173(3) 0.9053(3) 0.36048(15) 0.0353(9) Uani 1 1 d . A 1 H3 H -0.1859 0.87 0.3671 0.042 Uiso 1 1 calc R A 1 C4 C -0.3134(4) 0.6842(4) 0.41451(19) 0.0560(13) Uani 1 1 d . A 1 H4A H -0.3938 0.6934 0.4105 0.084 Uiso 1 1 calc R A 1 H4B H -0.2896 0.7547 0.4114 0.084 Uiso 1 1 calc R A 1 H4C H -0.2972 0.6424 0.4477 0.084 Uiso 1 1 calc R A 1 C5 C -0.2727(4) 0.6927(4) 0.30212(19) 0.0592(14) Uani 1 1 d . A 1 H5A H -0.3537 0.7024 0.2997 0.089 Uiso 1 1 calc R A 1 H5B H -0.2353 0.655 0.2753 0.089 Uiso 1 1 calc R A 1 H5C H -0.2481 0.763 0.2986 0.089 Uiso 1 1 calc R A 1 C6 C -0.2995(4) 0.4834(4) 0.3717(2) 0.0580(14) Uani 1 1 d . A 1 H6A H -0.3801 0.5013 0.3681 0.087 Uiso 1 1 calc R A 1 H6B H -0.2857 0.4404 0.4049 0.087 Uiso 1 1 calc R A 1 H6C H -0.2653 0.4421 0.3456 0.087 Uiso 1 1 calc R A 1 C7 C -0.0472(5) 0.4595(4) 0.28296(18) 0.0598(14) Uani 1 1 d . A 1 H7A H -0.0008 0.3973 0.2714 0.09 Uiso 1 1 calc R A 1 H7B H -0.0391 0.5243 0.2583 0.09 Uiso 1 1 calc R A 1 H7C H -0.1256 0.4483 0.2869 0.09 Uiso 1 1 calc R A 1 C8 C 0.1494(4) 0.4941(4) 0.33252(19) 0.0542(13) Uani 1 1 d . A 1 H8A H 0.1915 0.4319 0.3192 0.081 Uiso 1 1 calc R A 1 H8B H 0.18 0.5004 0.3638 0.081 Uiso 1 1 calc R A 1 H8C H 0.1553 0.5594 0.3079 0.081 Uiso 1 1 calc R A 1 C9 C -0.0013(5) 0.3447(4) 0.3888(2) 0.0596(14) Uani 1 1 d . A 1 H9A H 0.0439 0.2873 0.373 0.089 Uiso 1 1 calc R A 1 H9B H -0.0781 0.3293 0.3959 0.089 Uiso 1 1 calc R A 1 H9C H 0.0302 0.3486 0.4202 0.089 Uiso 1 1 calc R A 1 C10 C 0.1482(4) 0.5544(4) 0.47368(19) 0.0571(14) Uani 1 1 d . A 1 H10A H 0.1833 0.5039 0.5014 0.086 Uiso 1 1 calc R A 1 H10B H 0.1275 0.5144 0.4492 0.086 Uiso 1 1 calc R A 1 H10C H 0.0812 0.5971 0.4868 0.086 Uiso 1 1 calc R A 1 C11 C 0.2853(8) 0.7164(7) 0.4917(3) 0.132(4) Uani 1 1 d . A 1 H11A H 0.3158 0.6632 0.5197 0.198 Uiso 1 1 calc R A 1 H11B H 0.218 0.7602 0.5039 0.198 Uiso 1 1 calc R A 1 H11C H 0.3411 0.7627 0.4775 0.198 Uiso 1 1 calc R A 1 C12 C 0.3774(5) 0.5548(5) 0.4223(3) 0.109(3) Uani 1 1 d . A 1 H12A H 0.4049 0.5039 0.4517 0.163 Uiso 1 1 calc R A 1 H12B H 0.4355 0.598 0.4076 0.163 Uiso 1 1 calc R A 1 H12C H 0.3585 0.5151 0.3974 0.163 Uiso 1 1 calc R A 1 C13 C 0.3742(6) 0.7174(5) 0.3031(3) 0.093(2) Uani 1 1 d . A 1 H13A H 0.424 0.7568 0.2788 0.139 Uiso 1 1 calc R A 1 H13B H 0.3248 0.6863 0.2851 0.139 Uiso 1 1 calc R A 1 H13C H 0.4188 0.6598 0.3249 0.139 Uiso 1 1 calc R A 1 C14 C 0.2020(5) 0.9148(5) 0.2964(2) 0.0758(19) Uani 1 1 d . A 1 H14A H 0.2517 0.9513 0.2709 0.114 Uiso 1 1 calc R A 1 H14B H 0.1558 0.9677 0.3146 0.114 Uiso 1 1 calc R A 1 H14C H 0.1537 0.8791 0.2801 0.114 Uiso 1 1 calc R A 1 C15 C 0.3843(5) 0.8864(5) 0.3665(3) 0.085(2) Uani 1 1 d . A 1 H15A H 0.432 0.9183 0.3385 0.128 Uiso 1 1 calc R A 1 H15B H 0.431 0.837 0.3908 0.128 Uiso 1 1 calc R A 1 H15C H 0.3405 0.9433 0.3829 0.128 Uiso 1 1 calc R A 1 C16 C -0.0805(4) 0.8094(4) 0.46939(17) 0.0515(13) Uani 1 1 d . A 1 H16A H -0.0759 0.8259 0.503 0.077 Uiso 1 1 calc R A 1 H16B H -0.0096 0.7684 0.4589 0.077 Uiso 1 1 calc R A 1 H16C H -0.1409 0.7669 0.4701 0.077 Uiso 1 1 calc R A 1 C17 C 0.0056(5) 1.0180(4) 0.4255(2) 0.0644(15) Uani 1 1 d . A 1 H17A H 0.0066 1.0335 0.4596 0.097 Uiso 1 1 calc R A 1 H17B H -0.0069 1.0856 0.4018 0.097 Uiso 1 1 calc R A 1 H17C H 0.0773 0.9765 0.4163 0.097 Uiso 1 1 calc R A 1 C18 C -0.2422(6) 1.0130(5) 0.4492(2) 0.084(2) Uani 1 1 d . A 1 H18A H -0.2311 1.0275 0.4826 0.126 Uiso 1 1 calc R A 1 H18B H -0.3024 0.9694 0.4519 0.126 Uiso 1 1 calc R A 1 H18C H -0.2623 1.0811 0.4266 0.126 Uiso 1 1 calc R A 1 C19 C -0.1134(5) 0.9876(5) 0.24566(17) 0.0652(16) Uani 1 1 d . A 1 H19A H -0.1413 1.0488 0.2204 0.098 Uiso 1 1 calc R A 1 H19B H -0.1401 0.923 0.2398 0.098 Uiso 1 1 calc R A 1 H19C H -0.0316 0.9766 0.2431 0.098 Uiso 1 1 calc R A 1 C20 C -0.3219(4) 1.0355(5) 0.3100(2) 0.0719(17) Uani 1 1 d . A 1 H20A H -0.3464 1.0946 0.2831 0.108 Uiso 1 1 calc R A 1 H20B H -0.3549 1.0529 0.3425 0.108 Uiso 1 1 calc R A 1 H20C H -0.3461 0.9695 0.3043 0.108 Uiso 1 1 calc R A 1 C21 C -0.1211(6) 1.1465(4) 0.3152(2) 0.0779(19) Uani 1 1 d . A 1 H21A H -0.1493 1.2018 0.2875 0.117 Uiso 1 1 calc R A 1 H21B H -0.0393 1.1382 0.3135 0.117 Uiso 1 1 calc R A 1 H21C H -0.1512 1.168 0.3473 0.117 Uiso 1 1 calc R A 1 C22 C 0.0344(4) 0.7351(4) 0.20705(19) 0.0468(11) Uani 1 1 d . A 1 C23 C 0.0259(3) 0.7352(3) 0.15554(8) 0.0425(11) Uani 1 1 d G A 1 C24 C 0.0437(3) 0.8244(2) 0.11981(13) 0.0627(15) Uani 1 1 d G A 1 H24 H 0.0623 0.8863 0.1299 0.075 Uiso 1 1 calc R A 1 C25 C 0.0343(3) 0.8231(3) 0.06924(11) 0.0698(18) Uani 1 1 d G A 1 H25 H 0.0465 0.8841 0.0448 0.084 Uiso 1 1 calc R A 1 C26 C 0.0071(3) 0.7326(3) 0.05440(8) 0.0660(16) Uani 1 1 d G A 1 H26 H 0.0007 0.7317 0.0198 0.079 Uiso 1 1 calc R A 1 C27 C -0.0107(3) 0.6434(3) 0.09014(12) 0.0739(18) Uani 1 1 d G A 1 H27 H -0.0293 0.5816 0.08 0.089 Uiso 1 1 calc R A 1 C28 C -0.0014(3) 0.6447(2) 0.14071(11) 0.0624(15) Uani 1 1 d G A 1 H28 H -0.0136 0.5838 0.1651 0.075 Uiso 1 1 calc R A 1 Ce1A Ce -0.460467(19) 0.729538(18) -0.144772(9) 0.03337(7) Uani 1 1 d . B 2 Si1A Si -0.62480(10) 0.54884(10) -0.18221(4) 0.0378(3) Uani 1 1 d . B 2 Si2A Si -0.39241(10) 0.43514(9) -0.14572(4) 0.0362(3) Uani 1 1 d . B 2 Si3A Si -0.27423(11) 0.69102(11) -0.04457(5) 0.0461(3) Uani 1 1 d . B 2 Si4A Si -0.15832(11) 0.77779(12) -0.15146(6) 0.0530(4) Uani 1 1 d . B 2 Si5A Si -0.57379(11) 0.99834(9) -0.13364(5) 0.0399(3) Uani 1 1 d . B 2 Si6A Si -0.71999(10) 0.83608(10) -0.06500(5) 0.0398(3) Uani 1 1 d . B 2 N1A N -0.4403(3) 0.7558(3) -0.24257(16) 0.0503(10) Uani 1 1 d . B 2 C1A C -0.5090(3) 0.5456(3) -0.14221(14) 0.0320(9) Uani 1 1 d . B 2 H1A H -0.5434 0.5277 -0.1074 0.038 Uiso 1 1 calc R B 2 C2A C -0.2708(4) 0.7158(4) -0.11422(17) 0.0469(11) Uani 1 1 d . B 2 H2A H -0.2431 0.6402 -0.1192 0.056 Uiso 1 1 calc R B 2 C3A C -0.6175(4) 0.8639(3) -0.11825(16) 0.0389(10) Uani 1 1 d . B 2 H3A H -0.6667 0.8696 -0.1465 0.047 Uiso 1 1 calc R B 2 C4A C -0.7103(4) 0.6857(4) -0.19706(18) 0.0484(12) Uani 1 1 d . B 2 H4A1 H -0.77 0.6823 -0.2183 0.073 Uiso 1 1 calc R B 2 H4A2 H -0.6623 0.7368 -0.2148 0.073 Uiso 1 1 calc R B 2 H4A3 H -0.7431 0.7093 -0.1658 0.073 Uiso 1 1 calc R B 2 C5A C -0.7285(4) 0.4589(4) -0.1526(2) 0.0622(15) Uani 1 1 d . B 2 H5A1 H -0.7876 0.4641 -0.1755 0.093 Uiso 1 1 calc R B 2 H5A2 H -0.7613 0.4811 -0.121 0.093 Uiso 1 1 calc R B 2 H5A3 H -0.6908 0.3846 -0.1459 0.093 Uiso 1 1 calc R B 2 C6A C -0.5748(5) 0.5113(4) -0.24555(18) 0.0609(14) Uani 1 1 d . B 2 H6A1 H -0.6392 0.5143 -0.2652 0.091 Uiso 1 1 calc R B 2 H6A2 H -0.5332 0.4382 -0.241 0.091 Uiso 1 1 calc R B 2 H6A3 H -0.526 0.5616 -0.2634 0.091 Uiso 1 1 calc R B 2 C7A C -0.4323(5) 0.3027(4) -0.1525(2) 0.0686(16) Uani 1 1 d . B 2 H7A1 H -0.3648 0.2495 -0.1541 0.103 Uiso 1 1 calc R B 2 H7A2 H -0.4711 0.3115 -0.1834 0.103 Uiso 1 1 calc R B 2 H7A3 H -0.4817 0.2782 -0.1236 0.103 Uiso 1 1 calc R B 2 C8A C -0.3149(4) 0.4035(4) -0.08752(17) 0.0508(12) Uani 1 1 d . B 2 H8A1 H -0.2535 0.3446 -0.0906 0.076 Uiso 1 1 calc R B 2 H8A2 H -0.3658 0.3822 -0.0586 0.076 Uiso 1 1 calc R B 2 H8A3 H -0.2847 0.4672 -0.0828 0.076 Uiso 1 1 calc R B 2 C9A C -0.2935(4) 0.4732(4) -0.20012(19) 0.0559(13) Uani 1 1 d . B 2 H9A1 H -0.2316 0.4142 -0.2019 0.084 Uiso 1 1 calc R B 2 H9A2 H -0.2642 0.5378 -0.1959 0.084 Uiso 1 1 calc R B 2 H9A3 H -0.3326 0.4878 -0.2312 0.084 Uiso 1 1 calc R B 2 C10A C -0.4144(4) 0.6505(5) -0.0197(2) 0.0713(17) Uani 1 1 d . B 2 H10D H -0.4185 0.6375 0.0171 0.107 Uiso 1 1 calc R B 2 H10E H -0.4232 0.5847 -0.0317 0.107 Uiso 1 1 calc R B 2 H10F H -0.4741 0.7082 -0.0316 0.107 Uiso 1 1 calc R B 2 C11A C -0.2557(6) 0.8095(5) -0.0169(3) 0.089(2) Uani 1 1 d . B 2 H11D H -0.2587 0.7905 0.0198 0.134 Uiso 1 1 calc R B 2 H11E H -0.3155 0.8689 -0.0268 0.134 Uiso 1 1 calc R B 2 H11F H -0.1832 0.8316 -0.0292 0.134 Uiso 1 1 calc R B 2 C12A C -0.1652(4) 0.5796(4) -0.01710(19) 0.0543(13) Uani 1 1 d . B 2 H12D H -0.1724 0.5719 0.0196 0.081 Uiso 1 1 calc R B 2 H12E H -0.0908 0.5966 -0.0295 0.081 Uiso 1 1 calc R B 2 H12F H -0.1757 0.5122 -0.0271 0.081 Uiso 1 1 calc R B 2 C13A C -0.0158(5) 0.7011(6) -0.1394(3) 0.108(3) Uani 1 1 d . B 2 H13D H 0.0405 0.7387 -0.1603 0.161 Uiso 1 1 calc R B 2 H13E H -0.0112 0.6289 -0.1476 0.161 Uiso 1 1 calc R B 2 H13F H -0.0023 0.6954 -0.1038 0.161 Uiso 1 1 calc R B 2 C14A C -0.1572(5) 0.9194(5) -0.1425(3) 0.085(2) Uani 1 1 d . B 2 H14D H -0.0954 0.9483 -0.1636 0.127 Uiso 1 1 calc R B 2 H14E H -0.1474 0.9205 -0.1072 0.127 Uiso 1 1 calc R B 2 H14F H -0.2281 0.9635 -0.1522 0.127 Uiso 1 1 calc R B 2 C15A C -0.1746(5) 0.7851(5) -0.2200(2) 0.0691(17) Uani 1 1 d . B 2 H15D H -0.1143 0.8192 -0.2397 0.104 Uiso 1 1 calc R B 2 H15E H -0.2468 0.8275 -0.2289 0.104 Uiso 1 1 calc R B 2 H15F H -0.1712 0.7124 -0.2273 0.104 Uiso 1 1 calc R B 2 C16A C -0.4936(5) 1.0262(4) -0.0841(2) 0.0665(16) Uani 1 1 d . B 2 H16D H -0.4722 1.0981 -0.0938 0.1 Uiso 1 1 calc R B 2 H16E H -0.4263 0.9726 -0.0798 0.1 Uiso 1 1 calc R B 2 H16F H -0.5399 1.0228 -0.0524 0.1 Uiso 1 1 calc R B 2 C17A C -0.4755(5) 1.0014(5) -0.1917(2) 0.0717(17) Uani 1 1 d . B 2 H17D H -0.4508 1.072 -0.2005 0.107 Uiso 1 1 calc R B 2 H17E H -0.514 0.988 -0.2196 0.107 Uiso 1 1 calc R B 2 H17F H -0.4104 0.9458 -0.1853 0.107 Uiso 1 1 calc R B 2 C18A C -0.6889(5) 1.1136(4) -0.1476(3) 0.0767(19) Uani 1 1 d . B 2 H18D H -0.6575 1.181 -0.1551 0.115 Uiso 1 1 calc R B 2 H18E H -0.7427 1.1152 -0.1184 0.115 Uiso 1 1 calc R B 2 H18F H -0.7267 1.105 -0.1767 0.115 Uiso 1 1 calc R B 2 C19A C -0.7350(4) 0.6899(4) -0.05027(17) 0.0465(11) Uani 1 1 d . B 2 H19D H -0.7897 0.678 -0.0217 0.07 Uiso 1 1 calc R B 2 H19E H -0.6627 0.6473 -0.0418 0.07 Uiso 1 1 calc R B 2 H19F H -0.7604 0.6682 -0.0796 0.07 Uiso 1 1 calc R B 2 C20A C -0.6835(5) 0.8750(4) -0.00585(19) 0.0612(14) Uani 1 1 d . B 2 H20D H -0.7407 0.8583 0.0211 0.092 Uiso 1 1 calc R B 2 H20E H -0.6798 0.9522 -0.0116 0.092 Uiso 1 1 calc R B 2 H20F H -0.6108 0.8349 0.0039 0.092 Uiso 1 1 calc R B 2 C21A C -0.8643(4) 0.9093(5) -0.0787(2) 0.0741(19) Uani 1 1 d . B 2 H21D H -0.9162 0.8928 -0.0495 0.111 Uiso 1 1 calc R B 2 H21E H -0.8893 0.8864 -0.1079 0.111 Uiso 1 1 calc R B 2 H21F H -0.8625 0.9869 -0.086 0.111 Uiso 1 1 calc R B 2 C22A C -0.4293(4) 0.7609(4) -0.28538(18) 0.0425(11) Uani 1 1 d . B 2 C23A C -0.4135(3) 0.7664(3) -0.33766(10) 0.0509(13) Uani 1 1 d G B 2 C24A C -0.3204(3) 0.8065(3) -0.36289(15) 0.0724(17) Uani 1 1 d G B 2 H24A H -0.2676 0.8283 -0.3447 0.087 Uiso 1 1 calc R B 2 C25A C -0.3045(4) 0.8146(3) -0.41480(15) 0.101(3) Uani 1 1 d G B 2 H25A H -0.2408 0.842 -0.432 0.122 Uiso 1 1 calc R B 2 C26A C -0.3817(5) 0.7827(4) -0.44147(10) 0.111(3) Uani 1 1 d G B 2 H26A H -0.3708 0.7883 -0.4769 0.133 Uiso 1 1 calc R B 2 C27A C -0.4748(4) 0.7426(4) -0.41624(15) 0.099(3) Uani 1 1 d G B 2 H27A H -0.5276 0.7208 -0.4345 0.119 Uiso 1 1 calc R B 2 C28A C -0.4907(3) 0.7345(3) -0.36433(15) 0.0735(17) Uani 1 1 d G B 2 H28A H -0.5544 0.7071 -0.3471 0.088 Uiso 1 1 calc R B 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 Ce 0.03169(13) 0.03165(13) 0.03559(13) -0.00621(10) -0.00410(10) -0.00515(9) Si1 0.0335(6) 0.0443(7) 0.0448(7) -0.0029(6) -0.0092(5) -0.0103(5) Si2 0.0439(7) 0.0343(6) 0.0419(7) -0.0052(5) -0.0023(6) -0.0065(5) Si3 0.0529(9) 0.0543(8) 0.0559(8) 0.0083(7) -0.0228(7) -0.0148(7) Si4 0.0343(7) 0.0490(7) 0.0515(8) -0.0028(6) 0.0001(6) -0.0111(5) Si5 0.0574(8) 0.0398(7) 0.0360(6) -0.0072(5) -0.0025(6) -0.0002(6) Si6 0.0443(7) 0.0363(6) 0.0424(7) -0.0014(5) -0.0119(6) -0.0007(5) N 0.058(3) 0.060(3) 0.046(2) -0.013(2) -0.003(2) 0.000(2) C1 0.036(2) 0.038(2) 0.036(2) -0.0060(18) -0.0044(18) -0.0036(17) C2 0.039(2) 0.048(3) 0.041(2) -0.004(2) -0.009(2) -0.005(2) C3 0.039(2) 0.029(2) 0.037(2) -0.0015(17) -0.0060(18) -0.0041(17) C4 0.033(3) 0.063(3) 0.070(3) -0.011(3) 0.006(2) -0.006(2) C5 0.059(3) 0.058(3) 0.062(3) 0.000(3) -0.023(3) -0.015(3) C6 0.051(3) 0.062(3) 0.066(3) -0.002(3) -0.010(3) -0.025(2) C7 0.084(4) 0.055(3) 0.047(3) -0.020(2) -0.006(3) -0.015(3) C8 0.051(3) 0.053(3) 0.055(3) -0.015(2) 0.004(2) 0.004(2) C9 0.065(4) 0.037(3) 0.071(4) -0.001(2) -0.001(3) -0.003(2) C10 0.059(3) 0.053(3) 0.053(3) 0.013(2) -0.010(2) -0.013(2) C11 0.227(10) 0.114(6) 0.076(5) 0.020(4) -0.072(6) -0.092(7) C12 0.044(3) 0.083(5) 0.170(7) 0.048(5) -0.015(4) 0.004(3) C13 0.086(5) 0.091(5) 0.094(5) -0.018(4) 0.044(4) -0.021(4) C14 0.065(4) 0.080(4) 0.069(4) 0.028(3) -0.001(3) -0.018(3) C15 0.077(5) 0.069(4) 0.114(5) 0.004(4) -0.027(4) -0.032(3) C16 0.055(3) 0.054(3) 0.041(3) 0.002(2) 0.000(2) -0.007(2) C17 0.101(5) 0.052(3) 0.049(3) -0.012(2) -0.019(3) -0.023(3) C18 0.089(5) 0.087(4) 0.063(4) -0.019(3) 0.008(3) 0.025(4) C19 0.073(4) 0.075(4) 0.041(3) -0.002(3) -0.012(3) 0.006(3) C20 0.052(3) 0.070(4) 0.085(4) 0.000(3) -0.021(3) 0.012(3) C21 0.126(6) 0.038(3) 0.070(4) 0.013(3) -0.037(4) -0.021(3) C22 0.042(3) 0.047(3) 0.049(3) -0.007(2) 0.000(2) 0.000(2) C23 0.031(2) 0.053(3) 0.041(2) -0.008(2) -0.0050(19) 0.002(2) C24 0.076(4) 0.044(3) 0.059(3) -0.003(3) -0.006(3) 0.012(3) C25 0.072(4) 0.076(4) 0.046(3) 0.004(3) -0.003(3) 0.018(3) C26 0.045(3) 0.109(5) 0.041(3) -0.007(3) -0.007(2) -0.009(3) C27 0.066(4) 0.117(5) 0.055(3) -0.031(3) 0.000(3) -0.044(4) C28 0.063(4) 0.093(4) 0.041(3) -0.009(3) -0.005(2) -0.041(3) Ce1A 0.02924(13) 0.03378(13) 0.03992(14) -0.01076(10) -0.00578(10) -0.00595(9) Si1A 0.0325(6) 0.0447(7) 0.0398(6) -0.0080(5) -0.0078(5) -0.0119(5) Si2A 0.0404(7) 0.0294(6) 0.0385(6) -0.0048(5) -0.0055(5) -0.0032(5) Si3A 0.0385(7) 0.0483(7) 0.0542(8) -0.0170(6) -0.0139(6) 0.0011(6) Si4A 0.0339(7) 0.0543(8) 0.0736(10) -0.0117(7) -0.0020(7) -0.0149(6) Si5A 0.0444(7) 0.0296(6) 0.0458(7) -0.0026(5) -0.0094(6) -0.0066(5) Si6A 0.0369(7) 0.0374(6) 0.0435(7) -0.0051(5) -0.0006(5) -0.0036(5) N1A 0.045(2) 0.053(2) 0.052(3) -0.007(2) 0.001(2) -0.0107(19) C1A 0.027(2) 0.039(2) 0.030(2) -0.0047(17) -0.0033(16) -0.0044(16) C2A 0.036(2) 0.053(3) 0.053(3) -0.005(2) -0.009(2) -0.009(2) C3A 0.039(2) 0.036(2) 0.041(2) -0.0033(19) -0.0033(19) -0.0057(18) C4A 0.036(2) 0.058(3) 0.050(3) -0.002(2) -0.015(2) -0.006(2) C5A 0.047(3) 0.063(3) 0.081(4) -0.010(3) -0.001(3) -0.027(3) C6A 0.068(4) 0.072(4) 0.048(3) -0.020(3) -0.020(3) -0.009(3) C7A 0.083(4) 0.039(3) 0.089(4) -0.016(3) -0.019(3) -0.009(3) C8A 0.049(3) 0.047(3) 0.052(3) -0.004(2) -0.009(2) 0.005(2) C9A 0.050(3) 0.055(3) 0.059(3) -0.013(3) 0.003(2) 0.003(2) C10A 0.046(3) 0.105(5) 0.061(3) -0.018(3) 0.006(3) -0.005(3) C11A 0.096(5) 0.077(4) 0.105(5) -0.044(4) -0.056(4) 0.015(4) C12A 0.049(3) 0.053(3) 0.063(3) -0.015(3) -0.017(2) -0.002(2) C13A 0.037(3) 0.118(6) 0.149(7) 0.011(5) 0.003(4) 0.003(4) C14A 0.083(5) 0.061(4) 0.121(6) -0.019(4) -0.002(4) -0.042(3) C15A 0.060(4) 0.072(4) 0.071(4) -0.001(3) 0.014(3) -0.022(3) C16A 0.079(4) 0.059(3) 0.070(4) -0.002(3) -0.025(3) -0.032(3) C17A 0.088(5) 0.068(4) 0.064(4) -0.006(3) 0.010(3) -0.040(3) C18A 0.068(4) 0.040(3) 0.118(5) 0.002(3) -0.029(4) 0.000(3) C19A 0.050(3) 0.047(3) 0.043(3) -0.003(2) -0.001(2) -0.016(2) C20A 0.075(4) 0.056(3) 0.057(3) -0.022(3) 0.006(3) -0.015(3) C21A 0.048(3) 0.075(4) 0.081(4) 0.017(3) 0.004(3) 0.008(3) C22A 0.034(2) 0.042(2) 0.049(3) -0.008(2) 0.003(2) -0.0025(19) C23A 0.056(3) 0.049(3) 0.042(3) -0.008(2) 0.004(2) 0.007(2) C24A 0.070(4) 0.074(4) 0.067(4) -0.004(3) 0.011(3) -0.009(3) C25A 0.105(6) 0.119(6) 0.060(4) 0.002(4) 0.033(4) 0.006(5) C26A 0.163(9) 0.097(6) 0.057(4) -0.004(4) 0.010(5) 0.008(6) C27A 0.150(8) 0.092(5) 0.061(4) -0.021(4) -0.034(4) -0.011(5) C28A 0.093(5) 0.075(4) 0.055(3) -0.011(3) -0.006(3) -0.018(3) #----------------------------------------------------------------------------# # 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 Ce C2 2.486(5) . ? Ce C3 2.491(4) . ? Ce C1 2.497(4) . ? Ce N 2.607(4) . ? Si1 C1 1.842(4) . ? Si1 C4 1.870(5) . ? Si1 C5 1.875(5) . ? Si1 C6 1.896(5) . ? Si2 C1 1.854(4) . ? Si2 C9 1.871(4) . ? Si2 C8 1.875(5) . ? Si2 C7 1.884(5) . ? Si3 C2 1.845(4) . ? Si3 C11 1.867(7) . ? Si3 C10 1.874(5) . ? Si3 C12 1.887(6) . ? Si4 C2 1.844(4) . ? Si4 C15 1.860(6) . ? Si4 C13 1.870(6) . ? Si4 C14 1.895(5) . ? Si5 C3 1.848(4) . ? Si5 C17 1.873(6) . ? Si5 C18 1.877(5) . ? Si5 C16 1.883(4) . ? Si6 C3 1.838(4) . ? Si6 C20 1.874(5) . ? Si6 C21 1.879(6) . ? Si6 C19 1.881(5) . ? N C22 1.147(6) . ? C22 C23 1.410(5) . ? C23 C24 1.39 . ? C23 C28 1.39 . ? C24 C25 1.39 . ? C25 C26 1.39 . ? C26 C27 1.39 . ? C27 C28 1.39 . ? Ce1A C2A 2.492(4) . ? Ce1A C3A 2.498(4) . ? Ce1A C1A 2.506(4) . ? Ce1A N1A 2.606(4) . ? Si1A C1A 1.848(4) . ? Si1A C5A 1.873(5) . ? Si1A C4A 1.882(4) . ? Si1A C6A 1.886(5) . ? Si2A C1A 1.840(4) . ? Si2A C9A 1.860(5) . ? Si2A C8A 1.862(5) . ? Si2A C7A 1.882(5) . ? Si3A C2A 1.856(5) . ? Si3A C11A 1.862(6) . ? Si3A C12A 1.879(5) . ? Si3A C10A 1.891(5) . ? Si4A C2A 1.824(5) . ? Si4A C15A 1.871(6) . ? Si4A C13A 1.874(6) . ? Si4A C14A 1.874(6) . ? Si5A C16A 1.848(5) . ? Si5A C3A 1.849(4) . ? Si5A C18A 1.872(5) . ? Si5A C17A 1.885(5) . ? Si6A C3A 1.840(4) . ? Si6A C20A 1.874(5) . ? Si6A C19A 1.877(4) . ? Si6A C21A 1.886(5) . ? N1A C22A 1.147(6) . ? C22A C23A 1.403(5) . ? C23A C24A 1.39 . ? C23A C28A 1.39 . ? C24A C25A 1.39 . ? C25A C26A 1.39 . ? C26A C27A 1.39 . ? C27A C28A 1.39 . ? 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 C2 Ce C3 108.90(15) . . ? C2 Ce C1 117.31(13) . . ? C3 Ce C1 103.93(13) . . ? C2 Ce N 119.27(14) . . ? C3 Ce N 110.18(13) . . ? C1 Ce N 95.80(14) . . ? C1 Si1 C4 111.5(2) . . ? C1 Si1 C5 110.3(2) . . ? C4 Si1 C5 107.9(2) . . ? C1 Si1 C6 115.1(2) . . ? C4 Si1 C6 104.7(2) . . ? C5 Si1 C6 107.0(2) . . ? C1 Si2 C9 114.1(2) . . ? C1 Si2 C8 110.9(2) . . ? C9 Si2 C8 105.7(2) . . ? C1 Si2 C7 112.7(2) . . ? C9 Si2 C7 107.9(2) . . ? C8 Si2 C7 104.9(2) . . ? C2 Si3 C11 110.3(3) . . ? C2 Si3 C10 113.1(2) . . ? C11 Si3 C10 106.4(3) . . ? C2 Si3 C12 112.3(3) . . ? C11 Si3 C12 108.8(4) . . ? C10 Si3 C12 105.6(3) . . ? C2 Si4 C15 116.3(3) . . ? C2 Si4 C13 112.6(3) . . ? C15 Si4 C13 108.1(3) . . ? C2 Si4 C14 108.0(2) . . ? C15 Si4 C14 105.6(3) . . ? C13 Si4 C14 105.5(3) . . ? C3 Si5 C17 112.2(2) . . ? C3 Si5 C18 114.6(3) . . ? C17 Si5 C18 107.8(3) . . ? C3 Si5 C16 108.7(2) . . ? C17 Si5 C16 107.5(2) . . ? C18 Si5 C16 105.6(2) . . ? C3 Si6 C20 110.5(2) . . ? C3 Si6 C21 113.3(2) . . ? C20 Si6 C21 108.5(3) . . ? C3 Si6 C19 112.9(2) . . ? C20 Si6 C19 105.2(3) . . ? C21 Si6 C19 105.9(3) . . ? C22 N Ce 170.6(4) . . ? Si1 C1 Si2 116.7(2) . . ? Si1 C1 Ce 119.99(18) . . ? Si2 C1 Ce 107.17(18) . . ? Si4 C2 Si3 119.1(2) . . ? Si4 C2 Ce 105.57(19) . . ? Si3 C2 Ce 128.9(2) . . ? Si6 C3 Si5 117.8(2) . . ? Si6 C3 Ce 122.8(2) . . ? Si5 C3 Ce 112.35(17) . . ? N C22 C23 179.4(5) . . ? C24 C23 C28 120 . . ? C24 C23 C22 120.9(3) . . ? C28 C23 C22 119.1(3) . . ? C25 C24 C23 120 . . ? C26 C25 C24 120 . . ? C25 C26 C27 120 . . ? C28 C27 C26 120 . . ? C27 C28 C23 120 . . ? C2A Ce1A C3A 120.60(16) . . ? C2A Ce1A C1A 110.06(14) . . ? C3A Ce1A C1A 114.94(13) . . ? C2A Ce1A N1A 107.88(14) . . ? C3A Ce1A N1A 109.00(13) . . ? C1A Ce1A N1A 89.73(13) . . ? C1A Si1A C5A 113.3(2) . . ? C1A Si1A C4A 113.3(2) . . ? C5A Si1A C4A 104.6(2) . . ? C1A Si1A C6A 112.8(2) . . ? C5A Si1A C6A 107.6(3) . . ? C4A Si1A C6A 104.5(2) . . ? C1A Si2A C9A 109.66(19) . . ? C1A Si2A C8A 111.4(2) . . ? C9A Si2A C8A 108.6(2) . . ? C1A Si2A C7A 115.7(2) . . ? C9A Si2A C7A 107.1(3) . . ? C8A Si2A C7A 104.0(2) . . ? C2A Si3A C11A 114.2(3) . . ? C2A Si3A C12A 114.6(2) . . ? C11A Si3A C12A 105.1(3) . . ? C2A Si3A C10A 107.9(2) . . ? C11A Si3A C10A 108.2(3) . . ? C12A Si3A C10A 106.5(3) . . ? C2A Si4A C15A 110.1(2) . . ? C2A Si4A C13A 113.6(3) . . ? C15A Si4A C13A 105.9(3) . . ? C2A Si4A C14A 113.4(3) . . ? C15A Si4A C14A 105.7(3) . . ? C13A Si4A C14A 107.6(3) . . ? C16A Si5A C3A 112.3(2) . . ? C16A Si5A C18A 108.0(3) . . ? C3A Si5A C18A 115.6(2) . . ? C16A Si5A C17A 105.8(3) . . ? C3A Si5A C17A 108.1(2) . . ? C18A Si5A C17A 106.4(3) . . ? C3A Si6A C20A 113.2(2) . . ? C3A Si6A C19A 111.7(2) . . ? C20A Si6A C19A 107.2(2) . . ? C3A Si6A C21A 112.0(2) . . ? C20A Si6A C21A 106.9(3) . . ? C19A Si6A C21A 105.4(2) . . ? C22A N1A Ce1A 175.9(4) . . ? Si2A C1A Si1A 115.6(2) . . ? Si2A C1A Ce1A 117.31(18) . . ? Si1A C1A Ce1A 111.65(17) . . ? Si4A C2A Si3A 120.5(3) . . ? Si4A C2A Ce1A 123.0(2) . . ? Si3A C2A Ce1A 111.7(2) . . ? Si6A C3A Si5A 119.3(2) . . ? Si6A C3A Ce1A 124.84(19) . . ? Si5A C3A Ce1A 108.45(18) . . ? N1A C22A C23A 178.9(5) . . ? C24A C23A C28A 120 . . ? C24A C23A C22A 119.1(3) . . ? C28A C23A C22A 120.9(3) . . ? C25A C24A C23A 120 . . ? C24A C25A C26A 120 . . ? C27A C26A C25A 120 . . ? C26A C27A C28A 120 . . ? C27A C28A C23A 120 . . ? #===END data_(7)-sep1602 _database_code_depnum_ccdc_archive 'CCDC 229456' _audit_creation_date 2002-09-18T09:48:28-00:00 _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_name_common '[Me2SiNCPhCH(SiMe3)CPhN]' _chemical_formula_moiety 'C20 H26 N2 Si2' _chemical_formula_sum 'C20 H26 N2 Si2' _chemical_formula_weight 350.61 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _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 10.4609(3) _cell_length_b 9.9181(3) _cell_length_c 19.2816(6) _cell_angle_alpha 90 _cell_angle_beta 93.388(1) _cell_angle_gamma 90 _cell_volume 1997.01(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10610 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _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 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.166 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.181 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_unetI/netI 0.0452 _diffrn_reflns_number 10181 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.933 _diffrn_measured_fraction_theta_max 0.933 _reflns_number_total 3304 _reflns_number_gt 2777 _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^)+(0.0336P)^2^+1.6806P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_number_reflns 3304 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1025 _refine_ls_wR_factor_gt 0.0973 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.276 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.045 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Si1 Si 0.32714(6) 0.18346(6) 0.08267(3) 0.02574(18) Uani 1 1 d . . . Si2 Si 0.35209(6) 0.57862(6) 0.16031(3) 0.02522(18) Uani 1 1 d . . . N1 N 0.28734(17) 0.31556(18) 0.02634(8) 0.0251(4) Uani 1 1 d . . . N2 N 0.26088(18) 0.21900(18) 0.16147(9) 0.0276(4) Uani 1 1 d . . . C1 C 0.2363(2) 0.4237(2) 0.04820(10) 0.0217(5) Uani 1 1 d . . . C2 C 0.2194(2) 0.4562(2) 0.12394(10) 0.0208(5) Uani 1 1 d . . . H2 H 0.145(2) 0.508(2) 0.1270(10) 0.017(5) Uiso 1 1 d . . . C3 C 0.2129(2) 0.3354(2) 0.17220(10) 0.0226(5) Uani 1 1 d . . . C4 C 0.1935(2) 0.5292(2) -0.00427(10) 0.0221(5) Uani 1 1 d . . . C5 C 0.2384(2) 0.5200(2) -0.07058(11) 0.0268(5) Uani 1 1 d . . . H5 H 0.295(2) 0.451(3) -0.0800(12) 0.032(6) Uiso 1 1 d . . . C6 C 0.2013(2) 0.6121(3) -0.12171(12) 0.0322(5) Uani 1 1 d . . . H6 H 0.231(2) 0.604(3) -0.1680(13) 0.040(7) Uiso 1 1 d . . . C7 C 0.1178(2) 0.7151(2) -0.10756(12) 0.0351(6) Uani 1 1 d . . . H7 H 0.088(3) 0.779(3) -0.1417(13) 0.046(7) Uiso 1 1 d . . . C8 C 0.0727(3) 0.7256(2) -0.04214(12) 0.0345(6) Uani 1 1 d . . . H8 H 0.011(3) 0.791(3) -0.0325(12) 0.043(7) Uiso 1 1 d . . . C9 C 0.1098(2) 0.6332(2) 0.00923(12) 0.0303(5) Uani 1 1 d . . . H9 H 0.079(2) 0.641(3) 0.0539(13) 0.038(7) Uiso 1 1 d . . . C10 C 0.1505(2) 0.3603(2) 0.23948(10) 0.0242(5) Uani 1 1 d . . . C11 C 0.1943(3) 0.2878(3) 0.29807(12) 0.0353(6) Uani 1 1 d . . . H11 H 0.260(3) 0.228(3) 0.2933(13) 0.044(8) Uiso 1 1 d . . . C12 C 0.1423(3) 0.3075(3) 0.36168(13) 0.0432(7) Uani 1 1 d . . . H12 H 0.179(3) 0.262(3) 0.4029(15) 0.055(8) Uiso 1 1 d . . . C13 C 0.0420(3) 0.3972(3) 0.36657(12) 0.0364(6) Uani 1 1 d . . . H13 H 0.009(2) 0.410(3) 0.4100(13) 0.040(7) Uiso 1 1 d . . . C14 C -0.0049(2) 0.4680(2) 0.30911(11) 0.0304(5) Uani 1 1 d . . . H14 H -0.072(2) 0.528(2) 0.3136(11) 0.029(6) Uiso 1 1 d . . . C15 C 0.0506(2) 0.4509(2) 0.24601(11) 0.0256(5) Uani 1 1 d . . . H15 H 0.015(2) 0.502(2) 0.2065(11) 0.023(6) Uiso 1 1 d . . . C16 C 0.4750(3) 0.4824(3) 0.21329(16) 0.0429(7) Uani 1 1 d . . . H16A H 0.515(3) 0.420(4) 0.1862(17) 0.073(11) Uiso 1 1 d . . . H16C H 0.436(3) 0.439(3) 0.2502(18) 0.076(11) Uiso 1 1 d . . . H16B H 0.541(3) 0.547(3) 0.2316(14) 0.054(8) Uiso 1 1 d . . . C17 C 0.2755(3) 0.7064(3) 0.21483(17) 0.0465(7) Uani 1 1 d . . . H17B H 0.248(3) 0.665(3) 0.2559(17) 0.065(10) Uiso 1 1 d . . . H17A H 0.206(4) 0.751(4) 0.1913(18) 0.086(12) Uiso 1 1 d . . . H17C H 0.342(3) 0.769(3) 0.2298(15) 0.065(9) Uiso 1 1 d . . . C18 C 0.4306(3) 0.6643(3) 0.08822(14) 0.0390(6) Uani 1 1 d . . . H18C H 0.496(3) 0.720(3) 0.1080(15) 0.058(9) Uiso 1 1 d . . . H18A H 0.366(3) 0.718(3) 0.0602(15) 0.059(9) Uiso 1 1 d . . . H18B H 0.464(3) 0.603(3) 0.0563(15) 0.059(9) Uiso 1 1 d . . . C19 C 0.2516(3) 0.0281(3) 0.04640(15) 0.0395(6) Uani 1 1 d . . . H19C H 0.269(3) -0.039(4) 0.0785(17) 0.078(11) Uiso 1 1 d . . . H19B H 0.154(4) 0.043(4) 0.0368(17) 0.085(11) Uiso 1 1 d . . . H19A H 0.285(3) 0.007(3) 0.0044(16) 0.057(9) Uiso 1 1 d . . . C20 C 0.5026(3) 0.1606(3) 0.09313(16) 0.0432(7) Uani 1 1 d . . . H20A H 0.534(3) 0.141(4) 0.052(2) 0.082(11) Uiso 1 1 d . . . H20B H 0.524(4) 0.094(4) 0.127(2) 0.095(13) Uiso 1 1 d . . . H20C H 0.546(4) 0.238(4) 0.1057(19) 0.090(13) Uiso 1 1 d . . . 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 Si1 0.0322(4) 0.0214(3) 0.0244(3) 0.0015(2) 0.0079(2) 0.0061(3) Si2 0.0270(4) 0.0240(3) 0.0248(3) -0.0027(2) 0.0022(2) 0.0006(3) N1 0.0336(11) 0.0212(10) 0.0210(9) 0.0000(7) 0.0060(7) 0.0025(8) N2 0.0362(11) 0.0232(10) 0.0241(9) 0.0027(7) 0.0067(8) 0.0037(8) C1 0.0209(11) 0.0229(11) 0.0213(10) 0.0018(8) 0.0019(8) -0.0013(9) C2 0.0229(12) 0.0197(11) 0.0201(10) 0.0000(8) 0.0028(8) 0.0047(9) C3 0.0241(12) 0.0215(12) 0.0223(10) 0.0014(8) 0.0021(8) 0.0006(9) C4 0.0248(11) 0.0205(11) 0.0208(10) 0.0000(8) -0.0012(8) -0.0026(9) C5 0.0280(13) 0.0276(13) 0.0250(11) 0.0016(9) 0.0029(9) -0.0014(10) C6 0.0355(14) 0.0365(14) 0.0245(12) 0.0079(10) 0.0022(10) -0.0010(11) C7 0.0414(15) 0.0294(14) 0.0333(13) 0.0115(10) -0.0072(11) 0.0015(11) C8 0.0401(15) 0.0274(13) 0.0354(13) 0.0022(10) -0.0035(11) 0.0104(11) C9 0.0356(14) 0.0301(13) 0.0253(12) -0.0003(10) 0.0022(10) 0.0053(10) C10 0.0276(12) 0.0242(12) 0.0212(10) -0.0002(8) 0.0045(9) -0.0025(9) C11 0.0452(16) 0.0350(15) 0.0266(12) 0.0059(10) 0.0089(10) 0.0125(12) C12 0.0628(19) 0.0433(16) 0.0242(12) 0.0090(11) 0.0086(12) 0.0132(13) C13 0.0501(16) 0.0372(15) 0.0237(12) 0.0001(10) 0.0154(11) 0.0022(12) C14 0.0308(14) 0.0301(13) 0.0314(12) -0.0051(10) 0.0106(10) -0.0011(11) C15 0.0266(12) 0.0277(13) 0.0228(11) 0.0006(9) 0.0038(9) -0.0015(9) C16 0.0392(16) 0.0434(17) 0.0445(16) 0.0034(13) -0.0096(13) -0.0030(14) C17 0.0469(18) 0.0406(17) 0.0528(18) -0.0241(14) 0.0092(14) -0.0055(14) C18 0.0362(16) 0.0410(16) 0.0401(15) 0.0048(12) 0.0037(12) -0.0111(13) C19 0.0533(19) 0.0236(13) 0.0429(16) -0.0025(11) 0.0125(13) 0.0041(12) C20 0.0376(16) 0.0525(19) 0.0403(16) 0.0034(14) 0.0102(12) 0.0116(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 Si1 N1 1.7367(18) . ? Si1 N2 1.7429(18) . ? Si1 C20 1.849(3) . ? Si1 C19 1.850(3) . ? Si2 C16 1.858(3) . ? Si2 C17 1.858(3) . ? Si2 C18 1.861(3) . ? Si2 C2 1.944(2) . ? N1 C1 1.281(3) . ? N2 C3 1.280(3) . ? C1 C4 1.505(3) . ? C1 C2 1.516(3) . ? C2 C3 1.521(3) . ? C3 C10 1.507(3) . ? C4 C9 1.387(3) . ? C4 C5 1.391(3) . ? C5 C6 1.383(3) . ? C6 C7 1.382(4) . ? C7 C8 1.377(3) . ? C8 C9 1.388(3) . ? C10 C15 1.390(3) . ? C10 C11 1.393(3) . ? C11 C12 1.385(3) . ? C12 C13 1.384(4) . ? C13 C14 1.377(3) . ? C14 C15 1.389(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 Si1 N2 107.44(9) . . ? N1 Si1 C20 111.14(12) . . ? N2 Si1 C20 111.91(12) . . ? N1 Si1 C19 108.10(12) . . ? N2 Si1 C19 108.36(11) . . ? C20 Si1 C19 109.76(15) . . ? C16 Si2 C17 110.27(16) . . ? C16 Si2 C18 108.88(14) . . ? C17 Si2 C18 109.58(15) . . ? C16 Si2 C2 109.50(12) . . ? C17 Si2 C2 107.92(12) . . ? C18 Si2 C2 110.69(11) . . ? C1 N1 Si1 121.02(14) . . ? C3 N2 Si1 120.20(15) . . ? N1 C1 C4 118.32(18) . . ? N1 C1 C2 124.72(18) . . ? C4 C1 C2 116.92(18) . . ? C1 C2 C3 115.71(17) . . ? C1 C2 Si2 111.05(14) . . ? C3 C2 Si2 109.16(14) . . ? N2 C3 C10 118.74(19) . . ? N2 C3 C2 125.39(19) . . ? C10 C3 C2 115.78(18) . . ? C9 C4 C5 118.2(2) . . ? C9 C4 C1 123.82(19) . . ? C5 C4 C1 117.95(19) . . ? C6 C5 C4 121.1(2) . . ? C7 C6 C5 120.1(2) . . ? C8 C7 C6 119.5(2) . . ? C7 C8 C9 120.5(2) . . ? C4 C9 C8 120.7(2) . . ? C15 C10 C11 118.2(2) . . ? C15 C10 C3 123.39(19) . . ? C11 C10 C3 118.4(2) . . ? C12 C11 C10 121.2(2) . . ? C11 C12 C13 119.4(2) . . ? C14 C13 C12 120.6(2) . . ? C13 C14 C15 119.7(2) . . ? C10 C15 C14 120.9(2) . . ? #===END data_(D)-aug1297 _database_code_depnum_ccdc_archive 'CCDC 229457' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C22 H58 Br2 Mg2 O2 Si4' _chemical_formula_weight 675.48 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 16.184(2) _cell_length_b 9.244(2) _cell_length_c 25.873(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.910(10) _cell_angle_gamma 90.00 _cell_volume 3683.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.218 _exptl_crystal_density_method ? _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 2.381 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6694 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0783 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 24.99 _reflns_number_total 6462 _reflns_number_observed 4335 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1274P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6461 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1151 _refine_ls_R_factor_obs 0.0738 _refine_ls_wR_factor_all 0.2054 _refine_ls_wR_factor_obs 0.1761 _refine_ls_goodness_of_fit_all 1.024 _refine_ls_goodness_of_fit_obs 1.078 _refine_ls_restrained_S_all 1.025 _refine_ls_restrained_S_obs 1.078 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Br1 Br 0.40207(5) 0.40222(8) 0.22988(3) 0.0365(2) Uani 1 d . . Br2 Br 0.57616(5) 0.67110(8) 0.26069(3) 0.0392(2) Uani 1 d . . Si1 Si 0.37127(13) 0.4519(2) 0.05902(8) 0.0297(4) Uani 1 d . . Si2 Si 0.45878(14) 0.7620(2) 0.08715(8) 0.0334(5) Uani 1 d . . Si3 Si 0.4994(2) 0.2847(2) 0.40056(8) 0.0410(5) Uani 1 d . . Si4 Si 0.63346(13) 0.5489(2) 0.42775(8) 0.0391(5) Uani 1 d . . Mg1 Mg 0.50543(15) 0.5023(2) 0.17982(9) 0.0295(5) Uani 1 d . . Mg2 Mg 0.47878(15) 0.5599(2) 0.31307(9) 0.0293(5) Uani 1 d . . O1 O 0.5978(3) 0.3475(5) 0.1910(2) 0.0428(13) Uani 1 d . . O2 O 0.3933(3) 0.7216(5) 0.3095(2) 0.0391(12) Uani 1 d . . C1 C 0.4639(4) 0.5650(7) 0.0972(3) 0.0284(15) Uani 1 d . . H1 H 0.5124 0.5337 0.0834 0.034 Uiso 1 calc R . C2 C 0.3518(6) 0.4516(9) -0.0162(3) 0.048(2) Uani 1 d . . H2A H 0.3019 0.3897 -0.0337 0.073 Uiso 1 calc R . H2B H 0.4034 0.4146 -0.0240 0.073 Uiso 1 calc R . H2C H 0.3399 0.5505 -0.0302 0.073 Uiso 1 calc R . C3 C 0.3915(5) 0.2580(8) 0.0807(3) 0.042(2) Uani 1 d . . H3A H 0.3421 0.1988 0.0602 0.064 Uiso 1 calc R . H3B H 0.3988 0.2501 0.1196 0.064 Uiso 1 calc R . H3C H 0.4443 0.2240 0.0735 0.064 Uiso 1 calc R . C4 C 0.2665(5) 0.5114(9) 0.0700(3) 0.045(2) Uani 1 d . . H4A H 0.2191 0.4489 0.0491 0.067 Uiso 1 calc R . H4B H 0.2541 0.6117 0.0579 0.067 Uiso 1 calc R . H4C H 0.2719 0.5045 0.1087 0.067 Uiso 1 calc R . C5 C 0.5707(5) 0.8394(9) 0.1128(3) 0.051(2) Uani 1 d . . H5A H 0.5681 0.9445 0.1074 0.077 Uiso 1 calc R . H5B H 0.6072 0.7966 0.0928 0.077 Uiso 1 calc R . H5C H 0.5956 0.8178 0.1516 0.077 Uiso 1 calc R . C6 C 0.3919(6) 0.8497(8) 0.1253(3) 0.047(2) Uani 1 d . . H6A H 0.3904 0.9544 0.1191 0.071 Uiso 1 calc R . H6B H 0.4174 0.8299 0.1642 0.071 Uiso 1 calc R . H6C H 0.3327 0.8109 0.1127 0.071 Uiso 1 calc R . C7 C 0.4156(6) 0.8206(9) 0.0143(3) 0.054(2) Uani 1 d . . H7A H 0.4149 0.9265 0.0124 0.081 Uiso 1 calc R . H7B H 0.3565 0.7835 -0.0015 0.081 Uiso 1 calc R . H7C H 0.4530 0.7823 -0.0060 0.081 Uiso 1 calc R . C8 C 0.6263(6) 0.2578(9) 0.2396(3) 0.058(2) Uani 1 d . . H8A H 0.6093 0.3040 0.2693 0.069 Uiso 1 calc R . H8B H 0.6904 0.2494 0.2514 0.069 Uiso 1 calc R . C9 C 0.5862(9) 0.1089(10) 0.2285(4) 0.087(4) Uani 1 d . . H9A H 0.6060 0.0501 0.2615 0.130 Uiso 1 calc R . H9B H 0.6039 0.0627 0.1994 0.130 Uiso 1 calc R . H9C H 0.5228 0.1173 0.2173 0.130 Uiso 1 calc R . C10 C 0.6498(6) 0.3301(11) 0.1549(4) 0.068(3) Uani 1 d . . H10A H 0.6123 0.3410 0.1169 0.081 Uiso 1 calc R . H10B H 0.6747 0.2314 0.1592 0.081 Uiso 1 calc R . C11 C 0.7201(7) 0.4363(14) 0.1662(4) 0.089(4) Uani 1 d . . H11A H 0.7539 0.4215 0.1410 0.133 Uiso 1 calc R . H11B H 0.7579 0.4245 0.2036 0.133 Uiso 1 calc R . H11C H 0.6955 0.5341 0.1614 0.133 Uiso 1 calc R . C12 C 0.5248(5) 0.4758(7) 0.3933(2) 0.031(2) Uani 1 d . . H12 H 0.4877 0.5270 0.4121 0.038 Uiso 1 calc R . C13 C 0.3807(6) 0.2526(9) 0.3698(3) 0.055(2) Uani 1 d . . H13A H 0.3678 0.1505 0.3738 0.082 Uiso 1 calc R . H13B H 0.3634 0.2776 0.3311 0.082 Uiso 1 calc R . H13C H 0.3486 0.3130 0.3881 0.082 Uiso 1 calc R . C14 C 0.5562(7) 0.1628(9) 0.3656(4) 0.073(3) Uani 1 d . . H14A H 0.5410 0.0621 0.3704 0.109 Uiso 1 calc R . H14B H 0.6191 0.1757 0.3812 0.109 Uiso 1 calc R . H14C H 0.5385 0.1861 0.3268 0.109 Uiso 1 calc R . C15 C 0.5271(7) 0.2213(10) 0.4732(3) 0.076(3) Uani 1 d . . H15A H 0.5118 0.1189 0.4738 0.114 Uiso 1 calc R . H15B H 0.4945 0.2784 0.4922 0.114 Uiso 1 calc R . H15C H 0.5895 0.2336 0.4912 0.114 Uiso 1 calc R . C16 C 0.7167(5) 0.4764(11) 0.3975(4) 0.061(3) Uani 1 d . . H16A H 0.7736 0.5175 0.4168 0.092 Uiso 1 calc R . H16B H 0.7006 0.5031 0.3590 0.092 Uiso 1 calc R . H16C H 0.7192 0.3708 0.4010 0.092 Uiso 1 calc R . C17 C 0.6740(6) 0.5114(11) 0.5023(3) 0.071(3) Uani 1 d . . H17A H 0.7319 0.5536 0.5177 0.107 Uiso 1 calc R . H17B H 0.6771 0.4066 0.5084 0.107 Uiso 1 calc R . H17C H 0.6342 0.5543 0.5200 0.107 Uiso 1 calc R . C18 C 0.6330(5) 0.7503(9) 0.4214(3) 0.051(2) Uani 1 d . . H18A H 0.6913 0.7879 0.4399 0.077 Uiso 1 calc R . H18B H 0.5915 0.7916 0.4381 0.077 Uiso 1 calc R . H18C H 0.6161 0.7771 0.3829 0.077 Uiso 1 calc R . C19 C 0.3679(6) 0.7645(9) 0.3580(3) 0.052(2) Uani 1 d . . H19A H 0.4187 0.7544 0.3910 0.063 Uiso 1 calc R . H19B H 0.3502 0.8675 0.3547 0.063 Uiso 1 calc R . C20 C 0.2968(6) 0.6769(10) 0.3641(4) 0.064(3) Uani 1 d . . H20A H 0.2822 0.7084 0.3964 0.096 Uiso 1 calc R . H20B H 0.3145 0.5750 0.3682 0.096 Uiso 1 calc R . H20C H 0.2460 0.6881 0.3319 0.096 Uiso 1 calc R . C21 C 0.3395(6) 0.7856(9) 0.2602(3) 0.058(2) Uani 1 d . . H21A H 0.2778 0.7766 0.2586 0.070 Uiso 1 calc R . H21B H 0.3474 0.7325 0.2288 0.070 Uiso 1 calc R . C22 C 0.3610(9) 0.9433(10) 0.2561(4) 0.088(4) Uani 1 d . . H22A H 0.3231 0.9833 0.2219 0.133 Uiso 1 calc R . H22B H 0.4217 0.9524 0.2569 0.133 Uiso 1 calc R . H22C H 0.3522 0.9965 0.2867 0.133 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0456(4) 0.0330(4) 0.0325(4) -0.0059(3) 0.0145(3) -0.0133(3) Br2 0.0517(5) 0.0341(4) 0.0329(4) -0.0064(3) 0.0145(3) -0.0175(4) Si1 0.0379(11) 0.0216(10) 0.0309(10) -0.0033(8) 0.0126(8) -0.0027(8) Si2 0.0469(12) 0.0214(10) 0.0354(11) 0.0009(8) 0.0179(9) -0.0039(9) Si3 0.0611(14) 0.0249(11) 0.0400(12) 0.0081(9) 0.0200(10) 0.0044(10) Si4 0.0382(12) 0.0412(12) 0.0334(11) 0.0032(9) 0.0045(9) 0.0022(10) Mg1 0.0384(13) 0.0203(12) 0.0310(12) 0.0002(9) 0.0123(10) -0.0002(10) Mg2 0.0370(13) 0.0215(12) 0.0282(12) 0.0009(9) 0.0082(10) 0.0017(10) O1 0.057(3) 0.039(3) 0.035(3) 0.004(2) 0.019(2) 0.016(3) O2 0.055(3) 0.030(3) 0.032(3) 0.003(2) 0.010(2) 0.014(2) C1 0.034(4) 0.022(3) 0.032(4) 0.003(3) 0.014(3) 0.002(3) C2 0.069(6) 0.043(5) 0.031(4) -0.009(4) 0.012(4) -0.004(4) C3 0.046(5) 0.028(4) 0.055(5) -0.005(4) 0.018(4) -0.005(4) C4 0.041(4) 0.043(5) 0.052(5) -0.003(4) 0.015(4) 0.001(4) C5 0.065(6) 0.032(4) 0.062(5) -0.011(4) 0.027(4) -0.022(4) C6 0.074(6) 0.023(4) 0.051(5) -0.002(4) 0.027(4) 0.006(4) C7 0.081(6) 0.034(5) 0.050(5) 0.018(4) 0.025(5) 0.003(4) C8 0.084(7) 0.045(5) 0.043(5) 0.011(4) 0.018(5) 0.022(5) C9 0.151(11) 0.030(5) 0.081(7) -0.003(5) 0.039(7) -0.001(6) C10 0.078(7) 0.077(7) 0.056(6) 0.014(5) 0.032(5) 0.045(6) C11 0.060(6) 0.132(11) 0.082(8) 0.028(8) 0.034(6) 0.009(7) C12 0.043(4) 0.024(4) 0.024(3) -0.001(3) 0.006(3) 0.004(3) C13 0.075(6) 0.038(5) 0.054(5) -0.005(4) 0.026(5) -0.017(5) C14 0.101(8) 0.028(5) 0.101(8) 0.010(5) 0.049(7) 0.017(5) C15 0.116(9) 0.052(6) 0.058(6) 0.030(5) 0.024(6) 0.001(6) C16 0.034(5) 0.077(7) 0.072(6) -0.003(5) 0.014(4) 0.000(5) C17 0.083(7) 0.077(7) 0.037(5) 0.007(5) -0.005(5) -0.013(6) C18 0.059(5) 0.044(5) 0.045(5) -0.003(4) 0.006(4) -0.010(4) C19 0.078(6) 0.040(5) 0.037(4) 0.003(4) 0.015(4) 0.023(5) C20 0.069(6) 0.057(6) 0.067(6) 0.013(5) 0.024(5) 0.019(5) C21 0.077(6) 0.056(6) 0.042(5) 0.013(4) 0.017(4) 0.027(5) C22 0.173(12) 0.034(5) 0.070(7) 0.010(5) 0.055(8) 0.018(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Mg2 2.580(2) . ? Br1 Mg1 2.582(2) . ? Br2 Mg1 2.579(2) . ? Br2 Mg2 2.587(2) . ? Si1 C1 1.846(7) . ? Si1 C2 1.873(7) . ? Si1 C3 1.876(8) . ? Si1 C4 1.884(7) . ? Si2 C1 1.838(7) . ? Si2 C6 1.860(7) . ? Si2 C5 1.870(8) . ? Si2 C7 1.877(8) . ? Si3 C12 1.837(7) . ? Si3 C14 1.856(9) . ? Si3 C13 1.862(9) . ? Si3 C15 1.885(8) . ? Si4 C12 1.838(7) . ? Si4 C18 1.869(8) . ? Si4 C17 1.870(8) . ? Si4 C16 1.876(8) . ? Mg1 O1 2.024(5) . ? Mg1 C1 2.114(7) . ? Mg2 O2 2.020(5) . ? Mg2 C12 2.125(6) . ? O1 C10 1.444(9) . ? O1 C8 1.458(9) . ? O2 C21 1.432(9) . ? O2 C19 1.491(8) . ? C8 C9 1.512(13) . ? C10 C11 1.463(14) . ? C19 C20 1.454(12) . ? C21 C22 1.510(13) . ? 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 Mg2 Br1 Mg1 89.79(7) . . ? Mg1 Br2 Mg2 89.69(7) . . ? C1 Si1 C2 114.0(3) . . ? C1 Si1 C3 110.0(3) . . ? C2 Si1 C3 105.5(4) . . ? C1 Si1 C4 112.0(3) . . ? C2 Si1 C4 106.6(4) . . ? C3 Si1 C4 108.4(4) . . ? C1 Si2 C6 111.4(3) . . ? C1 Si2 C5 109.4(4) . . ? C6 Si2 C5 107.7(4) . . ? C1 Si2 C7 114.5(3) . . ? C6 Si2 C7 108.0(4) . . ? C5 Si2 C7 105.4(4) . . ? C12 Si3 C14 112.0(4) . . ? C12 Si3 C13 110.1(4) . . ? C14 Si3 C13 107.2(4) . . ? C12 Si3 C15 114.1(4) . . ? C14 Si3 C15 107.1(5) . . ? C13 Si3 C15 106.0(4) . . ? C12 Si4 C18 110.3(3) . . ? C12 Si4 C17 114.3(4) . . ? C18 Si4 C17 105.4(4) . . ? C12 Si4 C16 111.6(4) . . ? C18 Si4 C16 107.6(4) . . ? C17 Si4 C16 107.2(4) . . ? O1 Mg1 C1 109.2(2) . . ? O1 Mg1 Br2 100.8(2) . . ? C1 Mg1 Br2 125.3(2) . . ? O1 Mg1 Br1 103.8(2) . . ? C1 Mg1 Br1 123.5(2) . . ? Br2 Mg1 Br1 90.24(7) . . ? O2 Mg2 C12 110.2(2) . . ? O2 Mg2 Br1 103.4(2) . . ? C12 Mg2 Br1 122.9(2) . . ? O2 Mg2 Br2 101.6(2) . . ? C12 Mg2 Br2 124.7(2) . . ? Br1 Mg2 Br2 90.11(7) . . ? C10 O1 C8 113.6(6) . . ? C10 O1 Mg1 122.5(5) . . ? C8 O1 Mg1 123.3(5) . . ? C21 O2 C19 113.1(6) . . ? C21 O2 Mg2 124.5(4) . . ? C19 O2 Mg2 121.4(4) . . ? Si2 C1 Si1 119.4(4) . . ? Si2 C1 Mg1 113.7(3) . . ? Si1 C1 Mg1 109.8(3) . . ? O1 C8 C9 110.5(7) . . ? O1 C10 C11 111.6(8) . . ? Si3 C12 Si4 121.0(4) . . ? Si3 C12 Mg2 115.4(3) . . ? Si4 C12 Mg2 109.6(3) . . ? C20 C19 O2 112.0(7) . . ? O2 C21 C22 111.8(8) . . ? _refine_diff_density_max 1.465 _refine_diff_density_min -1.744 _refine_diff_density_rms 0.147 #===END data_(15)-apr2297 _database_code_depnum_ccdc_archive 'CCDC 229458' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H48 Mg O Si4' _chemical_formula_weight 417.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M C222(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 9.676(4) _cell_length_b 16.620(8) _cell_length_c 17.173(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2761.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.003 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.243 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius CAD4' _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4864 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 24.97 _reflns_number_total 2447 _reflns_number_gt 2354 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0587P)^2^+0.2368P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(14) _refine_ls_number_reflns 2447 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg Mg 0.41150(8) 0.0000 0.0000 0.0203(2) Uani 1 2 d S . . Si1 Si 0.27648(6) -0.12451(3) 0.14200(3) 0.02643(15) Uani 1 1 d . . . Si2 Si 0.26685(6) 0.06554(3) 0.15510(3) 0.02579(15) Uani 1 1 d . . . O O 0.62273(18) 0.0000 0.0000 0.0276(4) Uani 1 2 d S . . C1 C 0.35135(18) -0.02572(10) 0.11735(10) 0.0218(4) Uani 1 1 d . . . H1 H 0.4416 -0.0263 0.1457 0.026 Uiso 1 1 calc R . . C2 C 0.4063(2) -0.20628(12) 0.12556(14) 0.0402(5) Uani 1 1 d . . . H2C H 0.3652 -0.2584 0.1389 0.060 Uiso 1 1 calc R . . H2B H 0.4875 -0.1968 0.1585 0.060 Uiso 1 1 calc R . . H2A H 0.4344 -0.2065 0.0707 0.060 Uiso 1 1 calc R . . C3 C 0.1174(3) -0.14934(14) 0.08432(14) 0.0425(5) Uani 1 1 d . . . H3C H 0.0827 -0.2023 0.1000 0.064 Uiso 1 1 calc R . . H3B H 0.1401 -0.1501 0.0287 0.064 Uiso 1 1 calc R . . H3A H 0.0463 -0.1086 0.0941 0.064 Uiso 1 1 calc R . . C4 C 0.2230(3) -0.13473(14) 0.24719(13) 0.0479(6) Uani 1 1 d . . . H4C H 0.1843 -0.1885 0.2559 0.072 Uiso 1 1 calc R . . H4B H 0.1530 -0.0940 0.2595 0.072 Uiso 1 1 calc R . . H4A H 0.3037 -0.1270 0.2808 0.072 Uiso 1 1 calc R . . C5 C 0.0773(2) 0.06591(15) 0.13304(15) 0.0440(5) Uani 1 1 d . . . H5C H 0.0355 0.1151 0.1538 0.066 Uiso 1 1 calc R . . H5B H 0.0337 0.0189 0.1572 0.066 Uiso 1 1 calc R . . H5A H 0.0636 0.0639 0.0765 0.066 Uiso 1 1 calc R . . C6 C 0.3479(3) 0.15745(12) 0.10977(13) 0.0423(5) Uani 1 1 d . . . H6C H 0.3027 0.2059 0.1300 0.063 Uiso 1 1 calc R . . H6B H 0.3366 0.1552 0.0531 0.063 Uiso 1 1 calc R . . H6A H 0.4465 0.1590 0.1226 0.063 Uiso 1 1 calc R . . C7 C 0.2874(3) 0.08119(14) 0.26311(12) 0.0409(5) Uani 1 1 d . . . H7C H 0.2398 0.1307 0.2786 0.061 Uiso 1 1 calc R . . H7B H 0.3858 0.0856 0.2759 0.061 Uiso 1 1 calc R . . H7A H 0.2472 0.0354 0.2911 0.061 Uiso 1 1 calc R . . C8 C 0.7048(2) 0.05678(13) -0.04452(12) 0.0339(5) Uani 1 1 d . . . H8B H 0.6517 0.0741 -0.0909 0.041 Uiso 1 1 calc R . . H8A H 0.7899 0.0297 -0.0629 0.041 Uiso 1 1 calc R . . C9 C 0.7436(2) 0.12929(13) 0.00244(16) 0.0454(5) Uani 1 1 d . . . H9C H 0.7988 0.1659 -0.0297 0.068 Uiso 1 1 calc R . . H9B H 0.7978 0.1125 0.0478 0.068 Uiso 1 1 calc R . . H9A H 0.6597 0.1569 0.0199 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0207(4) 0.0201(4) 0.0200(4) 0.0012(3) 0.000 0.000 Si1 0.0322(3) 0.0230(3) 0.0241(3) 0.00393(18) 0.0006(2) -0.0045(2) Si2 0.0278(3) 0.0244(3) 0.0252(3) 0.00055(18) 0.00457(19) 0.0032(2) O 0.0228(9) 0.0339(9) 0.0260(9) 0.0067(8) 0.000 0.000 C1 0.0214(9) 0.0219(8) 0.0221(9) 0.0005(7) -0.0001(7) 0.0000(7) C2 0.0482(13) 0.0237(9) 0.0487(13) 0.0031(9) -0.0061(11) 0.0030(9) C3 0.0380(12) 0.0425(12) 0.0470(13) 0.0016(10) -0.0033(10) -0.0160(10) C4 0.0701(17) 0.0418(12) 0.0317(10) 0.0104(9) 0.0085(11) -0.0097(13) C5 0.0324(11) 0.0468(12) 0.0527(13) 0.0047(11) 0.0024(10) 0.0133(10) C6 0.0608(15) 0.0250(9) 0.0412(12) 0.0016(9) 0.0041(11) -0.0025(10) C7 0.0502(14) 0.0434(11) 0.0291(10) -0.0083(8) 0.0070(10) 0.0037(11) C8 0.0277(10) 0.0441(11) 0.0297(10) 0.0056(9) 0.0039(8) -0.0084(9) C9 0.0415(12) 0.0368(11) 0.0580(13) -0.0001(10) 0.0029(12) -0.0054(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg O 2.044(2) . ? Mg C1 2.1408(17) 2 ? Mg C1 2.1408(17) . ? Si1 C1 1.8438(19) . ? Si1 C2 1.872(2) . ? Si1 C3 1.876(2) . ? Si1 C4 1.887(2) . ? Si2 C1 1.8411(19) . ? Si2 C5 1.872(2) . ? Si2 C7 1.883(2) . ? Si2 C6 1.885(2) . ? O C8 1.451(2) . ? O C8 1.451(2) 2 ? C8 C9 1.498(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 O Mg C1 105.78(5) . 2 ? O Mg C1 105.78(5) . . ? C1 Mg C1 148.45(10) 2 . ? C1 Si1 C2 110.36(10) . . ? C1 Si1 C3 113.39(9) . . ? C2 Si1 C3 108.14(11) . . ? C1 Si1 C4 114.06(9) . . ? C2 Si1 C4 105.26(11) . . ? C3 Si1 C4 105.10(12) . . ? C1 Si2 C5 111.49(10) . . ? C1 Si2 C7 114.43(9) . . ? C5 Si2 C7 107.59(12) . . ? C1 Si2 C6 109.72(10) . . ? C5 Si2 C6 108.74(11) . . ? C7 Si2 C6 104.53(11) . . ? C8 O C8 113.6(2) . 2 ? C8 O Mg 123.19(11) . . ? C8 O Mg 123.19(11) 2 . ? Si2 C1 Si1 118.58(10) . . ? Si2 C1 Mg 106.72(8) . . ? Si1 C1 Mg 120.05(9) . . ? O C8 C9 112.13(16) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.274 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.078 #===END data_(17)-nov1601 _database_code_depnum_ccdc_archive 'CCDC 229459' _audit_creation_date 2001-11-27T09:51:54-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[Ce{N(SiMe3)2}2{Me3SiNC(C6H4tBu)CHC(C6H4tBu)NSiMe3}]' ; _chemical_formula_moiety 'C41 H81 Ce1 N4 Si6' _chemical_formula_sum 'C41 H81 Ce N4 Si6' _chemical_formula_weight 938.76 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _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 12.6286(6) _cell_length_b 18.6283(11) _cell_length_c 22.8848(11) _cell_angle_alpha 90 _cell_angle_beta 93.537(3) _cell_angle_gamma 90 _cell_volume 5373.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 83789 _cell_measurement_theta_min 4.076 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.16 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1988 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.009 _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 0.840 _exptl_absorpt_correction_T_max 0.893 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 38785 _diffrn_reflns_av_R_equivalents 0.1192 _diffrn_reflns_av_unetI/netI 0.0869 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 22.95 _diffrn_reflns_theta_full 22.95 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 7374 _reflns_number_gt 5325 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+3.3862P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 7374 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1218 _refine_ls_wR_factor_gt 0.1103 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.884 _refine_diff_density_min -0.92 _refine_diff_density_rms 0.091 #----------------------------------------------------------------------------# # 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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 Ce Ce 0.49426(3) 0.26470(2) 0.612283(14) 0.02883(14) Uani 1 1 d . . . Si1 Si 0.41263(14) 0.42473(11) 0.70789(7) 0.0382(5) Uani 1 1 d . . . Si2 Si 0.28462(14) 0.13410(10) 0.68290(7) 0.0360(5) Uani 1 1 d . . . Si3 Si 0.71405(15) 0.22631(12) 0.71158(8) 0.0450(5) Uani 1 1 d . . . Si4 Si 0.74433(15) 0.34963(12) 0.63000(8) 0.0455(5) Uani 1 1 d . . . Si5 Si 0.57640(14) 0.16286(11) 0.50180(8) 0.0401(5) Uani 1 1 d . . . Si6 Si 0.45713(15) 0.29075(11) 0.45292(8) 0.0421(5) Uani 1 1 d . . . N1 N 0.6693(4) 0.2828(3) 0.6567(2) 0.0324(13) Uani 1 1 d . . . N2 N 0.5087(4) 0.2410(3) 0.5113(2) 0.0334(13) Uani 1 1 d . . . N3 N 0.3853(4) 0.3627(3) 0.65064(19) 0.0313(13) Uani 1 1 d . . . N4 N 0.3346(3) 0.1998(3) 0.63812(18) 0.0278(12) Uani 1 1 d . . . C1 C 0.3002(5) 0.3621(3) 0.6138(3) 0.0325(15) Uani 1 1 d . . . C2 C 0.2688(5) 0.3008(4) 0.5784(2) 0.0313(15) Uani 1 1 d . . . H2 H 0.2413 0.3115 0.5398 0.038 Uiso 1 1 calc R . . C3 C 0.2732(4) 0.2285(4) 0.5926(2) 0.0283(15) Uani 1 1 d . . . C4 C 0.2281(5) 0.4259(3) 0.6060(3) 0.0320(16) Uani 1 1 d . . . C5 C 0.2610(5) 0.4915(4) 0.5863(2) 0.0339(16) Uani 1 1 d . . . H5 H 0.3318 0.4974 0.5754 0.041 Uiso 1 1 calc R . . C6 C 0.1909(5) 0.5493(4) 0.5822(3) 0.0392(17) Uani 1 1 d . . . H6 H 0.2146 0.594 0.5678 0.047 Uiso 1 1 calc R . . C7 C 0.0861(5) 0.5431(4) 0.5986(3) 0.0365(16) Uani 1 1 d . . . C8 C 0.0554(5) 0.4765(4) 0.6178(3) 0.0441(18) Uani 1 1 d . . . H8 H -0.0151 0.4706 0.6291 0.053 Uiso 1 1 calc R . . C9 C 0.1227(5) 0.4182(4) 0.6210(3) 0.0443(18) Uani 1 1 d . . . H9 H 0.0977 0.3729 0.6334 0.053 Uiso 1 1 calc R . . C10 C 0.0073(5) 0.6059(4) 0.5962(3) 0.0438(18) Uani 1 1 d . . . C11 C 0.0555(7) 0.6755(4) 0.5739(3) 0.067(2) Uani 1 1 d . . . H11A H 0.0022 0.7138 0.5734 0.101 Uiso 1 1 calc R . . H11B H 0.0782 0.668 0.5342 0.101 Uiso 1 1 calc R . . H11C H 0.1168 0.6892 0.5998 0.101 Uiso 1 1 calc R . . C12 C -0.0311(6) 0.6188(4) 0.6575(3) 0.060(2) Uani 1 1 d . . . H12A H -0.0815 0.6588 0.6563 0.09 Uiso 1 1 calc R . . H12B H 0.0297 0.6304 0.6846 0.09 Uiso 1 1 calc R . . H12C H -0.066 0.5754 0.671 0.09 Uiso 1 1 calc R . . C13 C -0.0893(6) 0.5851(5) 0.5540(4) 0.078(3) Uani 1 1 d . . . H13A H -0.1408 0.6245 0.5521 0.117 Uiso 1 1 calc R . . H13B H -0.1228 0.5417 0.5686 0.117 Uiso 1 1 calc R . . H13C H -0.065 0.5759 0.5149 0.117 Uiso 1 1 calc R . . C14 C 0.2093(4) 0.1804(3) 0.5512(2) 0.0296(15) Uani 1 1 d . . . C15 C 0.1057(5) 0.1984(4) 0.5298(3) 0.0346(16) Uani 1 1 d . . . H15 H 0.0706 0.2385 0.5454 0.042 Uiso 1 1 calc R . . C16 C 0.0551(5) 0.1575(4) 0.4857(2) 0.0344(16) Uani 1 1 d . . . H16 H -0.0156 0.1694 0.4726 0.041 Uiso 1 1 calc R . . C17 C 0.1041(5) 0.1001(4) 0.4604(3) 0.0343(16) Uani 1 1 d . . . C18 C 0.2043(5) 0.0814(4) 0.4837(3) 0.0385(17) Uani 1 1 d . . . H18 H 0.2391 0.041 0.4683 0.046 Uiso 1 1 calc R . . C19 C 0.2547(5) 0.1202(3) 0.5288(3) 0.0344(16) Uani 1 1 d . . . H19 H 0.3223 0.1048 0.5447 0.041 Uiso 1 1 calc R . . C20 C 0.0525(5) 0.0626(4) 0.4060(3) 0.0480(19) Uani 1 1 d . . . C21 C 0.0696(10) 0.1118(7) 0.3537(4) 0.129(5) Uani 1 1 d . . . H21A H 0.0394 0.1592 0.3608 0.193 Uiso 1 1 calc R . . H21B H 0.0346 0.091 0.3182 0.193 Uiso 1 1 calc R . . H21C H 0.1458 0.1165 0.3486 0.193 Uiso 1 1 calc R . . C22 C -0.0653(6) 0.0550(6) 0.4098(4) 0.095(4) Uani 1 1 d . . . H22A H -0.0964 0.1022 0.4167 0.143 Uiso 1 1 calc R . . H22B H -0.0799 0.0227 0.4421 0.143 Uiso 1 1 calc R . . H22C H -0.0965 0.0352 0.373 0.143 Uiso 1 1 calc R . . C23 C 0.0981(8) -0.0089(6) 0.3949(5) 0.130(5) Uani 1 1 d . . . H23A H 0.0623 -0.0296 0.3596 0.196 Uiso 1 1 calc R . . H23B H 0.0881 -0.0404 0.4284 0.196 Uiso 1 1 calc R . . H23C H 0.174 -0.0039 0.3892 0.196 Uiso 1 1 calc R . . C24 C 0.2934(6) 0.4592(5) 0.7410(3) 0.067(2) Uani 1 1 d . . . H24A H 0.251 0.4873 0.7119 0.101 Uiso 1 1 calc R . . H24B H 0.3147 0.4899 0.7745 0.101 Uiso 1 1 calc R . . H24C H 0.2512 0.4189 0.7542 0.101 Uiso 1 1 calc R . . C25 C 0.4929(6) 0.5011(4) 0.6814(3) 0.054(2) Uani 1 1 d . . . H25A H 0.5561 0.4824 0.6637 0.08 Uiso 1 1 calc R . . H25B H 0.5146 0.5324 0.7144 0.08 Uiso 1 1 calc R . . H25C H 0.4501 0.5287 0.652 0.08 Uiso 1 1 calc R . . C26 C 0.4922(6) 0.3717(4) 0.7639(3) 0.0495(19) Uani 1 1 d . . . H26A H 0.5559 0.353 0.7467 0.074 Uiso 1 1 calc R . . H26B H 0.4496 0.3315 0.7771 0.074 Uiso 1 1 calc R . . H26C H 0.5131 0.4025 0.7973 0.074 Uiso 1 1 calc R . . C27 C 0.1371(5) 0.1288(4) 0.6754(3) 0.053(2) Uani 1 1 d . . . H27A H 0.1145 0.1147 0.6353 0.079 Uiso 1 1 calc R . . H27B H 0.1069 0.1758 0.684 0.079 Uiso 1 1 calc R . . H27C H 0.1124 0.0931 0.7029 0.079 Uiso 1 1 calc R . . C28 C 0.3172(5) 0.1612(4) 0.7607(3) 0.051(2) Uani 1 1 d . . . H28A H 0.3944 0.165 0.7677 0.076 Uiso 1 1 calc R . . H28B H 0.2899 0.125 0.7869 0.076 Uiso 1 1 calc R . . H28C H 0.2845 0.2077 0.7681 0.076 Uiso 1 1 calc R . . C29 C 0.3409(6) 0.0438(4) 0.6699(3) 0.052(2) Uani 1 1 d . . . H29A H 0.4185 0.0463 0.6738 0.078 Uiso 1 1 calc R . . H29B H 0.3181 0.0276 0.6304 0.078 Uiso 1 1 calc R . . H29C H 0.3158 0.0099 0.6987 0.078 Uiso 1 1 calc R . . C30 C 0.5984(6) 0.1715(4) 0.7322(3) 0.056(2) Uani 1 1 d . . . H30A H 0.5673 0.1467 0.6975 0.084 Uiso 1 1 calc R . . H30B H 0.5451 0.203 0.7482 0.084 Uiso 1 1 calc R . . H30C H 0.6222 0.1361 0.7619 0.084 Uiso 1 1 calc R . . C31 C 0.7687(6) 0.2720(5) 0.7798(3) 0.071(3) Uani 1 1 d . . . H31A H 0.83 0.3014 0.7708 0.107 Uiso 1 1 calc R . . H31B H 0.7907 0.2359 0.8092 0.107 Uiso 1 1 calc R . . H31C H 0.7139 0.3028 0.7951 0.107 Uiso 1 1 calc R . . C32 C 0.8180(6) 0.1610(5) 0.6909(4) 0.076(3) Uani 1 1 d . . . H32A H 0.8809 0.1874 0.6798 0.113 Uiso 1 1 calc R . . H32B H 0.7903 0.1319 0.6577 0.113 Uiso 1 1 calc R . . H32C H 0.8373 0.1297 0.7243 0.113 Uiso 1 1 calc R . . C33 C 0.6682(6) 0.3940(4) 0.5673(3) 0.067(2) Uani 1 1 d . . . H33A H 0.6008 0.4122 0.5803 0.1 Uiso 1 1 calc R . . H33B H 0.6542 0.3591 0.5357 0.1 Uiso 1 1 calc R . . H33C H 0.7098 0.4341 0.5529 0.1 Uiso 1 1 calc R . . C34 C 0.7805(6) 0.4224(4) 0.6851(3) 0.064(2) Uani 1 1 d . . . H34A H 0.821 0.4015 0.7188 0.095 Uiso 1 1 calc R . . H34B H 0.7156 0.4445 0.6982 0.095 Uiso 1 1 calc R . . H34C H 0.8236 0.4589 0.667 0.095 Uiso 1 1 calc R . . C35 C 0.8726(6) 0.3167(5) 0.6019(4) 0.079(3) Uani 1 1 d . . . H35A H 0.9147 0.2928 0.6336 0.118 Uiso 1 1 calc R . . H35B H 0.9126 0.3575 0.5876 0.118 Uiso 1 1 calc R . . H35C H 0.8573 0.2827 0.5698 0.118 Uiso 1 1 calc R . . C36 C 0.5831(5) 0.1130(4) 0.5737(3) 0.0469(18) Uani 1 1 d . . . H36A H 0.6156 0.1439 0.6045 0.07 Uiso 1 1 calc R . . H36B H 0.626 0.0695 0.5703 0.07 Uiso 1 1 calc R . . H36C H 0.5113 0.0998 0.5836 0.07 Uiso 1 1 calc R . . C37 C 0.5140(6) 0.0995(4) 0.4467(3) 0.055(2) Uani 1 1 d . . . H37A H 0.5085 0.1227 0.4082 0.082 Uiso 1 1 calc R . . H37B H 0.443 0.0864 0.4581 0.082 Uiso 1 1 calc R . . H37C H 0.5577 0.0562 0.4449 0.082 Uiso 1 1 calc R . . C38 C 0.7175(5) 0.1761(5) 0.4834(3) 0.065(2) Uani 1 1 d . . . H38A H 0.7528 0.2091 0.5117 0.097 Uiso 1 1 calc R . . H38B H 0.7192 0.1963 0.4439 0.097 Uiso 1 1 calc R . . H38C H 0.7544 0.1298 0.4849 0.097 Uiso 1 1 calc R . . C39 C 0.5537(6) 0.2987(5) 0.3939(3) 0.058(2) Uani 1 1 d . . . H39A H 0.6207 0.3187 0.4105 0.087 Uiso 1 1 calc R . . H39B H 0.5242 0.3303 0.3628 0.087 Uiso 1 1 calc R . . H39C H 0.5667 0.251 0.3776 0.087 Uiso 1 1 calc R . . C40 C 0.4267(6) 0.3854(4) 0.4730(3) 0.060(2) Uani 1 1 d . . . H40A H 0.4905 0.4078 0.4915 0.09 Uiso 1 1 calc R . . H40B H 0.3701 0.3857 0.5005 0.09 Uiso 1 1 calc R . . H40C H 0.4036 0.4122 0.4377 0.09 Uiso 1 1 calc R . . C41 C 0.3321(6) 0.2523(4) 0.4179(3) 0.055(2) Uani 1 1 d . . . H41A H 0.2793 0.2474 0.4473 0.083 Uiso 1 1 calc R . . H41B H 0.3468 0.205 0.4015 0.083 Uiso 1 1 calc R . . H41C H 0.3045 0.2843 0.3866 0.083 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 Ce 0.0268(2) 0.0333(2) 0.0262(2) -0.00196(17) 0.00024(13) -0.00014(18) Si1 0.0426(11) 0.0380(13) 0.0336(10) -0.0088(8) -0.0014(8) 0.0017(9) Si2 0.0366(10) 0.0412(13) 0.0299(10) 0.0021(8) 0.0003(8) -0.0046(9) Si3 0.0381(11) 0.0546(15) 0.0410(11) -0.0011(10) -0.0076(8) 0.0036(10) Si4 0.0405(11) 0.0547(15) 0.0419(11) -0.0096(10) 0.0058(9) -0.0162(10) Si5 0.0397(11) 0.0456(14) 0.0355(10) -0.0076(9) 0.0059(8) 0.0014(9) Si6 0.0463(11) 0.0493(14) 0.0306(10) 0.0050(9) 0.0026(8) -0.0018(9) N1 0.029(3) 0.040(4) 0.028(3) -0.002(2) 0.004(2) 0.001(2) N2 0.031(3) 0.041(4) 0.029(3) 0.000(2) 0.002(2) 0.001(2) N3 0.032(3) 0.035(4) 0.026(3) -0.003(2) -0.007(2) -0.007(2) N4 0.027(3) 0.034(3) 0.022(3) 0.003(2) -0.002(2) 0.000(2) C1 0.048(4) 0.019(4) 0.032(3) 0.000(3) 0.007(3) -0.004(3) C2 0.040(4) 0.028(5) 0.027(3) -0.001(3) 0.006(3) 0.002(3) C3 0.022(3) 0.034(5) 0.028(3) 0.000(3) 0.001(3) -0.003(3) C4 0.030(4) 0.028(4) 0.037(4) -0.004(3) -0.005(3) 0.001(3) C5 0.032(4) 0.033(5) 0.037(4) 0.004(3) 0.000(3) -0.001(3) C6 0.046(4) 0.031(5) 0.040(4) 0.001(3) 0.000(3) -0.002(3) C7 0.041(4) 0.030(5) 0.038(4) 0.000(3) -0.004(3) 0.002(3) C8 0.026(4) 0.043(5) 0.063(5) -0.002(4) 0.001(3) 0.007(3) C9 0.036(4) 0.037(5) 0.060(5) 0.005(4) 0.003(3) -0.007(3) C10 0.041(4) 0.043(5) 0.047(4) -0.005(3) -0.004(3) 0.016(3) C11 0.087(6) 0.041(6) 0.074(5) 0.010(4) 0.010(5) 0.019(5) C12 0.071(5) 0.052(6) 0.058(5) 0.001(4) 0.007(4) 0.020(4) C13 0.065(5) 0.084(7) 0.079(6) -0.019(5) -0.039(5) 0.033(5) C14 0.031(4) 0.034(4) 0.024(3) 0.001(3) -0.001(3) 0.001(3) C15 0.036(4) 0.031(4) 0.036(4) -0.001(3) -0.006(3) 0.004(3) C16 0.026(3) 0.040(5) 0.037(4) 0.000(3) -0.004(3) -0.004(3) C17 0.035(4) 0.032(4) 0.037(4) -0.005(3) 0.003(3) 0.000(3) C18 0.039(4) 0.040(5) 0.037(4) -0.007(3) 0.002(3) 0.001(3) C19 0.033(4) 0.034(5) 0.036(4) 0.005(3) -0.003(3) 0.005(3) C20 0.046(4) 0.055(6) 0.042(4) -0.010(4) -0.003(3) -0.003(4) C21 0.192(12) 0.141(12) 0.052(6) -0.019(6) -0.011(7) -0.085(10) C22 0.050(5) 0.133(10) 0.100(7) -0.074(7) -0.017(5) -0.008(5) C23 0.109(8) 0.113(10) 0.159(10) -0.104(8) -0.079(7) 0.047(7) C24 0.067(5) 0.082(7) 0.053(5) -0.021(4) 0.006(4) 0.013(5) C25 0.064(5) 0.042(5) 0.053(4) -0.009(4) -0.013(4) -0.006(4) C26 0.065(5) 0.042(5) 0.040(4) -0.005(3) -0.006(3) 0.003(4) C27 0.042(4) 0.075(6) 0.042(4) 0.008(4) 0.001(3) -0.019(4) C28 0.051(4) 0.061(6) 0.039(4) 0.001(4) 0.002(3) -0.008(4) C29 0.075(5) 0.035(5) 0.046(4) 0.008(3) 0.003(4) -0.004(4) C30 0.071(5) 0.057(6) 0.040(4) 0.005(4) 0.007(4) -0.005(4) C31 0.070(5) 0.089(7) 0.050(5) -0.009(5) -0.023(4) 0.003(5) C32 0.058(5) 0.088(8) 0.079(6) -0.006(5) -0.009(4) 0.024(5) C33 0.089(6) 0.063(6) 0.049(5) 0.007(4) 0.001(4) -0.028(5) C34 0.066(5) 0.061(6) 0.064(5) -0.018(4) 0.006(4) -0.023(4) C35 0.056(5) 0.103(8) 0.081(6) -0.039(5) 0.030(4) -0.035(5) C36 0.050(4) 0.045(5) 0.045(4) -0.001(3) 0.002(3) 0.009(4) C37 0.068(5) 0.051(6) 0.045(4) -0.018(4) 0.007(4) 0.003(4) C38 0.050(5) 0.075(7) 0.070(5) -0.005(5) 0.017(4) 0.004(4) C39 0.062(5) 0.073(6) 0.040(4) 0.005(4) 0.008(4) -0.003(4) C40 0.073(5) 0.050(6) 0.058(5) 0.014(4) 0.007(4) 0.002(4) C41 0.061(5) 0.061(6) 0.044(4) 0.005(4) -0.006(4) -0.003(4) #----------------------------------------------------------------------------# # 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 Ce N2 2.370(5) . ? Ce N1 2.400(5) . ? Ce N4 2.455(5) . ? Ce N3 2.479(5) . ? Si1 N3 1.764(5) . ? Si1 C24 1.843(7) . ? Si1 C26 1.863(6) . ? Si1 C25 1.870(7) . ? Si2 N4 1.739(5) . ? Si2 C29 1.857(7) . ? Si2 C27 1.863(6) . ? Si2 C28 1.871(6) . ? Si3 N1 1.708(5) . ? Si3 C30 1.866(7) . ? Si3 C32 1.872(8) . ? Si3 C31 1.872(7) . ? Si4 N1 1.700(5) . ? Si4 C33 1.870(7) . ? Si4 C35 1.882(8) . ? Si4 C34 1.888(7) . ? Si5 N2 1.709(5) . ? Si5 C37 1.866(7) . ? Si5 C38 1.873(7) . ? Si5 C36 1.887(7) . ? Si6 N2 1.721(5) . ? Si6 C41 1.869(7) . ? Si6 C40 1.868(8) . ? Si6 C39 1.882(7) . ? N3 C1 1.325(7) . ? N4 C3 1.368(7) . ? C1 C2 1.442(8) . ? C1 C4 1.501(8) . ? C2 C3 1.386(8) . ? C3 C14 1.504(8) . ? C4 C5 1.376(9) . ? C4 C9 1.403(8) . ? C5 C6 1.393(9) . ? C6 C7 1.402(9) . ? C7 C8 1.379(9) . ? C7 C10 1.535(9) . ? C8 C9 1.379(9) . ? C10 C12 1.532(10) . ? C10 C11 1.532(10) . ? C10 C13 1.558(9) . ? C14 C19 1.373(8) . ? C14 C15 1.409(8) . ? C15 C16 1.388(8) . ? C16 C17 1.381(8) . ? C17 C18 1.387(8) . ? C17 C20 1.537(9) . ? C18 C19 1.383(8) . ? C20 C23 1.478(11) . ? C20 C22 1.502(10) . ? C20 C21 1.534(12) . ? 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 Ce N1 108.37(16) . . ? N2 Ce N4 104.88(16) . . ? N1 Ce N4 135.75(15) . . ? N2 Ce N3 124.05(16) . . ? N1 Ce N3 105.25(15) . . ? N4 Ce N3 78.21(16) . . ? N3 Si1 C24 114.0(3) . . ? N3 Si1 C26 103.7(3) . . ? C24 Si1 C26 108.8(3) . . ? N3 Si1 C25 110.0(3) . . ? C24 Si1 C25 109.9(4) . . ? C26 Si1 C25 110.3(3) . . ? N4 Si2 C29 112.7(3) . . ? N4 Si2 C27 112.3(3) . . ? C29 Si2 C27 109.1(4) . . ? N4 Si2 C28 107.7(3) . . ? C29 Si2 C28 109.4(3) . . ? C27 Si2 C28 105.2(3) . . ? N1 Si3 C30 107.2(3) . . ? N1 Si3 C32 114.8(3) . . ? C30 Si3 C32 106.3(4) . . ? N1 Si3 C31 114.9(3) . . ? C30 Si3 C31 106.9(4) . . ? C32 Si3 C31 106.2(4) . . ? N1 Si4 C33 109.2(3) . . ? N1 Si4 C35 113.3(4) . . ? C33 Si4 C35 107.1(4) . . ? N1 Si4 C34 113.7(3) . . ? C33 Si4 C34 106.7(4) . . ? C35 Si4 C34 106.5(4) . . ? N2 Si5 C37 115.5(3) . . ? N2 Si5 C38 114.0(3) . . ? C37 Si5 C38 107.4(3) . . ? N2 Si5 C36 107.7(3) . . ? C37 Si5 C36 105.8(3) . . ? C38 Si5 C36 105.6(3) . . ? N2 Si6 C41 113.3(3) . . ? N2 Si6 C40 113.0(3) . . ? C41 Si6 C40 106.6(3) . . ? N2 Si6 C39 111.6(3) . . ? C41 Si6 C39 106.9(3) . . ? C40 Si6 C39 104.8(4) . . ? Si4 N1 Si3 123.3(3) . . ? Si4 N1 Ce 118.0(2) . . ? Si3 N1 Ce 118.6(3) . . ? Si5 N2 Si6 121.9(3) . . ? Si5 N2 Ce 110.6(2) . . ? Si6 N2 Ce 127.5(3) . . ? C1 N3 Si1 126.3(4) . . ? C1 N3 Ce 102.3(4) . . ? Si1 N3 Ce 131.1(2) . . ? C3 N4 Si2 121.0(4) . . ? C3 N4 Ce 93.4(3) . . ? Si2 N4 Ce 145.3(2) . . ? N3 C1 C2 123.3(6) . . ? N3 C1 C4 122.0(5) . . ? C2 C1 C4 114.6(5) . . ? C3 C2 C1 129.2(5) . . ? N4 C3 C2 124.9(5) . . ? N4 C3 C14 120.3(6) . . ? C2 C3 C14 114.7(5) . . ? C5 C4 C9 118.8(6) . . ? C5 C4 C1 123.3(6) . . ? C9 C4 C1 117.9(6) . . ? C4 C5 C6 120.4(6) . . ? C5 C6 C7 121.6(6) . . ? C8 C7 C6 116.6(6) . . ? C8 C7 C10 120.2(6) . . ? C6 C7 C10 123.2(6) . . ? C9 C8 C7 122.8(6) . . ? C8 C9 C4 119.8(7) . . ? C12 C10 C11 109.2(6) . . ? C12 C10 C7 109.1(5) . . ? C11 C10 C7 112.8(6) . . ? C12 C10 C13 109.1(6) . . ? C11 C10 C13 108.4(6) . . ? C7 C10 C13 108.3(6) . . ? C19 C14 C15 117.8(5) . . ? C19 C14 C3 120.1(5) . . ? C15 C14 C3 121.9(6) . . ? C16 C15 C14 119.9(6) . . ? C17 C16 C15 122.1(6) . . ? C16 C17 C18 117.1(5) . . ? C16 C17 C20 120.9(5) . . ? C18 C17 C20 121.9(6) . . ? C17 C18 C19 121.5(6) . . ? C14 C19 C18 121.4(6) . . ? C23 C20 C22 108.9(8) . . ? C23 C20 C17 113.5(6) . . ? C22 C20 C17 111.6(6) . . ? C23 C20 C21 109.1(8) . . ? C22 C20 C21 106.8(8) . . ? C17 C20 C21 106.7(6) . . ? #===END data_(16)-aug701 _database_code_depnum_ccdc_archive 'CCDC 229460' _audit_creation_date 2001-08-08T11:24:00-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[CeCl{Me3SiNC(Ph)CHC(Ph)NSiMe3}2]' _chemical_formula_moiety 'C42 H58 Ce1 Cl1 N4 Si4' _chemical_formula_sum 'C42 H58 Ce Cl N4 Si4' _chemical_formula_weight 906.85 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9825(9) _cell_length_b 12.4284(10) _cell_length_c 15.9086(15) _cell_angle_alpha 94.607(4) _cell_angle_beta 94.084(5) _cell_angle_gamma 90.114(4) _cell_volume 2355.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9822 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 938 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.156 _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 0.874 _exptl_absorpt_correction_T_max 0.911 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 15186 _diffrn_reflns_av_R_equivalents 0.0917 _diffrn_reflns_av_unetI/netI 0.1599 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 8244 _reflns_number_gt 5313 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+2.0647P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 8244 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1252 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1271 _refine_ls_wR_factor_gt 0.107 _refine_ls_goodness_of_fit_ref 1.01 _refine_ls_restrained_S_all 1.01 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.605 _refine_diff_density_min -0.942 _refine_diff_density_rms 0.138 #----------------------------------------------------------------------------# # 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' Ce Ce -0.2486 2.6331 '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' 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 Ce Ce 0.66841(3) 0.66759(3) 0.73347(3) 0.02648(14) Uani 1 1 d . . . Cl Cl 0.49752(14) 0.52792(14) 0.69004(13) 0.0429(5) Uani 1 1 d . . . Si1 Si 0.68775(16) 0.82307(16) 0.53847(14) 0.0348(5) Uani 1 1 d . . . Si2 Si 0.78024(16) 0.41867(15) 0.59944(14) 0.0331(5) Uani 1 1 d . . . Si3 Si 0.72237(16) 0.58104(16) 0.95671(14) 0.0347(5) Uani 1 1 d . . . Si4 Si 0.39320(15) 0.79896(16) 0.80922(14) 0.0348(5) Uani 1 1 d . . . N1 N 0.7472(4) 0.7756(4) 0.6318(4) 0.0304(14) Uani 1 1 d . . . N2 N 0.7992(4) 0.5422(4) 0.6612(4) 0.0275(14) Uani 1 1 d . . . N3 N 0.7304(4) 0.6759(4) 0.8823(4) 0.0272(14) Uani 1 1 d . . . N4 N 0.5385(4) 0.7971(4) 0.8019(4) 0.0267(14) Uani 1 1 d . . . C1 C 0.8512(5) 0.7859(5) 0.6670(5) 0.0291(18) Uani 1 1 d . . . C2 C 0.9078(5) 0.7038(5) 0.7091(5) 0.0269(17) Uani 1 1 d . . . H2 H 0.9619 0.7278 0.7532 0.032 Uiso 1 1 calc R . . C3 C 0.8942(5) 0.5897(5) 0.6940(4) 0.0254(16) Uani 1 1 d . . . C4 C 0.5422(6) 0.7673(7) 0.5307(6) 0.053(2) Uani 1 1 d . . . H4A H 0.502 0.7989 0.5781 0.08 Uiso 1 1 calc R . . H4B H 0.5449 0.6887 0.5326 0.08 Uiso 1 1 calc R . . H4C H 0.5034 0.7849 0.4773 0.08 Uiso 1 1 calc R . . C5 C 0.7690(7) 0.7661(7) 0.4511(6) 0.062(3) Uani 1 1 d . . . H5A H 0.8446 0.7973 0.4573 0.093 Uiso 1 1 calc R . . H5B H 0.732 0.7833 0.397 0.093 Uiso 1 1 calc R . . H5C H 0.7735 0.6876 0.4528 0.093 Uiso 1 1 calc R . . C6 C 0.6803(7) 0.9725(6) 0.5313(6) 0.054(2) Uani 1 1 d . . . H6A H 0.6379 1.0051 0.5771 0.081 Uiso 1 1 calc R . . H6B H 0.643 0.9876 0.4767 0.081 Uiso 1 1 calc R . . H6C H 0.7562 1.0031 0.5363 0.081 Uiso 1 1 calc R . . C7 C 0.6855(6) 0.4513(6) 0.5084(5) 0.051(2) Uani 1 1 d . . . H7A H 0.7216 0.5047 0.4769 0.076 Uiso 1 1 calc R . . H7B H 0.6158 0.481 0.5288 0.076 Uiso 1 1 calc R . . H7C H 0.6691 0.3857 0.4712 0.076 Uiso 1 1 calc R . . C8 C 0.7134(6) 0.3168(6) 0.6593(6) 0.048(2) Uani 1 1 d . . . H8A H 0.7642 0.2997 0.7074 0.072 Uiso 1 1 calc R . . H8B H 0.6971 0.2511 0.6222 0.072 Uiso 1 1 calc R . . H8C H 0.6436 0.3459 0.6801 0.072 Uiso 1 1 calc R . . C9 C 0.9110(6) 0.3640(6) 0.5554(5) 0.046(2) Uani 1 1 d . . . H9A H 0.9637 0.3451 0.6017 0.069 Uiso 1 1 calc R . . H9B H 0.9449 0.4188 0.524 0.069 Uiso 1 1 calc R . . H9C H 0.8928 0.2995 0.5173 0.069 Uiso 1 1 calc R . . C10 C 0.9143(5) 0.8908(5) 0.6665(5) 0.0299(18) Uani 1 1 d . . . C11 C 0.8651(6) 0.9875(6) 0.6932(5) 0.039(2) Uani 1 1 d . . . H11 H 0.7907 0.9876 0.7104 0.047 Uiso 1 1 calc R . . C12 C 0.9241(6) 1.0842(5) 0.6947(5) 0.042(2) Uani 1 1 d . . . H12 H 0.8894 1.1501 0.7122 0.05 Uiso 1 1 calc R . . C13 C 1.0315(7) 1.0853(6) 0.6713(6) 0.054(3) Uani 1 1 d . . . H13 H 1.0719 1.1514 0.6736 0.065 Uiso 1 1 calc R . . C14 C 1.0805(7) 0.9902(7) 0.6445(6) 0.059(3) Uani 1 1 d . . . H14 H 1.1543 0.9909 0.6265 0.07 Uiso 1 1 calc R . . C15 C 1.0227(6) 0.8925(6) 0.6435(5) 0.043(2) Uani 1 1 d . . . H15 H 1.0584 0.8268 0.6269 0.052 Uiso 1 1 calc R . . C16 C 0.9935(5) 0.5223(5) 0.7188(5) 0.0277(17) Uani 1 1 d . . . C17 C 0.9805(6) 0.4337(6) 0.7662(5) 0.039(2) Uani 1 1 d . . . H17 H 0.9095 0.4179 0.7854 0.047 Uiso 1 1 calc R . . C18 C 1.0705(7) 0.3696(6) 0.7848(5) 0.045(2) Uani 1 1 d . . . H18 H 1.0615 0.3095 0.8172 0.054 Uiso 1 1 calc R . . C19 C 1.1733(7) 0.3916(7) 0.7571(5) 0.049(2) Uani 1 1 d . . . H19 H 1.2349 0.346 0.7693 0.059 Uiso 1 1 calc R . . C20 C 1.1872(6) 0.4793(7) 0.7119(6) 0.046(2) Uani 1 1 d . . . H20 H 1.2585 0.4948 0.693 0.055 Uiso 1 1 calc R . . C21 C 1.0988(5) 0.5443(6) 0.6939(5) 0.0360(19) Uani 1 1 d . . . H21 H 1.1097 0.6059 0.6638 0.043 Uiso 1 1 calc R . . C22 C 0.7714(5) 0.7756(5) 0.8939(4) 0.0279(17) Uani 1 1 d . . . C23 C 0.7263(5) 0.8628(5) 0.8514(4) 0.0249(16) Uani 1 1 d . . . H23 H 0.7773 0.9185 0.8421 0.03 Uiso 1 1 calc R . . C24 C 0.6131(6) 0.8767(5) 0.8210(4) 0.0271(17) Uani 1 1 d . . . C25 C 0.6391(8) 0.4680(6) 0.9003(6) 0.072(3) Uani 1 1 d . . . H25A H 0.5673 0.4952 0.8778 0.109 Uiso 1 1 calc R . . H25B H 0.6257 0.4134 0.9397 0.109 Uiso 1 1 calc R . . H25C H 0.6802 0.4356 0.8537 0.109 Uiso 1 1 calc R . . C26 C 0.8558(6) 0.5245(6) 0.9980(5) 0.048(2) Uani 1 1 d . . . H26A H 0.9018 0.5822 1.0285 0.071 Uiso 1 1 calc R . . H26B H 0.8958 0.4918 0.9508 0.071 Uiso 1 1 calc R . . H26C H 0.8405 0.4694 1.0365 0.071 Uiso 1 1 calc R . . C27 C 0.6473(7) 0.6464(7) 1.0453(6) 0.062(3) Uani 1 1 d . . . H27A H 0.6933 0.7056 1.074 0.094 Uiso 1 1 calc R . . H27B H 0.6332 0.5931 1.0856 0.094 Uiso 1 1 calc R . . H27C H 0.576 0.675 1.0231 0.094 Uiso 1 1 calc R . . C28 C 0.3617(6) 0.6816(6) 0.8689(5) 0.047(2) Uani 1 1 d . . . H28A H 0.4015 0.6899 0.925 0.07 Uiso 1 1 calc R . . H28B H 0.3859 0.6151 0.8383 0.07 Uiso 1 1 calc R . . H28C H 0.281 0.6777 0.8749 0.07 Uiso 1 1 calc R . . C29 C 0.3408(6) 0.9224(6) 0.8699(6) 0.056(3) Uani 1 1 d . . . H29A H 0.356 0.9864 0.8402 0.084 Uiso 1 1 calc R . . H29B H 0.3791 0.9298 0.9266 0.084 Uiso 1 1 calc R . . H29C H 0.2601 0.9153 0.8745 0.084 Uiso 1 1 calc R . . C30 C 0.3169(6) 0.7829(6) 0.7027(5) 0.049(2) Uani 1 1 d . . . H30A H 0.3334 0.8448 0.671 0.074 Uiso 1 1 calc R . . H30B H 0.2362 0.7791 0.7089 0.074 Uiso 1 1 calc R . . H30C H 0.3409 0.7164 0.672 0.074 Uiso 1 1 calc R . . C31 C 0.8711(5) 0.8038(5) 0.9537(5) 0.0292(18) Uani 1 1 d . . . C32 C 0.8635(7) 0.8839(6) 1.0201(5) 0.048(2) Uani 1 1 d . . . H32 H 0.7954 0.9218 1.0262 0.058 Uiso 1 1 calc R . . C33 C 0.9562(7) 0.9086(6) 1.0778(6) 0.053(2) Uani 1 1 d . . . H33 H 0.9496 0.9611 1.124 0.064 Uiso 1 1 calc R . . C34 C 1.0555(7) 0.8574(6) 1.0677(6) 0.050(2) Uani 1 1 d . . . H34 H 1.1189 0.8763 1.1053 0.06 Uiso 1 1 calc R . . C35 C 1.0635(6) 0.7789(7) 1.0031(6) 0.054(2) Uani 1 1 d . . . H35 H 1.1323 0.7421 0.9971 0.065 Uiso 1 1 calc R . . C36 C 0.9720(6) 0.7519(6) 0.9460(5) 0.041(2) Uani 1 1 d . . . H36 H 0.9793 0.6973 0.9014 0.049 Uiso 1 1 calc R . . C37 C 0.5800(5) 0.9930(5) 0.8099(5) 0.0281(17) Uani 1 1 d . . . C38 C 0.6084(6) 1.0755(6) 0.8721(5) 0.043(2) Uani 1 1 d . . . H38 H 0.6507 1.0601 0.9225 0.052 Uiso 1 1 calc R . . C39 C 0.5750(8) 1.1799(6) 0.8607(7) 0.059(3) Uani 1 1 d . . . H39 H 0.5944 1.2357 0.9036 0.07 Uiso 1 1 calc R . . C40 C 0.5151(8) 1.2043(7) 0.7891(6) 0.057(3) Uani 1 1 d . . . H40 H 0.4919 1.2763 0.7823 0.068 Uiso 1 1 calc R . . C41 C 0.4884(7) 1.1240(7) 0.7268(6) 0.051(2) Uani 1 1 d . . . H41 H 0.4485 1.1403 0.6757 0.061 Uiso 1 1 calc R . . C42 C 0.5196(6) 1.0194(6) 0.7387(5) 0.040(2) Uani 1 1 d . . . H42 H 0.4985 0.9639 0.6959 0.048 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 Ce 0.0218(2) 0.0261(2) 0.0311(3) -0.00127(17) 0.00286(17) -0.00025(16) Cl 0.0274(9) 0.0435(11) 0.0558(15) -0.0061(10) 0.0004(9) -0.0055(9) Si1 0.0307(11) 0.0376(12) 0.0366(15) 0.0067(10) 0.0012(10) 0.0013(10) Si2 0.0311(11) 0.0284(11) 0.0384(15) -0.0057(10) 0.0030(10) -0.0010(9) Si3 0.0338(11) 0.0353(11) 0.0355(14) 0.0065(10) 0.0030(10) -0.0025(10) Si4 0.0246(10) 0.0384(12) 0.0417(15) 0.0007(10) 0.0075(10) 0.0043(10) N1 0.023(3) 0.035(3) 0.034(4) 0.008(3) -0.001(3) 0.003(3) N2 0.021(3) 0.027(3) 0.034(4) -0.002(3) 0.003(3) -0.006(3) N3 0.022(3) 0.026(3) 0.033(4) 0.000(3) 0.003(3) 0.001(3) N4 0.028(3) 0.024(3) 0.027(4) -0.003(3) 0.001(3) 0.007(3) C1 0.024(4) 0.031(4) 0.031(5) -0.006(3) 0.006(3) 0.007(3) C2 0.016(3) 0.030(4) 0.032(5) -0.007(3) -0.001(3) 0.003(3) C3 0.025(4) 0.028(4) 0.024(5) 0.003(3) 0.003(3) 0.002(3) C4 0.037(4) 0.068(6) 0.056(7) 0.020(5) -0.008(4) 0.000(4) C5 0.078(6) 0.062(6) 0.048(7) 0.004(5) 0.015(5) 0.010(5) C6 0.065(6) 0.051(5) 0.049(6) 0.015(4) 0.004(5) 0.008(4) C7 0.055(5) 0.051(5) 0.043(6) -0.003(4) -0.007(4) -0.011(4) C8 0.040(4) 0.037(4) 0.067(7) 0.003(4) 0.007(4) -0.004(4) C9 0.047(5) 0.044(5) 0.044(6) -0.014(4) 0.010(4) -0.002(4) C10 0.021(4) 0.029(4) 0.040(5) 0.008(3) 0.000(3) -0.004(3) C11 0.034(4) 0.037(4) 0.047(6) 0.003(4) 0.006(4) 0.003(4) C12 0.044(5) 0.020(4) 0.063(6) 0.010(4) 0.002(4) -0.001(4) C13 0.051(5) 0.034(5) 0.078(7) 0.007(5) 0.007(5) -0.014(4) C14 0.042(5) 0.055(6) 0.083(8) 0.013(5) 0.020(5) -0.010(5) C15 0.035(4) 0.030(4) 0.066(7) 0.000(4) 0.013(4) 0.002(4) C16 0.022(4) 0.030(4) 0.031(5) 0.001(3) 0.003(3) -0.001(3) C17 0.043(5) 0.038(4) 0.035(5) -0.004(4) 0.004(4) -0.003(4) C18 0.053(5) 0.037(5) 0.044(6) 0.000(4) 0.003(4) 0.016(4) C19 0.044(5) 0.058(6) 0.039(6) -0.007(5) -0.017(4) 0.025(4) C20 0.030(4) 0.052(5) 0.053(6) -0.005(5) -0.002(4) 0.000(4) C21 0.027(4) 0.038(4) 0.043(6) 0.003(4) 0.004(4) 0.004(4) C22 0.022(4) 0.037(4) 0.025(5) -0.002(3) 0.003(3) -0.001(3) C23 0.029(4) 0.022(4) 0.024(4) 0.005(3) 0.001(3) -0.005(3) C24 0.036(4) 0.028(4) 0.017(4) -0.003(3) 0.005(3) 0.002(3) C25 0.095(7) 0.051(5) 0.071(8) 0.023(5) -0.012(6) -0.037(6) C26 0.066(5) 0.041(5) 0.036(6) 0.006(4) 0.005(4) 0.015(4) C27 0.052(5) 0.098(7) 0.044(6) 0.030(5) 0.022(5) 0.023(5) C28 0.033(4) 0.055(5) 0.052(6) 0.000(4) 0.010(4) -0.003(4) C29 0.052(5) 0.056(5) 0.062(7) -0.014(5) 0.034(5) -0.002(4) C30 0.030(4) 0.052(5) 0.065(7) 0.002(5) -0.006(4) 0.003(4) C31 0.027(4) 0.024(4) 0.036(5) 0.006(3) -0.002(3) -0.006(3) C32 0.050(5) 0.043(5) 0.050(6) 0.000(4) -0.007(4) 0.000(4) C33 0.063(6) 0.044(5) 0.047(6) -0.008(4) -0.021(5) -0.001(5) C34 0.045(5) 0.045(5) 0.056(7) 0.008(5) -0.023(5) -0.012(4) C35 0.036(5) 0.056(6) 0.072(8) 0.018(5) -0.001(5) 0.002(4) C36 0.029(4) 0.048(5) 0.043(6) 0.000(4) 0.000(4) 0.000(4) C37 0.030(4) 0.026(4) 0.030(5) 0.005(3) 0.009(4) 0.010(3) C38 0.058(5) 0.034(4) 0.036(6) -0.004(4) 0.003(4) 0.005(4) C39 0.088(7) 0.021(4) 0.068(8) 0.001(4) 0.014(6) -0.001(4) C40 0.079(7) 0.035(5) 0.060(8) 0.019(5) 0.020(6) 0.020(5) C41 0.052(5) 0.055(6) 0.048(6) 0.015(5) 0.004(4) 0.011(4) C42 0.042(4) 0.037(5) 0.044(6) 0.009(4) 0.006(4) 0.006(4) #----------------------------------------------------------------------------# # 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 Ce N1 2.423(6) . ? Ce N3 2.425(6) . ? Ce N4 2.483(5) . ? Ce N2 2.487(5) . ? Ce Cl 2.6973(16) . ? Si1 N1 1.747(6) . ? Si1 C5 1.849(8) . ? Si1 C4 1.867(7) . ? Si1 C6 1.872(8) . ? Si2 N2 1.760(5) . ? Si2 C7 1.847(9) . ? Si2 C8 1.858(7) . ? Si2 C9 1.868(7) . ? Si3 N3 1.743(6) . ? Si3 C26 1.847(8) . ? Si3 C25 1.855(7) . ? Si3 C27 1.859(8) . ? Si4 N4 1.753(5) . ? Si4 C28 1.856(8) . ? Si4 C30 1.864(8) . ? Si4 C29 1.879(7) . ? N1 C1 1.331(8) . ? N2 C3 1.334(7) . ? N3 C22 1.325(8) . ? N4 C24 1.334(7) . ? C1 C2 1.413(10) . ? C1 C10 1.507(9) . ? C2 C3 1.427(8) . ? C3 C16 1.505(9) . ? C10 C15 1.375(9) . ? C10 C11 1.390(9) . ? C11 C12 1.391(9) . ? C12 C13 1.364(10) . ? C13 C14 1.371(11) . ? C14 C15 1.396(9) . ? C16 C21 1.382(8) . ? C16 C17 1.398(10) . ? C17 C18 1.371(10) . ? C18 C19 1.372(10) . ? C19 C20 1.369(11) . ? C20 C21 1.361(10) . ? C22 C23 1.411(9) . ? C22 C31 1.496(9) . ? C23 C24 1.423(9) . ? C24 C37 1.520(9) . ? C31 C36 1.380(9) . ? C31 C32 1.400(10) . ? C32 C33 1.407(10) . ? C33 C34 1.364(11) . ? C34 C35 1.367(11) . ? C35 C36 1.396(10) . ? C37 C42 1.364(10) . ? C37 C38 1.391(9) . ? C38 C39 1.381(11) . ? C39 C40 1.357(12) . ? C40 C41 1.370(11) . ? C41 C42 1.377(10) . ? 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 Ce N3 124.27(17) . . ? N1 Ce N4 101.79(18) . . ? N3 Ce N4 75.82(18) . . ? N1 Ce N2 76.33(18) . . ? N3 Ce N2 105.53(18) . . ? N4 Ce N2 178.1(2) . . ? N1 Ce Cl 122.14(14) . . ? N3 Ce Cl 113.57(12) . . ? N4 Ce Cl 90.29(12) . . ? N2 Ce Cl 90.41(11) . . ? N1 Si1 C5 107.4(4) . . ? N1 Si1 C4 103.3(3) . . ? C5 Si1 C4 111.9(4) . . ? N1 Si1 C6 118.2(3) . . ? C5 Si1 C6 107.6(4) . . ? C4 Si1 C6 108.6(4) . . ? N2 Si2 C7 104.3(3) . . ? N2 Si2 C8 110.8(3) . . ? C7 Si2 C8 110.0(4) . . ? N2 Si2 C9 114.0(3) . . ? C7 Si2 C9 106.7(4) . . ? C8 Si2 C9 110.7(4) . . ? N3 Si3 C26 116.9(3) . . ? N3 Si3 C25 104.6(4) . . ? C26 Si3 C25 107.3(4) . . ? N3 Si3 C27 106.8(3) . . ? C26 Si3 C27 109.9(4) . . ? C25 Si3 C27 111.3(4) . . ? N4 Si4 C28 105.4(3) . . ? N4 Si4 C30 111.4(3) . . ? C28 Si4 C30 109.3(4) . . ? N4 Si4 C29 114.3(3) . . ? C28 Si4 C29 107.0(4) . . ? C30 Si4 C29 109.2(4) . . ? C1 N1 Si1 130.0(5) . . ? C1 N1 Ce 98.9(4) . . ? Si1 N1 Ce 131.0(3) . . ? C3 N2 Si2 128.9(4) . . ? C3 N2 Ce 97.3(4) . . ? Si2 N2 Ce 133.2(2) . . ? C22 N3 Si3 128.2(5) . . ? C22 N3 Ce 100.7(4) . . ? Si3 N3 Ce 131.1(3) . . ? C24 N4 Si4 129.1(4) . . ? C24 N4 Ce 96.4(4) . . ? Si4 N4 Ce 133.8(3) . . ? N1 C1 C2 123.8(6) . . ? N1 C1 C10 120.4(6) . . ? C2 C1 C10 115.8(6) . . ? C1 C2 C3 128.4(6) . . ? N2 C3 C2 123.4(6) . . ? N2 C3 C16 120.1(5) . . ? C2 C3 C16 116.5(5) . . ? C15 C10 C11 118.8(6) . . ? C15 C10 C1 121.0(6) . . ? C11 C10 C1 120.1(6) . . ? C10 C11 C12 120.3(6) . . ? C13 C12 C11 120.6(7) . . ? C12 C13 C14 119.5(7) . . ? C13 C14 C15 120.5(7) . . ? C10 C15 C14 120.3(7) . . ? C21 C16 C17 118.3(7) . . ? C21 C16 C3 121.3(6) . . ? C17 C16 C3 120.3(6) . . ? C18 C17 C16 119.9(7) . . ? C17 C18 C19 120.4(8) . . ? C20 C19 C18 120.0(8) . . ? C21 C20 C19 120.0(7) . . ? C20 C21 C16 121.3(7) . . ? N3 C22 C23 123.6(6) . . ? N3 C22 C31 121.8(7) . . ? C23 C22 C31 114.6(5) . . ? C22 C23 C24 127.3(6) . . ? N4 C24 C23 125.1(6) . . ? N4 C24 C37 120.2(6) . . ? C23 C24 C37 114.7(5) . . ? C36 C31 C32 118.1(7) . . ? C36 C31 C22 121.7(6) . . ? C32 C31 C22 120.2(6) . . ? C31 C32 C33 120.4(8) . . ? C34 C33 C32 120.2(8) . . ? C33 C34 C35 119.7(8) . . ? C34 C35 C36 120.9(8) . . ? C31 C36 C35 120.6(7) . . ? C42 C37 C38 117.7(7) . . ? C42 C37 C24 120.7(6) . . ? C38 C37 C24 121.6(7) . . ? C39 C38 C37 120.0(8) . . ? C40 C39 C38 121.2(8) . . ? C39 C40 C41 119.3(8) . . ? C40 C41 C42 119.7(9) . . ? C37 C42 C41 122.1(8) . . ? #===END