# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2189 data_gunko-1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[{Li(Me3SiNCPhNCH2CH2CH2NMe2)}2]' _chemical_formula_analytical ? _chemical_formula_sum 'C30 H52 Li2 N6 Si2' _chemical_formula_weight 566.84 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 17.151(4) _cell_length_b 9.616(7) _cell_length_c 22.314(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.27(4) _cell_angle_gamma 90.00 _cell_volume 3550.2(31) _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 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.061 _exptl_crystal_density_method ? _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 0.126 _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 3221 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 24.98 _reflns_number_total 3122 _reflns_number_observed 2471 _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_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+2.7343P] 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 3122 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_obs 0.0417 _refine_ls_wR_factor_all 0.1077 _refine_ls_wR_factor_obs 0.0982 _refine_ls_goodness_of_fit_all 1.026 _refine_ls_goodness_of_fit_obs 1.058 _refine_ls_restrained_S_all 1.026 _refine_ls_restrained_S_obs 1.058 _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 Li Li -0.0467(2) 0.1080(3) 0.28230(14) 0.0304(7) Uani 1 d . . Si Si -0.00648(3) -0.19193(5) 0.13288(2) 0.0295(2) Uani 1 d . . N1 N -0.02079(9) -0.0360(2) 0.16410(7) 0.0262(3) Uani 1 d . . N2 N -0.08586(9) 0.1513(2) 0.19095(7) 0.0273(4) Uani 1 d . . N3 N -0.11741(9) 0.2276(2) 0.32303(7) 0.0292(4) Uani 1 d . . C1 C -0.08253(10) 0.0511(2) 0.15088(8) 0.0242(4) Uani 1 d . . C2 C -0.14676(13) 0.2599(2) 0.17086(9) 0.0388(5) Uani 1 d . . H2A H -0.20060(13) 0.2162(2) 0.15556(9) 0.047 Uiso 1 calc R . H2B H -0.13515(13) 0.3122(2) 0.13598(9) 0.047 Uiso 1 calc R . C3 C -0.14854(14) 0.3601(2) 0.22296(9) 0.0403(5) Uani 1 d . . H3A H -0.18299(14) 0.4404(2) 0.20513(9) 0.048 Uiso 1 calc R . H3B H -0.09311(14) 0.3956(2) 0.24087(9) 0.048 Uiso 1 calc R . C4 C -0.17956(12) 0.2988(2) 0.27500(9) 0.0386(5) Uani 1 d . . H4A H -0.20313(12) 0.3745(2) 0.29473(9) 0.046 Uiso 1 calc R . H4B H -0.22335(12) 0.2320(2) 0.25694(9) 0.046 Uiso 1 calc R . C5 C -0.06470(14) 0.3282(2) 0.36330(10) 0.0462(6) Uani 1 d . . H5A H -0.03845(14) 0.3867(2) 0.33836(10) 0.069 Uiso 1 calc R . H5B H -0.02341(14) 0.2788(2) 0.39484(10) 0.069 Uiso 1 calc R . H5C H -0.09685(14) 0.3868(2) 0.38371(10) 0.069 Uiso 1 calc R . C6 C -0.15561(14) 0.1421(2) 0.36143(11) 0.0447(5) Uani 1 d . . H6A H -0.19132(14) 0.0738(2) 0.33520(11) 0.067 Uiso 1 calc R . H6B H -0.18729(14) 0.2016(2) 0.38185(11) 0.067 Uiso 1 calc R . H6C H -0.11386(14) 0.0936(2) 0.39298(11) 0.067 Uiso 1 calc R . C7 C -0.14653(11) 0.0400(2) 0.09003(8) 0.0278(4) Uani 1 d . . C8 C -0.21232(12) -0.0463(2) 0.08451(9) 0.0406(5) Uani 1 d . . H8 H -0.21864(12) -0.0959(2) 0.11974(9) 0.049 Uiso 1 calc R . C9 C -0.26909(14) -0.0608(3) 0.02800(11) 0.0512(6) Uani 1 d . . H9 H -0.31381(14) -0.1214(3) 0.02450(11) 0.061 Uiso 1 calc R . C10 C -0.26132(14) 0.0115(2) -0.02294(10) 0.0480(6) Uani 1 d . . H10 H -0.30039(14) 0.0009(2) -0.06171(10) 0.058 Uiso 1 calc R . C11 C -0.19721(13) 0.0989(2) -0.01778(9) 0.0436(5) Uani 1 d . . H11 H -0.19202(13) 0.1503(2) -0.05287(9) 0.052 Uiso 1 calc R . C12 C -0.13971(12) 0.1126(2) 0.03853(9) 0.0361(5) Uani 1 d . . H12 H -0.09498(12) 0.1730(2) 0.04166(9) 0.043 Uiso 1 calc R . C13 C -0.02487(14) -0.1957(2) 0.04653(10) 0.0462(6) Uani 1 d . . H13A H 0.00797(14) -0.1239(2) 0.03371(10) 0.069 Uiso 1 calc R . H13B H -0.08220(14) -0.1779(2) 0.02695(10) 0.069 Uiso 1 calc R . H13C H -0.01003(14) -0.2872(2) 0.03365(10) 0.069 Uiso 1 calc R . C14 C 0.10136(12) -0.2397(2) 0.16771(11) 0.0450(5) Uani 1 d . . H14A H 0.13650(12) -0.1687(2) 0.15712(11) 0.067 Uiso 1 calc R . H14B H 0.11259(12) -0.3299(2) 0.15133(11) 0.067 Uiso 1 calc R . H14C H 0.11165(12) -0.2456(2) 0.21297(11) 0.067 Uiso 1 calc R . C15 C -0.07031(14) -0.3301(2) 0.15446(11) 0.0459(6) Uani 1 d . . H15A H -0.12750(14) -0.3078(2) 0.13675(11) 0.069 Uiso 1 calc R . H15B H -0.05895(14) -0.3354(2) 0.19980(11) 0.069 Uiso 1 calc R . H15C H -0.05803(14) -0.4198(2) 0.13817(11) 0.069 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 Li 0.029(2) 0.036(2) 0.0250(15) 0.0045(14) 0.0056(13) 0.0087(14) Si 0.0295(3) 0.0258(3) 0.0308(3) -0.0034(2) 0.0038(2) -0.0020(2) N1 0.0244(8) 0.0265(8) 0.0252(8) -0.0003(6) 0.0021(6) -0.0022(6) N2 0.0262(8) 0.0306(8) 0.0231(8) 0.0011(7) 0.0028(6) 0.0066(7) N3 0.0306(9) 0.0286(8) 0.0280(8) 0.0013(7) 0.0071(7) 0.0036(7) C1 0.0224(9) 0.0273(9) 0.0222(9) 0.0047(7) 0.0048(7) -0.0040(7) C2 0.0423(12) 0.0427(12) 0.0281(10) 0.0052(9) 0.0037(9) 0.0166(10) C3 0.0501(13) 0.0330(11) 0.0372(11) 0.0094(9) 0.0104(10) 0.0196(10) C4 0.0332(11) 0.0454(12) 0.0373(11) 0.0020(10) 0.0094(9) 0.0152(10) C5 0.0482(13) 0.0438(13) 0.0420(12) -0.0084(10) 0.0038(10) -0.0021(10) C6 0.0522(14) 0.0397(12) 0.0500(13) 0.0062(10) 0.0272(11) 0.0057(10) C7 0.0244(9) 0.0329(10) 0.0244(9) -0.0011(8) 0.0035(7) 0.0014(8) C8 0.0330(11) 0.0514(13) 0.0325(11) 0.0072(10) -0.0001(9) -0.0120(10) C9 0.0366(12) 0.0573(15) 0.0488(14) 0.0027(12) -0.0081(10) -0.0154(11) C10 0.0460(13) 0.0527(14) 0.0322(11) -0.0043(10) -0.0128(9) 0.0031(11) C11 0.0501(13) 0.0530(14) 0.0235(10) 0.0050(10) 0.0022(9) 0.0017(11) C12 0.0351(11) 0.0436(12) 0.0275(10) 0.0031(9) 0.0044(8) -0.0059(9) C13 0.0558(14) 0.0470(13) 0.0358(11) -0.0108(10) 0.0123(10) 0.0020(11) C14 0.0362(12) 0.0349(11) 0.0605(14) -0.0036(11) 0.0067(10) 0.0045(10) C15 0.0457(13) 0.0334(12) 0.0554(14) -0.0005(10) 0.0075(11) -0.0086(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 Li N1 1.989(3) 6_556 ? Li N2 2.015(3) . ? Li N3 2.050(3) . ? Li N2 2.232(3) 6_556 ? Li C1 2.386(4) 6_556 ? Li Li 2.420(6) 6_556 ? Si N1 1.698(2) . ? Si C15 1.864(2) . ? Si C14 1.865(2) . ? Si C13 1.869(2) . ? N1 C1 1.321(2) . ? N1 Li 1.989(3) 6_556 ? N2 C1 1.327(2) . ? N2 C2 1.461(2) . ? N2 Li 2.232(3) 6_556 ? N3 C5 1.461(3) . ? N3 C6 1.461(3) . ? N3 C4 1.467(2) . ? C1 C7 1.508(2) . ? C1 Li 2.386(4) 6_556 ? C2 C3 1.516(3) . ? C3 C4 1.518(3) . ? C7 C12 1.376(3) . ? C7 C8 1.379(3) . ? C8 C9 1.382(3) . ? C9 C10 1.369(3) . ? C10 C11 1.364(3) . ? C11 C12 1.384(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 Li N2 137.6(2) 6_556 . ? N1 Li N3 116.3(2) 6_556 . ? N2 Li N3 104.70(15) . . ? N1 Li N2 65.12(11) 6_556 6_556 ? N2 Li N2 106.07(15) . 6_556 ? N3 Li N2 117.2(2) . 6_556 ? N1 Li C1 33.62(8) 6_556 6_556 ? N2 Li C1 133.4(2) . 6_556 ? N3 Li C1 114.36(14) . 6_556 ? N2 Li C1 33.18(7) 6_556 6_556 ? N1 Li Li 89.25(14) 6_556 6_556 ? N2 Li Li 59.60(13) . 6_556 ? N3 Li Li 145.67(10) . 6_556 ? N2 Li Li 51.13(12) 6_556 6_556 ? C1 Li Li 73.81(15) 6_556 6_556 ? N1 Si C15 111.42(10) . . ? N1 Si C14 106.32(9) . . ? C15 Si C14 107.59(11) . . ? N1 Si C13 115.90(9) . . ? C15 Si C13 107.54(11) . . ? C14 Si C13 107.72(11) . . ? C1 N1 Si 131.45(13) . . ? C1 N1 Li 89.9(2) . 6_556 ? Si N1 Li 137.49(13) . 6_556 ? C1 N2 C2 117.8(2) . . ? C1 N2 Li 118.00(15) . . ? C2 N2 Li 118.64(15) . . ? C1 N2 Li 79.80(13) . 6_556 ? C2 N2 Li 144.2(2) . 6_556 ? Li N2 Li 69.26(15) . 6_556 ? C5 N3 C6 108.2(2) . . ? C5 N3 C4 110.7(2) . . ? C6 N3 C4 109.8(2) . . ? C5 N3 Li 107.6(2) . . ? C6 N3 Li 110.7(2) . . ? C4 N3 Li 109.83(14) . . ? N1 C1 N2 119.0(2) . . ? N1 C1 C7 120.5(2) . . ? N2 C1 C7 120.5(2) . . ? N1 C1 Li 56.50(12) . 6_556 ? N2 C1 Li 67.03(12) . 6_556 ? C7 C1 Li 156.17(14) . 6_556 ? N2 C2 C3 112.1(2) . . ? C2 C3 C4 115.0(2) . . ? N3 C4 C3 114.0(2) . . ? C12 C7 C8 118.6(2) . . ? C12 C7 C1 120.9(2) . . ? C8 C7 C1 120.5(2) . . ? C7 C8 C9 120.4(2) . . ? C10 C9 C8 120.5(2) . . ? C11 C10 C9 119.7(2) . . ? C10 C11 C12 120.1(2) . . ? C7 C12 C11 120.8(2) . . ? _refine_diff_density_max 0.290 _refine_diff_density_min -0.216 _refine_diff_density_rms 0.040 #===END data_gunko-2 _audit_creation_date 1999-12-21T10:41:53-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[AlCl2{Me3SiNC(Ph)N(CH2)3NMe2}]' _chemical_formula_moiety 'C15 H26 Al1 Cl2 N3 Si1' _chemical_formula_structural 'C15 H26 AL CL2 N3 SI' _chemical_formula_sum 'C15 H26 Al Cl2 N3 Si' _chemical_formula_weight 374.36 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.8881(3) _cell_length_b 11.4278(5) _cell_length_c 10.3472(5) _cell_angle_alpha 90 _cell_angle_beta 109.373(2) _cell_angle_gamma 90 _cell_volume 991.47(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4777 _cell_measurement_theta_min 4.246 _cell_measurement_theta_max 30.034 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.432 _exptl_absorpt_correction_T_min 0.8813 _exptl_absorpt_correction_T_max 0.8813 #----------------------------------------------------------------------------# # 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 8799 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.32 _diffrn_reflns_theta_max 30 _diffrn_reflns_theta_full 30 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 4202 _reflns_number_gt 3972 _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^)+(0.0304P)^2^+0.2161P] 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 4202 _refine_ls_number_parameters 199 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 -0.01(5) _refine_diff_density_max 0.25 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.041 #----------------------------------------------------------------------------# # 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' Al Al 0.0645 0.0514 '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 Al Al 0.21673(6) 0.13591(5) 0.84595(5) 0.02081(11) Uani 1 1 d . . . Cl1 Cl 0.44982(5) 0.05273(5) 0.89837(5) 0.03164(11) Uani 1 1 d . . . Cl2 Cl 0.23747(7) 0.30754(5) 0.93792(6) 0.04133(13) Uani 1 1 d . . . Si Si 0.31116(6) 0.21494(5) 0.55461(5) 0.02503(11) Uani 1 1 d . . . N1 N 0.19085(17) 0.17184(15) 0.64877(15) 0.0251(3) Uani 1 1 d . . . N2 N 0.00317(17) 0.11425(17) 0.72689(16) 0.0296(4) Uani 1 1 d . . . N3 N 0.15689(17) 0.04162(16) 0.99538(15) 0.0247(3) Uani 1 1 d . . . C1 C 0.03621(19) 0.15240(18) 0.61873(17) 0.0235(3) Uani 1 1 d . . . C2 C -0.08982(19) 0.17248(18) 0.48284(18) 0.0246(4) Uani 1 1 d . . . C3 C -0.1744(2) 0.2765(2) 0.4584(2) 0.0346(5) Uani 1 1 d . . . H3 H -0.1522 0.3346 0.5279 0.042 Uiso 1 1 calc R . . C4 C -0.2915(3) 0.2961(2) 0.3328(2) 0.0417(5) Uani 1 1 d . . . H4 H -0.3481 0.3681 0.316 0.05 Uiso 1 1 calc R . . C5 C -0.3258(2) 0.2113(2) 0.2324(2) 0.0385(5) Uani 1 1 d . . . H5 H -0.4065 0.2249 0.1467 0.046 Uiso 1 1 calc R . . C6 C -0.2434(3) 0.1067(2) 0.2560(2) 0.0367(5) Uani 1 1 d . . . H6 H -0.2674 0.0482 0.1868 0.044 Uiso 1 1 calc R . . C7 C -0.1247(2) 0.0874(2) 0.3818(2) 0.0318(4) Uani 1 1 d . . . H7 H -0.0676 0.0156 0.3982 0.038 Uiso 1 1 calc R . . C8 C 0.1998(3) 0.2945(2) 0.3938(2) 0.0391(5) Uani 1 1 d . . . H8A H 0.1182 0.2429 0.3339 0.059 Uiso 1 1 calc R . . H8B H 0.2741 0.3184 0.3468 0.059 Uiso 1 1 calc R . . H8C H 0.1487 0.3639 0.4163 0.059 Uiso 1 1 calc R . . C9 C 0.4071(2) 0.0829(2) 0.5109(2) 0.0342(4) Uani 1 1 d . . . H9A H 0.3249 0.0315 0.4513 0.051 Uiso 1 1 calc R . . H9B H 0.466 0.0409 0.5951 0.051 Uiso 1 1 calc R . . H9C H 0.4809 0.1067 0.4634 0.051 Uiso 1 1 calc R . . C10 C 0.4657(3) 0.3134(2) 0.6671(2) 0.0392(5) Uani 1 1 d . . . H10A H 0.4144 0.3827 0.6897 0.059 Uiso 1 1 calc R . . H10B H 0.5392 0.3376 0.6194 0.059 Uiso 1 1 calc R . . H10C H 0.5251 0.2719 0.7515 0.059 Uiso 1 1 calc R . . C11 C -0.1540(2) 0.1082(2) 0.7403(2) 0.0374(5) Uani 1 1 d . . . H11A H -0.2299 0.0713 0.6577 0.045 Uiso 1 1 calc R . . H11B H -0.1928 0.1881 0.7489 0.045 Uiso 1 1 calc R . . C12 C -0.1446(2) 0.0369(2) 0.8660(2) 0.0368(5) Uani 1 1 d . . . H12A H -0.132 -0.0466 0.8466 0.044 Uiso 1 1 calc R . . H12B H -0.2465 0.0452 0.8845 0.044 Uiso 1 1 calc R . . C13 C -0.0082(2) 0.0724(2) 0.9939(2) 0.0323(4) Uani 1 1 d . . . H13A H -0.0132 0.1582 1.0054 0.039 Uiso 1 1 calc R . . H13B H -0.0255 0.0352 1.0742 0.039 Uiso 1 1 calc R . . C14 C 0.1650(3) -0.0866(2) 0.9708(2) 0.0362(5) Uani 1 1 d . . . H14A H 0.0933 -0.1058 0.8786 0.054 Uiso 1 1 calc R . . H14B H 0.1326 -0.1301 1.0388 0.054 Uiso 1 1 calc R . . H14C H 0.2745 -0.108 0.9787 0.054 Uiso 1 1 calc R . . C15 C 0.2672(3) 0.0654(3) 1.13593(19) 0.0389(5) Uani 1 1 d . . . H15A H 0.2653 0.1491 1.1559 0.058 Uiso 1 1 calc R . . H15B H 0.3756 0.0423 1.1425 0.058 Uiso 1 1 calc R . . H15C H 0.2333 0.0204 1.2022 0.058 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 Al 0.0173(2) 0.0245(3) 0.0199(2) -0.0009(2) 0.00519(17) 0.0009(2) Cl1 0.01895(17) 0.0445(3) 0.0292(2) 0.0008(2) 0.00502(15) 0.00713(19) Cl2 0.0569(3) 0.0257(2) 0.0472(3) -0.0084(2) 0.0251(2) -0.0041(2) Si 0.0231(2) 0.0291(3) 0.0244(2) 0.0015(2) 0.00989(18) -0.0010(2) N1 0.0194(6) 0.0330(9) 0.0217(6) 0.0022(6) 0.0050(5) 0.0003(6) N2 0.0175(6) 0.0431(11) 0.0255(7) 0.0082(7) 0.0035(5) -0.0011(6) N3 0.0260(6) 0.0272(8) 0.0211(6) -0.0006(6) 0.0079(5) -0.0003(6) C1 0.0197(7) 0.0252(9) 0.0228(7) 0.0011(7) 0.0034(6) 0.0006(7) C2 0.0196(7) 0.0281(9) 0.0240(8) 0.0025(7) 0.0042(6) -0.0016(7) C3 0.0350(10) 0.0296(11) 0.0327(10) -0.0011(8) 0.0024(8) 0.0045(8) C4 0.0376(10) 0.0368(12) 0.0418(11) 0.0113(11) 0.0012(9) 0.0115(10) C5 0.0291(9) 0.0517(14) 0.0264(8) 0.0099(10) -0.0019(7) -0.0041(10) C6 0.0360(10) 0.0429(13) 0.0256(9) -0.0035(9) 0.0028(7) -0.0094(9) C7 0.0326(9) 0.0294(11) 0.0301(9) -0.0002(8) 0.0061(7) 0.0044(8) C8 0.0415(11) 0.0452(14) 0.0338(10) 0.0121(10) 0.0166(8) 0.0039(10) C9 0.0339(9) 0.0384(12) 0.0324(9) -0.0022(9) 0.0140(8) 0.0022(9) C10 0.0361(10) 0.0379(12) 0.0462(11) -0.0048(11) 0.0172(9) -0.0114(10) C11 0.0192(8) 0.0544(15) 0.0384(10) 0.0104(10) 0.0095(7) 0.0002(8) C12 0.0235(8) 0.0525(15) 0.0382(10) 0.0074(10) 0.0154(7) -0.0031(9) C13 0.0317(8) 0.0398(13) 0.0299(8) 0.0004(9) 0.0164(7) 0.0022(9) C14 0.0403(11) 0.0253(10) 0.0442(12) 0.0039(9) 0.0156(9) 0.0024(9) C15 0.0405(10) 0.0532(15) 0.0196(8) 0.0020(9) 0.0055(7) -0.0027(11) #----------------------------------------------------------------------------# # 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 Al N2 1.9053(15) . ? Al N1 2.0182(16) . ? Al N3 2.0929(16) . ? Al Cl2 2.1610(8) . ? Al Cl1 2.1782(6) . ? Al C1 2.3738(17) . ? Si N1 1.7396(16) . ? Si C10 1.856(2) . ? Si C9 1.861(2) . ? Si C8 1.866(2) . ? N1 C1 1.324(2) . ? N2 C1 1.322(2) . ? N2 C11 1.451(2) . ? N3 C15 1.484(2) . ? N3 C14 1.493(3) . ? N3 C13 1.504(2) . ? C1 C2 1.496(2) . ? C2 C3 1.384(3) . ? C2 C7 1.386(3) . ? C3 C4 1.387(3) . ? C4 C5 1.379(4) . ? C5 C6 1.381(4) . ? C6 C7 1.394(3) . ? C11 C12 1.514(3) . ? C12 C13 1.524(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 N2 Al N1 67.53(6) . . ? N2 Al N3 88.17(7) . . ? N1 Al N3 151.64(7) . . ? N2 Al Cl2 108.90(6) . . ? N1 Al Cl2 103.00(6) . . ? N3 Al Cl2 98.48(5) . . ? N2 Al Cl1 139.95(7) . . ? N1 Al Cl1 96.92(5) . . ? N3 Al Cl1 92.59(5) . . ? Cl2 Al Cl1 110.56(3) . . ? N2 Al C1 33.78(6) . . ? N1 Al C1 33.86(6) . . ? N3 Al C1 121.24(6) . . ? Cl2 Al C1 107.16(6) . . ? Cl1 Al C1 123.77(5) . . ? N1 Si C10 106.55(9) . . ? N1 Si C9 108.83(10) . . ? C10 Si C9 109.90(11) . . ? N1 Si C8 113.24(9) . . ? C10 Si C8 109.08(12) . . ? C9 Si C8 109.19(11) . . ? C1 N1 Si 134.38(13) . . ? C1 N1 Al 87.96(11) . . ? Si N1 Al 137.62(8) . . ? C1 N2 C11 126.01(15) . . ? C1 N2 Al 92.93(11) . . ? C11 N2 Al 136.80(14) . . ? C15 N3 C14 107.03(18) . . ? C15 N3 C13 106.99(15) . . ? C14 N3 C13 109.29(16) . . ? C15 N3 Al 112.50(13) . . ? C14 N3 Al 109.92(12) . . ? C13 N3 Al 110.97(12) . . ? N2 C1 N1 111.20(15) . . ? N2 C1 C2 122.61(15) . . ? N1 C1 C2 126.18(16) . . ? N2 C1 Al 53.28(9) . . ? N1 C1 Al 58.17(9) . . ? C2 C1 Al 172.80(14) . . ? C3 C2 C7 119.51(17) . . ? C3 C2 C1 119.68(17) . . ? C7 C2 C1 120.80(17) . . ? C2 C3 C4 120.2(2) . . ? C5 C4 C3 120.1(2) . . ? C4 C5 C6 120.23(18) . . ? C5 C6 C7 119.6(2) . . ? C2 C7 C6 120.3(2) . . ? N2 C11 C12 109.10(16) . . ? C11 C12 C13 113.84(19) . . ? N3 C13 C12 116.07(17) . . ? #===END data_gunko-3 _audit_creation_date 2000-02-17T14:16:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[GaCl2(Me3SiNCPhNCH2CH2CH2NMe2)]' _chemical_formula_moiety 'C15 H26 Cl2 Ga1 N3 Si1' _chemical_formula_structural 'C15 H26 CL2 GA N3 SI' _chemical_formula_sum 'C15 H26 Cl2 Ga N3 Si' _chemical_formula_weight 417.1 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.8921(2) _cell_length_b 11.4453(3) _cell_length_c 10.4095(3) _cell_angle_alpha 90 _cell_angle_beta 109.221(2) _cell_angle_gamma 90 _cell_volume 1000.35(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4555 _cell_measurement_theta_min 4.529 _cell_measurement_theta_max 27.878 _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 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.702 _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 0.620 _exptl_absorpt_correction_T_max 0.646 #----------------------------------------------------------------------------# # 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 8110 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 4.61 _diffrn_reflns_theta_max 27.9 _diffrn_reflns_theta_full 27.9 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 4427 _reflns_number_gt 4347 _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 'SHELXCS-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^)+(0.0146P)^2^+0.2507P] 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 4427 _refine_ls_number_parameters 199 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0568 _refine_ls_wR_factor_gt 0.0564 _refine_ls_goodness_of_fit_ref 1.08 _refine_ls_restrained_S_all 1.08 _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 -0.003(6) _refine_diff_density_max 0.257 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.047 #----------------------------------------------------------------------------# # 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' Ga Ga 0.2307 1.6083 '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 Ga Ga 0.22207(2) 0.136146(19) 0.851022(18) 0.02074(6) Uani 1 1 d . . . Cl1 Cl 0.45610(6) 0.04924(5) 0.90110(5) 0.03302(12) Uani 1 1 d . . . Cl2 Cl 0.24651(8) 0.30883(5) 0.94726(6) 0.04120(14) Uani 1 1 d . . . Si Si 0.31220(7) 0.21583(5) 0.55207(6) 0.02572(12) Uani 1 1 d . . . N1 N 0.1910(2) 0.17468(15) 0.64536(17) 0.0254(4) Uani 1 1 d . . . N2 N 0.00448(18) 0.11588(17) 0.72563(16) 0.0287(4) Uani 1 1 d . . . N3 N 0.1551(2) 0.03742(15) 0.99830(16) 0.0258(3) Uani 1 1 d . . . C1 C 0.0378(2) 0.15438(17) 0.61798(19) 0.0236(4) Uani 1 1 d . . . C2 C -0.0888(2) 0.17255(17) 0.4834(2) 0.0247(4) Uani 1 1 d . . . C3 C -0.1726(3) 0.2771(2) 0.4578(2) 0.0360(5) Uani 1 1 d . . . H3 H -0.1497 0.3362 0.5256 0.043 Uiso 1 1 calc R . . C4 C -0.2905(3) 0.2950(2) 0.3326(3) 0.0440(6) Uani 1 1 d . . . H4 H -0.3476 0.3667 0.315 0.053 Uiso 1 1 calc R . . C5 C -0.3248(3) 0.2094(2) 0.2341(2) 0.0390(6) Uani 1 1 d . . . H5 H -0.4046 0.2223 0.1485 0.047 Uiso 1 1 calc R . . C6 C -0.2432(3) 0.1048(2) 0.2597(2) 0.0368(5) Uani 1 1 d . . . H6 H -0.2679 0.0453 0.1924 0.044 Uiso 1 1 calc R . . C7 C -0.1245(3) 0.0865(2) 0.3847(2) 0.0323(5) Uani 1 1 d . . . H7 H -0.0679 0.0147 0.402 0.039 Uiso 1 1 calc R . . C8 C 0.2025(3) 0.2953(2) 0.3921(2) 0.0410(5) Uani 1 1 d . . . H8A H 0.1211 0.2439 0.3324 0.061 Uiso 1 1 calc R . . H8B H 0.2774 0.319 0.3458 0.061 Uiso 1 1 calc R . . H8C H 0.1514 0.3648 0.4141 0.061 Uiso 1 1 calc R . . C9 C 0.4068(3) 0.0826(2) 0.5100(2) 0.0350(5) Uani 1 1 d . . . H9A H 0.3244 0.0317 0.4506 0.052 Uiso 1 1 calc R . . H9B H 0.464 0.0407 0.594 0.052 Uiso 1 1 calc R . . H9C H 0.4817 0.1052 0.4634 0.052 Uiso 1 1 calc R . . C10 C 0.4677(3) 0.3128(2) 0.6645(3) 0.0404(5) Uani 1 1 d . . . H10A H 0.4173 0.3822 0.6875 0.061 Uiso 1 1 calc R . . H10B H 0.5416 0.3366 0.6173 0.061 Uiso 1 1 calc R . . H10C H 0.5262 0.2708 0.748 0.061 Uiso 1 1 calc R . . C11 C -0.1516(2) 0.1111(2) 0.7418(2) 0.0348(5) Uani 1 1 d . . . H11A H -0.2298 0.0773 0.659 0.042 Uiso 1 1 calc R . . H11B H -0.187 0.1911 0.7542 0.042 Uiso 1 1 calc R . . C12 C -0.1435(3) 0.0371(2) 0.8638(2) 0.0365(5) Uani 1 1 d . . . H12A H -0.1299 -0.0456 0.8419 0.044 Uiso 1 1 calc R . . H12B H -0.2463 0.0435 0.8809 0.044 Uiso 1 1 calc R . . C13 C -0.0097(3) 0.0697(2) 0.9937(2) 0.0309(4) Uani 1 1 d . . . H13A H -0.0132 0.1552 1.0068 0.037 Uiso 1 1 calc R . . H13B H -0.031 0.0316 1.0714 0.037 Uiso 1 1 calc R . . C14 C 0.1639(3) -0.0898(2) 0.9720(3) 0.0378(5) Uani 1 1 d . . . H14A H 0.0923 -0.1082 0.8803 0.057 Uiso 1 1 calc R . . H14B H 0.1318 -0.1344 1.039 0.057 Uiso 1 1 calc R . . H14C H 0.2734 -0.1105 0.9793 0.057 Uiso 1 1 calc R . . C15 C 0.2636(3) 0.0610(3) 1.1382(2) 0.0393(6) Uani 1 1 d . . . H15A H 0.2616 0.1445 1.1581 0.059 Uiso 1 1 calc R . . H15B H 0.3722 0.0378 1.1456 0.059 Uiso 1 1 calc R . . H15C H 0.2287 0.0161 1.2035 0.059 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 Ga 0.01701(9) 0.02480(10) 0.01876(9) -0.00057(8) 0.00364(6) 0.00072(8) Cl1 0.0202(2) 0.0459(3) 0.0300(2) 0.0005(2) 0.00438(18) 0.0087(2) Cl2 0.0547(4) 0.0253(3) 0.0466(3) -0.0083(2) 0.0207(3) -0.0040(2) Si 0.0246(3) 0.0289(3) 0.0246(3) 0.0018(2) 0.0093(2) -0.0011(2) N1 0.0196(8) 0.0353(9) 0.0199(7) 0.0016(6) 0.0046(6) -0.0003(6) N2 0.0151(7) 0.0443(12) 0.0239(8) 0.0081(8) 0.0027(6) -0.0019(7) N3 0.0293(9) 0.0271(9) 0.0204(8) 0.0000(7) 0.0074(6) 0.0005(7) C1 0.0229(9) 0.0241(11) 0.0206(8) 0.0005(8) 0.0030(7) 0.0002(7) C2 0.0209(9) 0.0275(10) 0.0228(9) 0.0031(7) 0.0031(7) -0.0018(7) C3 0.0374(12) 0.0293(11) 0.0333(12) -0.0011(9) 0.0007(10) 0.0066(9) C4 0.0390(13) 0.0405(14) 0.0418(13) 0.0122(11) -0.0012(11) 0.0114(10) C5 0.0270(11) 0.0533(15) 0.0279(11) 0.0101(11) -0.0029(9) -0.0026(10) C6 0.0350(11) 0.0453(14) 0.0240(10) -0.0042(9) 0.0011(8) -0.0096(9) C7 0.0344(12) 0.0288(10) 0.0292(11) 0.0005(8) 0.0043(9) 0.0012(9) C8 0.0459(14) 0.0469(14) 0.0333(12) 0.0122(11) 0.0174(10) 0.0079(11) C9 0.0346(12) 0.0393(12) 0.0321(11) -0.0007(9) 0.0125(9) 0.0004(9) C10 0.0383(13) 0.0381(12) 0.0479(14) -0.0053(11) 0.0182(11) -0.0100(10) C11 0.0187(9) 0.0506(16) 0.0338(11) 0.0083(10) 0.0070(7) 0.0000(9) C12 0.0222(10) 0.0524(14) 0.0370(12) 0.0061(11) 0.0125(8) -0.0041(9) C13 0.0322(11) 0.0381(12) 0.0277(10) 0.0022(9) 0.0170(8) 0.0007(9) C14 0.0432(13) 0.0244(11) 0.0469(14) 0.0035(10) 0.0163(11) -0.0013(9) C15 0.0411(13) 0.0526(15) 0.0200(10) 0.0022(10) 0.0044(9) -0.0034(11) #----------------------------------------------------------------------------# # 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 Ga N2 1.9592(15) . ? Ga N1 2.1130(17) . ? Ga N3 2.1407(18) . ? Ga Cl2 2.1940(6) . ? Ga Cl1 2.2085(5) . ? Ga C1 2.4486(18) . ? Si N1 1.7364(18) . ? Si C10 1.857(2) . ? Si C9 1.862(2) . ? Si C8 1.866(2) . ? N1 C1 1.317(3) . ? N2 C1 1.325(3) . ? N2 C11 1.453(3) . ? N3 C15 1.483(2) . ? N3 C14 1.488(3) . ? N3 C13 1.497(3) . ? C1 C2 1.495(3) . ? C2 C7 1.383(3) . ? C2 C3 1.388(3) . ? C3 C4 1.393(3) . ? C4 C5 1.378(4) . ? C5 C6 1.379(3) . ? C6 C7 1.395(3) . ? C11 C12 1.509(3) . ? C12 C13 1.525(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 N2 Ga N1 65.08(7) . . ? N2 Ga N3 88.18(7) . . ? N1 Ga N3 149.47(6) . . ? N2 Ga Cl2 109.78(6) . . ? N1 Ga Cl2 103.58(5) . . ? N3 Ga Cl2 99.07(5) . . ? N2 Ga Cl1 138.69(6) . . ? N1 Ga Cl1 97.58(5) . . ? N3 Ga Cl1 93.20(5) . . ? Cl2 Ga Cl1 110.73(2) . . ? N2 Ga C1 32.66(7) . . ? N1 Ga C1 32.52(7) . . ? N3 Ga C1 120.09(6) . . ? Cl2 Ga C1 108.00(5) . . ? Cl1 Ga C1 122.92(5) . . ? N1 Si C10 106.27(10) . . ? N1 Si C9 108.71(10) . . ? C10 Si C9 109.73(12) . . ? N1 Si C8 113.14(10) . . ? C10 Si C8 109.44(13) . . ? C9 Si C8 109.48(12) . . ? C1 N1 Si 135.63(14) . . ? C1 N1 Ga 87.90(12) . . ? Si N1 Ga 136.47(9) . . ? C1 N2 C11 126.74(16) . . ? C1 N2 Ga 94.43(12) . . ? C11 N2 Ga 134.34(14) . . ? C15 N3 C14 107.58(19) . . ? C15 N3 C13 107.46(17) . . ? C14 N3 C13 110.21(18) . . ? C15 N3 Ga 111.29(14) . . ? C14 N3 Ga 109.92(14) . . ? C13 N3 Ga 110.31(12) . . ? N1 C1 N2 112.27(16) . . ? N1 C1 C2 125.77(18) . . ? N2 C1 C2 121.96(17) . . ? N1 C1 Ga 59.58(10) . . ? N2 C1 Ga 52.91(9) . . ? C2 C1 Ga 172.79(15) . . ? C7 C2 C3 119.57(19) . . ? C7 C2 C1 121.02(18) . . ? C3 C2 C1 119.41(19) . . ? C2 C3 C4 119.8(2) . . ? C5 C4 C3 120.4(2) . . ? C6 C5 C4 119.96(19) . . ? C5 C6 C7 120.0(2) . . ? C2 C7 C6 120.3(2) . . ? N2 C11 C12 109.61(17) . . ? C11 C12 C13 114.60(19) . . ? N3 C13 C12 115.97(18) . . ? #===END data_gunko-5 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[{CeCl2(Me3SiNCPhN(CH2)3NMe2)2}2].2(C5H12)' _chemical_formula_analytical ? _chemical_formula_sum 'C70 H128 Ce2 Cl2 N12 Si4' _chemical_formula_weight 1601.34 _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' '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' 'Ce' 'Ce' -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 10.034(4) _cell_length_b 18.888(3) _cell_length_c 22.335(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.28(2) _cell_angle_gamma 90.00 _cell_volume 4221.2(20) _cell_formula_units_Z 2 _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 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method ? _exptl_crystal_F_000 1676 _exptl_absorpt_coefficient_mu 1.228 _exptl_absorpt_correction_type ? _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 6230 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0669 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 23.00 _reflns_number_total 5853 _reflns_number_observed 4426 _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_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+2.9698P] 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 5853 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_obs 0.0383 _refine_ls_wR_factor_all 0.0881 _refine_ls_wR_factor_obs 0.0770 _refine_ls_goodness_of_fit_all 1.044 _refine_ls_goodness_of_fit_obs 1.061 _refine_ls_restrained_S_all 1.044 _refine_ls_restrained_S_obs 1.061 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ce Ce 0.44908(3) -0.03645(2) 0.092422(13) 0.02384(10) Uani 1 d . . Cl Cl 0.33597(12) 0.03291(8) -0.01364(5) 0.0348(3) Uani 1 d . . Si1 Si 0.12001(15) -0.13844(9) 0.04896(7) 0.0359(4) Uani 1 d . . Si2 Si 0.4221(2) 0.16250(8) 0.13403(7) 0.0365(4) Uani 1 d . . N1 N 0.2881(4) -0.1354(2) 0.0714(2) 0.0303(11) Uani 1 d . . N2 N 0.4966(4) -0.1619(2) 0.1086(2) 0.0386(12) Uani 1 d . . N3 N 0.6680(4) -0.0444(2) 0.1747(2) 0.0328(11) Uani 1 d . . N4 N 0.4032(4) 0.0741(2) 0.1492(2) 0.0296(10) Uani 1 d . . N5 N 0.3160(4) -0.0284(2) 0.1822(2) 0.0319(11) Uani 1 d . . N6 N 0.0477(6) -0.1153(3) 0.3088(2) 0.059(2) Uani 1 d . . C1 C 0.3762(5) -0.1845(3) 0.0909(2) 0.0308(13) Uani 1 d . . C2 C 0.6104(5) -0.2083(3) 0.1253(3) 0.050(2) Uani 1 d . . H2A H 0.6655(5) -0.2137(3) 0.0906(3) 0.060 Uiso 1 calc R . H2B H 0.5773(5) -0.2557(3) 0.1358(3) 0.060 Uiso 1 calc R . C3 C 0.6958(6) -0.1784(3) 0.1782(3) 0.054(2) Uani 1 d . . H3A H 0.6404(6) -0.1750(3) 0.2129(3) 0.065 Uiso 1 calc R . H3B H 0.7691(6) -0.2122(3) 0.1890(3) 0.065 Uiso 1 calc R . C4 C 0.7564(5) -0.1064(3) 0.1678(3) 0.042(2) Uani 1 d . . H4A H 0.8363(5) -0.1008(3) 0.1962(3) 0.051 Uiso 1 calc R . H4B H 0.7870(5) -0.1055(3) 0.1267(3) 0.051 Uiso 1 calc R . C5 C 0.3365(5) -0.2604(3) 0.0955(3) 0.0361(14) Uani 1 d . . C6 C 0.3111(7) -0.3013(3) 0.0451(3) 0.061(2) Uani 1 d . . H6 H 0.3209(7) -0.2816(3) 0.0065(3) 0.074 Uiso 1 calc R . C7 C 0.2714(9) -0.3707(4) 0.0501(4) 0.088(3) Uani 1 d . . H7 H 0.2546(9) -0.3983(4) 0.0148(4) 0.106 Uiso 1 calc R . C8 C 0.2561(9) -0.3999(4) 0.1039(5) 0.096(3) Uani 1 d . . H8 H 0.2269(9) -0.4475(4) 0.1064(5) 0.115 Uiso 1 calc R . C9 C 0.2826(7) -0.3610(4) 0.1553(4) 0.078(3) Uani 1 d . . H9 H 0.2737(7) -0.3819(4) 0.1935(4) 0.094 Uiso 1 calc R . C10 C 0.3230(6) -0.2901(3) 0.1512(3) 0.051(2) Uani 1 d . . H10 H 0.3410(6) -0.2627(3) 0.1865(3) 0.061 Uiso 1 calc R . C11 C 0.0500(5) -0.0512(3) 0.0670(3) 0.044(2) Uani 1 d . . H11A H 0.0622(5) -0.0431(3) 0.1104(3) 0.067 Uiso 1 calc R . H11B H -0.0456(5) -0.0501(3) 0.0542(3) 0.067 Uiso 1 calc R . H11C H 0.0962(5) -0.0140(3) 0.0460(3) 0.067 Uiso 1 calc R . C12 C 0.0219(6) -0.2078(3) 0.0867(3) 0.050(2) Uani 1 d . . H12A H 0.0570(6) -0.2548(3) 0.0779(3) 0.075 Uiso 1 calc R . H12B H -0.0723(6) -0.2049(3) 0.0718(3) 0.075 Uiso 1 calc R . H12C H 0.0298(6) -0.2000(3) 0.1302(3) 0.075 Uiso 1 calc R . C13 C 0.0949(6) -0.1517(4) -0.0335(3) 0.061(2) Uani 1 d . . H13A H 0.1314(6) -0.1978(4) -0.0441(3) 0.091 Uiso 1 calc R . H13B H 0.1409(6) -0.1141(4) -0.0541(3) 0.091 Uiso 1 calc R . H13C H -0.0009(6) -0.1502(4) -0.0459(3) 0.091 Uiso 1 calc R . C14 C 0.6264(6) -0.0401(4) 0.2365(2) 0.056(2) Uani 1 d . . H14A H 0.5722(6) -0.0816(4) 0.2448(2) 0.084 Uiso 1 calc R . H14B H 0.5736(6) 0.0030(4) 0.2409(2) 0.084 Uiso 1 calc R . H14C H 0.7058(6) -0.0388(4) 0.2648(2) 0.084 Uiso 1 calc R . C15 C 0.7487(6) 0.0191(3) 0.1647(3) 0.047(2) Uani 1 d . . H15A H 0.7783(6) 0.0181(3) 0.1239(3) 0.070 Uiso 1 calc R . H15B H 0.8269(6) 0.0198(3) 0.1938(3) 0.070 Uiso 1 calc R . H15C H 0.6947(6) 0.0616(3) 0.1699(3) 0.070 Uiso 1 calc R . C16 C 0.3158(5) 0.0412(3) 0.1825(2) 0.0297(12) Uani 1 d . . C17 C 0.2172(6) -0.0699(3) 0.2132(2) 0.0383(14) Uani 1 d . . H17A H 0.1833(6) -0.1089(3) 0.1867(2) 0.046 Uiso 1 calc R . H17B H 0.1406(6) -0.0391(3) 0.2210(2) 0.046 Uiso 1 calc R . C18 C 0.2744(6) -0.1004(4) 0.2714(3) 0.054(2) Uani 1 d . . H18A H 0.3007(6) -0.0614(4) 0.2994(3) 0.065 Uiso 1 calc R . H18B H 0.3556(6) -0.1280(4) 0.2643(3) 0.065 Uiso 1 calc R . C19 C 0.1735(7) -0.1485(3) 0.2999(3) 0.062(2) Uani 1 d . . H19A H 0.1569(7) -0.1906(3) 0.2739(3) 0.074 Uiso 1 calc R . H19B H 0.2137(7) -0.1653(3) 0.3392(3) 0.074 Uiso 1 calc R . C20 C 0.2207(6) 0.0825(3) 0.2185(3) 0.0384(15) Uani 1 d . . C21 C 0.2585(8) 0.1005(3) 0.2773(3) 0.061(2) Uani 1 d . . H21 H 0.3436(8) 0.0864(3) 0.2948(3) 0.073 Uiso 1 calc R . C22 C 0.1723(11) 0.1392(4) 0.3111(4) 0.089(3) Uani 1 d . . H22 H 0.1984(11) 0.1527(4) 0.3513(4) 0.106 Uiso 1 calc R . C23 C 0.0482(10) 0.1572(4) 0.2847(5) 0.102(4) Uani 1 d . . H23 H -0.0125(10) 0.1822(4) 0.3076(5) 0.122 Uiso 1 calc R . C24 C 0.0105(8) 0.1403(4) 0.2269(5) 0.083(3) Uani 1 d . . H24 H -0.0748(8) 0.1544(4) 0.2096(5) 0.100 Uiso 1 calc R . C25 C 0.0960(6) 0.1025(3) 0.1928(3) 0.056(2) Uani 1 d . . H25 H 0.0697(6) 0.0905(3) 0.1524(3) 0.067 Uiso 1 calc R . C26 C 0.2699(7) 0.2042(4) 0.0975(5) 0.135(5) Uani 1 d . . H26A H 0.2393(7) 0.1770(4) 0.0618(5) 0.203 Uiso 1 calc R . H26B H 0.2904(7) 0.2528(4) 0.0858(5) 0.203 Uiso 1 calc R . H26C H 0.1996(7) 0.2050(4) 0.1257(5) 0.203 Uiso 1 calc R . C27 C 0.4783(13) 0.2139(5) 0.2007(3) 0.158(6) Uani 1 d . . H27A H 0.4117(13) 0.2105(5) 0.2305(3) 0.237 Uiso 1 calc R . H27B H 0.4895(13) 0.2635(5) 0.1894(3) 0.237 Uiso 1 calc R . H27C H 0.5639(13) 0.1951(5) 0.2178(3) 0.237 Uiso 1 calc R . C28 C 0.5507(7) 0.1707(3) 0.0797(3) 0.066(2) Uani 1 d . . H28A H 0.5233(7) 0.1437(3) 0.0435(3) 0.098 Uiso 1 calc R . H28B H 0.6358(7) 0.1522(3) 0.0976(3) 0.098 Uiso 1 calc R . H28C H 0.5614(7) 0.2207(3) 0.0693(3) 0.098 Uiso 1 calc R . C29 C 0.0602(9) -0.0582(4) 0.3510(4) 0.102(3) Uani 1 d . . H29A H -0.0280(9) -0.0374(4) 0.3554(4) 0.153 Uiso 1 calc R . H29B H 0.1199(9) -0.0220(4) 0.3365(4) 0.153 Uiso 1 calc R . H29C H 0.0972(9) -0.0760(4) 0.3899(4) 0.153 Uiso 1 calc R . C30 C -0.0462(7) -0.1681(4) 0.3284(3) 0.076(2) Uani 1 d . . H30A H -0.0540(7) -0.2069(4) 0.2992(3) 0.114 Uiso 1 calc R . H30B H -0.1339(7) -0.1461(4) 0.3313(3) 0.114 Uiso 1 calc R . H30C H -0.0136(7) -0.1866(4) 0.3677(3) 0.114 Uiso 1 calc R . C31 C 0.5069(14) -0.5765(9) 0.0926(6) 0.225(9) Uani 1 d . . H31A H 0.6026(14) -0.5824(9) 0.0879(6) 0.338 Uiso 1 calc R . H31B H 0.4801(14) -0.6078(9) 0.1246(6) 0.338 Uiso 1 calc R . H31C H 0.4887(14) -0.5272(9) 0.1030(6) 0.338 Uiso 1 calc R . C32 C 0.4284(15) -0.5954(11) 0.0343(9) 0.256(11) Uani 1 d . . H32A H 0.4571(15) -0.5643(11) 0.0020(9) 0.307 Uiso 1 calc R . H32B H 0.4486(15) -0.6449(11) 0.0236(9) 0.307 Uiso 1 calc R . C33 C 0.3021(16) -0.5887(7) 0.0377(7) 0.156(5) Uani 1 d . . H33A H 0.2808(16) -0.5386(7) 0.0457(7) 0.188 Uiso 1 calc R . H33B H 0.2738(16) -0.6175(7) 0.0715(7) 0.188 Uiso 1 calc R . C34 C 0.2248(23) -0.6124(12) -0.0203(8) 0.308(15) Uani 1 d . . H34A H 0.2705(23) -0.5948(12) -0.0552(8) 0.369 Uiso 1 calc R . H34B H 0.2230(23) -0.6647(12) -0.0222(8) 0.369 Uiso 1 calc R . C35 C 0.0946(18) -0.5865(11) -0.0232(8) 0.239(9) Uani 1 d . . H35A H 0.0466(18) -0.6022(11) -0.0607(8) 0.359 Uiso 1 calc R . H35B H 0.0964(18) -0.5346(11) -0.0220(8) 0.359 Uiso 1 calc R . H35C H 0.0490(18) -0.6045(11) 0.0110(8) 0.359 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 Ce 0.0179(2) 0.0262(2) 0.0281(2) 0.0010(2) 0.00609(11) 0.0013(2) Cl 0.0201(7) 0.0517(8) 0.0334(7) 0.0081(7) 0.0067(5) 0.0065(7) Si1 0.0197(8) 0.0457(10) 0.0427(10) 0.0037(8) 0.0041(7) -0.0055(7) Si2 0.0357(10) 0.0284(9) 0.0476(10) -0.0038(7) 0.0174(8) -0.0048(7) N1 0.017(2) 0.033(3) 0.041(3) 0.005(2) 0.002(2) 0.001(2) N2 0.023(3) 0.025(3) 0.067(3) 0.004(2) -0.007(2) 0.001(2) N3 0.024(2) 0.038(3) 0.036(3) -0.001(2) -0.002(2) 0.000(2) N4 0.024(3) 0.032(3) 0.033(3) -0.001(2) 0.008(2) 0.000(2) N5 0.036(3) 0.027(3) 0.034(3) 0.005(2) 0.013(2) -0.004(2) N6 0.064(4) 0.053(4) 0.066(4) 0.008(3) 0.034(3) -0.013(3) C1 0.025(3) 0.030(3) 0.038(3) 0.000(3) 0.008(3) 0.001(3) C2 0.022(3) 0.035(4) 0.091(5) 0.007(3) -0.003(3) 0.001(3) C3 0.031(4) 0.052(4) 0.076(5) 0.016(4) -0.012(3) 0.014(3) C4 0.025(3) 0.044(4) 0.057(4) 0.005(3) -0.002(3) -0.001(3) C5 0.021(3) 0.030(3) 0.059(4) 0.004(3) 0.015(3) 0.001(3) C6 0.062(5) 0.048(4) 0.077(5) -0.009(4) 0.024(4) -0.014(4) C7 0.096(7) 0.057(5) 0.115(7) -0.026(5) 0.034(6) -0.033(5) C8 0.084(7) 0.044(5) 0.165(10) 0.004(6) 0.043(7) -0.015(5) C9 0.052(5) 0.068(6) 0.120(7) 0.051(5) 0.037(5) 0.009(4) C10 0.043(4) 0.051(4) 0.060(4) 0.018(3) 0.009(3) 0.005(3) C11 0.018(3) 0.056(4) 0.059(4) 0.017(3) 0.002(3) -0.001(3) C12 0.033(4) 0.050(4) 0.068(4) 0.004(3) 0.016(3) -0.009(3) C13 0.036(4) 0.096(6) 0.049(4) 0.004(4) -0.003(3) -0.013(4) C14 0.050(4) 0.082(5) 0.036(3) 0.003(4) 0.000(3) 0.010(4) C15 0.037(4) 0.049(4) 0.054(4) -0.007(3) -0.004(3) -0.007(3) C16 0.026(3) 0.036(3) 0.027(3) 0.001(3) 0.005(2) 0.000(3) C17 0.038(4) 0.034(3) 0.046(4) -0.003(3) 0.022(3) -0.002(3) C18 0.047(4) 0.066(5) 0.050(4) 0.020(4) 0.005(3) -0.002(4) C19 0.069(5) 0.049(4) 0.069(5) 0.027(4) 0.018(4) -0.007(4) C20 0.042(4) 0.028(3) 0.049(4) -0.005(3) 0.028(3) -0.010(3) C21 0.090(6) 0.046(4) 0.052(4) -0.008(3) 0.034(4) -0.026(4) C22 0.138(9) 0.060(5) 0.077(6) -0.033(4) 0.074(7) -0.053(6) C23 0.098(8) 0.058(6) 0.164(10) -0.053(6) 0.103(8) -0.049(6) C24 0.051(5) 0.045(5) 0.159(9) -0.035(5) 0.047(6) -0.012(4) C25 0.030(4) 0.044(4) 0.097(5) -0.025(4) 0.026(4) -0.005(3) C26 0.044(5) 0.077(6) 0.288(14) 0.095(8) 0.033(7) 0.022(5) C27 0.317(17) 0.091(7) 0.070(6) -0.038(5) 0.051(8) -0.127(9) C28 0.070(5) 0.047(4) 0.086(5) 0.014(4) 0.045(4) 0.001(4) C29 0.122(8) 0.094(7) 0.097(7) -0.023(5) 0.066(6) -0.042(6) C30 0.063(5) 0.082(6) 0.087(6) 0.021(5) 0.027(4) -0.013(4) C31 0.163(14) 0.369(24) 0.130(11) -0.012(13) -0.081(11) 0.033(15) C32 0.112(13) 0.399(30) 0.261(22) 0.026(20) 0.045(14) 0.104(16) C33 0.184(15) 0.123(10) 0.167(13) -0.014(9) 0.049(12) 0.013(11) C34 0.301(29) 0.412(33) 0.194(18) -0.165(20) -0.086(20) 0.137(26) C35 0.211(20) 0.316(24) 0.194(17) -0.017(16) 0.036(16) 0.050(19) _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 2.438(4) . ? Ce N1 2.492(4) . ? Ce N5 2.496(4) . ? Ce N4 2.503(4) . ? Ce N3 2.761(4) . ? Ce Cl 2.8662(14) . ? Ce Cl 2.8842(15) 3_655 ? Ce C1 2.890(5) . ? Ce C16 2.895(5) . ? Cl Ce 2.8842(15) 3_655 ? Si1 N1 1.724(4) . ? Si1 C11 1.848(6) . ? Si1 C13 1.858(6) . ? Si1 C12 1.877(6) . ? Si2 N4 1.717(4) . ? Si2 C27 1.830(7) . ? Si2 C28 1.842(6) . ? Si2 C26 1.853(8) . ? N1 C1 1.332(6) . ? N2 C1 1.314(7) . ? N2 C2 1.466(7) . ? N3 C14 1.473(7) . ? N3 C15 1.474(7) . ? N3 C4 1.483(7) . ? N4 C16 1.344(6) . ? N5 C16 1.314(6) . ? N5 C17 1.476(6) . ? N6 C29 1.433(8) . ? N6 C19 1.437(8) . ? N6 C30 1.461(8) . ? C1 C5 1.493(7) . ? C2 C3 1.516(8) . ? C3 C4 1.515(8) . ? C5 C6 1.373(8) . ? C5 C10 1.381(8) . ? C6 C7 1.376(9) . ? C7 C8 1.342(11) . ? C8 C9 1.373(11) . ? C9 C10 1.403(9) . ? C16 C20 1.512(7) . ? C17 C18 1.495(8) . ? C18 C19 1.533(8) . ? C20 C21 1.382(8) . ? C20 C25 1.389(8) . ? C21 C22 1.397(10) . ? C22 C23 1.381(13) . ? C23 C24 1.356(12) . ? C24 C25 1.386(9) . ? C31 C32 1.51(2) . ? C32 C33 1.28(2) . ? C33 C34 1.53(2) . ? C34 C35 1.39(2) . ? 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 54.24(14) . . ? N2 Ce N5 92.90(15) . . ? N1 Ce N5 79.57(14) . . ? N2 Ce N4 140.99(15) . . ? N1 Ce N4 125.45(14) . . ? N5 Ce N4 54.03(14) . . ? N2 Ce N3 73.23(14) . . ? N1 Ce N3 123.83(13) . . ? N5 Ce N3 85.13(13) . . ? N4 Ce N3 82.86(13) . . ? N2 Ce Cl 128.86(12) . . ? N1 Ce Cl 88.63(10) . . ? N5 Ce Cl 115.70(10) . . ? N4 Ce Cl 87.75(10) . . ? N3 Ce Cl 145.23(10) . . ? N2 Ce Cl 88.05(11) . 3_655 ? N1 Ce Cl 113.95(10) . 3_655 ? N5 Ce Cl 163.38(10) . 3_655 ? N4 Ce Cl 117.63(10) . 3_655 ? N3 Ce Cl 79.25(9) . 3_655 ? Cl Ce Cl 75.71(4) . 3_655 ? N2 Ce C1 26.87(14) . . ? N1 Ce C1 27.39(14) . . ? N5 Ce C1 85.30(14) . . ? N4 Ce C1 139.20(14) . . ? N3 Ce C1 98.22(14) . . ? Cl Ce C1 110.40(11) . . ? Cl Ce C1 102.45(11) 3_655 . ? N2 Ce C16 119.0(2) . . ? N1 Ce C16 100.63(14) . . ? N5 Ce C16 26.94(13) . . ? N4 Ce C16 27.62(14) . . ? N3 Ce C16 87.19(13) . . ? Cl Ce C16 99.65(10) . . ? Cl Ce C16 144.80(11) 3_655 . ? C1 Ce C16 111.62(15) . . ? Ce Cl Ce 104.29(4) . 3_655 ? N1 Si1 C11 106.7(2) . . ? N1 Si1 C13 110.5(3) . . ? C11 Si1 C13 108.1(3) . . ? N1 Si1 C12 115.3(3) . . ? C11 Si1 C12 107.7(3) . . ? C13 Si1 C12 108.3(3) . . ? N4 Si2 C27 112.8(3) . . ? N4 Si2 C28 107.8(3) . . ? C27 Si2 C28 107.6(4) . . ? N4 Si2 C26 113.6(3) . . ? C27 Si2 C26 109.1(5) . . ? C28 Si2 C26 105.6(4) . . ? C1 N1 Si1 133.1(4) . . ? C1 N1 Ce 93.2(3) . . ? Si1 N1 Ce 133.3(2) . . ? C1 N2 C2 124.3(5) . . ? C1 N2 Ce 96.1(3) . . ? C2 N2 Ce 139.3(3) . . ? C14 N3 C15 107.1(5) . . ? C14 N3 C4 110.7(4) . . ? C15 N3 C4 106.6(4) . . ? C14 N3 Ce 110.7(3) . . ? C15 N3 Ce 105.9(3) . . ? C4 N3 Ce 115.2(3) . . ? C16 N4 Si2 130.2(4) . . ? C16 N4 Ce 92.6(3) . . ? Si2 N4 Ce 133.2(2) . . ? C16 N5 C17 121.9(4) . . ? C16 N5 Ce 93.7(3) . . ? C17 N5 Ce 139.7(3) . . ? C29 N6 C19 112.7(6) . . ? C29 N6 C30 110.1(6) . . ? C19 N6 C30 109.7(5) . . ? N2 C1 N1 116.4(5) . . ? N2 C1 C5 122.4(5) . . ? N1 C1 C5 121.1(5) . . ? N2 C1 Ce 57.0(3) . . ? N1 C1 Ce 59.4(3) . . ? C5 C1 Ce 175.3(4) . . ? N2 C2 C3 111.1(5) . . ? C4 C3 C2 115.2(5) . . ? N3 C4 C3 116.3(5) . . ? C6 C5 C10 119.0(6) . . ? C6 C5 C1 121.2(5) . . ? C10 C5 C1 119.7(6) . . ? C5 C6 C7 120.4(7) . . ? C8 C7 C6 121.2(8) . . ? C7 C8 C9 120.1(8) . . ? C8 C9 C10 119.6(7) . . ? C5 C10 C9 119.7(7) . . ? N5 C16 N4 117.4(5) . . ? N5 C16 C20 121.3(5) . . ? N4 C16 C20 121.3(5) . . ? N5 C16 Ce 59.3(3) . . ? N4 C16 Ce 59.7(3) . . ? C20 C16 Ce 167.0(4) . . ? N5 C17 C18 112.6(5) . . ? C17 C18 C19 111.5(5) . . ? N6 C19 C18 114.4(5) . . ? C21 C20 C25 120.1(6) . . ? C21 C20 C16 119.5(6) . . ? C25 C20 C16 120.4(5) . . ? C20 C21 C22 120.3(8) . . ? C23 C22 C21 118.2(8) . . ? C24 C23 C22 121.9(8) . . ? C23 C24 C25 120.2(9) . . ? C24 C25 C20 119.3(7) . . ? C33 C32 C31 112.3(17) . . ? C32 C33 C34 111.3(16) . . ? C35 C34 C33 110.6(17) . . ? _refine_diff_density_max 0.408 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.081 #===END