#Copyright The Royal Society of Chemistry, 1998 #P.B. Hitchcock, M.F. Lappert and M.Layh, J. Chem. Soc. Dalton Trans., #Compound 2' data_dec194 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Cu2{Me3SiNC(tBu)CHSiMe3}2]' _chemical_formula_analytical ? _chemical_formula_sum 'C24 H56 Cu2 N2 Si4' _chemical_formula_weight 612.15 _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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.210(4) _cell_length_b 9.412(3) _cell_length_c 11.624(4) _cell_angle_alpha 102.83(3) _cell_angle_beta 91.97(3) _cell_angle_gamma 118.86(3) _cell_volume 848.5(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method ? _exptl_crystal_F_000 328 _exptl_absorpt_coefficient_mu 1.408 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2979 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0793 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2979 _reflns_number_observed 2012 _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^)+(0.1223P)^2^+0.7510P] 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 2979 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1058 _refine_ls_R_factor_obs 0.0610 _refine_ls_wR_factor_all 0.1907 _refine_ls_wR_factor_obs 0.1510 _refine_ls_goodness_of_fit_all 0.912 _refine_ls_goodness_of_fit_obs 0.882 _refine_ls_restrained_S_all 0.912 _refine_ls_restrained_S_obs 0.882 _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 Cu Cu 0.10653(9) -0.00871(10) -0.06033(7) 0.0356(3) Uani 1 d . . Si1 Si 0.0484(2) -0.1784(3) -0.3238(2) 0.0459(5) Uani 1 d . . Si2 Si -0.1968(3) 0.1134(2) -0.1385(2) 0.0446(5) Uani 1 d . . N N -0.0534(6) -0.1489(6) -0.2045(5) 0.0356(12) Uani 1 d . . C1 C -0.2061(8) -0.2002(8) -0.1811(5) 0.0349(14) Uani 1 d . . C2 C -0.2414(8) -0.0840(8) -0.0981(6) 0.0359(15) Uani 1 d . . H2 H -0.3602(8) -0.1445(8) -0.0898(6) 0.043 Uiso 1 calc R . C3 C -0.3537(9) -0.3815(8) -0.2338(6) 0.045(2) Uani 1 d . . C4 C -0.4749(11) -0.3813(12) -0.3284(8) 0.080(3) Uani 1 d . . H4A H -0.4162(11) -0.3402(12) -0.3910(8) 0.121 Uiso 1 calc R . H4B H -0.5168(11) -0.3096(12) -0.2917(8) 0.121 Uiso 1 calc R . H4C H -0.5672(11) -0.4940(12) -0.3615(8) 0.121 Uiso 1 calc R . C5 C -0.2946(11) -0.5026(10) -0.2900(9) 0.071(3) Uani 1 d . . H5A H -0.2350(11) -0.4658(10) -0.3534(9) 0.107 Uiso 1 calc R . H5B H -0.3901(11) -0.6137(10) -0.3217(9) 0.107 Uiso 1 calc R . H5C H -0.2214(11) -0.5046(10) -0.2304(9) 0.107 Uiso 1 calc R . C6 C -0.4460(11) -0.4476(10) -0.1345(8) 0.072(3) Uani 1 d . . H6A H -0.4865(11) -0.3752(10) -0.0964(8) 0.108 Uiso 1 calc R . H6B H -0.3706(11) -0.4496(10) -0.0767(8) 0.108 Uiso 1 calc R . H6C H -0.5393(11) -0.5596(10) -0.1679(8) 0.108 Uiso 1 calc R . C7 C -0.0748(11) -0.2378(12) -0.4732(7) 0.067(2) Uani 1 d . . H7A H -0.1133(11) -0.1599(12) -0.4750(7) 0.101 Uiso 1 calc R . H7B H -0.1697(11) -0.3496(12) -0.4887(7) 0.101 Uiso 1 calc R . H7C H -0.0051(11) -0.2347(12) -0.5332(7) 0.101 Uiso 1 calc R . C8 C 0.2357(10) 0.0321(12) -0.3094(8) 0.072(3) Uani 1 d . . H8A H 0.3053(10) 0.0703(12) -0.2332(8) 0.108 Uiso 1 calc R . H8B H 0.1998(10) 0.1109(12) -0.3153(8) 0.108 Uiso 1 calc R . H8C H 0.2985(10) 0.0237(12) -0.3722(8) 0.108 Uiso 1 calc R . C9 C 0.1271(14) -0.3259(16) -0.3156(10) 0.100(4) Uani 1 d . . H9A H 0.1903(14) -0.2923(16) -0.2375(10) 0.150 Uiso 1 calc R . H9B H 0.1978(14) -0.3230(16) -0.3748(10) 0.150 Uiso 1 calc R . H9C H 0.0334(14) -0.4384(16) -0.3303(10) 0.150 Uiso 1 calc R . C10 C -0.3247(13) 0.1924(12) -0.0552(9) 0.075(3) Uani 1 d . . H10A H -0.3052(13) 0.2945(12) -0.0729(9) 0.113 Uiso 1 calc R . H10B H -0.2930(13) 0.2145(12) 0.0292(9) 0.113 Uiso 1 calc R . H10C H -0.4418(13) 0.1089(12) -0.0789(9) 0.113 Uiso 1 calc R . C11 C -0.2672(15) 0.0691(13) -0.3022(8) 0.085(3) Uani 1 d . . H11A H -0.2422(15) 0.1725(13) -0.3204(8) 0.128 Uiso 1 calc R . H11B H -0.3861(15) -0.0083(13) -0.3221(8) 0.128 Uiso 1 calc R . H11C H -0.2093(15) 0.0207(13) -0.3479(8) 0.128 Uiso 1 calc R . C12 C 0.0254(11) 0.2874(11) -0.1033(11) 0.093(4) Uani 1 d . . H12A H 0.0334(11) 0.3815(11) -0.1278(11) 0.140 Uiso 1 calc R . H12B H 0.0937(11) 0.2495(11) -0.1452(11) 0.140 Uiso 1 calc R . H12C H 0.0639(11) 0.3212(11) -0.0188(11) 0.140 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 Cu 0.0316(4) 0.0354(5) 0.0360(5) 0.0014(3) 0.0008(3) 0.0176(3) Si1 0.0411(11) 0.0556(13) 0.0392(11) 0.0020(9) 0.0064(8) 0.0276(10) Si2 0.0492(11) 0.0415(11) 0.0539(12) 0.0132(9) 0.0072(9) 0.0310(10) N 0.033(3) 0.031(3) 0.039(3) 0.002(2) 0.000(2) 0.017(2) C1 0.035(3) 0.035(4) 0.032(3) 0.007(3) 0.002(3) 0.017(3) C2 0.027(3) 0.036(4) 0.037(4) 0.002(3) 0.000(3) 0.014(3) C3 0.045(4) 0.031(4) 0.047(4) 0.000(3) 0.003(3) 0.015(3) C4 0.055(5) 0.072(6) 0.070(6) -0.018(5) -0.029(4) 0.017(5) C5 0.068(6) 0.035(4) 0.096(7) 0.001(4) 0.023(5) 0.021(4) C6 0.068(6) 0.039(5) 0.081(6) 0.008(4) 0.032(5) 0.007(4) C7 0.069(5) 0.076(6) 0.045(5) 0.009(4) 0.008(4) 0.031(5) C8 0.046(5) 0.084(7) 0.059(5) 0.013(5) 0.016(4) 0.016(4) C9 0.108(8) 0.139(11) 0.102(9) 0.024(7) 0.028(7) 0.101(9) C10 0.096(7) 0.072(6) 0.087(7) 0.017(5) 0.025(6) 0.065(6) C11 0.134(9) 0.092(7) 0.069(6) 0.038(6) 0.022(6) 0.080(7) C12 0.064(6) 0.055(6) 0.165(11) 0.047(7) 0.008(6) 0.027(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N 1.921(5) . ? Cu C2 1.943(6) 2 ? Cu Cu 2.499(2) 2 ? Cu Si2 2.945(2) 2 ? Si1 N 1.746(6) . ? Si1 C7 1.854(8) . ? Si1 C9 1.867(10) . ? Si1 C8 1.861(8) . ? Si2 C2 1.872(7) . ? Si2 C10 1.866(8) . ? Si2 C12 1.857(9) . ? Si2 C11 1.875(9) . ? Si2 Cu 2.945(2) 2 ? N C1 1.309(8) . ? C1 C2 1.460(9) . ? C1 C3 1.541(9) . ? C2 Cu 1.943(6) 2 ? C3 C6 1.523(11) . ? C3 C5 1.521(10) . ? C3 C4 1.540(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Cu C2 166.2(2) . 2 ? N Cu Cu 94.5(2) . 2 ? C2 Cu Cu 81.2(2) 2 2 ? N Cu Si2 128.1(2) . 2 ? C2 Cu Si2 38.6(2) 2 2 ? Cu Cu Si2 83.86(6) 2 2 ? N Si1 C7 114.2(3) . . ? N Si1 C9 112.9(4) . . ? C7 Si1 C9 111.2(5) . . ? N Si1 C8 105.4(3) . . ? C7 Si1 C8 105.3(4) . . ? C9 Si1 C8 107.1(5) . . ? C2 Si2 C10 106.6(4) . . ? C2 Si2 C12 116.7(4) . . ? C10 Si2 C12 108.0(5) . . ? C2 Si2 C11 111.3(4) . . ? C10 Si2 C11 107.4(5) . . ? C12 Si2 C11 106.5(5) . . ? C2 Si2 Cu 40.4(2) . 2 ? C10 Si2 Cu 94.6(3) . 2 ? C12 Si2 Cu 85.6(3) . 2 ? C11 Si2 Cu 149.6(3) . 2 ? C1 N Si1 139.5(5) . . ? C1 N Cu 109.7(4) . . ? Si1 N Cu 110.7(3) . . ? N C1 C2 119.6(5) . . ? N C1 C3 123.6(6) . . ? C2 C1 C3 116.8(5) . . ? C1 C2 Si2 116.4(5) . . ? C1 C2 Cu 114.0(4) . 2 ? Si2 C2 Cu 101.0(3) . 2 ? C6 C3 C5 106.3(7) . . ? C6 C3 C1 109.7(6) . . ? C5 C3 C1 112.1(6) . . ? C6 C3 C4 109.8(7) . . ? C5 C3 C4 109.7(7) . . ? C1 C3 C4 109.2(6) . . ? _refine_diff_density_max 0.661 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.102 #=END #P.B. Hitchcock, M.F. Lappert and M. Layh, J. Chem. Soc., Dalton Trans. #Compound 4 data_feb1795 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Li(dme)3][Cu{Me3SiNC(tBu)CHSiMe3}2]' _chemical_formula_analytical ? _chemical_formula_sum 'C36 H86 Cu Li N2 O6 Si4' _chemical_formula_weight 825.91 _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' '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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' _cell_length_a 9.653(12) _cell_length_b 14.164(14) _cell_length_c 18.277(15) _cell_angle_alpha 90.00 _cell_angle_beta 94.93(9) _cell_angle_gamma 90.00 _cell_volume 2489.7(45) _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 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_method ? _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.572 _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 3681 _diffrn_reflns_av_R_equivalents 0.1068 _diffrn_reflns_av_sigmaI/netI 0.1331 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 23.00 _reflns_number_total 3456 _reflns_number_observed 1654 _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 ; In the anion the ligand is disordered in a 57:43 ratio between conformations in which there are resolved alternative sites for C(7),C(8), and N, a common SiMe3 group on N, and the other SiMe3 group and the t-butyl group overlapping Refinement on F^2^ for ALL reflections except for 9 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^)+(0.1215P)^2^+5.2483P] 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 3447 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1953 _refine_ls_R_factor_obs 0.0978 _refine_ls_wR_factor_all 0.3233 _refine_ls_wR_factor_obs 0.2235 _refine_ls_goodness_of_fit_all 1.045 _refine_ls_goodness_of_fit_obs 1.205 _refine_ls_restrained_S_all 1.189 _refine_ls_restrained_S_obs 1.205 _refine_ls_shift/esd_max -0.208 _refine_ls_shift/esd_mean 0.001 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 Cu Cu 0.0000 0.24998(10) 0.2500 0.0799(6) Uani 1 d S . Si1 Si -0.0753(3) 0.3359(2) 0.09969(12) 0.0768(8) Uani 1 d . . Li Li 0.5000 0.7026(12) 0.2500 0.064(6) Uani 1 d S . O1 O 0.5747(5) 0.7987(4) 0.3329(3) 0.062(2) Uani 1 d . . O2 O 0.7123(5) 0.7237(4) 0.2285(3) 0.064(2) Uani 1 d . . O3 C 0.4855(7) 0.5899(4) 0.1783(4) 0.048(2) Uani 1 d . . C1 C 0.4920(9) 0.8559(7) 0.3754(5) 0.090(3) Uani 1 d . . H1A H 0.4072(9) 0.8216(7) 0.3849(5) 0.135 Uiso 1 calc R . H1B H 0.4670(9) 0.9141(7) 0.3485(5) 0.135 Uiso 1 calc R . H1C H 0.5445(9) 0.8715(7) 0.4221(5) 0.135 Uiso 1 calc R . C2 C 0.6983(9) 0.8432(6) 0.3170(5) 0.078(3) Uani 1 d . . H2A H 0.7455(9) 0.8707(6) 0.3623(5) 0.094 Uiso 1 calc R . H2B H 0.6775(9) 0.8948(6) 0.2812(5) 0.094 Uiso 1 calc R . C3 C 0.7893(9) 0.7725(7) 0.2860(4) 0.081(3) Uani 1 d . . H3A H 0.8702(9) 0.8043(7) 0.2669(4) 0.097 Uiso 1 calc R . H3B H 0.8241(9) 0.7275(7) 0.3247(4) 0.097 Uiso 1 calc R . C4 C 0.7984(9) 0.6613(7) 0.1919(5) 0.089(3) Uani 1 d . . H4A H 0.7424(9) 0.6286(7) 0.1524(5) 0.133 Uiso 1 calc R . H4B H 0.8401(9) 0.6149(7) 0.2270(5) 0.133 Uiso 1 calc R . H4C H 0.8722(9) 0.6974(7) 0.1710(5) 0.133 Uiso 1 calc R . C5 C 0.4559(11) 0.5069(7) 0.2150(7) 0.150(6) Uani 1 d . . H5A H 0.4769(11) 0.4512(7) 0.1852(7) 0.180 Uiso 1 calc R . H5B H 0.3564(11) 0.5049(7) 0.2243(7) 0.180 Uiso 1 calc R . C6 C 0.4280(12) 0.5898(8) 0.1083(8) 0.162(6) Uani 1 d . . H6A H 0.4509(12) 0.6490(8) 0.0843(8) 0.243 Uiso 1 calc R . H6B H 0.3268(12) 0.5839(8) 0.1080(8) 0.243 Uiso 1 calc R . H6C H 0.4647(12) 0.5365(8) 0.0818(8) 0.243 Uiso 1 calc R . C10 C 0.3207(10) 0.2698(6) 0.1821(5) 0.083(3) Uani 1 d . . H10A H 0.4169(10) 0.2912(6) 0.1804(5) 0.124 Uiso 1 calc R 1 H10B H 0.3136(10) 0.2311(6) 0.2261(5) 0.124 Uiso 1 calc R 1 H10C H 0.2592(10) 0.3246(6) 0.1837(5) 0.124 Uiso 1 calc R 1 C11 C 0.2786(12) 0.2735(9) 0.0377(6) 0.130(5) Uani 1 d . . H11A H 0.3759(12) 0.2843(9) 0.0285(6) 0.196 Uiso 1 calc R 1 H11B H 0.2355(12) 0.3337(9) 0.0494(6) 0.196 Uiso 1 calc R 1 H11C H 0.2286(12) 0.2463(9) -0.0062(6) 0.196 Uiso 1 calc R 1 C12 C 0.3860(12) 0.1220(7) 0.1060(6) 0.128(5) Uani 1 d . . H12A H 0.4741(12) 0.1486(7) 0.0926(6) 0.192 Uiso 1 calc R 1 H12B H 0.3550(12) 0.0725(7) 0.0709(6) 0.192 Uiso 1 calc R 1 H12C H 0.3994(12) 0.0951(7) 0.1555(6) 0.192 Uiso 1 calc R 1 C13 C -0.0791(10) 0.3157(7) -0.0022(4) 0.095(3) Uani 1 d . . H13A H 0.0156(10) 0.3042(7) -0.0157(4) 0.143 Uiso 1 calc R . H13B H -0.1174(10) 0.3716(7) -0.0283(4) 0.143 Uiso 1 calc R . H13C H -0.1375(10) 0.2608(7) -0.0158(4) 0.143 Uiso 1 calc R . C14 C 0.0129(11) 0.4499(6) 0.1210(6) 0.114(4) Uani 1 d . . H14A H 0.1107(11) 0.4452(6) 0.1107(6) 0.170 Uiso 1 calc R . H14B H 0.0074(11) 0.4652(6) 0.1729(6) 0.170 Uiso 1 calc R . H14C H -0.0327(11) 0.4998(6) 0.0905(6) 0.170 Uiso 1 calc R . C15 C -0.2521(10) 0.3567(7) 0.1213(5) 0.102(4) Uani 1 d . . H15A H -0.3073(10) 0.2993(7) 0.1116(5) 0.153 Uiso 1 calc R . H15B H -0.2924(10) 0.4084(7) 0.0908(5) 0.153 Uiso 1 calc R . H15C H -0.2524(10) 0.3737(7) 0.1733(5) 0.153 Uiso 1 calc R . C16 C -0.2312(8) 0.0863(6) 0.0425(4) 0.075(3) Uani 1 d . . H16A H -0.2464(8) 0.1545(6) 0.0466(4) 0.113 Uiso 1 calc R 1 H16B H -0.3192(8) 0.0530(6) 0.0465(4) 0.113 Uiso 1 calc R 1 H16C H -0.1963(8) 0.0722(6) -0.0050(4) 0.113 Uiso 1 calc R 1 C17 C -0.1912(9) 0.0722(6) 0.1940(4) 0.075(3) Uani 1 d . . H17A H -0.2081(9) 0.1402(6) 0.1980(4) 0.113 Uiso 1 calc R 1 H17B H -0.1314(9) 0.0509(6) 0.2369(4) 0.113 Uiso 1 calc R 1 H17C H -0.2800(9) 0.0384(6) 0.1919(4) 0.113 Uiso 1 calc R 1 C18 C -0.0812(11) -0.0664(10) 0.1078(5) 0.148(5) Uani 1 d . . H18A H -0.0128(11) -0.0860(10) 0.1476(5) 0.222 Uiso 1 calc R 1 H18B H -0.0458(11) -0.0811(10) 0.0604(5) 0.222 Uiso 1 calc R 1 H18C H -0.1687(11) -0.1003(10) 0.1120(5) 0.222 Uiso 1 calc R 1 Si2 Si -0.1088(3) 0.0492(2) 0.11352(15) 0.0558(10) Uani 0.573(5) d P 1 N N 0.0340(17) 0.2489(12) 0.1572(7) 0.053(5) Uani 0.427(5) d P 1 C7 C 0.1193(14) 0.1809(9) 0.1239(6) 0.047(4) Uani 0.573(5) d P 1 C8 C 0.0718(19) 0.0976(11) 0.1108(7) 0.060(5) Uani 0.573(5) d P 1 H8 H 0.1388(19) 0.0530(11) 0.0976(7) 0.071 Uiso 0.573(5) calc PR 1 C9 C 0.2720(5) 0.2030(3) 0.1045(2) 0.0708(14) Uani 0.573(5) d P 1 Si21 Si 0.2720(5) 0.2030(3) 0.1045(2) 0.0708(14) Uani 0.427(5) d P 2 N11 N -0.0259(15) 0.2443(9) 0.1426(5) 0.059(4) Uani 0.573(5) d P 2 C71 C -0.0040(16) 0.1496(13) 0.1191(8) 0.040(5) Uani 0.427(5) d P 2 C81 C 0.1063(25) 0.1261(17) 0.0926(9) 0.060(7) Uani 0.427(5) d P 2 H81 H 0.1086(25) 0.0688(17) 0.0657(9) 0.072 Uiso 0.427(5) calc PR 2 C91 C -0.1088(3) 0.0492(2) 0.11352(15) 0.0558(10) Uani 0.427(5) d P 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 Cu 0.167(2) 0.0409(7) 0.0318(7) 0.000 0.0061(8) 0.000 Si1 0.127(2) 0.0527(14) 0.0502(13) 0.0168(11) 0.0069(14) 0.018(2) Li 0.079(14) 0.034(9) 0.076(12) 0.000 -0.017(10) 0.000 O1 0.058(3) 0.060(3) 0.068(3) -0.010(3) -0.002(3) -0.007(3) O2 0.054(3) 0.064(3) 0.072(3) -0.012(3) -0.013(3) 0.003(3) O3 0.030(4) 0.019(3) 0.090(5) -0.032(4) -0.020(4) -0.004(3) C1 0.060(6) 0.113(7) 0.095(7) -0.050(6) -0.003(5) 0.006(6) C2 0.083(6) 0.084(6) 0.066(5) -0.017(5) 0.002(5) -0.041(6) C3 0.074(6) 0.103(7) 0.062(5) -0.018(5) -0.011(5) -0.016(6) C4 0.059(6) 0.098(7) 0.109(7) -0.031(6) 0.003(5) 0.010(6) C5 0.089(9) 0.067(6) 0.297(19) -0.080(9) 0.034(9) 0.005(6) C6 0.114(10) 0.098(9) 0.274(17) -0.080(10) 0.014(11) -0.007(8) C10 0.098(7) 0.071(6) 0.079(6) -0.017(5) 0.011(5) -0.029(5) C11 0.120(9) 0.147(11) 0.127(10) -0.005(8) 0.026(8) -0.011(8) C12 0.140(10) 0.079(7) 0.156(11) -0.014(7) -0.039(8) -0.024(7) C13 0.132(8) 0.110(7) 0.046(5) 0.033(5) 0.018(5) 0.042(7) C14 0.132(9) 0.063(6) 0.141(9) 0.013(6) -0.014(8) 0.007(6) C15 0.131(9) 0.087(7) 0.090(7) -0.003(6) 0.022(6) 0.011(7) C16 0.075(6) 0.079(6) 0.068(5) 0.005(5) -0.016(5) 0.005(5) C17 0.084(6) 0.081(6) 0.061(5) -0.016(5) 0.013(5) -0.021(5) C18 0.126(9) 0.245(15) 0.070(7) 0.016(8) -0.017(6) 0.095(10) Si2 0.059(2) 0.074(2) 0.032(2) 0.0034(15) -0.0102(14) -0.009(2) N 0.070(11) 0.057(9) 0.026(7) -0.001(7) -0.028(7) 0.036(9) C7 0.060(9) 0.069(9) 0.010(5) 0.017(6) -0.007(6) -0.030(8) C8 0.090(12) 0.064(9) 0.024(7) 0.040(7) 0.006(7) 0.009(9) C9 0.070(3) 0.065(3) 0.078(3) 0.004(2) 0.006(2) -0.016(2) Si21 0.070(3) 0.065(3) 0.078(3) 0.004(2) 0.006(2) -0.016(2) N11 0.112(12) 0.050(7) 0.008(4) -0.007(5) -0.035(6) 0.047(8) C71 0.029(10) 0.064(12) 0.024(8) 0.009(8) -0.014(7) 0.034(9) C81 0.100(18) 0.075(15) 0.000(8) -0.009(9) -0.020(10) 0.051(14) C91 0.059(2) 0.074(2) 0.032(2) 0.0034(15) -0.0102(14) -0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N 1.756(15) 4_556 ? Cu N 1.756(15) . ? Cu N11 1.958(10) . ? Cu N11 1.958(10) 4_556 ? Si1 N11 1.570(12) . ? Si1 C15 1.809(10) . ? Si1 C14 1.851(10) . ? Si1 C13 1.882(8) . ? Si1 N 1.88(2) . ? Li O3 2.061(15) . ? Li O3 2.061(15) 4_656 ? Li O1 2.117(12) 4_656 ? Li O1 2.117(12) . ? Li O2 2.140(6) 4_656 ? Li O2 2.140(6) . ? O1 C2 1.402(9) . ? O1 C1 1.415(9) . ? O2 C3 1.414(9) . ? O2 C4 1.420(9) . ? O3 C6 1.351(15) . ? O3 C5 1.396(13) . ? C2 C3 1.476(12) . ? C5 C5 1.47(2) 4_656 ? C10 Si21 1.736(9) . ? C10 C9 1.736(9) . ? C11 Si21 1.583(12) . ? C11 C9 1.583(12) . ? C12 Si21 1.589(12) . ? C12 C9 1.589(12) . ? C16 C91 1.758(8) . ? C16 Si2 1.758(8) . ? C17 C91 1.762(8) . ? C17 Si2 1.762(8) . ? C18 C91 1.665(14) . ? C18 Si2 1.665(14) . ? Si2 C8 1.88(2) . ? N C7 1.44(2) . ? C7 C8 1.28(2) . ? C7 C9 1.577(13) . ? Si21 C81 1.93(3) . ? N11 C71 1.43(2) . ? C71 C81 1.25(3) . ? C71 C91 1.74(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 N Cu N 179.0(11) 4_556 . ? N11 Cu N11 175.3(8) . 4_556 ? N11 Si1 C15 106.1(6) . . ? N11 Si1 C14 120.1(6) . . ? C15 Si1 C14 103.7(5) . . ? N11 Si1 C13 110.4(5) . . ? C15 Si1 C13 107.6(5) . . ? C14 Si1 C13 108.1(5) . . ? C15 Si1 N 118.6(6) . . ? C14 Si1 N 103.2(6) . . ? C13 Si1 N 114.5(6) . . ? O3 Li O3 78.6(7) . 4_656 ? O3 Li O1 92.4(3) . 4_656 ? O3 Li O1 162.3(5) 4_656 4_656 ? O3 Li O1 162.3(5) . . ? O3 Li O1 92.4(3) 4_656 . ? O1 Li O1 100.0(8) 4_656 . ? O3 Li O2 102.2(4) . 4_656 ? O3 Li O2 90.3(4) 4_656 4_656 ? O1 Li O2 76.6(4) 4_656 4_656 ? O1 Li O2 92.9(4) . 4_656 ? O3 Li O2 90.3(4) . . ? O3 Li O2 102.2(4) 4_656 . ? O1 Li O2 92.9(4) 4_656 . ? O1 Li O2 76.6(4) . . ? O2 Li O2 163.9(10) 4_656 . ? C2 O1 C1 112.8(6) . . ? C2 O1 Li 112.6(5) . . ? C1 O1 Li 125.9(5) . . ? C3 O2 C4 111.3(6) . . ? C3 O2 Li 112.5(5) . . ? C4 O2 Li 127.4(6) . . ? C6 O3 C5 111.7(8) . . ? C6 O3 Li 127.1(7) . . ? C5 O3 Li 110.6(7) . . ? O1 C2 C3 108.7(7) . . ? O2 C3 C2 108.9(7) . . ? O3 C5 C5 106.9(7) . 4_656 ? C18 Si2 C16 110.4(5) . . ? C18 Si2 C17 108.7(5) . . ? C16 Si2 C17 103.8(4) . . ? C18 Si2 C8 101.7(7) . . ? C16 Si2 C8 116.0(5) . . ? C17 Si2 C8 116.2(5) . . ? C7 N Cu 125.2(10) . . ? C7 N Si1 121.2(9) . . ? Cu N Si1 113.0(9) . . ? C8 C7 N 119.3(14) . . ? C8 C7 C9 117.9(13) . . ? N C7 C9 122.9(11) . . ? C7 C8 Si2 130.5(14) . . ? C7 C9 C11 113.6(6) . . ? C7 C9 C12 120.8(7) . . ? C11 C9 C12 113.3(7) . . ? C7 C9 C10 96.7(6) . . ? C11 C9 C10 105.1(6) . . ? C12 C9 C10 103.9(5) . . ? C11 Si21 C12 113.3(7) . . ? C11 Si21 C10 105.1(6) . . ? C12 Si21 C10 103.9(5) . . ? C11 Si21 C81 110.9(7) . . ? C12 Si21 C81 99.2(8) . . ? C10 Si21 C81 124.3(7) . . ? C71 N11 Si1 132.2(9) . . ? C71 N11 Cu 109.3(9) . . ? Si1 N11 Cu 118.3(7) . . ? C81 C71 N11 121.2(19) . . ? C81 C71 C91 105.7(16) . . ? N11 C71 C91 133.1(13) . . ? C71 C81 Si21 122.0(17) . . ? C18 C91 C71 135.3(7) . . ? C18 C91 C16 110.4(5) . . ? C71 C91 C16 98.6(6) . . ? C18 C91 C17 108.7(5) . . ? C71 C91 C17 95.9(6) . . ? C16 C91 C17 103.8(4) . . ? _refine_diff_density_max 0.505 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.085 #=END #P.B. Hitchcock, M.F. Lappert and M. Layh, J. Chem. Soc. Dalton Trans., #Compound 3 data_jul1395 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Me3SiCHC(tBu)N(SiMe3)CuPPh3]' _chemical_formula_analytical ? _chemical_formula_sum 'C30 H43 Cu N P Si2' _chemical_formula_weight 568.34 _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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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' 'Cu' 'Cu' 0.3201 1.2651 '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 12.135(4) _cell_length_b 14.805(5) _cell_length_c 17.896(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.40(3) _cell_angle_gamma 90.00 _cell_volume 3099.7(17) _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 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.218 _exptl_crystal_density_method ? _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.852 _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 5708 _diffrn_reflns_av_R_equivalents 0.1491 _diffrn_reflns_av_sigmaI/netI 0.2021 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5446 _reflns_number_observed 2509 _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^)+(0.1220P)^2^+1.7804P] 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 5446 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2135 _refine_ls_R_factor_obs 0.1007 _refine_ls_wR_factor_all 0.2862 _refine_ls_wR_factor_obs 0.2171 _refine_ls_goodness_of_fit_all 1.032 _refine_ls_goodness_of_fit_obs 1.169 _refine_ls_restrained_S_all 1.032 _refine_ls_restrained_S_obs 1.169 _refine_ls_shift/esd_max -0.006 _refine_ls_shift/esd_mean 0.001 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 Cu Cu 0.09537(11) 0.19998(9) 0.32950(8) 0.0360(4) Uani 1 d . . P P 0.2416(2) 0.1869(2) 0.2844(2) 0.0292(7) Uani 1 d . . Si1 Si -0.1191(3) 0.1422(2) 0.3837(2) 0.0366(8) Uani 1 d . . Si2 Si 0.1617(3) 0.2757(2) 0.5421(2) 0.0400(8) Uani 1 d . . N N -0.0207(7) 0.2227(5) 0.3754(5) 0.031(2) Uani 1 d . . C1 C -0.0086(8) 0.3119(7) 0.3982(6) 0.029(2) Uani 1 d . . C2 C 0.0668(9) 0.3395(7) 0.4639(6) 0.038(3) Uani 1 d . . H2 H 0.0712(9) 0.4032(7) 0.4707(6) 0.045 Uiso 1 calc R . C3 C -0.0800(8) 0.3832(6) 0.3400(6) 0.025(2) Uani 1 d . . C4 C -0.0886(13) 0.3571(9) 0.2580(7) 0.072(4) Uani 1 d . . H4A H -0.0119(13) 0.3542(9) 0.2501(7) 0.109 Uiso 1 calc R . H4B H -0.1342(13) 0.4022(9) 0.2230(7) 0.109 Uiso 1 calc R . H4C H -0.1255(13) 0.2979(9) 0.2473(7) 0.109 Uiso 1 calc R . C5 C -0.0283(12) 0.4763(8) 0.3516(9) 0.086(6) Uani 1 d . . H5A H -0.0212(12) 0.4961(8) 0.4050(9) 0.129 Uiso 1 calc R . H5B H -0.0776(12) 0.5185(8) 0.3155(9) 0.129 Uiso 1 calc R . H5C H 0.0474(12) 0.4750(8) 0.3420(9) 0.129 Uiso 1 calc R . C6 C -0.1984(10) 0.3871(10) 0.3504(9) 0.070(4) Uani 1 d . . H6A H -0.1946(10) 0.4042(10) 0.4039(9) 0.104 Uiso 1 calc R . H6B H -0.2346(10) 0.3276(10) 0.3393(9) 0.104 Uiso 1 calc R . H6C H -0.2434(10) 0.4319(10) 0.3148(9) 0.104 Uiso 1 calc R . C7 C -0.1672(12) 0.1512(9) 0.4720(8) 0.070(4) Uani 1 d . . H7A H -0.2024(12) 0.2104(9) 0.4737(8) 0.105 Uiso 1 calc R . H7B H -0.1016(12) 0.1442(9) 0.5174(8) 0.105 Uiso 1 calc R . H7C H -0.2233(12) 0.1036(9) 0.4722(8) 0.105 Uiso 1 calc R . C8 C -0.0522(15) 0.0340(9) 0.3757(13) 0.121(8) Uani 1 d . . H8A H -0.0281(15) 0.0324(9) 0.3276(13) 0.182 Uiso 1 calc R . H8B H -0.1071(15) -0.0147(9) 0.3751(13) 0.182 Uiso 1 calc R . H8C H 0.0146(15) 0.0260(9) 0.4201(13) 0.182 Uiso 1 calc R . C9 C -0.2554(13) 0.1384(12) 0.3046(9) 0.107(7) Uani 1 d . . H9A H -0.2977(13) 0.1949(12) 0.3045(9) 0.161 Uiso 1 calc R . H9B H -0.3019(13) 0.0874(12) 0.3134(9) 0.161 Uiso 1 calc R . H9C H -0.2380(13) 0.1311(12) 0.2545(9) 0.161 Uiso 1 calc R . C10 C 0.0896(10) 0.2472(8) 0.6177(7) 0.053(3) Uani 1 d . . H10A H 0.1420(10) 0.2130(8) 0.6591(7) 0.079 Uiso 1 calc R . H10B H 0.0216(10) 0.2106(8) 0.5950(7) 0.079 Uiso 1 calc R . H10C H 0.0668(10) 0.3029(8) 0.6391(7) 0.079 Uiso 1 calc R . C11 C 0.2817(9) 0.3565(9) 0.5856(8) 0.059(4) Uani 1 d . . H11A H 0.3370(9) 0.3268(9) 0.6286(8) 0.088 Uiso 1 calc R . H11B H 0.2507(9) 0.4101(9) 0.6049(8) 0.088 Uiso 1 calc R . H11C H 0.3197(9) 0.3744(9) 0.5459(8) 0.088 Uiso 1 calc R . C12 C 0.2300(13) 0.1711(9) 0.5167(7) 0.077(5) Uani 1 d . . H12A H 0.2784(13) 0.1439(9) 0.5640(7) 0.116 Uiso 1 calc R . H12B H 0.2768(13) 0.1865(9) 0.4816(7) 0.116 Uiso 1 calc R . H12C H 0.1705(13) 0.1281(9) 0.4912(7) 0.116 Uiso 1 calc R . C13 C 0.2113(7) 0.1689(6) 0.1813(6) 0.025(2) Uani 1 d . . C14 C 0.2906(9) 0.1299(7) 0.1468(6) 0.032(3) Uani 1 d . . H14 H 0.3627(9) 0.1108(7) 0.1783(6) 0.039 Uiso 1 calc R . C15 C 0.2658(10) 0.1189(8) 0.0682(7) 0.043(3) Uani 1 d . . H15 H 0.3198(10) 0.0910(8) 0.0457(7) 0.052 Uiso 1 calc R . C16 C 0.1631(9) 0.1480(7) 0.0219(7) 0.040(3) Uani 1 d . . H16 H 0.1475(9) 0.1426(7) -0.0328(7) 0.048 Uiso 1 calc R . C17 C 0.0821(9) 0.1852(8) 0.0543(7) 0.044(3) Uani 1 d . . H17 H 0.0098(9) 0.2035(8) 0.0224(7) 0.053 Uiso 1 calc R . C18 C 0.1077(8) 0.1954(7) 0.1338(6) 0.038(3) Uani 1 d . . H18 H 0.0523(8) 0.2213(7) 0.1563(6) 0.045 Uiso 1 calc R . C19 C 0.3315(8) 0.0926(7) 0.3279(6) 0.029(2) Uani 1 d . . C20 C 0.4502(9) 0.1009(7) 0.3615(7) 0.043(3) Uani 1 d . . H20 H 0.4879(9) 0.1569(7) 0.3605(7) 0.051 Uiso 1 calc R . C21 C 0.5116(10) 0.0246(9) 0.3966(7) 0.053(3) Uani 1 d . . H21 H 0.5920(10) 0.0281(9) 0.4179(7) 0.063 Uiso 1 calc R . C22 C 0.4551(10) -0.0555(8) 0.4002(7) 0.045(3) Uani 1 d . . H22 H 0.4968(10) -0.1064(8) 0.4251(7) 0.054 Uiso 1 calc R . C23 C 0.3414(10) -0.0626(8) 0.3688(7) 0.054(4) Uani 1 d . . H23 H 0.3042(10) -0.1187(8) 0.3705(7) 0.065 Uiso 1 calc R . C24 C 0.2774(10) 0.0131(7) 0.3333(7) 0.042(3) Uani 1 d . . H24 H 0.1968(10) 0.0085(7) 0.3134(7) 0.051 Uiso 1 calc R . C25 C 0.3330(8) 0.2858(7) 0.3023(6) 0.029(2) Uani 1 d . . C26 C 0.4139(9) 0.3037(8) 0.2624(7) 0.040(3) Uani 1 d . . H26 H 0.4213(9) 0.2639(8) 0.2224(7) 0.048 Uiso 1 calc R . C27 C 0.4839(10) 0.3782(8) 0.2800(8) 0.051(3) Uani 1 d . . H27 H 0.5419(10) 0.3886(8) 0.2543(8) 0.061 Uiso 1 calc R . C28 C 0.4679(10) 0.4381(7) 0.3361(8) 0.054(4) Uani 1 d . . H28 H 0.5144(10) 0.4906(7) 0.3476(8) 0.064 Uiso 1 calc R . C29 C 0.3887(10) 0.4236(8) 0.3741(7) 0.047(3) Uani 1 d . . H29 H 0.3807(10) 0.4653(8) 0.4127(7) 0.056 Uiso 1 calc R . C30 C 0.3175(9) 0.3482(7) 0.3580(6) 0.037(3) Uani 1 d . . H30 H 0.2597(9) 0.3391(7) 0.3842(6) 0.045 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 Cu 0.0310(7) 0.0330(8) 0.0465(9) -0.0017(7) 0.0148(6) 0.0062(6) P 0.0226(13) 0.032(2) 0.032(2) -0.0044(13) 0.0060(11) 0.0068(12) Si1 0.040(2) 0.023(2) 0.046(2) -0.0043(14) 0.010(2) -0.0070(14) Si2 0.038(2) 0.031(2) 0.044(2) 0.0008(15) 0.001(2) 0.0125(14) N 0.034(5) 0.019(5) 0.039(5) 0.000(4) 0.008(4) 0.004(4) C1 0.031(5) 0.024(6) 0.034(6) 0.001(5) 0.012(5) -0.003(5) C2 0.039(6) 0.026(6) 0.037(7) -0.004(5) -0.010(5) 0.001(5) C3 0.022(5) 0.020(5) 0.033(6) 0.009(4) 0.005(5) 0.003(4) C4 0.101(12) 0.067(10) 0.048(9) 0.023(8) 0.017(8) 0.038(9) C5 0.073(10) 0.029(7) 0.120(13) 0.034(8) -0.036(9) -0.014(7) C6 0.035(7) 0.067(10) 0.101(12) 0.026(9) 0.007(7) 0.017(7) C7 0.072(9) 0.064(9) 0.065(10) -0.014(8) 0.004(8) -0.041(8) C8 0.110(14) 0.026(8) 0.259(26) -0.002(12) 0.103(16) -0.006(9) C9 0.102(13) 0.120(15) 0.069(11) 0.005(10) -0.033(9) -0.079(12) C10 0.046(7) 0.042(7) 0.062(9) 0.004(7) 0.000(7) -0.002(6) C11 0.032(7) 0.069(9) 0.067(9) 0.004(8) -0.002(6) 0.008(7) C12 0.103(11) 0.072(10) 0.040(8) 0.003(7) -0.009(8) 0.056(9) C13 0.013(5) 0.026(5) 0.034(6) 0.002(5) 0.003(4) 0.002(4) C14 0.030(6) 0.027(6) 0.040(7) -0.002(5) 0.007(5) -0.005(5) C15 0.044(7) 0.046(7) 0.044(8) 0.002(6) 0.019(6) 0.006(6) C16 0.037(6) 0.039(7) 0.038(7) 0.000(6) -0.002(6) -0.009(6) C17 0.033(6) 0.045(7) 0.044(7) 0.007(6) -0.008(5) 0.004(6) C18 0.027(5) 0.039(6) 0.047(7) -0.001(6) 0.011(5) -0.010(5) C19 0.028(5) 0.023(5) 0.030(6) -0.003(5) -0.002(5) 0.015(5) C20 0.035(6) 0.030(6) 0.055(8) 0.007(6) -0.001(6) 0.001(5) C21 0.032(6) 0.055(8) 0.061(9) 0.005(7) -0.005(6) 0.009(6) C22 0.052(8) 0.035(7) 0.046(8) 0.007(6) 0.011(6) 0.010(6) C23 0.044(7) 0.038(7) 0.071(10) 0.000(7) -0.003(7) -0.006(6) C24 0.039(7) 0.033(7) 0.053(8) -0.002(6) 0.009(6) -0.001(6) C25 0.022(5) 0.028(6) 0.034(6) 0.003(5) 0.002(4) 0.011(5) C26 0.039(6) 0.034(6) 0.047(7) -0.003(6) 0.012(5) 0.007(6) C27 0.031(6) 0.046(8) 0.068(9) 0.007(7) -0.002(6) -0.009(6) C28 0.041(7) 0.014(6) 0.083(10) 0.001(6) -0.023(7) -0.002(5) C29 0.048(7) 0.033(7) 0.056(8) -0.016(6) 0.005(7) 0.003(6) C30 0.037(6) 0.027(6) 0.038(7) -0.003(5) -0.006(5) 0.015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N 1.840(8) . ? Cu P 2.145(3) . ? P C13 1.802(10) . ? P C19 1.815(9) . ? P C25 1.813(10) . ? Si1 N 1.721(8) . ? Si1 C8 1.818(14) . ? Si1 C7 1.829(14) . ? Si1 C9 1.870(13) . ? Si2 C2 1.823(10) . ? Si2 C10 1.844(12) . ? Si2 C12 1.868(12) . ? Si2 C11 1.885(12) . ? N C1 1.379(12) . ? C1 C2 1.348(13) . ? C1 C3 1.571(13) . ? C3 C4 1.49(2) . ? C3 C6 1.497(14) . ? C3 C5 1.507(14) . ? C13 C18 1.374(13) . ? C13 C14 1.399(13) . ? C14 C15 1.366(15) . ? C15 C16 1.370(15) . ? C16 C17 1.382(15) . ? C17 C18 1.382(15) . ? C19 C24 1.364(14) . ? C19 C20 1.412(14) . ? C20 C21 1.406(15) . ? C21 C22 1.38(2) . ? C22 C23 1.348(15) . ? C23 C24 1.41(2) . ? C25 C26 1.385(14) . ? C25 C30 1.408(14) . ? C26 C27 1.377(15) . ? C27 C28 1.39(2) . ? C28 C29 1.33(2) . ? C29 C30 1.394(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Cu P 173.0(3) . . ? C13 P C19 105.1(4) . . ? C13 P C25 104.5(5) . . ? C19 P C25 106.0(4) . . ? C13 P Cu 115.7(3) . . ? C19 P Cu 111.8(4) . . ? C25 P Cu 112.9(3) . . ? N Si1 C8 105.6(6) . . ? N Si1 C7 114.3(5) . . ? C8 Si1 C7 112.5(8) . . ? N Si1 C9 116.8(6) . . ? C8 Si1 C9 103.8(9) . . ? C7 Si1 C9 103.6(7) . . ? C2 Si2 C10 110.8(5) . . ? C2 Si2 C12 118.2(5) . . ? C10 Si2 C12 108.4(6) . . ? C2 Si2 C11 104.4(5) . . ? C10 Si2 C11 107.9(6) . . ? C12 Si2 C11 106.4(6) . . ? C1 N Si1 131.3(7) . . ? C1 N Cu 105.8(6) . . ? Si1 N Cu 122.9(5) . . ? C2 C1 N 122.8(9) . . ? C2 C1 C3 120.2(9) . . ? N C1 C3 116.8(8) . . ? C1 C2 Si2 131.1(8) . . ? C4 C3 C6 108.2(10) . . ? C4 C3 C5 106.8(10) . . ? C6 C3 C5 109.0(10) . . ? C4 C3 C1 111.1(9) . . ? C6 C3 C1 108.8(8) . . ? C5 C3 C1 112.8(8) . . ? C18 C13 C14 117.9(10) . . ? C18 C13 P 119.6(8) . . ? C14 C13 P 122.4(7) . . ? C15 C14 C13 120.9(10) . . ? C14 C15 C16 120.1(11) . . ? C15 C16 C17 120.4(11) . . ? C16 C17 C18 119.0(10) . . ? C13 C18 C17 121.6(10) . . ? C24 C19 C20 120.1(10) . . ? C24 C19 P 116.7(8) . . ? C20 C19 P 123.0(8) . . ? C21 C20 C19 118.7(10) . . ? C22 C21 C20 120.0(11) . . ? C23 C22 C21 120.9(11) . . ? C22 C23 C24 120.4(11) . . ? C19 C24 C23 119.9(10) . . ? C26 C25 C30 119.2(10) . . ? C26 C25 P 123.1(8) . . ? C30 C25 P 117.7(8) . . ? C27 C26 C25 120.9(11) . . ? C26 C27 C28 118.7(12) . . ? C29 C28 C27 121.5(11) . . ? C28 C29 C30 121.0(11) . . ? C29 C30 C25 118.6(11) . . ? _refine_diff_density_max 1.222 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.125