# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'John Arnold' _publ_contact_author_email ARNOLD@BERKELEY.EDU _publ_section_title ; Aluminium, Zinc, Gallium, and Cadmium Complexes Supported by a Monoanionic [N2P2] Ligand ; loop_ _publ_author_name 'John Arnold' 'Stefan Minasian' #===end data_sgm332 _database_code_depnum_ccdc_archive 'CCDC 701676' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H51 Al Cl2 N2 P2 Si' _chemical_formula_sum 'C22 H51 Al Cl2 N2 P2 Si' _chemical_formula_weight 531.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 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' Al Al 0.0567 0.0519 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0718 0.0712 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1240 0.1597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0879 0.0952 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N -0.0030 0.0033 '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 7.8709(9) _cell_length_b 13.2010(15) _cell_length_c 15.9297(18) _cell_angle_alpha 109.071(2) _cell_angle_beta 91.737(2) _cell_angle_gamma 96.951(2) _cell_volume 1548.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 7758 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 33.37 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.140 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.387 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.615954 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type ? _diffrn_radiation_source syncrotron _diffrn_radiation_monochromator mirrors _diffrn_measurement_device_type 'Beamline 11.3.1 ALS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 27403 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.0703 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 33.75 _reflns_number_total 9502 _reflns_number_gt 7500 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'Bruker SAINT v7.23a' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+0.4556P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9502 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1597 _refine_ls_wR_factor_gt 0.1495 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.55361(6) 0.05011(4) 0.31044(3) 0.03606(12) Uani 1 1 d . . . Cl2 Cl 0.63051(7) 0.31392(4) 0.42421(4) 0.04582(14) Uani 1 1 d . . . P2 P 0.23286(6) 0.21472(4) 0.45233(3) 0.03037(11) Uani 1 1 d . . . P1 P -0.07448(8) -0.22679(4) 0.20281(4) 0.03941(13) Uani 1 1 d . . . Si1 Si 0.24537(7) 0.13121(4) 0.16771(3) 0.03231(12) Uani 1 1 d . . . Al1 Al 0.42759(7) 0.19385(4) 0.33246(4) 0.02834(12) Uani 1 1 d . . . N1 N 0.16757(18) 0.08752(12) 0.25570(10) 0.0278(3) Uani 1 1 d . . . N2 N 0.3890(2) 0.23565(13) 0.23469(11) 0.0318(3) Uani 1 1 d . . . C9 C 0.0271(2) 0.14594(15) 0.29884(12) 0.0294(3) Uani 1 1 d . . . H9A H -0.0839 0.1078 0.2665 0.035 Uiso 1 1 calc R . . H9B H 0.0428 0.2197 0.2947 0.035 Uiso 1 1 calc R . . C10 C 0.0216(2) 0.15425(16) 0.39691(13) 0.0319(4) Uani 1 1 d . . . H10A H -0.0086 0.0814 0.4017 0.038 Uiso 1 1 calc R . . H10B H -0.0660 0.1997 0.4251 0.038 Uiso 1 1 calc R . . C7 C 0.1403(2) -0.02866(14) 0.24568(13) 0.0321(4) Uani 1 1 d . . . H7A H 0.1338 -0.0353 0.3057 0.038 Uiso 1 1 calc R . . H7B H 0.2418 -0.0612 0.2197 0.038 Uiso 1 1 calc R . . C4 C 0.4948(3) 0.31840(19) 0.20620(16) 0.0430(5) Uani 1 1 d . . . C8 C -0.0195(3) -0.09414(15) 0.18818(14) 0.0365(4) Uani 1 1 d . . . H8A H -0.0005 -0.1054 0.1248 0.044 Uiso 1 1 calc R . . H8B H -0.1173 -0.0526 0.2036 0.044 Uiso 1 1 calc R . . C22 C 0.1624(3) 0.41111(17) 0.44642(17) 0.0457(5) Uani 1 1 d . . . H22A H 0.1549 0.4875 0.4782 0.069 Uiso 1 1 calc R . . H22B H 0.0498 0.3746 0.4170 0.069 Uiso 1 1 calc R . . H22C H 0.2465 0.4056 0.4016 0.069 Uiso 1 1 calc R . . C20 C 0.2183(3) 0.35757(18) 0.51256(14) 0.0418(5) Uani 1 1 d . . . H20A H 0.3364 0.3935 0.5383 0.050 Uiso 1 1 calc R . . C19 C 0.2659(3) 0.0291(2) 0.49509(17) 0.0491(5) Uani 1 1 d . . . H19A H 0.2875 -0.0019 0.5419 0.074 Uiso 1 1 calc R . . H19B H 0.3542 0.0136 0.4524 0.074 Uiso 1 1 calc R . . H19C H 0.1527 -0.0029 0.4643 0.074 Uiso 1 1 calc R . . C17 C 0.2709(3) 0.1506(2) 0.53652(14) 0.0433(5) Uani 1 1 d . . . H17A H 0.1774 0.1642 0.5782 0.052 Uiso 1 1 calc R . . C11 C -0.2559(3) -0.28420(17) 0.11642(15) 0.0421(5) Uani 1 1 d . . . H11A H -0.2138 -0.2837 0.0579 0.051 Uiso 1 1 calc R . . C6 C 0.3386(3) 0.0199(2) 0.08565(15) 0.0483(5) Uani 1 1 d . . . H6A H 0.2730 -0.0014 0.0279 0.072 Uiso 1 1 calc R . . H6B H 0.3335 -0.0423 0.1066 0.072 Uiso 1 1 calc R . . H6C H 0.4584 0.0450 0.0794 0.072 Uiso 1 1 calc R . . C5 C 0.0641(3) 0.1616(2) 0.10625(16) 0.0512(6) Uani 1 1 d . . . H5A H 0.0513 0.1120 0.0446 0.077 Uiso 1 1 calc R . . H5B H 0.0877 0.2363 0.1066 0.077 Uiso 1 1 calc R . . H5C H -0.0420 0.1525 0.1352 0.077 Uiso 1 1 calc R . . C16 C 0.1218(4) -0.3200(3) 0.0538(2) 0.0687(8) Uani 1 1 d . . . H16A H 0.2226 -0.3562 0.0349 0.103 Uiso 1 1 calc R . . H16B H 0.1329 -0.2517 0.0412 0.103 Uiso 1 1 calc R . . H16C H 0.0182 -0.3669 0.0211 0.103 Uiso 1 1 calc R . . C21 C 0.1023(4) 0.3756(2) 0.58934(16) 0.0582(7) Uani 1 1 d . . . H21A H 0.1013 0.4534 0.6184 0.087 Uiso 1 1 calc R . . H21B H 0.1454 0.3446 0.6326 0.087 Uiso 1 1 calc R . . H21C H -0.0146 0.3404 0.5665 0.087 Uiso 1 1 calc R . . C14 C 0.1093(4) -0.2975(2) 0.1515(2) 0.0566(6) Uani 1 1 d . . . H14A H 0.2142 -0.2452 0.1800 0.068 Uiso 1 1 calc R . . C3 C 0.4873(4) 0.4315(2) 0.2721(2) 0.0567(6) Uani 1 1 d . . . H3A H 0.5326 0.4357 0.3314 0.085 Uiso 1 1 calc R . . H3B H 0.3680 0.4460 0.2748 0.085 Uiso 1 1 calc R . . H3C H 0.5564 0.4854 0.2526 0.085 Uiso 1 1 calc R . . C1 C 0.4242(4) 0.3175(3) 0.11526(19) 0.0641(8) Uani 1 1 d . . . H1A H 0.4269 0.2460 0.0709 0.096 Uiso 1 1 calc R . . H1B H 0.4949 0.3725 0.0976 0.096 Uiso 1 1 calc R . . H1C H 0.3057 0.3333 0.1191 0.096 Uiso 1 1 calc R . . C18 C 0.4430(4) 0.2028(3) 0.59091(19) 0.0623(7) Uani 1 1 d . . . H18A H 0.4621 0.1681 0.6355 0.093 Uiso 1 1 calc R . . H18B H 0.4399 0.2802 0.6208 0.093 Uiso 1 1 calc R . . H18C H 0.5364 0.1933 0.5510 0.093 Uiso 1 1 calc R . . C2 C 0.6795(3) 0.2942(3) 0.1983(2) 0.0647(8) Uani 1 1 d . . . H2A H 0.7271 0.2946 0.2560 0.097 Uiso 1 1 calc R . . H2B H 0.7484 0.3495 0.1803 0.097 Uiso 1 1 calc R . . H2C H 0.6815 0.2229 0.1535 0.097 Uiso 1 1 calc R . . C12 C -0.4003(3) -0.2153(3) 0.1374(2) 0.0698(9) Uani 1 1 d . . . H12A H -0.4950 -0.2467 0.0913 0.105 Uiso 1 1 calc R . . H12B H -0.3581 -0.1417 0.1390 0.105 Uiso 1 1 calc R . . H12C H -0.4408 -0.2130 0.1955 0.105 Uiso 1 1 calc R . . C15 C 0.1282(6) -0.3959(3) 0.1775(3) 0.0996(14) Uani 1 1 d . . . H15A H 0.2262 -0.4291 0.1496 0.149 Uiso 1 1 calc R . . H15B H 0.0235 -0.4482 0.1574 0.149 Uiso 1 1 calc R . . H15C H 0.1472 -0.3743 0.2424 0.149 Uiso 1 1 calc R . . C13 C -0.3209(5) -0.4004(2) 0.1083(3) 0.0832(11) Uani 1 1 d . . . H13A H -0.4165 -0.4288 0.0624 0.125 Uiso 1 1 calc R . . H13B H -0.3602 -0.4027 0.1655 0.125 Uiso 1 1 calc R . . H13C H -0.2279 -0.4446 0.0917 0.125 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0289(2) 0.0370(2) 0.0453(3) 0.01534(19) 0.00339(17) 0.01114(16) Cl2 0.0338(2) 0.0437(3) 0.0529(3) 0.0105(2) -0.0081(2) -0.00326(19) P2 0.0282(2) 0.0355(2) 0.0285(2) 0.01021(18) 0.00316(16) 0.00935(17) P1 0.0470(3) 0.0324(2) 0.0370(3) 0.0121(2) -0.0009(2) -0.0025(2) Si1 0.0287(2) 0.0395(3) 0.0289(2) 0.0117(2) 0.00205(18) 0.00492(19) Al1 0.0243(2) 0.0305(3) 0.0318(3) 0.0118(2) 0.00286(19) 0.00575(19) N1 0.0250(6) 0.0265(7) 0.0312(7) 0.0082(6) 0.0037(5) 0.0046(5) N2 0.0291(7) 0.0337(7) 0.0356(8) 0.0161(6) 0.0034(6) 0.0023(6) C9 0.0236(7) 0.0317(8) 0.0325(8) 0.0099(7) 0.0014(6) 0.0049(6) C10 0.0260(8) 0.0359(9) 0.0357(9) 0.0133(7) 0.0060(7) 0.0063(6) C7 0.0304(8) 0.0260(8) 0.0370(9) 0.0071(7) -0.0005(7) 0.0033(6) C4 0.0400(10) 0.0456(11) 0.0502(12) 0.0270(10) 0.0079(9) -0.0006(8) C8 0.0356(9) 0.0299(9) 0.0407(10) 0.0099(8) -0.0040(8) -0.0008(7) C22 0.0492(12) 0.0322(10) 0.0539(13) 0.0092(9) 0.0059(10) 0.0131(9) C20 0.0394(10) 0.0396(10) 0.0384(10) -0.0002(8) -0.0004(8) 0.0127(8) C19 0.0482(12) 0.0607(14) 0.0541(13) 0.0366(12) 0.0089(10) 0.0168(10) C17 0.0435(11) 0.0603(13) 0.0346(10) 0.0230(9) 0.0058(8) 0.0181(10) C11 0.0413(11) 0.0363(10) 0.0413(10) 0.0072(8) 0.0010(8) -0.0067(8) C6 0.0504(12) 0.0526(13) 0.0375(11) 0.0069(9) 0.0133(9) 0.0108(10) C5 0.0440(12) 0.0751(17) 0.0411(11) 0.0277(11) -0.0027(9) 0.0111(11) C16 0.0545(15) 0.0660(18) 0.076(2) 0.0074(15) 0.0145(14) 0.0157(13) C21 0.0678(16) 0.0654(16) 0.0382(11) 0.0044(11) 0.0127(11) 0.0309(13) C14 0.0591(15) 0.0420(12) 0.0667(16) 0.0133(11) -0.0024(13) 0.0145(11) C3 0.0695(17) 0.0383(11) 0.0671(16) 0.0269(11) 0.0070(13) -0.0016(11) C1 0.081(2) 0.0683(17) 0.0555(15) 0.0404(14) 0.0061(14) 0.0001(15) C18 0.0661(17) 0.0741(18) 0.0476(13) 0.0228(13) -0.0171(12) 0.0110(14) C2 0.0427(13) 0.0779(19) 0.084(2) 0.0425(16) 0.0241(13) 0.0014(12) C12 0.0404(13) 0.0697(18) 0.0741(19) -0.0076(15) -0.0046(12) 0.0037(12) C15 0.105(3) 0.068(2) 0.144(4) 0.054(2) 0.007(3) 0.031(2) C13 0.087(2) 0.0480(15) 0.101(3) 0.0240(16) -0.021(2) -0.0293(16) _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 Cl1 Al1 2.1792(7) . ? Cl2 Al1 2.2206(7) . ? P2 C10 1.8193(19) . ? P2 C20 1.835(2) . ? P2 C17 1.839(2) . ? P2 Al1 2.4509(7) . ? P1 C8 1.843(2) . ? P1 C11 1.856(2) . ? P1 C14 1.880(3) . ? Si1 N2 1.7048(17) . ? Si1 N1 1.7796(16) . ? Si1 C5 1.861(2) . ? Si1 C6 1.862(2) . ? Si1 Al1 2.7741(8) . ? Al1 N2 1.8429(17) . ? Al1 N1 2.3844(16) . ? N1 C7 1.477(2) . ? N1 C9 1.481(2) . ? N2 C4 1.490(2) . ? C9 C10 1.532(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C7 C8 1.522(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C4 C2 1.526(3) . ? C4 C3 1.529(4) . ? C4 C1 1.531(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C22 C20 1.529(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C20 C21 1.522(3) . ? C20 H20A 1.0000 . ? C19 C17 1.517(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C17 C18 1.540(4) . ? C17 H17A 1.0000 . ? C11 C12 1.519(4) . ? C11 C13 1.519(3) . ? C11 H11A 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C16 C14 1.495(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C14 C15 1.508(4) . ? C14 H14A 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? 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 C10 P2 C20 106.60(9) . . ? C10 P2 C17 106.80(10) . . ? C20 P2 C17 107.04(11) . . ? C10 P2 Al1 105.38(6) . . ? C20 P2 Al1 111.79(8) . . ? C17 P2 Al1 118.53(7) . . ? C8 P1 C11 99.15(10) . . ? C8 P1 C14 100.96(11) . . ? C11 P1 C14 104.24(12) . . ? N2 Si1 N1 95.10(7) . . ? N2 Si1 C5 119.04(11) . . ? N1 Si1 C5 109.86(9) . . ? N2 Si1 C6 115.95(10) . . ? N1 Si1 C6 109.77(10) . . ? C5 Si1 C6 106.40(12) . . ? N2 Si1 Al1 40.38(5) . . ? N1 Si1 Al1 58.38(5) . . ? C5 Si1 Al1 143.19(9) . . ? C6 Si1 Al1 110.39(9) . . ? N2 Al1 Cl1 116.57(6) . . ? N2 Al1 Cl2 108.56(6) . . ? Cl1 Al1 Cl2 98.30(3) . . ? N2 Al1 N1 73.68(6) . . ? Cl1 Al1 N1 91.58(4) . . ? Cl2 Al1 N1 167.20(5) . . ? N2 Al1 P2 123.66(6) . . ? Cl1 Al1 P2 111.48(3) . . ? Cl2 Al1 P2 91.32(3) . . ? N1 Al1 P2 77.44(4) . . ? N2 Al1 Si1 36.82(5) . . ? Cl1 Al1 Si1 97.81(3) . . ? Cl2 Al1 Si1 145.18(3) . . ? N1 Al1 Si1 39.46(4) . . ? P2 Al1 Si1 110.97(3) . . ? C7 N1 C9 113.05(14) . . ? C7 N1 Si1 120.70(12) . . ? C9 N1 Si1 112.56(11) . . ? C7 N1 Al1 118.25(11) . . ? C9 N1 Al1 105.90(10) . . ? Si1 N1 Al1 82.16(6) . . ? C4 N2 Si1 125.85(14) . . ? C4 N2 Al1 128.65(14) . . ? Si1 N2 Al1 102.81(8) . . ? N1 C9 C10 112.26(14) . . ? N1 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? N1 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 P2 107.97(12) . . ? C9 C10 H10A 110.1 . . ? P2 C10 H10A 110.1 . . ? C9 C10 H10B 110.1 . . ? P2 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? N1 C7 C8 115.55(15) . . ? N1 C7 H7A 108.4 . . ? C8 C7 H7A 108.4 . . ? N1 C7 H7B 108.4 . . ? C8 C7 H7B 108.4 . . ? H7A C7 H7B 107.5 . . ? N2 C4 C2 110.03(19) . . ? N2 C4 C3 110.07(18) . . ? C2 C4 C3 111.0(2) . . ? N2 C4 C1 110.53(19) . . ? C2 C4 C1 108.2(2) . . ? C3 C4 C1 106.9(2) . . ? C7 C8 P1 112.44(14) . . ? C7 C8 H8A 109.1 . . ? P1 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? P1 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C20 C22 111.20(19) . . ? C21 C20 P2 114.11(18) . . ? C22 C20 P2 109.14(14) . . ? C21 C20 H20A 107.4 . . ? C22 C20 H20A 107.4 . . ? P2 C20 H20A 107.4 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C19 C17 C18 110.9(2) . . ? C19 C17 P2 111.94(15) . . ? C18 C17 P2 110.10(18) . . ? C19 C17 H17A 107.9 . . ? C18 C17 H17A 107.9 . . ? P2 C17 H17A 107.9 . . ? C12 C11 C13 110.4(2) . . ? C12 C11 P1 110.44(16) . . ? C13 C11 P1 111.0(2) . . ? C12 C11 H11A 108.3 . . ? C13 C11 H11A 108.3 . . ? P1 C11 H11A 108.3 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C14 C15 111.8(3) . . ? C16 C14 P1 116.9(2) . . ? C15 C14 P1 112.8(3) . . ? C16 C14 H14A 104.6 . . ? C15 C14 H14A 104.6 . . ? P1 C14 H14A 104.6 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 P2 Al1 N2 51.36(10) . . . . ? C20 P2 Al1 N2 -64.04(10) . . . . ? C17 P2 Al1 N2 170.75(11) . . . . ? C10 P2 Al1 Cl1 -95.74(7) . . . . ? C20 P2 Al1 Cl1 148.85(8) . . . . ? C17 P2 Al1 Cl1 23.65(10) . . . . ? C10 P2 Al1 Cl2 164.81(7) . . . . ? C20 P2 Al1 Cl2 49.40(8) . . . . ? C17 P2 Al1 Cl2 -75.81(10) . . . . ? C10 P2 Al1 N1 -9.03(7) . . . . ? C20 P2 Al1 N1 -124.43(9) . . . . ? C17 P2 Al1 N1 110.36(10) . . . . ? C10 P2 Al1 Si1 12.15(7) . . . . ? C20 P2 Al1 Si1 -103.25(8) . . . . ? C17 P2 Al1 Si1 131.54(9) . . . . ? N1 Si1 Al1 N2 -152.29(11) . . . . ? C5 Si1 Al1 N2 -71.31(17) . . . . ? C6 Si1 Al1 N2 106.47(12) . . . . ? N2 Si1 Al1 Cl1 -124.77(9) . . . . ? N1 Si1 Al1 Cl1 82.94(6) . . . . ? C5 Si1 Al1 Cl1 163.93(14) . . . . ? C6 Si1 Al1 Cl1 -18.30(9) . . . . ? N2 Si1 Al1 Cl2 -7.87(10) . . . . ? N1 Si1 Al1 Cl2 -160.15(8) . . . . ? C5 Si1 Al1 Cl2 -79.17(15) . . . . ? C6 Si1 Al1 Cl2 98.61(10) . . . . ? N2 Si1 Al1 N1 152.29(11) . . . . ? C5 Si1 Al1 N1 80.98(15) . . . . ? C6 Si1 Al1 N1 -101.24(10) . . . . ? N2 Si1 Al1 P2 118.59(9) . . . . ? N1 Si1 Al1 P2 -33.70(6) . . . . ? C5 Si1 Al1 P2 47.28(15) . . . . ? C6 Si1 Al1 P2 -134.94(9) . . . . ? N2 Si1 N1 C7 -135.89(14) . . . . ? C5 Si1 N1 C7 100.71(16) . . . . ? C6 Si1 N1 C7 -15.97(17) . . . . ? Al1 Si1 N1 C7 -118.29(14) . . . . ? N2 Si1 N1 C9 86.41(13) . . . . ? C5 Si1 N1 C9 -36.99(16) . . . . ? C6 Si1 N1 C9 -153.66(13) . . . . ? Al1 Si1 N1 C9 104.02(12) . . . . ? N2 Si1 N1 Al1 -17.60(7) . . . . ? C5 Si1 N1 Al1 -141.01(10) . . . . ? C6 Si1 N1 Al1 102.32(9) . . . . ? N2 Al1 N1 C7 137.61(14) . . . . ? Cl1 Al1 N1 C7 20.34(12) . . . . ? Cl2 Al1 N1 C7 -120.3(2) . . . . ? P2 Al1 N1 C7 -91.33(12) . . . . ? Si1 Al1 N1 C7 120.73(14) . . . . ? N2 Al1 N1 C9 -94.43(12) . . . . ? Cl1 Al1 N1 C9 148.30(10) . . . . ? Cl2 Al1 N1 C9 7.6(3) . . . . ? P2 Al1 N1 C9 36.63(10) . . . . ? Si1 Al1 N1 C9 -111.31(12) . . . . ? N2 Al1 N1 Si1 16.88(7) . . . . ? Cl1 Al1 N1 Si1 -100.39(5) . . . . ? Cl2 Al1 N1 Si1 118.9(2) . . . . ? P2 Al1 N1 Si1 147.94(5) . . . . ? N1 Si1 N2 C4 -173.95(17) . . . . ? C5 Si1 N2 C4 -57.9(2) . . . . ? C6 Si1 N2 C4 71.1(2) . . . . ? Al1 Si1 N2 C4 162.6(2) . . . . ? N1 Si1 N2 Al1 23.43(9) . . . . ? C5 Si1 N2 Al1 139.52(10) . . . . ? C6 Si1 N2 Al1 -91.48(12) . . . . ? Cl1 Al1 N2 C4 -96.44(18) . . . . ? Cl2 Al1 N2 C4 13.33(19) . . . . ? N1 Al1 N2 C4 -179.88(19) . . . . ? P2 Al1 N2 C4 117.97(17) . . . . ? Si1 Al1 N2 C4 -161.9(2) . . . . ? Cl1 Al1 N2 Si1 65.50(9) . . . . ? Cl2 Al1 N2 Si1 175.27(6) . . . . ? N1 Al1 N2 Si1 -17.94(7) . . . . ? P2 Al1 N2 Si1 -80.09(9) . . . . ? C7 N1 C9 C10 68.05(19) . . . . ? Si1 N1 C9 C10 -150.92(12) . . . . ? Al1 N1 C9 C10 -62.94(15) . . . . ? N1 C9 C10 P2 54.27(17) . . . . ? C20 P2 C10 C9 100.89(14) . . . . ? C17 P2 C10 C9 -144.95(13) . . . . ? Al1 P2 C10 C9 -18.04(13) . . . . ? C9 N1 C7 C8 61.4(2) . . . . ? Si1 N1 C7 C8 -76.13(19) . . . . ? Al1 N1 C7 C8 -174.12(13) . . . . ? Si1 N2 C4 C2 -103.8(2) . . . . ? Al1 N2 C4 C2 54.3(3) . . . . ? Si1 N2 C4 C3 133.52(19) . . . . ? Al1 N2 C4 C3 -68.4(2) . . . . ? Si1 N2 C4 C1 15.7(3) . . . . ? Al1 N2 C4 C1 173.76(18) . . . . ? N1 C7 C8 P1 -164.91(13) . . . . ? C11 P1 C8 C7 -174.79(15) . . . . ? C14 P1 C8 C7 -68.23(17) . . . . ? C10 P2 C20 C21 66.75(19) . . . . ? C17 P2 C20 C21 -47.3(2) . . . . ? Al1 P2 C20 C21 -178.59(15) . . . . ? C10 P2 C20 C22 -58.33(18) . . . . ? C17 P2 C20 C22 -172.33(16) . . . . ? Al1 P2 C20 C22 56.33(17) . . . . ? C10 P2 C17 C19 59.84(18) . . . . ? C20 P2 C17 C19 173.70(16) . . . . ? Al1 P2 C17 C19 -58.82(18) . . . . ? C10 P2 C17 C18 -176.31(17) . . . . ? C20 P2 C17 C18 -62.4(2) . . . . ? Al1 P2 C17 C18 65.04(19) . . . . ? C8 P1 C11 C12 -61.4(2) . . . . ? C14 P1 C11 C12 -165.3(2) . . . . ? C8 P1 C11 C13 175.7(2) . . . . ? C14 P1 C11 C13 71.9(2) . . . . ? C8 P1 C14 C16 -65.3(2) . . . . ? C11 P1 C14 C16 37.1(2) . . . . ? C8 P1 C14 C15 162.9(3) . . . . ? C11 P1 C14 C15 -94.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 33.75 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.812 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.077 #===end data_freds _database_code_depnum_ccdc_archive 'CCDC 701677' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H51 Cd Cl N2 P2 Si' _chemical_formula_sum 'C22 H51 Cd Cl N2 P2 Si' _chemical_formula_weight 581.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 '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 -0.0031 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0833 0.0850 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1013 0.1134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1408 0.1896 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.9197 1.4096 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 23.375(8) _cell_length_b 16.608(6) _cell_length_c 15.136(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5876(3) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 17428 _cell_measurement_theta_min 3.50 _cell_measurement_theta_max 32.95 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 1.243 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.832113 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator mirrors _diffrn_measurement_device_type 'Beamline 11.3.1 ALS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 79744 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 34.02 _reflns_number_total 17336 _reflns_number_gt 16147 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.255(12) _refine_ls_number_reflns 17336 _refine_ls_number_parameters 523 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0868 _refine_ls_wR_factor_gt 0.0854 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.146 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.315816(8) 0.487607(11) 0.840571(11) 0.01930(5) Uani 1 1 d . . . Cd2 Cd 0.567003(8) 0.009062(10) 0.720371(12) 0.01851(5) Uani 1 1 d . . . Cl1 Cl 0.25144(4) 0.47316(5) 0.71082(6) 0.04100(18) Uani 1 1 d . . . Cl2 Cl 0.50060(4) 0.01370(5) 0.84907(6) 0.03723(18) Uani 1 1 d . . . P1 P 0.29082(3) 0.36305(4) 0.93976(5) 0.02118(15) Uani 1 1 d . . . P2 P 0.27212(3) 0.61061(4) 0.92484(5) 0.02191(14) Uani 1 1 d . . . P3 P 0.52770(3) 0.12417(4) 0.61850(5) 0.01960(14) Uani 1 1 d . . . P4 P 0.54174(3) -0.12302(4) 0.63467(5) 0.02103(14) Uani 1 1 d . . . Si1 Si 0.43872(4) 0.49601(5) 0.92111(8) 0.0241(2) Uani 1 1 d . . . Si2 Si 0.69217(4) 0.00554(5) 0.64402(8) 0.02317(19) Uani 1 1 d . . . N4 N 0.63665(11) 0.00883(13) 0.5649(2) 0.0205(5) Uani 1 1 d . . . N3 N 0.65887(12) 0.01345(15) 0.74150(19) 0.0275(6) Uani 1 1 d . . . N2 N 0.38099(11) 0.50338(13) 0.9971(2) 0.0212(5) Uani 1 1 d . . . N1 N 0.40691(11) 0.50140(14) 0.8209(2) 0.0258(6) Uani 1 1 d . . . C42 C 0.47857(13) -0.11964(18) 0.5615(2) 0.0277(6) Uani 1 1 d . . . H42A H 0.4866 -0.0769 0.5167 0.033 Uiso 1 1 calc R . . C31 C 0.62055(12) -0.06010(16) 0.5084(2) 0.0231(6) Uani 1 1 d . . . H31A H 0.6536 -0.0740 0.4705 0.028 Uiso 1 1 calc R . . H31B H 0.5889 -0.0432 0.4691 0.028 Uiso 1 1 calc R . . C36 C 0.45238(12) 0.12499(19) 0.5789(2) 0.0295(6) Uani 1 1 d . . . H36A H 0.4460 0.0723 0.5484 0.035 Uiso 1 1 calc R . . C28 C 0.73536(14) -0.0888(2) 0.6252(2) 0.0376(8) Uani 1 1 d . . . H28A H 0.7729 -0.0744 0.6011 0.056 Uiso 1 1 calc R . . H28B H 0.7153 -0.1238 0.5833 0.056 Uiso 1 1 calc R . . H28C H 0.7404 -0.1172 0.6814 0.056 Uiso 1 1 calc R . . C27 C 0.74483(14) 0.0883(2) 0.6179(2) 0.0384(8) Uani 1 1 d . . . H27A H 0.7803 0.0647 0.5950 0.058 Uiso 1 1 calc R . . H27B H 0.7532 0.1189 0.6718 0.058 Uiso 1 1 calc R . . H27C H 0.7284 0.1244 0.5734 0.058 Uiso 1 1 calc R . . C33 C 0.54275(14) 0.22585(17) 0.6639(2) 0.0292(7) Uani 1 1 d . . . H33A H 0.5238 0.2674 0.6261 0.035 Uiso 1 1 calc R . . C39 C 0.53984(15) -0.21983(18) 0.6953(2) 0.0334(7) Uani 1 1 d . . . H39A H 0.5367 -0.2647 0.6515 0.040 Uiso 1 1 calc R . . C44 C 0.46832(16) -0.1970(2) 0.5098(2) 0.0427(8) Uani 1 1 d . . . H44A H 0.4344 -0.1907 0.4725 0.064 Uiso 1 1 calc R . . H44B H 0.4624 -0.2417 0.5511 0.064 Uiso 1 1 calc R . . H44C H 0.5017 -0.2085 0.4726 0.064 Uiso 1 1 calc R . . C32 C 0.60185(12) -0.13597(17) 0.5587(2) 0.0286(6) Uani 1 1 d . . . H32A H 0.6350 -0.1563 0.5928 0.034 Uiso 1 1 calc R . . H32B H 0.5915 -0.1779 0.5150 0.034 Uiso 1 1 calc R . . C35 C 0.60786(13) 0.24067(19) 0.6648(2) 0.0350(7) Uani 1 1 d . . . H35A H 0.6157 0.2943 0.6890 0.052 Uiso 1 1 calc R . . H35B H 0.6227 0.2374 0.6044 0.052 Uiso 1 1 calc R . . H35C H 0.6265 0.1998 0.7016 0.052 Uiso 1 1 calc R . . C23 C 0.68243(12) 0.0227(2) 0.8312(3) 0.0282(7) Uani 1 1 d . . . C1 C 0.43219(14) 0.49651(19) 0.7340(3) 0.0339(10) Uani 1 1 d . . . C26 C 0.74805(18) 0.0167(3) 0.8339(4) 0.0567(11) Uani 1 1 d . . . H26A H 0.7600 -0.0356 0.8103 0.085 Uiso 1 1 calc R . . H26B H 0.7612 0.0219 0.8951 0.085 Uiso 1 1 calc R . . H26C H 0.7647 0.0599 0.7980 0.085 Uiso 1 1 calc R . . C16 C 0.17157(13) 0.3928(2) 0.9532(2) 0.0376(7) Uani 1 1 d . . . H16A H 0.1384 0.3961 0.9925 0.056 Uiso 1 1 calc R . . H16B H 0.1648 0.3515 0.9082 0.056 Uiso 1 1 calc R . . H16C H 0.1774 0.4450 0.9244 0.056 Uiso 1 1 calc R . . C4 C 0.49846(19) 0.5074(2) 0.7359(3) 0.0536(12) Uani 1 1 d . . . H4A H 0.5155 0.4658 0.7736 0.080 Uiso 1 1 calc R . . H4B H 0.5078 0.5607 0.7596 0.080 Uiso 1 1 calc R . . H4C H 0.5137 0.5025 0.6758 0.080 Uiso 1 1 calc R . . C13 C 0.34677(15) 0.2469(2) 0.8386(2) 0.0430(8) Uani 1 1 d . . . H13A H 0.3462 0.1924 0.8139 0.064 Uiso 1 1 calc R . . H13B H 0.3799 0.2528 0.8778 0.064 Uiso 1 1 calc R . . H13C H 0.3494 0.2863 0.7906 0.064 Uiso 1 1 calc R . . C43 C 0.42395(13) -0.0932(2) 0.6106(3) 0.0418(8) Uani 1 1 d . . . H43A H 0.3917 -0.0922 0.5691 0.063 Uiso 1 1 calc R . . H43B H 0.4296 -0.0393 0.6354 0.063 Uiso 1 1 calc R . . H43C H 0.4158 -0.1313 0.6584 0.063 Uiso 1 1 calc R . . C25 C 0.65842(15) -0.0420(2) 0.8924(2) 0.0392(8) Uani 1 1 d . . . H25A H 0.6692 -0.0953 0.8703 0.059 Uiso 1 1 calc R . . H25B H 0.6166 -0.0377 0.8944 0.059 Uiso 1 1 calc R . . H25C H 0.6740 -0.0345 0.9520 0.059 Uiso 1 1 calc R . . C12 C 0.23946(16) 0.2500(2) 0.8304(2) 0.0485(9) Uani 1 1 d . . . H12A H 0.2403 0.1960 0.8043 0.073 Uiso 1 1 calc R . . H12B H 0.2402 0.2905 0.7833 0.073 Uiso 1 1 calc R . . H12C H 0.2045 0.2564 0.8654 0.073 Uiso 1 1 calc R . . C3 C 0.41976(15) 0.4146(2) 0.6923(2) 0.0412(8) Uani 1 1 d . . . H3A H 0.3783 0.4058 0.6904 0.062 Uiso 1 1 calc R . . H3B H 0.4378 0.3722 0.7276 0.062 Uiso 1 1 calc R . . H3C H 0.4352 0.4133 0.6321 0.062 Uiso 1 1 calc R . . C20 C 0.19539(12) 0.6116(2) 0.9564(2) 0.0319(7) Uani 1 1 d . . . H20A H 0.1889 0.5616 0.9918 0.038 Uiso 1 1 calc R . . C38 C 0.43984(14) 0.1903(2) 0.5111(2) 0.0408(8) Uani 1 1 d . . . H38A H 0.3996 0.1871 0.4931 0.061 Uiso 1 1 calc R . . H38B H 0.4645 0.1827 0.4594 0.061 Uiso 1 1 calc R . . H38C H 0.4473 0.2433 0.5372 0.061 Uiso 1 1 calc R . . C24 C 0.66537(16) 0.1056(2) 0.8665(2) 0.0419(8) Uani 1 1 d . . . H24A H 0.6808 0.1475 0.8276 0.063 Uiso 1 1 calc R . . H24B H 0.6808 0.1127 0.9262 0.063 Uiso 1 1 calc R . . H24C H 0.6236 0.1098 0.8683 0.063 Uiso 1 1 calc R . . C8 C 0.34906(12) 0.35878(16) 1.0211(2) 0.0257(6) Uani 1 1 d . . . H8A H 0.3374 0.3222 1.0695 0.031 Uiso 1 1 calc R . . H8B H 0.3831 0.3348 0.9923 0.031 Uiso 1 1 calc R . . C10 C 0.30681(12) 0.61075(17) 1.03365(19) 0.0255(6) Uani 1 1 d . . . H10A H 0.3046 0.6658 1.0584 0.031 Uiso 1 1 calc R . . H10B H 0.2850 0.5748 1.0734 0.031 Uiso 1 1 calc R . . C9 C 0.37007(12) 0.58384(17) 1.0340(2) 0.0280(6) Uani 1 1 d . . . H9A H 0.3927 0.6236 1.0000 0.034 Uiso 1 1 calc R . . H9B H 0.3842 0.5849 1.0957 0.034 Uiso 1 1 calc R . . C2 C 0.40696(17) 0.5616(2) 0.6739(2) 0.0483(9) Uani 1 1 d . . . H2A H 0.3653 0.5559 0.6718 0.073 Uiso 1 1 calc R . . H2B H 0.4227 0.5558 0.6142 0.073 Uiso 1 1 calc R . . H2C H 0.4168 0.6149 0.6972 0.073 Uiso 1 1 calc R . . C11 C 0.29219(14) 0.26138(18) 0.8908(2) 0.0299(7) Uani 1 1 d . . . H11A H 0.2902 0.2209 0.9396 0.036 Uiso 1 1 calc R . . C41 C 0.59493(15) -0.2312(2) 0.7489(2) 0.0445(9) Uani 1 1 d . . . H41A H 0.5934 -0.2828 0.7803 0.067 Uiso 1 1 calc R . . H41B H 0.5987 -0.1873 0.7917 0.067 Uiso 1 1 calc R . . H41C H 0.6279 -0.2309 0.7089 0.067 Uiso 1 1 calc R . . C19 C 0.26838(17) 0.7071(2) 0.7759(2) 0.0477(9) Uani 1 1 d . . . H19A H 0.2764 0.7595 0.7487 0.072 Uiso 1 1 calc R . . H19B H 0.2273 0.6960 0.7725 0.072 Uiso 1 1 calc R . . H19C H 0.2895 0.6650 0.7444 0.072 Uiso 1 1 calc R . . C21 C 0.17865(15) 0.6824(2) 1.0168(3) 0.0494(10) Uani 1 1 d . . . H21A H 0.1378 0.6790 1.0310 0.074 Uiso 1 1 calc R . . H21B H 0.1864 0.7334 0.9865 0.074 Uiso 1 1 calc R . . H21C H 0.2011 0.6799 1.0715 0.074 Uiso 1 1 calc R . . C18 C 0.35005(15) 0.7310(2) 0.8771(3) 0.0458(9) Uani 1 1 d . . . H18A H 0.3560 0.7833 0.8486 0.069 Uiso 1 1 calc R . . H18B H 0.3728 0.6899 0.8467 0.069 Uiso 1 1 calc R . . H18C H 0.3619 0.7342 0.9391 0.069 Uiso 1 1 calc R . . C37 C 0.40916(14) 0.1288(2) 0.6553(3) 0.0486(9) Uani 1 1 d . . . H37A H 0.3702 0.1288 0.6314 0.073 Uiso 1 1 calc R . . H37B H 0.4154 0.1782 0.6894 0.073 Uiso 1 1 calc R . . H37C H 0.4143 0.0819 0.6938 0.073 Uiso 1 1 calc R . . C7 C 0.36649(12) 0.43979(17) 1.06147(19) 0.0246(6) Uani 1 1 d . . . H7A H 0.3347 0.4593 1.0990 0.030 Uiso 1 1 calc R . . H7B H 0.4000 0.4309 1.1003 0.030 Uiso 1 1 calc R . . C34 C 0.51957(16) 0.2320(2) 0.7583(2) 0.0443(9) Uani 1 1 d . . . H34A H 0.5277 0.2858 0.7820 0.066 Uiso 1 1 calc R . . H34B H 0.5381 0.1913 0.7955 0.066 Uiso 1 1 calc R . . H34C H 0.4781 0.2229 0.7579 0.066 Uiso 1 1 calc R . . C17 C 0.28696(14) 0.70861(18) 0.8722(2) 0.0310(7) Uani 1 1 d . . . H17A H 0.2644 0.7510 0.9036 0.037 Uiso 1 1 calc R . . C5 C 0.48056(13) 0.4015(2) 0.9487(3) 0.0420(9) Uani 1 1 d . . . H5A H 0.5178 0.4165 0.9734 0.063 Uiso 1 1 calc R . . H5B H 0.4862 0.3697 0.8949 0.063 Uiso 1 1 calc R . . H5C H 0.4593 0.3696 0.9921 0.063 Uiso 1 1 calc R . . C15 C 0.21398(15) 0.2982(2) 1.0676(2) 0.0378(8) Uani 1 1 d . . . H15A H 0.1787 0.3072 1.1011 0.057 Uiso 1 1 calc R . . H15B H 0.2460 0.2916 1.1087 0.057 Uiso 1 1 calc R . . H15C H 0.2100 0.2495 1.0316 0.057 Uiso 1 1 calc R . . C40 C 0.48777(15) -0.2224(2) 0.7564(3) 0.0492(10) Uani 1 1 d . . . H40A H 0.4871 -0.2739 0.7880 0.074 Uiso 1 1 calc R . . H40B H 0.4528 -0.2169 0.7212 0.074 Uiso 1 1 calc R . . H40C H 0.4901 -0.1782 0.7990 0.074 Uiso 1 1 calc R . . C14 C 0.22532(12) 0.37067(17) 1.0075(2) 0.0263(6) Uani 1 1 d . . . H14A H 0.2319 0.4172 1.0481 0.032 Uiso 1 1 calc R . . C6 C 0.49166(14) 0.5793(2) 0.9483(3) 0.0428(9) Uani 1 1 d . . . H6A H 0.5263 0.5558 0.9740 0.064 Uiso 1 1 calc R . . H6B H 0.4743 0.6167 0.9906 0.064 Uiso 1 1 calc R . . H6C H 0.5016 0.6085 0.8941 0.064 Uiso 1 1 calc R . . C22 C 0.15518(14) 0.6061(3) 0.8772(3) 0.0569(11) Uani 1 1 d . . . H22A H 0.1154 0.6067 0.8978 0.085 Uiso 1 1 calc R . . H22B H 0.1625 0.5560 0.8450 0.085 Uiso 1 1 calc R . . H22C H 0.1617 0.6521 0.8380 0.085 Uiso 1 1 calc R . . C30 C 0.56614(11) 0.11581(17) 0.51351(19) 0.0236(5) Uani 1 1 d . . . H30A H 0.5444 0.0790 0.4746 0.028 Uiso 1 1 calc R . . H30B H 0.5663 0.1695 0.4850 0.028 Uiso 1 1 calc R . . C29 C 0.62789(12) 0.08575(17) 0.5183(2) 0.0266(6) Uani 1 1 d . . . H29A H 0.6425 0.0799 0.4573 0.032 Uiso 1 1 calc R . . H29B H 0.6513 0.1275 0.5479 0.032 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 Cd1 0.01782(10) 0.02436(9) 0.01572(10) 0.00038(10) -0.00117(8) -0.00032(6) Cd2 0.01779(10) 0.02170(9) 0.01603(11) -0.00079(10) 0.00120(8) -0.00070(6) Cl1 0.0403(4) 0.0586(5) 0.0241(4) -0.0069(4) -0.0144(4) 0.0042(4) Cl2 0.0384(4) 0.0496(4) 0.0237(4) -0.0005(3) 0.0144(3) -0.0032(3) P1 0.0235(3) 0.0213(3) 0.0187(4) -0.0007(3) 0.0006(3) -0.0019(3) P2 0.0210(3) 0.0227(3) 0.0221(4) 0.0015(3) 0.0000(3) 0.0023(3) P3 0.0194(3) 0.0203(3) 0.0190(3) -0.0005(3) 0.0004(3) 0.0020(2) P4 0.0240(3) 0.0191(3) 0.0200(4) -0.0003(2) -0.0004(3) -0.0013(3) Si1 0.0159(4) 0.0330(4) 0.0233(6) 0.0018(3) -0.0009(3) -0.0015(3) Si2 0.0161(4) 0.0320(4) 0.0214(5) -0.0031(3) 0.0003(4) 0.0003(3) N4 0.0206(12) 0.0219(11) 0.0190(13) -0.0040(9) -0.0012(10) -0.0014(8) N3 0.0218(13) 0.0429(15) 0.0178(16) -0.0036(10) -0.0006(11) -0.0020(10) N2 0.0169(12) 0.0241(11) 0.0226(15) -0.0016(8) 0.0006(10) -0.0003(8) N1 0.0160(12) 0.0392(14) 0.0224(16) 0.0009(9) 0.0030(11) -0.0038(9) C42 0.0312(15) 0.0273(14) 0.0246(15) 0.0048(11) -0.0052(12) -0.0031(12) C31 0.0219(13) 0.0274(13) 0.0198(14) -0.0059(11) 0.0007(10) 0.0012(10) C36 0.0221(14) 0.0371(16) 0.0293(16) -0.0024(12) -0.0011(12) 0.0042(12) C28 0.0290(16) 0.0505(19) 0.0332(19) -0.0085(15) -0.0024(13) 0.0163(14) C27 0.0316(17) 0.055(2) 0.0289(17) -0.0008(15) 0.0002(14) -0.0159(15) C33 0.0382(17) 0.0211(13) 0.0282(16) -0.0011(11) -0.0044(13) 0.0048(12) C39 0.050(2) 0.0207(13) 0.0293(18) 0.0053(11) -0.0059(14) -0.0040(13) C44 0.050(2) 0.0416(19) 0.0368(19) -0.0041(15) -0.0196(16) -0.0075(15) C32 0.0306(15) 0.0211(13) 0.0342(16) -0.0037(11) 0.0063(12) 0.0007(11) C35 0.0391(17) 0.0326(16) 0.0333(17) -0.0018(13) -0.0027(14) -0.0088(13) C23 0.0246(15) 0.0417(16) 0.0185(18) -0.0019(15) -0.0046(12) -0.0016(12) C1 0.0252(17) 0.0473(19) 0.029(2) 0.0025(13) 0.0076(13) -0.0033(13) C26 0.0309(19) 0.104(3) 0.035(2) -0.012(2) -0.0048(19) 0.0031(19) C16 0.0256(15) 0.047(2) 0.040(2) -0.0019(16) 0.0007(14) -0.0001(14) C4 0.035(2) 0.091(3) 0.035(3) -0.0044(19) 0.0194(19) -0.0125(17) C13 0.058(2) 0.0366(17) 0.0345(18) -0.0087(16) 0.0170(17) 0.0046(14) C43 0.0277(16) 0.046(2) 0.052(2) 0.0063(17) 0.0022(16) 0.0004(14) C25 0.0473(19) 0.0424(19) 0.0278(17) 0.0080(14) -0.0118(15) -0.0031(16) C12 0.060(2) 0.0448(19) 0.041(2) -0.0191(17) -0.0011(18) -0.0136(16) C3 0.0411(18) 0.055(2) 0.0271(17) -0.0072(15) 0.0103(14) -0.0010(16) C20 0.0249(14) 0.0378(17) 0.0330(17) 0.0084(14) 0.0046(13) 0.0070(12) C38 0.0343(17) 0.048(2) 0.040(2) 0.0032(16) -0.0083(15) 0.0115(14) C24 0.057(2) 0.0418(19) 0.0269(17) -0.0084(14) -0.0152(15) 0.0017(16) C8 0.0248(13) 0.0256(13) 0.0269(15) 0.0074(11) -0.0049(11) 0.0015(11) C10 0.0267(14) 0.0252(14) 0.0244(14) -0.0045(11) -0.0013(11) 0.0026(10) C9 0.0299(15) 0.0251(14) 0.0288(16) -0.0057(11) -0.0050(12) -0.0001(11) C2 0.052(2) 0.060(2) 0.033(2) 0.0168(17) 0.0092(16) 0.0057(18) C11 0.0410(17) 0.0224(14) 0.0263(16) -0.0036(12) 0.0069(13) -0.0036(13) C41 0.0451(19) 0.050(2) 0.038(2) 0.0124(16) -0.0100(16) 0.0055(16) C19 0.058(2) 0.047(2) 0.038(2) 0.0203(16) -0.0075(17) 0.0012(17) C21 0.044(2) 0.045(2) 0.060(3) 0.0101(19) 0.0228(18) 0.0183(16) C18 0.048(2) 0.042(2) 0.047(2) 0.0133(16) -0.0007(17) -0.0134(16) C37 0.0266(17) 0.071(3) 0.048(2) -0.006(2) 0.0046(15) 0.0049(16) C7 0.0235(13) 0.0326(15) 0.0178(14) 0.0000(11) -0.0019(10) 0.0002(11) C34 0.055(2) 0.0377(18) 0.041(2) -0.0163(15) 0.0076(17) 0.0040(16) C17 0.0413(18) 0.0218(14) 0.0300(17) 0.0015(11) 0.0074(14) 0.0027(12) C5 0.0228(15) 0.053(2) 0.051(2) 0.0129(17) 0.0110(15) 0.0121(14) C15 0.0423(18) 0.0367(18) 0.0343(18) 0.0046(14) 0.0116(15) -0.0096(14) C40 0.045(2) 0.056(2) 0.046(2) 0.0209(18) 0.0003(17) -0.0145(17) C14 0.0246(14) 0.0289(14) 0.0254(15) -0.0016(11) 0.0040(12) -0.0023(11) C6 0.0243(16) 0.064(2) 0.040(2) -0.0015(17) -0.0035(14) -0.0138(15) C22 0.0261(17) 0.092(3) 0.053(2) 0.013(2) -0.0043(16) 0.0063(18) C30 0.0258(14) 0.0272(13) 0.0180(13) 0.0020(10) 0.0021(10) -0.0013(10) C29 0.0237(13) 0.0332(15) 0.0230(15) 0.0030(12) 0.0081(11) -0.0005(11) _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 Cd1 N1 2.162(3) . ? Cd1 Cl1 2.4858(11) . ? Cd1 P2 2.6160(10) . ? Cd1 P1 2.6220(10) . ? Cd1 Si1 3.1240(13) . ? Cd2 N3 2.172(3) . ? Cd2 Cl2 2.4920(11) . ? Cd2 P4 2.6160(10) . ? Cd2 P3 2.6223(9) . ? Cd2 Si2 3.1462(13) . ? P1 C8 1.837(3) . ? P1 C11 1.844(3) . ? P1 C14 1.847(3) . ? P2 C10 1.836(3) . ? P2 C17 1.845(3) . ? P2 C20 1.856(3) . ? P3 C30 1.831(3) . ? P3 C33 1.857(3) . ? P3 C36 1.860(3) . ? P4 C32 1.828(3) . ? P4 C42 1.846(3) . ? P4 C39 1.852(3) . ? Si1 N1 1.692(3) . ? Si1 N2 1.778(3) . ? Si1 C5 1.896(3) . ? Si1 C6 1.902(3) . ? Si2 N3 1.673(3) . ? Si2 N4 1.767(3) . ? Si2 C28 1.886(3) . ? Si2 C27 1.887(3) . ? N4 C29 1.474(4) . ? N4 C31 1.478(4) . ? N3 C23 1.472(5) . ? N2 C9 1.470(4) . ? N2 C7 1.476(4) . ? N1 C1 1.444(6) . ? C42 C44 1.524(4) . ? C42 C43 1.541(4) . ? C42 H42A 1.0000 . ? C31 C32 1.536(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C36 C38 1.522(4) . ? C36 C37 1.537(4) . ? C36 H36A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C33 C34 1.532(5) . ? C33 C35 1.542(4) . ? C33 H33A 1.0000 . ? C39 C40 1.529(5) . ? C39 C41 1.534(4) . ? C39 H39A 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C23 C25 1.527(5) . ? C23 C24 1.530(5) . ? C23 C26 1.538(5) . ? C1 C3 1.527(5) . ? C1 C2 1.531(5) . ? C1 C4 1.560(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C16 C14 1.546(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C13 C11 1.520(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C12 C11 1.546(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C20 C22 1.526(5) . ? C20 C21 1.540(5) . ? C20 H20A 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C8 C7 1.533(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C10 C9 1.545(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C11 H11A 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C19 C17 1.521(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C18 C17 1.523(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C17 H17A 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C15 C14 1.532(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C14 H14A 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C30 C29 1.529(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? 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 Cd1 Cl1 119.83(9) . . ? N1 Cd1 P2 111.66(7) . . ? Cl1 Cd1 P2 102.96(3) . . ? N1 Cd1 P1 112.46(7) . . ? Cl1 Cd1 P1 103.97(3) . . ? P2 Cd1 P1 104.47(3) . . ? N1 Cd1 Si1 31.07(9) . . ? Cl1 Cd1 Si1 150.38(3) . . ? P2 Cd1 Si1 97.69(3) . . ? P1 Cd1 Si1 90.96(3) . . ? N3 Cd2 Cl2 119.97(8) . . ? N3 Cd2 P4 108.92(7) . . ? Cl2 Cd2 P4 105.84(3) . . ? N3 Cd2 P3 114.11(8) . . ? Cl2 Cd2 P3 102.65(3) . . ? P4 Cd2 P3 103.93(3) . . ? N3 Cd2 Si2 30.17(8) . . ? Cl2 Cd2 Si2 150.10(3) . . ? P4 Cd2 Si2 90.70(3) . . ? P3 Cd2 Si2 97.09(3) . . ? C8 P1 C11 102.76(14) . . ? C8 P1 C14 104.21(14) . . ? C11 P1 C14 107.46(14) . . ? C8 P1 Cd1 104.42(9) . . ? C11 P1 Cd1 119.24(11) . . ? C14 P1 Cd1 116.64(10) . . ? C10 P2 C17 107.66(15) . . ? C10 P2 C20 101.31(14) . . ? C17 P2 C20 106.55(15) . . ? C10 P2 Cd1 105.43(9) . . ? C17 P2 Cd1 113.88(11) . . ? C20 P2 Cd1 120.65(11) . . ? C30 P3 C33 107.31(14) . . ? C30 P3 C36 100.68(13) . . ? C33 P3 C36 106.98(14) . . ? C30 P3 Cd2 106.45(9) . . ? C33 P3 Cd2 112.26(11) . . ? C36 P3 Cd2 121.77(10) . . ? C32 P4 C42 103.97(15) . . ? C32 P4 C39 103.17(15) . . ? C42 P4 C39 107.71(14) . . ? C32 P4 Cd2 103.71(10) . . ? C42 P4 Cd2 116.89(10) . . ? C39 P4 Cd2 119.19(11) . . ? N1 Si1 N2 104.07(14) . . ? N1 Si1 C5 117.91(17) . . ? N2 Si1 C5 107.82(15) . . ? N1 Si1 C6 116.19(16) . . ? N2 Si1 C6 107.70(16) . . ? C5 Si1 C6 102.65(18) . . ? N1 Si1 Cd1 41.27(9) . . ? N2 Si1 Cd1 63.73(10) . . ? C5 Si1 Cd1 121.57(12) . . ? C6 Si1 Cd1 135.67(12) . . ? N3 Si2 N4 104.70(15) . . ? N3 Si2 C28 116.59(16) . . ? N4 Si2 C28 108.46(14) . . ? N3 Si2 C27 115.50(15) . . ? N4 Si2 C27 108.35(15) . . ? C28 Si2 C27 102.97(18) . . ? N3 Si2 Cd2 40.73(10) . . ? N4 Si2 Cd2 64.24(10) . . ? C28 Si2 Cd2 124.68(12) . . ? C27 Si2 Cd2 132.05(12) . . ? C29 N4 C31 111.0(3) . . ? C29 N4 Si2 116.96(18) . . ? C31 N4 Si2 123.74(19) . . ? C23 N3 Si2 130.3(2) . . ? C23 N3 Cd2 120.6(2) . . ? Si2 N3 Cd2 109.10(15) . . ? C9 N2 C7 111.1(3) . . ? C9 N2 Si1 116.10(19) . . ? C7 N2 Si1 123.51(18) . . ? C1 N1 Si1 129.3(2) . . ? C1 N1 Cd1 121.5(2) . . ? Si1 N1 Cd1 107.66(15) . . ? C44 C42 C43 110.9(3) . . ? C44 C42 P4 114.1(2) . . ? C43 C42 P4 112.5(2) . . ? C44 C42 H42A 106.2 . . ? C43 C42 H42A 106.2 . . ? P4 C42 H42A 106.2 . . ? N4 C31 C32 114.9(3) . . ? N4 C31 H31A 108.5 . . ? C32 C31 H31A 108.5 . . ? N4 C31 H31B 108.5 . . ? C32 C31 H31B 108.5 . . ? H31A C31 H31B 107.5 . . ? C38 C36 C37 110.6(3) . . ? C38 C36 P3 113.9(2) . . ? C37 C36 P3 112.3(2) . . ? C38 C36 H36A 106.5 . . ? C37 C36 H36A 106.5 . . ? P3 C36 H36A 106.5 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C34 C33 C35 109.3(3) . . ? C34 C33 P3 109.8(2) . . ? C35 C33 P3 109.6(2) . . ? C34 C33 H33A 109.4 . . ? C35 C33 H33A 109.4 . . ? P3 C33 H33A 109.4 . . ? C40 C39 C41 110.2(3) . . ? C40 C39 P4 110.1(2) . . ? C41 C39 P4 110.4(2) . . ? C40 C39 H39A 108.7 . . ? C41 C39 H39A 108.7 . . ? P4 C39 H39A 108.7 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C31 C32 P4 115.74(19) . . ? C31 C32 H32A 108.3 . . ? P4 C32 H32A 108.3 . . ? C31 C32 H32B 108.3 . . ? P4 C32 H32B 108.3 . . ? H32A C32 H32B 107.4 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C23 C25 110.4(3) . . ? N3 C23 C24 108.6(3) . . ? C25 C23 C24 109.0(3) . . ? N3 C23 C26 113.0(4) . . ? C25 C23 C26 107.7(3) . . ? C24 C23 C26 108.0(3) . . ? N1 C1 C3 110.4(3) . . ? N1 C1 C2 110.1(3) . . ? C3 C1 C2 108.1(4) . . ? N1 C1 C4 112.5(4) . . ? C3 C1 C4 107.4(3) . . ? C2 C1 C4 108.2(3) . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C22 C20 C21 110.8(3) . . ? C22 C20 P2 113.1(2) . . ? C21 C20 P2 113.9(2) . . ? C22 C20 H20A 106.1 . . ? C21 C20 H20A 106.1 . . ? P2 C20 H20A 106.1 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C7 C8 P1 115.49(19) . . ? C7 C8 H8A 108.4 . . ? P1 C8 H8A 108.4 . . ? C7 C8 H8B 108.4 . . ? P1 C8 H8B 108.4 . . ? H8A C8 H8B 107.5 . . ? C9 C10 P2 115.2(2) . . ? C9 C10 H10A 108.5 . . ? P2 C10 H10A 108.5 . . ? C9 C10 H10B 108.5 . . ? P2 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? N2 C9 C10 115.3(2) . . ? N2 C9 H9A 108.4 . . ? C10 C9 H9A 108.4 . . ? N2 C9 H9B 108.4 . . ? C10 C9 H9B 108.4 . . ? H9A C9 H9B 107.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C13 C11 C12 110.0(3) . . ? C13 C11 P1 111.6(2) . . ? C12 C11 P1 109.6(2) . . ? C13 C11 H11A 108.5 . . ? C12 C11 H11A 108.5 . . ? P1 C11 H11A 108.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N2 C7 C8 115.2(2) . . ? N2 C7 H7A 108.5 . . ? C8 C7 H7A 108.5 . . ? N2 C7 H7B 108.5 . . ? C8 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C19 C17 C18 109.1(3) . . ? C19 C17 P2 110.3(2) . . ? C18 C17 P2 112.1(2) . . ? C19 C17 H17A 108.4 . . ? C18 C17 H17A 108.4 . . ? P2 C17 H17A 108.4 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C15 C14 C16 111.3(3) . . ? C15 C14 P1 114.8(2) . . ? C16 C14 P1 113.3(2) . . ? C15 C14 H14A 105.5 . . ? C16 C14 H14A 105.5 . . ? P1 C14 H14A 105.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C29 C30 P3 116.5(2) . . ? C29 C30 H30A 108.2 . . ? P3 C30 H30A 108.2 . . ? C29 C30 H30B 108.2 . . ? P3 C30 H30B 108.2 . . ? H30A C30 H30B 107.3 . . ? N4 C29 C30 115.9(2) . . ? N4 C29 H29A 108.3 . . ? C30 C29 H29A 108.3 . . ? N4 C29 H29B 108.3 . . ? C30 C29 H29B 108.3 . . ? H29A C29 H29B 107.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cd1 P1 C8 35.52(13) . . . . ? Cl1 Cd1 P1 C8 166.62(10) . . . . ? P2 Cd1 P1 C8 -85.76(10) . . . . ? Si1 Cd1 P1 C8 12.44(10) . . . . ? N1 Cd1 P1 C11 -78.40(15) . . . . ? Cl1 Cd1 P1 C11 52.70(13) . . . . ? P2 Cd1 P1 C11 160.33(13) . . . . ? Si1 Cd1 P1 C11 -101.47(13) . . . . ? N1 Cd1 P1 C14 149.88(14) . . . . ? Cl1 Cd1 P1 C14 -79.02(12) . . . . ? P2 Cd1 P1 C14 28.61(12) . . . . ? Si1 Cd1 P1 C14 126.81(11) . . . . ? N1 Cd1 P2 C10 -62.80(13) . . . . ? Cl1 Cd1 P2 C10 167.37(10) . . . . ? P1 Cd1 P2 C10 59.00(10) . . . . ? Si1 Cd1 P2 C10 -34.00(10) . . . . ? N1 Cd1 P2 C17 55.00(15) . . . . ? Cl1 Cd1 P2 C17 -74.83(12) . . . . ? P1 Cd1 P2 C17 176.80(12) . . . . ? Si1 Cd1 P2 C17 83.80(12) . . . . ? N1 Cd1 P2 C20 -176.37(15) . . . . ? Cl1 Cd1 P2 C20 53.80(13) . . . . ? P1 Cd1 P2 C20 -54.57(12) . . . . ? Si1 Cd1 P2 C20 -147.57(12) . . . . ? N3 Cd2 P3 C30 57.50(13) . . . . ? Cl2 Cd2 P3 C30 -171.11(10) . . . . ? P4 Cd2 P3 C30 -60.99(10) . . . . ? Si2 Cd2 P3 C30 31.50(10) . . . . ? N3 Cd2 P3 C33 -59.64(14) . . . . ? Cl2 Cd2 P3 C33 71.76(12) . . . . ? P4 Cd2 P3 C33 -178.13(11) . . . . ? Si2 Cd2 P3 C33 -85.64(12) . . . . ? N3 Cd2 P3 C36 171.71(14) . . . . ? Cl2 Cd2 P3 C36 -56.90(12) . . . . ? P4 Cd2 P3 C36 53.22(12) . . . . ? Si2 Cd2 P3 C36 145.71(12) . . . . ? N3 Cd2 P4 C32 -36.36(14) . . . . ? Cl2 Cd2 P4 C32 -166.62(11) . . . . ? P3 Cd2 P4 C32 85.64(11) . . . . ? Si2 Cd2 P4 C32 -11.84(11) . . . . ? N3 Cd2 P4 C42 -150.08(14) . . . . ? Cl2 Cd2 P4 C42 79.66(12) . . . . ? P3 Cd2 P4 C42 -28.08(11) . . . . ? Si2 Cd2 P4 C42 -125.56(11) . . . . ? N3 Cd2 P4 C39 77.53(16) . . . . ? Cl2 Cd2 P4 C39 -52.72(14) . . . . ? P3 Cd2 P4 C39 -160.47(13) . . . . ? Si2 Cd2 P4 C39 102.05(14) . . . . ? Cl1 Cd1 Si1 N1 14.25(14) . . . . ? P2 Cd1 Si1 N1 -119.82(12) . . . . ? P1 Cd1 Si1 N1 135.44(12) . . . . ? N1 Cd1 Si1 N2 166.78(15) . . . . ? Cl1 Cd1 Si1 N2 -178.97(9) . . . . ? P2 Cd1 Si1 N2 46.96(8) . . . . ? P1 Cd1 Si1 N2 -57.78(8) . . . . ? N1 Cd1 Si1 C5 -97.6(2) . . . . ? Cl1 Cd1 Si1 C5 -83.38(16) . . . . ? P2 Cd1 Si1 C5 142.55(15) . . . . ? P1 Cd1 Si1 C5 37.81(16) . . . . ? N1 Cd1 Si1 C6 77.9(2) . . . . ? Cl1 Cd1 Si1 C6 92.2(2) . . . . ? P2 Cd1 Si1 C6 -41.9(2) . . . . ? P1 Cd1 Si1 C6 -146.6(2) . . . . ? Cl2 Cd2 Si2 N3 -3.97(15) . . . . ? P4 Cd2 Si2 N3 -128.64(14) . . . . ? P3 Cd2 Si2 N3 127.23(14) . . . . ? N3 Cd2 Si2 N4 -172.87(16) . . . . ? Cl2 Cd2 Si2 N4 -176.84(9) . . . . ? P4 Cd2 Si2 N4 58.49(8) . . . . ? P3 Cd2 Si2 N4 -45.64(8) . . . . ? N3 Cd2 Si2 C28 91.8(2) . . . . ? Cl2 Cd2 Si2 C28 87.79(16) . . . . ? P4 Cd2 Si2 C28 -36.88(15) . . . . ? P3 Cd2 Si2 C28 -141.01(15) . . . . ? N3 Cd2 Si2 C27 -80.9(2) . . . . ? Cl2 Cd2 Si2 C27 -84.82(18) . . . . ? P4 Cd2 Si2 C27 150.51(17) . . . . ? P3 Cd2 Si2 C27 46.38(17) . . . . ? N3 Si2 N4 C29 101.7(2) . . . . ? C28 Si2 N4 C29 -133.2(2) . . . . ? C27 Si2 N4 C29 -22.1(3) . . . . ? Cd2 Si2 N4 C29 106.5(2) . . . . ? N3 Si2 N4 C31 -112.8(2) . . . . ? C28 Si2 N4 C31 12.3(3) . . . . ? C27 Si2 N4 C31 123.4(3) . . . . ? Cd2 Si2 N4 C31 -108.0(2) . . . . ? N4 Si2 N3 C23 -172.9(3) . . . . ? C28 Si2 N3 C23 67.3(3) . . . . ? C27 Si2 N3 C23 -53.9(3) . . . . ? Cd2 Si2 N3 C23 -179.5(4) . . . . ? N4 Si2 N3 Cd2 6.63(15) . . . . ? C28 Si2 N3 Cd2 -113.19(16) . . . . ? C27 Si2 N3 Cd2 125.69(16) . . . . ? Cl2 Cd2 N3 C23 -2.7(3) . . . . ? P4 Cd2 N3 C23 -124.7(2) . . . . ? P3 Cd2 N3 C23 119.7(2) . . . . ? Si2 Cd2 N3 C23 179.6(3) . . . . ? Cl2 Cd2 N3 Si2 177.72(9) . . . . ? P4 Cd2 N3 Si2 55.66(14) . . . . ? P3 Cd2 N3 Si2 -59.95(14) . . . . ? N1 Si1 N2 C9 -97.2(2) . . . . ? C5 Si1 N2 C9 136.8(2) . . . . ? C6 Si1 N2 C9 26.7(3) . . . . ? Cd1 Si1 N2 C9 -106.1(2) . . . . ? N1 Si1 N2 C7 119.2(2) . . . . ? C5 Si1 N2 C7 -6.8(3) . . . . ? C6 Si1 N2 C7 -116.9(3) . . . . ? Cd1 Si1 N2 C7 110.2(2) . . . . ? N2 Si1 N1 C1 -178.2(2) . . . . ? C5 Si1 N1 C1 -58.8(3) . . . . ? C6 Si1 N1 C1 63.6(3) . . . . ? Cd1 Si1 N1 C1 -166.0(3) . . . . ? N2 Si1 N1 Cd1 -12.20(13) . . . . ? C5 Si1 N1 Cd1 107.13(16) . . . . ? C6 Si1 N1 Cd1 -130.41(15) . . . . ? Cl1 Cd1 N1 C1 -4.6(2) . . . . ? P2 Cd1 N1 C1 -125.0(2) . . . . ? P1 Cd1 N1 C1 117.9(2) . . . . ? Si1 Cd1 N1 C1 167.3(3) . . . . ? Cl1 Cd1 N1 Si1 -171.94(8) . . . . ? P2 Cd1 N1 Si1 67.68(12) . . . . ? P1 Cd1 N1 Si1 -49.39(13) . . . . ? C32 P4 C42 C44 63.2(3) . . . . ? C39 P4 C42 C44 -45.9(3) . . . . ? Cd2 P4 C42 C44 176.7(2) . . . . ? C32 P4 C42 C43 -169.3(2) . . . . ? C39 P4 C42 C43 81.7(2) . . . . ? Cd2 P4 C42 C43 -55.7(2) . . . . ? C29 N4 C31 C32 -153.5(2) . . . . ? Si2 N4 C31 C32 59.2(3) . . . . ? C30 P3 C36 C38 -55.3(3) . . . . ? C33 P3 C36 C38 56.7(3) . . . . ? Cd2 P3 C36 C38 -172.41(19) . . . . ? C30 P3 C36 C37 178.0(2) . . . . ? C33 P3 C36 C37 -70.0(3) . . . . ? Cd2 P3 C36 C37 60.9(3) . . . . ? C30 P3 C33 C34 -171.2(2) . . . . ? C36 P3 C33 C34 81.4(3) . . . . ? Cd2 P3 C33 C34 -54.6(2) . . . . ? C30 P3 C33 C35 -51.1(2) . . . . ? C36 P3 C33 C35 -158.5(2) . . . . ? Cd2 P3 C33 C35 65.5(2) . . . . ? C32 P4 C39 C40 -174.6(2) . . . . ? C42 P4 C39 C40 -65.0(3) . . . . ? Cd2 P4 C39 C40 71.2(3) . . . . ? C32 P4 C39 C41 63.5(3) . . . . ? C42 P4 C39 C41 173.1(2) . . . . ? Cd2 P4 C39 C41 -50.7(3) . . . . ? N4 C31 C32 P4 57.2(3) . . . . ? C42 P4 C32 C31 76.8(2) . . . . ? C39 P4 C32 C31 -170.8(2) . . . . ? Cd2 P4 C32 C31 -45.9(2) . . . . ? Si2 N3 C23 C25 -126.6(3) . . . . ? Cd2 N3 C23 C25 53.9(4) . . . . ? Si2 N3 C23 C24 114.0(3) . . . . ? Cd2 N3 C23 C24 -65.5(3) . . . . ? Si2 N3 C23 C26 -5.9(4) . . . . ? Cd2 N3 C23 C26 174.6(2) . . . . ? Si1 N1 C1 C3 104.9(3) . . . . ? Cd1 N1 C1 C3 -59.4(3) . . . . ? Si1 N1 C1 C2 -135.9(3) . . . . ? Cd1 N1 C1 C2 59.9(3) . . . . ? Si1 N1 C1 C4 -15.1(4) . . . . ? Cd1 N1 C1 C4 -179.4(2) . . . . ? C10 P2 C20 C22 -176.2(3) . . . . ? C17 P2 C20 C22 71.3(3) . . . . ? Cd1 P2 C20 C22 -60.5(3) . . . . ? C10 P2 C20 C21 56.0(3) . . . . ? C17 P2 C20 C21 -56.4(3) . . . . ? Cd1 P2 C20 C21 171.7(2) . . . . ? C11 P1 C8 C7 169.0(2) . . . . ? C14 P1 C8 C7 -79.0(2) . . . . ? Cd1 P1 C8 C7 43.8(2) . . . . ? C17 P2 C10 C9 -86.5(2) . . . . ? C20 P2 C10 C9 161.9(2) . . . . ? Cd1 P2 C10 C9 35.4(2) . . . . ? C7 N2 C9 C10 -78.7(3) . . . . ? Si1 N2 C9 C10 133.3(2) . . . . ? P2 C10 C9 N2 -56.9(3) . . . . ? C8 P1 C11 C13 -66.5(3) . . . . ? C14 P1 C11 C13 -176.1(2) . . . . ? Cd1 P1 C11 C13 48.3(3) . . . . ? C8 P1 C11 C12 171.3(2) . . . . ? C14 P1 C11 C12 61.8(3) . . . . ? Cd1 P1 C11 C12 -73.9(2) . . . . ? C9 N2 C7 C8 152.6(2) . . . . ? Si1 N2 C7 C8 -62.2(3) . . . . ? P1 C8 C7 N2 -53.8(3) . . . . ? C10 P2 C17 C19 170.2(2) . . . . ? C20 P2 C17 C19 -81.8(3) . . . . ? Cd1 P2 C17 C19 53.7(3) . . . . ? C10 P2 C17 C18 48.4(3) . . . . ? C20 P2 C17 C18 156.4(2) . . . . ? Cd1 P2 C17 C18 -68.1(3) . . . . ? C8 P1 C14 C15 -62.7(3) . . . . ? C11 P1 C14 C15 45.9(3) . . . . ? Cd1 P1 C14 C15 -177.20(19) . . . . ? C8 P1 C14 C16 168.0(2) . . . . ? C11 P1 C14 C16 -83.5(2) . . . . ? Cd1 P1 C14 C16 53.5(2) . . . . ? C33 P3 C30 C29 87.8(2) . . . . ? C36 P3 C30 C29 -160.5(2) . . . . ? Cd2 P3 C30 C29 -32.6(2) . . . . ? C31 N4 C29 C30 78.2(3) . . . . ? Si2 N4 C29 C30 -132.1(2) . . . . ? P3 C30 C29 N4 53.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 34.02 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.580 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.075 #===end # Attachment '70167X.cif' data_sgm3131 _database_code_depnum_ccdc_archive 'CCDC 701678' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H51 Cl2 Ga N2 P2 Si' _chemical_formula_sum 'C22 H51 Cl2 Ga N2 P2 Si' _chemical_formula_weight 574.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 '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 -0.0031 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0833 0.0850 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1013 0.1134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1408 0.1896 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.1009 1.8770 '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 7.9503(7) _cell_length_b 13.2103(12) _cell_length_c 15.7869(15) _cell_angle_alpha 109.305(2) _cell_angle_beta 91.043(2) _cell_angle_gamma 96.357(2) _cell_volume 1552.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 8274 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 33.70 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 1.526 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.665 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type ? _diffrn_radiation_source 'Beamline 11.3.1 ALS' _diffrn_radiation_monochromator mirrors _diffrn_measurement_device_type syncrotron _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 27092 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 33.71 _reflns_number_total 9477 _reflns_number_gt 8748 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'Bruker SAINT v7.23a' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+0.2144P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9477 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1178 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.066089(18) 0.300084(12) 0.160639(10) 0.02584(6) Uani 1 1 d . . . Cl1 Cl -0.04923(5) 0.45235(3) 0.18793(3) 0.03476(9) Uani 1 1 d . . . Cl2 Cl -0.14081(5) 0.18231(4) 0.06952(3) 0.04514(11) Uani 1 1 d . . . P1 P 0.58598(6) 0.73011(3) 0.29696(3) 0.03863(10) Uani 1 1 d . . . P2 P 0.26846(5) 0.28449(3) 0.04796(2) 0.02713(8) Uani 1 1 d . . . Si1 Si 0.26146(5) 0.37180(4) 0.33073(3) 0.03134(10) Uani 1 1 d . . . N1 N 0.35389(15) 0.41866(10) 0.24903(8) 0.0279(2) Uani 1 1 d . . . N2 N 0.12039(16) 0.26658(11) 0.26395(9) 0.0306(2) Uani 1 1 d . . . C1 C -0.1702(3) 0.2181(2) 0.30377(19) 0.0613(6) Uani 1 1 d . . . H1A H -0.1679 0.2914 0.3468 0.092 Uiso 1 1 calc R . . H1B H -0.2401 0.1670 0.3256 0.092 Uiso 1 1 calc R . . H1C H -0.2183 0.2153 0.2453 0.092 Uiso 1 1 calc R . . C2 C 0.0118(3) 0.07335(16) 0.22692(16) 0.0544(5) Uani 1 1 d . . . H2A H 0.1286 0.0557 0.2216 0.082 Uiso 1 1 calc R . . H2B H -0.0352 0.0696 0.1680 0.082 Uiso 1 1 calc R . . H2C H -0.0571 0.0215 0.2484 0.082 Uiso 1 1 calc R . . C3 C 0.0764(4) 0.1865(2) 0.38480(16) 0.0632(6) Uani 1 1 d . . . H3A H 0.1922 0.1671 0.3803 0.095 Uiso 1 1 calc R . . H3B H 0.0030 0.1333 0.4027 0.095 Uiso 1 1 calc R . . H3C H 0.0763 0.2583 0.4299 0.095 Uiso 1 1 calc R . . C4 C 0.0105(2) 0.18766(16) 0.29368(13) 0.0418(4) Uani 1 1 d . . . C5 C 0.4312(3) 0.3361(2) 0.39510(14) 0.0524(5) Uani 1 1 d . . . H5A H 0.4529 0.3918 0.4545 0.079 Uiso 1 1 calc R . . H5B H 0.5352 0.3315 0.3624 0.079 Uiso 1 1 calc R . . H5C H 0.3945 0.2661 0.4022 0.079 Uiso 1 1 calc R . . C6 C 0.1641(3) 0.48276(17) 0.41251(13) 0.0494(4) Uani 1 1 d . . . H6A H 0.0703 0.5020 0.3821 0.059 Uiso 1 1 calc R . . H6B H 0.2495 0.5460 0.4372 0.059 Uiso 1 1 calc R . . H6C H 0.1210 0.4588 0.4614 0.059 Uiso 1 1 calc R . . C7 C 0.3760(2) 0.53305(12) 0.25737(11) 0.0322(3) Uani 1 1 d . . . H7A H 0.2746 0.5655 0.2840 0.039 Uiso 1 1 calc R . . H7B H 0.3819 0.5384 0.1964 0.039 Uiso 1 1 calc R . . C8 C 0.5330(2) 0.59944(12) 0.31429(11) 0.0345(3) Uani 1 1 d . . . H8A H 0.6305 0.5574 0.2991 0.041 Uiso 1 1 calc R . . H8B H 0.5134 0.6125 0.3786 0.041 Uiso 1 1 calc R . . C9 C 0.48483(17) 0.35675(12) 0.20042(10) 0.0283(3) Uani 1 1 d . . . H9A H 0.4708 0.2842 0.2066 0.034 Uiso 1 1 calc R . . H9B H 0.5977 0.3935 0.2280 0.034 Uiso 1 1 calc R . . C10 C 0.47794(18) 0.34410(12) 0.10050(10) 0.0300(3) Uani 1 1 d . . . H10A H 0.5634 0.2975 0.0700 0.036 Uiso 1 1 calc R . . H10B H 0.5059 0.4158 0.0936 0.036 Uiso 1 1 calc R . . C11 C 0.4019(4) 0.80137(19) 0.34830(17) 0.0610(6) Uani 1 1 d . . . H11A H 0.3004 0.7484 0.3194 0.073 Uiso 1 1 calc R . . C12 C 0.3845(3) 0.8230(2) 0.44626(19) 0.0681(7) Uani 1 1 d . . . H12A H 0.2842 0.8598 0.4650 0.102 Uiso 1 1 calc R . . H12B H 0.4857 0.8690 0.4799 0.102 Uiso 1 1 calc R . . H12C H 0.3724 0.7545 0.4583 0.102 Uiso 1 1 calc R . . C13 C 0.3769(6) 0.8976(3) 0.3230(3) 0.1087(14) Uani 1 1 d . . . H13A H 0.2786 0.9297 0.3523 0.163 Uiso 1 1 calc R . . H13B H 0.3572 0.8759 0.2576 0.163 Uiso 1 1 calc R . . H13C H 0.4782 0.9508 0.3423 0.163 Uiso 1 1 calc R . . C14 C 0.7630(2) 0.78920(14) 0.38340(12) 0.0410(4) Uani 1 1 d . . . H14A H 0.7203 0.7908 0.4430 0.049 Uiso 1 1 calc R . . C15 C 0.8254(5) 0.9043(2) 0.3891(2) 0.0857(10) Uani 1 1 d . . . H15A H 0.9188 0.9338 0.4352 0.129 Uiso 1 1 calc R . . H15B H 0.7324 0.9488 0.4051 0.129 Uiso 1 1 calc R . . H15C H 0.8654 0.9045 0.3308 0.129 Uiso 1 1 calc R . . C16 C 0.9069(3) 0.7204(2) 0.36371(18) 0.0637(6) Uani 1 1 d . . . H16A H 0.9992 0.7529 0.4100 0.096 Uiso 1 1 calc R . . H16B H 0.9485 0.7162 0.3047 0.096 Uiso 1 1 calc R . . H16C H 0.8663 0.6476 0.3636 0.096 Uiso 1 1 calc R . . C17 C 0.2266(2) 0.34710(16) -0.03704(11) 0.0405(4) Uani 1 1 d . . . H17A H 0.3178 0.3320 -0.0807 0.049 Uiso 1 1 calc R . . C18 C 0.0572(3) 0.2967(2) -0.08914(15) 0.0559(5) Uani 1 1 d . . . H18A H 0.0372 0.3311 -0.1341 0.084 Uiso 1 1 calc R . . H18B H -0.0342 0.3076 -0.0474 0.084 Uiso 1 1 calc R . . H18C H 0.0599 0.2191 -0.1193 0.084 Uiso 1 1 calc R . . C19 C 0.2332(3) 0.46941(17) 0.00468(14) 0.0458(4) Uani 1 1 d . . . H19A H 0.2104 0.5001 -0.0424 0.069 Uiso 1 1 calc R . . H19B H 0.3459 0.5002 0.0338 0.069 Uiso 1 1 calc R . . H19C H 0.1475 0.4866 0.0494 0.069 Uiso 1 1 calc R . . C20 C 0.2808(2) 0.14088(14) -0.01069(11) 0.0377(3) Uani 1 1 d . . . H20A H 0.1633 0.1055 -0.0334 0.045 Uiso 1 1 calc R . . C21 C 0.3905(3) 0.11952(19) -0.09093(13) 0.0541(5) Uani 1 1 d . . . H21A H 0.3918 0.0415 -0.1190 0.081 Uiso 1 1 calc R . . H21D H 0.5064 0.1545 -0.0709 0.081 Uiso 1 1 calc R . . H21B H 0.3442 0.1488 -0.1347 0.081 Uiso 1 1 calc R . . C22 C 0.3421(2) 0.09045(13) 0.05691(13) 0.0417(4) Uani 1 1 d . . . H22D H 0.3490 0.0134 0.0261 0.063 Uiso 1 1 calc R . . H22A H 0.2622 0.0988 0.1046 0.063 Uiso 1 1 calc R . . H22B H 0.4544 0.1268 0.0833 0.063 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 Ga1 0.02179(9) 0.02858(9) 0.02890(9) 0.01140(6) 0.00186(6) 0.00479(6) Cl1 0.02973(17) 0.03564(18) 0.04298(19) 0.01582(15) 0.00518(14) 0.01226(13) Cl2 0.03141(19) 0.0448(2) 0.0527(2) 0.01134(18) -0.01037(17) -0.00469(16) P1 0.0498(3) 0.03122(19) 0.0331(2) 0.01127(15) -0.00361(17) -0.00322(17) P2 0.02545(17) 0.03162(18) 0.02564(16) 0.00969(13) 0.00267(12) 0.00862(13) Si1 0.02788(19) 0.0404(2) 0.02539(18) 0.01039(16) 0.00113(14) 0.00468(16) N1 0.0245(5) 0.0263(5) 0.0307(6) 0.0070(4) 0.0028(4) 0.0027(4) N2 0.0291(6) 0.0339(6) 0.0323(6) 0.0166(5) 0.0022(5) 0.0009(5) C1 0.0394(10) 0.0797(16) 0.0772(15) 0.0435(13) 0.0211(10) 0.0027(10) C2 0.0640(13) 0.0390(9) 0.0664(13) 0.0289(9) 0.0052(10) -0.0037(9) C3 0.0763(16) 0.0735(15) 0.0532(12) 0.0429(12) 0.0053(11) -0.0024(12) C4 0.0389(8) 0.0466(9) 0.0478(9) 0.0277(8) 0.0083(7) 0.0007(7) C5 0.0402(9) 0.0842(15) 0.0391(9) 0.0290(10) -0.0058(7) 0.0086(9) C6 0.0523(11) 0.0535(10) 0.0353(8) 0.0039(7) 0.0128(8) 0.0087(8) C7 0.0307(7) 0.0259(6) 0.0366(7) 0.0065(5) -0.0028(6) 0.0021(5) C8 0.0357(7) 0.0290(6) 0.0362(7) 0.0099(5) -0.0059(6) -0.0026(6) C9 0.0218(6) 0.0311(6) 0.0316(6) 0.0100(5) 0.0007(5) 0.0035(5) C10 0.0231(6) 0.0345(7) 0.0339(7) 0.0131(5) 0.0059(5) 0.0048(5) C11 0.0697(15) 0.0472(11) 0.0614(13) 0.0082(9) -0.0085(11) 0.0213(10) C12 0.0543(13) 0.0675(15) 0.0740(16) 0.0092(12) 0.0142(12) 0.0155(11) C13 0.123(3) 0.085(2) 0.142(4) 0.057(2) 0.021(3) 0.047(2) C14 0.0452(9) 0.0353(8) 0.0364(8) 0.0084(6) -0.0003(7) -0.0086(7) C15 0.100(2) 0.0463(13) 0.100(2) 0.0264(13) -0.0280(19) -0.0334(14) C16 0.0402(10) 0.0663(14) 0.0636(13) -0.0034(11) -0.0048(10) -0.0014(9) C17 0.0407(8) 0.0576(10) 0.0315(7) 0.0225(7) 0.0066(6) 0.0168(7) C18 0.0592(12) 0.0695(13) 0.0434(10) 0.0251(10) -0.0149(9) 0.0101(10) C19 0.0468(10) 0.0535(10) 0.0524(10) 0.0352(9) 0.0071(8) 0.0146(8) C20 0.0353(8) 0.0359(7) 0.0354(7) 0.0014(6) -0.0008(6) 0.0107(6) C21 0.0616(12) 0.0605(12) 0.0362(9) 0.0037(8) 0.0092(8) 0.0289(10) C22 0.0452(9) 0.0292(7) 0.0501(10) 0.0102(7) 0.0045(7) 0.0105(6) _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 Ga1 N2 1.8805(13) . ? Ga1 Cl1 2.2185(4) . ? Ga1 Cl2 2.2501(4) . ? Ga1 P2 2.3938(4) . ? Ga1 Si1 2.8916(5) . ? P1 C8 1.8404(16) . ? P1 C14 1.8533(18) . ? P1 C11 1.879(3) . ? P2 C10 1.8191(15) . ? P2 C20 1.8301(17) . ? P2 C17 1.8368(17) . ? Si1 N2 1.7159(14) . ? Si1 N1 1.7459(13) . ? Si1 C6 1.8576(19) . ? Si1 C5 1.8668(19) . ? N1 C7 1.4630(19) . ? N1 C9 1.4643(18) . ? N2 C4 1.486(2) . ? C1 C4 1.531(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.531(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.527(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.526(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.530(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C13 1.485(4) . ? C11 C12 1.489(4) . ? C11 H11A 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.513(3) . ? C14 C15 1.519(3) . ? C14 H14A 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.524(3) . ? C17 C18 1.527(3) . ? C17 H17A 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.518(3) . ? C20 C22 1.531(3) . ? C20 H20A 1.0000 . ? C21 H21A 0.9800 . ? C21 H21D 0.9800 . ? C21 H21B 0.9800 . ? C22 H22D 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? 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 Ga1 Cl1 114.38(4) . . ? N2 Ga1 Cl2 113.47(4) . . ? Cl1 Ga1 Cl2 99.987(18) . . ? N2 Ga1 P2 119.40(4) . . ? Cl1 Ga1 P2 110.560(15) . . ? Cl2 Ga1 P2 95.879(18) . . ? N2 Ga1 Si1 34.59(4) . . ? Cl1 Ga1 Si1 94.464(15) . . ? Cl2 Ga1 Si1 147.687(17) . . ? P2 Ga1 Si1 105.883(15) . . ? C8 P1 C14 99.28(8) . . ? C8 P1 C11 100.53(11) . . ? C14 P1 C11 104.26(10) . . ? C10 P2 C20 106.93(7) . . ? C10 P2 C17 106.89(8) . . ? C20 P2 C17 107.84(9) . . ? C10 P2 Ga1 109.99(5) . . ? C20 P2 Ga1 108.47(6) . . ? C17 P2 Ga1 116.32(6) . . ? N2 Si1 N1 100.07(6) . . ? N2 Si1 C6 115.09(9) . . ? N1 Si1 C6 109.22(9) . . ? N2 Si1 C5 116.52(9) . . ? N1 Si1 C5 108.92(8) . . ? C6 Si1 C5 106.63(11) . . ? N2 Si1 Ga1 38.47(4) . . ? N1 Si1 Ga1 65.87(4) . . ? C6 Si1 Ga1 109.33(7) . . ? C5 Si1 Ga1 143.21(8) . . ? C7 N1 C9 114.64(12) . . ? C7 N1 Si1 122.69(10) . . ? C9 N1 Si1 115.16(10) . . ? C4 N2 Si1 126.47(11) . . ? C4 N2 Ga1 122.71(11) . . ? Si1 N2 Ga1 106.94(7) . . ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 C3 110.89(16) . . ? N2 C4 C2 110.06(15) . . ? C3 C4 C2 106.84(18) . . ? N2 C4 C1 110.35(16) . . ? C3 C4 C1 107.66(19) . . ? C2 C4 C1 110.96(19) . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 C8 115.02(13) . . ? N1 C7 H7A 108.5 . . ? C8 C7 H7A 108.5 . . ? N1 C7 H7B 108.5 . . ? C8 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C7 C8 P1 112.62(11) . . ? C7 C8 H8A 109.1 . . ? P1 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? P1 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? N1 C9 C10 112.71(12) . . ? N1 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? N1 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C9 C10 P2 110.85(10) . . ? C9 C10 H10A 109.5 . . ? P2 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? P2 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C13 C11 C12 111.5(3) . . ? C13 C11 P1 114.7(3) . . ? C12 C11 P1 117.00(18) . . ? C13 C11 H11A 103.9 . . ? C12 C11 H11A 103.9 . . ? P1 C11 H11A 103.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C16 C14 C15 110.4(2) . . ? C16 C14 P1 110.66(13) . . ? C15 C14 P1 110.92(17) . . ? C16 C14 H14A 108.3 . . ? C15 C14 H14A 108.3 . . ? P1 C14 H14A 108.3 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 111.19(16) . . ? C19 C17 P2 111.63(12) . . ? C18 C17 P2 110.70(14) . . ? C19 C17 H17A 107.7 . . ? C18 C17 H17A 107.7 . . ? P2 C17 H17A 107.7 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 111.31(15) . . ? C21 C20 P2 113.69(14) . . ? C22 C20 P2 108.84(11) . . ? C21 C20 H20A 107.6 . . ? C22 C20 H20A 107.6 . . ? P2 C20 H20A 107.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21D 109.5 . . ? H21A C21 H21D 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? H21D C21 H21B 109.5 . . ? C20 C22 H22D 109.5 . . ? C20 C22 H22A 109.5 . . ? H22D C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22D C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ga1 P2 C10 -44.95(7) . . . . ? Cl1 Ga1 P2 C10 90.88(5) . . . . ? Cl2 Ga1 P2 C10 -166.12(5) . . . . ? Si1 Ga1 P2 C10 -10.25(6) . . . . ? N2 Ga1 P2 C20 71.67(7) . . . . ? Cl1 Ga1 P2 C20 -152.49(6) . . . . ? Cl2 Ga1 P2 C20 -49.50(6) . . . . ? Si1 Ga1 P2 C20 106.37(6) . . . . ? N2 Ga1 P2 C17 -166.62(9) . . . . ? Cl1 Ga1 P2 C17 -30.78(8) . . . . ? Cl2 Ga1 P2 C17 72.21(8) . . . . ? Si1 Ga1 P2 C17 -131.92(7) . . . . ? Cl1 Ga1 Si1 N2 128.04(8) . . . . ? Cl2 Ga1 Si1 N2 11.37(8) . . . . ? P2 Ga1 Si1 N2 -119.10(7) . . . . ? N2 Ga1 Si1 N1 150.67(9) . . . . ? Cl1 Ga1 Si1 N1 -81.29(5) . . . . ? Cl2 Ga1 Si1 N1 162.04(5) . . . . ? P2 Ga1 Si1 N1 31.57(5) . . . . ? N2 Ga1 Si1 C6 -106.32(11) . . . . ? Cl1 Ga1 Si1 C6 21.72(8) . . . . ? Cl2 Ga1 Si1 C6 -94.95(8) . . . . ? P2 Ga1 Si1 C6 134.58(8) . . . . ? N2 Ga1 Si1 C5 61.02(14) . . . . ? Cl1 Ga1 Si1 C5 -170.94(12) . . . . ? Cl2 Ga1 Si1 C5 72.39(13) . . . . ? P2 Ga1 Si1 C5 -58.08(12) . . . . ? N2 Si1 N1 C7 131.98(12) . . . . ? C6 Si1 N1 C7 10.78(14) . . . . ? C5 Si1 N1 C7 -105.32(14) . . . . ? Ga1 Si1 N1 C7 113.95(12) . . . . ? N2 Si1 N1 C9 -79.96(11) . . . . ? C6 Si1 N1 C9 158.84(11) . . . . ? C5 Si1 N1 C9 42.74(13) . . . . ? Ga1 Si1 N1 C9 -97.99(10) . . . . ? N1 Si1 N2 C4 174.92(14) . . . . ? C6 Si1 N2 C4 -68.19(17) . . . . ? C5 Si1 N2 C4 57.75(17) . . . . ? Ga1 Si1 N2 C4 -158.08(18) . . . . ? N1 Si1 N2 Ga1 -27.00(8) . . . . ? C6 Si1 N2 Ga1 89.90(10) . . . . ? C5 Si1 N2 Ga1 -144.16(9) . . . . ? Cl1 Ga1 N2 C4 99.55(13) . . . . ? Cl2 Ga1 N2 C4 -14.30(14) . . . . ? P2 Ga1 N2 C4 -126.19(12) . . . . ? Si1 Ga1 N2 C4 159.10(18) . . . . ? Cl1 Ga1 N2 Si1 -59.55(7) . . . . ? Cl2 Ga1 N2 Si1 -173.40(5) . . . . ? P2 Ga1 N2 Si1 74.71(7) . . . . ? Si1 N2 C4 C3 -18.8(2) . . . . ? Ga1 N2 C4 C3 -173.64(15) . . . . ? Si1 N2 C4 C2 -136.75(15) . . . . ? Ga1 N2 C4 C2 68.36(19) . . . . ? Si1 N2 C4 C1 100.45(19) . . . . ? Ga1 N2 C4 C1 -54.4(2) . . . . ? C9 N1 C7 C8 -65.48(17) . . . . ? Si1 N1 C7 C8 82.74(16) . . . . ? N1 C7 C8 P1 164.07(11) . . . . ? C14 P1 C8 C7 174.59(12) . . . . ? C11 P1 C8 C7 68.08(14) . . . . ? C7 N1 C9 C10 -67.99(15) . . . . ? Si1 N1 C9 C10 141.34(10) . . . . ? N1 C9 C10 P2 -55.19(14) . . . . ? C20 P2 C10 C9 -99.98(12) . . . . ? C17 P2 C10 C9 144.74(11) . . . . ? Ga1 P2 C10 C9 17.60(12) . . . . ? C8 P1 C11 C13 -163.1(3) . . . . ? C14 P1 C11 C13 94.4(3) . . . . ? C8 P1 C11 C12 63.5(2) . . . . ? C14 P1 C11 C12 -39.0(2) . . . . ? C8 P1 C14 C16 61.34(17) . . . . ? C11 P1 C14 C16 164.79(17) . . . . ? C8 P1 C14 C15 -175.8(2) . . . . ? C11 P1 C14 C15 -72.3(2) . . . . ? C10 P2 C17 C19 -59.15(14) . . . . ? C20 P2 C17 C19 -173.82(13) . . . . ? Ga1 P2 C17 C19 64.14(14) . . . . ? C10 P2 C17 C18 176.41(14) . . . . ? C20 P2 C17 C18 61.74(16) . . . . ? Ga1 P2 C17 C18 -60.30(16) . . . . ? C10 P2 C20 C21 -67.87(15) . . . . ? C17 P2 C20 C21 46.78(16) . . . . ? Ga1 P2 C20 C21 173.55(12) . . . . ? C10 P2 C20 C22 56.82(14) . . . . ? C17 P2 C20 C22 171.47(12) . . . . ? Ga1 P2 C20 C22 -61.76(13) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 33.71 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.306 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.076