Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Raithby, P.' 'Ahrens, Birte' 'Al-Mandhary, Muna R. A.' 'Al-Suti, Mohammed K.' 'Feeder, Neil' 'Friend, Richard' 'Hisahm, Abdul Khader' 'Khan, Muhammad S.' 'Kohler, Anna' 'Mahon, M.' 'Male, Louise' 'Marseglia, Elisabeth A.' 'Teat, Simon J.' 'Tedesco, Emilio' _publ_contact_author_name 'Prof P Raithby' _publ_contact_author_address ; Department of Chemistry Sultan Qaboos University UNITED ARAB EMIRATES ; _publ_contact_author_email 'P.R.RAITHBY@BATH.AC.UK' _publ_section_title ; Structual characterisation of acetylide - functionalised oligopyridines and the synthesis, characterisation and optical spectroscopy of platinum di-ynes containing oligopyridyl linker groups in the backbone ; data_pr9819 _database_code_CSD 174647 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Compound 2a ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H24 N2 Si2' _chemical_formula_weight 348.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.024(3) _cell_length_b 10.645(4) _cell_length_c 17.768(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.68(3) _cell_angle_gamma 90.00 _cell_volume 2082.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 1.556 _exptl_absorpt_correction_type 'Semi-empirical based on psi scans' _exptl_absorpt_correction_T_min 0.5750 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe 4 circle diffractometer' _diffrn_measurement_method 'omega/2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4267 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.01 _diffrn_reflns_theta_max 55.09 _reflns_number_total 2016 _reflns_number_gt 1773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe XRD software' _computing_cell_refinement 'Stoe XRD software' _computing_data_reduction 'Stoe XRD software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (J. Barbour, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0894P)^2^+1.2719P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2016 _refine_ls_number_parameters 223 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1417 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.085 _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 N1 N 0.4759(3) 0.6438(2) 0.94784(13) 0.0238(8) Uani 1 1 d . . . Si1 Si 0.48833(10) 1.07186(8) 0.80395(5) 0.0340(4) Uani 1 1 d D . . C1 C 0.5074(5) 1.1971(3) 0.8755(2) 0.0591(14) Uani 1 1 d D . . H1A H 0.4313 1.2082 0.9011 0.089 Uiso 1 1 calc R . . H1B H 0.5289 1.2759 0.8510 0.089 Uiso 1 1 calc R . . H1C H 0.5722 1.1736 0.9125 0.089 Uiso 1 1 calc R . . C2 C 0.6331(4) 1.0349(4) 0.7591(2) 0.0523(13) Uani 1 1 d D . . H2A H 0.6922 1.0030 0.7974 0.078 Uiso 1 1 calc R . . H2B H 0.6650 1.1111 0.7364 0.078 Uiso 1 1 calc R . . H2C H 0.6184 0.9710 0.7201 0.078 Uiso 1 1 calc R . . C3 C 0.3702(4) 1.1170(4) 0.7317(2) 0.0576(13) Uani 1 1 d D . . H3A H 0.3600 1.0494 0.6945 0.086 Uiso 1 1 calc R . . H3B H 0.3948 1.1942 0.7066 0.086 Uiso 1 1 calc R . . H3C H 0.2932 1.1311 0.7558 0.086 Uiso 1 1 calc R . . C4 C 0.4418(3) 0.9262(3) 0.85157(18) 0.0310(10) Uani 1 1 d . . . C5 C 0.4164(3) 0.8307(3) 0.88250(17) 0.0257(9) Uani 1 1 d . . . C6 C 0.3837(3) 0.7156(3) 0.92111(17) 0.0253(10) Uani 1 1 d . . . C7 C 0.4483(3) 0.5388(3) 0.98538(17) 0.0240(9) Uani 1 1 d . . . C8 C 0.3292(3) 0.5066(3) 0.9981(2) 0.0360(12) Uani 1 1 d . . . H8 H 0.3120 0.4337 1.0266 0.043 Uiso 1 1 calc R . . C9 C 0.2357(4) 0.5810(3) 0.9693(2) 0.0375(11) Uani 1 1 d . . . H9 H 0.1536 0.5590 0.9768 0.045 Uiso 1 1 calc R . . C10 C 0.2627(3) 0.6873(3) 0.92954(18) 0.0271(10) Uani 1 1 d . . . H10 H 0.2002 0.7397 0.9085 0.033 Uiso 1 1 calc R . . N11 N 0.9749(3) 0.8483(2) 0.95721(14) 0.0244(8) Uani 1 1 d . A . Si11 Si 0.96298(11) 0.40758(9) 0.82066(6) 0.0401(4) Uani 0.50 1 d PD A 1 C11 C 0.9334(10) 0.4295(10) 0.7200(5) 0.066(3) Uiso 0.50 1 d PD A 1 H11A H 0.8467 0.4457 0.7098 0.098 Uiso 0.50 1 calc PR A 1 H11B H 0.9569 0.3535 0.6931 0.098 Uiso 0.50 1 calc PR A 1 H11C H 0.9806 0.5011 0.7028 0.098 Uiso 0.50 1 calc PR A 1 C12 C 1.1186(8) 0.3479(9) 0.8409(5) 0.054(3) Uiso 0.50 1 d PD A 1 H12A H 1.1774 0.4138 0.8303 0.081 Uiso 0.50 1 calc PR A 1 H12B H 1.1328 0.2747 0.8090 0.081 Uiso 0.50 1 calc PR A 1 H12C H 1.1279 0.3235 0.8940 0.081 Uiso 0.50 1 calc PR A 1 C13 C 0.8536(8) 0.2875(8) 0.8581(5) 0.053(2) Uiso 0.50 1 d PD A 1 H13A H 0.8598 0.2089 0.8298 0.079 Uiso 0.50 1 calc PR A 1 H13B H 0.7704 0.3198 0.8524 0.079 Uiso 0.50 1 calc PR A 1 H13C H 0.8741 0.2717 0.9116 0.079 Uiso 0.50 1 calc PR A 1 Si1' Si 0.96298(11) 0.40758(9) 0.82066(6) 0.0401(4) Uani 0.50 1 d PD A 2 C1' C 0.9885(11) 0.4565(9) 0.7215(5) 0.064(3) Uiso 0.50 1 d PD A 2 H1D H 0.9163 0.5003 0.7006 0.095 Uiso 0.50 1 calc PR A 2 H1E H 1.0038 0.3820 0.6910 0.095 Uiso 0.50 1 calc PR A 2 H1F H 1.0587 0.5128 0.7209 0.095 Uiso 0.50 1 calc PR A 2 C2' C 1.1028(8) 0.3299(9) 0.8640(5) 0.045(2) Uiso 0.50 1 d PD A 2 H2D H 1.1730 0.3851 0.8589 0.068 Uiso 0.50 1 calc PR A 2 H2E H 1.1168 0.2502 0.8382 0.068 Uiso 0.50 1 calc PR A 2 H2F H 1.0913 0.3138 0.9175 0.068 Uiso 0.50 1 calc PR A 2 C3' C 0.8266(9) 0.3095(9) 0.8220(5) 0.061(3) Uiso 0.50 1 d PD A 2 H3D H 0.8338 0.2395 0.7866 0.091 Uiso 0.50 1 calc PR A 2 H3E H 0.7551 0.3601 0.8071 0.091 Uiso 0.50 1 calc PR A 2 H3F H 0.8178 0.2764 0.8729 0.091 Uiso 0.50 1 calc PR A 2 C14 C 0.9363(3) 0.5569(3) 0.87039(19) 0.0327(10) Uani 1 1 d . . . C15 C 0.9133(3) 0.6558(3) 0.89874(17) 0.0251(9) Uani 1 1 d . A . C16 C 0.8816(3) 0.7758(3) 0.93197(17) 0.0249(10) Uani 1 1 d . . . C17 C 0.9476(3) 0.9605(3) 0.98708(18) 0.0253(9) Uani 1 1 d . . . C18 C 0.8287(3) 0.9999(3) 0.9943(2) 0.0345(12) Uani 1 1 d . A . H18 H 0.8125 1.0786 1.0170 0.041 Uiso 1 1 calc R . . C19 C 0.7346(4) 0.9245(3) 0.9683(2) 0.0354(10) Uani 1 1 d . . . H19 H 0.6528 0.9505 0.9726 0.043 Uiso 1 1 calc R A . C20 C 0.7608(3) 0.8100(3) 0.93580(18) 0.0278(10) Uani 1 1 d . A . H20 H 0.6977 0.7565 0.9167 0.033 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 N1 0.026(2) 0.0204(14) 0.0245(14) 0.0010(12) 0.0004(16) -0.0010(14) Si1 0.0390(8) 0.0288(6) 0.0338(6) 0.0098(4) -0.0031(6) -0.0052(5) C1 0.081(4) 0.042(2) 0.055(2) -0.0034(19) 0.007(3) -0.012(2) C2 0.053(3) 0.054(2) 0.051(2) 0.0081(19) 0.010(3) -0.008(2) C3 0.053(4) 0.062(3) 0.056(3) 0.027(2) -0.012(3) -0.005(2) C4 0.030(3) 0.030(2) 0.0322(18) 0.0047(15) -0.005(2) 0.0006(17) C5 0.022(2) 0.0246(18) 0.0302(17) 0.0017(15) -0.0046(19) 0.0046(16) C6 0.034(3) 0.0196(17) 0.0227(16) -0.0002(13) 0.002(2) 0.0019(17) C7 0.025(2) 0.0218(16) 0.0251(17) 0.0012(14) -0.001(2) -0.0002(14) C8 0.027(3) 0.0302(19) 0.051(2) 0.0160(17) 0.001(3) 0.000(2) C9 0.022(3) 0.038(2) 0.052(2) 0.0098(18) 0.003(2) -0.0020(19) C10 0.023(3) 0.0263(17) 0.0310(17) 0.0006(15) -0.004(2) 0.0082(17) N11 0.025(2) 0.0208(14) 0.0270(14) -0.0035(12) 0.0000(15) -0.0030(14) Si11 0.0410(8) 0.0315(6) 0.0480(7) -0.0188(4) 0.0059(7) -0.0014(5) Si1' 0.0410(8) 0.0315(6) 0.0480(7) -0.0188(4) 0.0059(7) -0.0014(5) C14 0.029(3) 0.033(2) 0.0362(18) -0.0051(16) 0.000(2) -0.0046(17) C15 0.021(2) 0.0251(18) 0.0288(17) -0.0026(15) -0.0048(19) -0.0069(16) C16 0.029(3) 0.0214(17) 0.0246(16) -0.0007(14) 0.001(2) -0.0049(17) C17 0.026(2) 0.0219(17) 0.0280(18) -0.0021(14) 0.000(2) -0.0038(15) C18 0.027(3) 0.0252(18) 0.051(2) -0.0140(17) -0.003(3) -0.0032(19) C19 0.022(3) 0.0326(19) 0.051(2) -0.0067(17) -0.004(2) 0.0028(18) C20 0.024(3) 0.0253(17) 0.0335(18) -0.0003(14) -0.007(2) -0.0093(17) _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 N1 C6 1.341(4) . ? N1 C7 1.344(4) . ? Si1 C1 1.848(4) . ? Si1 C3 1.848(4) . ? Si1 C4 1.851(3) . ? Si1 C2 1.859(4) . ? C4 C5 1.195(4) . ? C5 C6 1.457(4) . ? C6 C10 1.382(5) . ? C7 C8 1.386(5) . ? C7 C7 1.482(7) 3_667 ? C8 C9 1.380(5) . ? C9 C10 1.374(5) . ? N11 C16 1.346(4) . ? N11 C17 1.346(4) . ? Si11 C11 1.818(8) . ? Si11 C12 1.849(8) . ? Si11 C14 1.849(3) . ? Si11 C13 1.899(7) . ? C14 C15 1.199(4) . ? C15 C16 1.457(4) . ? C16 C20 1.386(5) . ? C17 C18 1.387(5) . ? C17 C17 1.485(7) 3_777 ? C18 C19 1.375(5) . ? C19 C20 1.384(5) . ? 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 C6 N1 C7 117.7(3) . . ? C1 Si1 C3 110.1(2) . . ? C1 Si1 C4 108.36(16) . . ? C3 Si1 C4 109.49(19) . . ? C1 Si1 C2 112.0(2) . . ? C3 Si1 C2 110.4(2) . . ? C4 Si1 C2 106.27(16) . . ? C5 C4 Si1 177.5(3) . . ? C4 C5 C6 178.9(3) . . ? N1 C6 C10 123.8(3) . . ? N1 C6 C5 116.4(3) . . ? C10 C6 C5 119.7(3) . . ? N1 C7 C8 121.7(3) . . ? N1 C7 C7 116.7(4) . 3_667 ? C8 C7 C7 121.5(3) . 3_667 ? C9 C8 C7 119.6(3) . . ? C10 C9 C8 119.2(3) . . ? C9 C10 C6 118.0(4) . . ? C16 N11 C17 117.3(3) . . ? C11 Si11 C12 110.9(5) . . ? C11 Si11 C14 109.6(3) . . ? C12 Si11 C14 111.7(3) . . ? C11 Si11 C13 110.1(5) . . ? C12 Si11 C13 107.4(4) . . ? C14 Si11 C13 107.1(3) . . ? C15 C14 Si11 175.5(4) . . ? C14 C15 C16 178.2(4) . . ? N11 C16 C20 123.7(3) . . ? N11 C16 C15 116.4(3) . . ? C20 C16 C15 120.0(3) . . ? N11 C17 C18 122.3(3) . . ? N11 C17 C17 116.1(4) . 3_777 ? C18 C17 C17 121.6(3) . 3_777 ? C19 C18 C17 119.6(3) . . ? C18 C19 C20 119.0(3) . . ? C19 C20 C16 118.1(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 C1 Si1 C4 C5 -96(7) . . . . ? C3 Si1 C4 C5 144(7) . . . . ? C2 Si1 C4 C5 25(7) . . . . ? Si1 C4 C5 C6 139(19) . . . . ? C7 N1 C6 C10 -0.5(4) . . . . ? C7 N1 C6 C5 178.3(3) . . . . ? C4 C5 C6 N1 -132(23) . . . . ? C4 C5 C6 C10 47(23) . . . . ? C6 N1 C7 C8 -1.7(5) . . . . ? C6 N1 C7 C7 -179.8(3) . . . 3_667 ? N1 C7 C8 C9 2.6(5) . . . . ? C7 C7 C8 C9 -179.4(4) 3_667 . . . ? C7 C8 C9 C10 -1.2(5) . . . . ? C8 C9 C10 C6 -0.8(5) . . . . ? N1 C6 C10 C9 1.7(5) . . . . ? C5 C6 C10 C9 -177.0(3) . . . . ? C11 Si11 C14 C15 29(4) . . . . ? C12 Si11 C14 C15 152(4) . . . . ? C13 Si11 C14 C15 -91(4) . . . . ? Si11 C14 C15 C16 25(13) . . . . ? C17 N11 C16 C20 -0.6(4) . . . . ? C17 N11 C16 C15 179.0(3) . . . . ? C14 C15 C16 N11 -159(10) . . . . ? C14 C15 C16 C20 21(10) . . . . ? C16 N11 C17 C18 2.0(4) . . . . ? C16 N11 C17 C17 -178.7(3) . . . 3_777 ? N11 C17 C18 C19 -1.9(5) . . . . ? C17 C17 C18 C19 178.8(4) 3_777 . . . ? C17 C18 C19 C20 0.4(5) . . . . ? C18 C19 C20 C16 0.9(5) . . . . ? N11 C16 C20 C19 -0.9(5) . . . . ? C15 C16 C20 C19 179.5(3) . . . . ? N1 C7 C7 N1 180.000(3) . . 3_667 3_667 ? N11 C17 C17 N11 180.0 . . 3_777 3_777 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C20 H20 N1 0.95 2.80 3.619(4) 144.8 . C8 H8 N1 0.95 2.50 2.812(5) 99.1 3_667 C10 H10 N11 0.95 2.91 3.660(4) 137.0 1_455 C18 H18 N11 0.95 2.49 2.804(5) 99.2 3_777 _diffrn_measured_fraction_theta_max 0.766 _diffrn_reflns_theta_full 55.00 _diffrn_measured_fraction_theta_full 0.767 _refine_diff_density_max 0.289 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.062 ###END data_pr9942 _database_code_CSD 174648 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Compound 3a ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H27 N3 Si2' _chemical_formula_weight 425.68 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' _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 6.3543(8) _cell_length_b 10.844(2) _cell_length_c 17.722(4) _cell_angle_alpha 84.891(8) _cell_angle_beta 86.268(10) _cell_angle_gamma 82.049(10) _cell_volume 1202.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11843 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 0.163 _exptl_absorpt_correction_type SORTAV _exptl_absorpt_correction_T_min 0.9557 _exptl_absorpt_correction_T_max 0.9886 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'not applicable' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7566 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.1355 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.44 _reflns_number_total 5373 _reflns_number_gt 2787 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius HKL Scalepack' _computing_data_reduction 'Nonius HKL Denzo & Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (J. Barbour, 1997)' _computing_publication_material SHELXL-97 _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^)+(0.0444P)^2^] 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 'methyls rigid, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5373 _refine_ls_number_parameters 277 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1393 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1248 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.936 _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 Si1 Si 0.55690(10) 0.25829(7) 0.16878(4) 0.0327(2) Uani 1 1 d . . . Si2 Si 0.14411(11) 1.25859(7) 0.87778(4) 0.0356(2) Uani 1 1 d . . . C1 C 0.4625(4) 0.1048(3) 0.18148(18) 0.0535(8) Uani 1 1 d . . . H1A H 0.5121 0.0607 0.2291 0.080 Uiso 1 1 calc R . . H1B H 0.5183 0.0558 0.1390 0.080 Uiso 1 1 calc R . . H1C H 0.3066 0.1160 0.1832 0.080 Uiso 1 1 calc R . . C2 C 0.5013(4) 0.3361(3) 0.07315(15) 0.0527(8) Uani 1 1 d . . . H2A H 0.3475 0.3480 0.0668 0.079 Uiso 1 1 calc R . . H2B H 0.5733 0.2839 0.0343 0.079 Uiso 1 1 calc R . . H2C H 0.5536 0.4175 0.0679 0.079 Uiso 1 1 calc R . . C3 C 0.8473(4) 0.2386(3) 0.18094(16) 0.0489(8) Uani 1 1 d . . . H3A H 0.9004 0.3192 0.1694 0.073 Uiso 1 1 calc R . . H3B H 0.9194 0.1784 0.1464 0.073 Uiso 1 1 calc R . . H3C H 0.8758 0.2076 0.2334 0.073 Uiso 1 1 calc R . . C4 C 0.4062(4) 0.3577(2) 0.23822(14) 0.0335(6) Uani 1 1 d . . . C5 C 0.2847(4) 0.4201(2) 0.27927(14) 0.0314(6) Uani 1 1 d . . . N1 N 0.1991(3) 0.55682(18) 0.37944(11) 0.0273(5) Uani 1 1 d D . . C6 C 0.1277(3) 0.4943(2) 0.32622(13) 0.0265(6) Uani 1 1 d D . . C7 C -0.0880(3) 0.4984(2) 0.31399(14) 0.0305(6) Uani 1 1 d D . . H7 H -0.1330 0.4507 0.2770 0.037 Uiso 1 1 calc R . . C8 C -0.2340(3) 0.5727(2) 0.35651(13) 0.0292(6) Uani 1 1 d D . . H8 H -0.3819 0.5773 0.3494 0.035 Uiso 1 1 calc R . . C9 C -0.1628(3) 0.6403(2) 0.40949(13) 0.0269(6) Uani 1 1 d D . . H9 H -0.2608 0.6946 0.4381 0.032 Uiso 1 1 calc R . . C10 C 0.0538(3) 0.6283(2) 0.42069(13) 0.0238(6) Uani 1 1 d D . . N2 N 0.0019(3) 0.78126(18) 0.51440(11) 0.0256(5) Uani 1 1 d D . . C11 C 0.1364(3) 0.6925(2) 0.48159(13) 0.0249(6) Uani 1 1 d D . . C12 C 0.3437(3) 0.6567(2) 0.50383(13) 0.0260(6) Uani 1 1 d D . . H12 H 0.4348 0.5934 0.4795 0.031 Uiso 1 1 calc R . . C13 C 0.4146(3) 0.7146(2) 0.56165(13) 0.0302(6) Uani 1 1 d D . . H13 H 0.5553 0.6916 0.5779 0.036 Uiso 1 1 calc R . . C14 C 0.2788(3) 0.8062(2) 0.59556(13) 0.0280(6) Uani 1 1 d D . . H14 H 0.3235 0.8468 0.6359 0.034 Uiso 1 1 calc R . . C15 C 0.0747(3) 0.8384(2) 0.56969(13) 0.0247(6) Uani 1 1 d D . . N3 N 0.0041(3) 0.99868(19) 0.65675(11) 0.0282(5) Uani 1 1 d D . . C16 C -0.0743(3) 0.9403(2) 0.60299(13) 0.0251(6) Uani 1 1 d D . . C17 C -0.2813(3) 0.9727(2) 0.57986(13) 0.0285(6) Uani 1 1 d D . . H17 H -0.3317 0.9305 0.5413 0.034 Uiso 1 1 calc R . . C18 C -0.4123(3) 1.0670(2) 0.61369(14) 0.0311(6) Uani 1 1 d D . . H18 H -0.5550 1.0895 0.5995 0.037 Uiso 1 1 calc R . . C19 C -0.3330(4) 1.1282(2) 0.66848(14) 0.0310(6) Uani 1 1 d D . . H19 H -0.4189 1.1946 0.6918 0.037 Uiso 1 1 calc R . . C20 C -0.1242(3) 1.0903(2) 0.68879(13) 0.0279(6) Uani 1 1 d D . . C21 C -0.0359(4) 1.1497(2) 0.74756(14) 0.0315(6) Uani 1 1 d . . . C22 C 0.0359(4) 1.1953(2) 0.79775(15) 0.0363(7) Uani 1 1 d . . . C23 C 0.4184(4) 1.2904(3) 0.85144(15) 0.0494(8) Uani 1 1 d . . . H23A H 0.5086 1.2121 0.8415 0.074 Uiso 1 1 calc R . . H23B H 0.4738 1.3278 0.8931 0.074 Uiso 1 1 calc R . . H23C H 0.4183 1.3483 0.8057 0.074 Uiso 1 1 calc R . . C24 C -0.0270(4) 1.4043(3) 0.90117(16) 0.0463(8) Uani 1 1 d . . . H24A H -0.0411 1.4623 0.8555 0.069 Uiso 1 1 calc R . . H24B H 0.0376 1.4430 0.9403 0.069 Uiso 1 1 calc R . . H24C H -0.1679 1.3848 0.9201 0.069 Uiso 1 1 calc R . . C25 C 0.1387(5) 1.1395(3) 0.96011(16) 0.0602(9) Uani 1 1 d . . . H25A H -0.0066 1.1194 0.9704 0.090 Uiso 1 1 calc R . . H25B H 0.1860 1.1727 1.0048 0.090 Uiso 1 1 calc R . . H25C H 0.2338 1.0637 0.9484 0.090 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 Si1 0.0358(4) 0.0306(5) 0.0312(5) -0.0101(4) 0.0024(3) 0.0001(3) Si2 0.0417(4) 0.0358(5) 0.0322(5) -0.0127(4) -0.0012(3) -0.0100(4) C1 0.0531(17) 0.038(2) 0.069(2) -0.0128(17) 0.0065(15) -0.0044(14) C2 0.0664(19) 0.053(2) 0.0364(18) -0.0077(16) 0.0001(14) 0.0012(16) C3 0.0388(15) 0.057(2) 0.052(2) -0.0216(17) 0.0038(13) -0.0005(14) C4 0.0319(14) 0.0329(18) 0.0351(16) -0.0066(14) -0.0033(11) 0.0009(12) C5 0.0312(14) 0.0318(17) 0.0323(16) -0.0054(13) -0.0060(11) -0.0036(12) N1 0.0272(11) 0.0258(13) 0.0292(12) -0.0094(10) 0.0012(9) -0.0017(9) C6 0.0285(13) 0.0256(16) 0.0256(14) -0.0063(12) 0.0008(10) -0.0031(11) C7 0.0348(14) 0.0295(17) 0.0298(15) -0.0089(13) -0.0019(11) -0.0096(12) C8 0.0251(12) 0.0322(17) 0.0323(15) -0.0074(13) -0.0015(11) -0.0076(11) C9 0.0257(13) 0.0235(16) 0.0320(15) -0.0089(12) 0.0031(10) -0.0034(11) C10 0.0245(13) 0.0215(15) 0.0257(14) -0.0051(12) 0.0006(10) -0.0035(10) N2 0.0259(10) 0.0216(13) 0.0302(12) -0.0083(10) 0.0029(9) -0.0047(9) C11 0.0262(13) 0.0231(15) 0.0263(14) -0.0037(12) 0.0025(10) -0.0072(11) C12 0.0258(13) 0.0226(15) 0.0293(15) -0.0059(12) 0.0015(10) -0.0015(11) C13 0.0256(13) 0.0330(17) 0.0326(16) -0.0034(13) -0.0026(11) -0.0049(12) C14 0.0314(13) 0.0288(16) 0.0257(15) -0.0074(12) -0.0013(11) -0.0078(11) C15 0.0286(13) 0.0221(15) 0.0244(14) -0.0036(12) -0.0008(10) -0.0065(11) N3 0.0301(11) 0.0268(13) 0.0303(12) -0.0093(10) -0.0010(9) -0.0085(9) C16 0.0273(13) 0.0222(15) 0.0268(15) -0.0047(12) 0.0015(10) -0.0067(11) C17 0.0342(14) 0.0267(16) 0.0267(15) -0.0079(12) -0.0026(11) -0.0078(12) C18 0.0278(13) 0.0268(16) 0.0392(16) -0.0064(13) -0.0042(11) -0.0019(11) C19 0.0372(15) 0.0219(16) 0.0332(16) -0.0093(13) 0.0041(11) 0.0002(12) C20 0.0354(14) 0.0225(16) 0.0274(15) -0.0055(12) 0.0011(11) -0.0089(12) C21 0.0336(14) 0.0244(16) 0.0367(17) -0.0094(13) 0.0019(12) -0.0015(12) C22 0.0396(15) 0.0325(18) 0.0387(17) -0.0117(14) 0.0014(12) -0.0069(13) C23 0.0457(16) 0.065(2) 0.0411(18) -0.0148(16) -0.0015(13) -0.0128(15) C24 0.0518(16) 0.045(2) 0.0445(18) -0.0189(16) 0.0004(13) -0.0088(14) C25 0.085(2) 0.052(2) 0.046(2) -0.0027(17) -0.0012(16) -0.0164(18) _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. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 0.8690 (0.0059) x + 7.9220 (0.0081) y - 10.8321 (0.0153) z = 0.4786 (0.0102) * -0.0045 (0.0016) N1 * 0.0144 (0.0017) C6 * -0.0083 (0.0017) C7 * -0.0069 (0.0017) C8 * 0.0165 (0.0017) C9 * -0.0111 (0.0016) C10 0.1273 (0.0049) C4 0.0719 (0.0039) C5 Rms deviation of fitted atoms = 0.0111 2.4132 (0.0052) x + 7.4095 (0.0080) y - 10.4754 (0.0145) z = 0.4136 (0.0134) Angle to previous plane (with approximate esd) = 14.74 ( 0.14 ) * -0.0089 (0.0015) N2 * 0.0013 (0.0015) C11 * 0.0038 (0.0016) C12 * -0.0016 (0.0016) C13 * -0.0059 (0.0016) C14 * 0.0113 (0.0016) C15 Rms deviation of fitted atoms = 0.0066 - 2.3269 (0.0054) x - 7.1029 (0.0082) y + 11.0860 (0.0142) z = 0.1780 (0.0165) Angle to previous plane (with approximate esd) = 2.49 ( 0.16 ) * -0.0004 (0.0015) N3 * 0.0010 (0.0016) C16 * -0.0039 (0.0016) C17 * 0.0062 (0.0017) C18 * -0.0056 (0.0017) C19 * 0.0028 (0.0016) C20 0.0270 (0.0039) C21 0.0921 (0.0049) C22 Rms deviation of fitted atoms = 0.0039 ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C1 1.837(3) . ? Si1 C4 1.841(3) . ? Si1 C3 1.852(2) . ? Si1 C2 1.857(3) . ? Si2 C22 1.840(3) . ? Si2 C23 1.846(2) . ? Si2 C24 1.853(3) . ? Si2 C25 1.862(3) . ? C4 C5 1.206(3) . ? C5 C6 1.457(3) . ? N1 C10 1.343(3) . ? N1 C6 1.345(3) . ? C6 C7 1.396(3) . ? C7 C8 1.374(3) . ? C8 C9 1.376(3) . ? C9 C10 1.390(3) . ? C10 C11 1.494(3) . ? N2 C11 1.343(3) . ? N2 C15 1.343(3) . ? C11 C12 1.393(3) . ? C12 C13 1.379(3) . ? C13 C14 1.376(3) . ? C14 C15 1.392(3) . ? C15 C16 1.489(3) . ? N3 C20 1.338(3) . ? N3 C16 1.347(3) . ? C16 C17 1.393(3) . ? C17 C18 1.381(3) . ? C18 C19 1.381(3) . ? C19 C20 1.394(3) . ? C20 C21 1.453(3) . ? C21 C22 1.199(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Si1 C4 107.80(12) . . ? C1 Si1 C3 109.35(13) . . ? C4 Si1 C3 112.35(12) . . ? C1 Si1 C2 111.19(14) . . ? C4 Si1 C2 106.92(12) . . ? C3 Si1 C2 109.22(13) . . ? C22 Si2 C23 109.37(11) . . ? C22 Si2 C24 109.09(12) . . ? C23 Si2 C24 110.29(13) . . ? C22 Si2 C25 107.35(13) . . ? C23 Si2 C25 111.06(14) . . ? C24 Si2 C25 109.62(13) . . ? C5 C4 Si1 171.6(2) . . ? C4 C5 C6 176.6(2) . . ? C10 N1 C6 117.43(18) . . ? N1 C6 C7 123.0(2) . . ? N1 C6 C5 117.82(19) . . ? C7 C6 C5 119.2(2) . . ? C8 C7 C6 118.6(2) . . ? C7 C8 C9 119.0(2) . . ? C8 C9 C10 119.4(2) . . ? N1 C10 C9 122.5(2) . . ? N1 C10 C11 116.38(19) . . ? C9 C10 C11 121.1(2) . . ? C11 N2 C15 117.72(19) . . ? N2 C11 C12 122.6(2) . . ? N2 C11 C10 117.47(19) . . ? C12 C11 C10 119.9(2) . . ? C13 C12 C11 119.0(2) . . ? C14 C13 C12 119.1(2) . . ? C13 C14 C15 118.8(2) . . ? N2 C15 C14 122.8(2) . . ? N2 C15 C16 116.76(19) . . ? C14 C15 C16 120.4(2) . . ? C20 N3 C16 118.0(2) . . ? N3 C16 C17 122.3(2) . . ? N3 C16 C15 115.7(2) . . ? C17 C16 C15 121.9(2) . . ? C18 C17 C16 119.1(2) . . ? C17 C18 C19 119.1(2) . . ? C18 C19 C20 118.5(2) . . ? N3 C20 C19 123.0(2) . . ? N3 C20 C21 116.5(2) . . ? C19 C20 C21 120.5(2) . . ? C22 C21 C20 177.8(3) . . ? C21 C22 Si2 177.2(3) . . ? 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 C1 Si1 C4 C5 -59.2(17) . . . . ? C3 Si1 C4 C5 -180(100) . . . . ? C2 Si1 C4 C5 60.4(17) . . . . ? Si1 C4 C5 C6 -4(6) . . . . ? C10 N1 C6 C7 -1.7(4) . . . . ? C10 N1 C6 C5 177.8(2) . . . . ? C4 C5 C6 N1 -173(5) . . . . ? C4 C5 C6 C7 6(5) . . . . ? N1 C6 C7 C8 2.1(4) . . . . ? C5 C6 C7 C8 -177.4(2) . . . . ? C6 C7 C8 C9 0.0(4) . . . . ? C7 C8 C9 C10 -2.3(4) . . . . ? C6 N1 C10 C9 -0.8(3) . . . . ? C6 N1 C10 C11 177.5(2) . . . . ? C8 C9 C10 N1 2.8(4) . . . . ? C8 C9 C10 C11 -175.3(2) . . . . ? C15 N2 C11 C12 1.4(3) . . . . ? C15 N2 C11 C10 179.4(2) . . . . ? N1 C10 C11 N2 168.4(2) . . . . ? C9 C10 C11 N2 -13.4(3) . . . . ? N1 C10 C11 C12 -13.5(3) . . . . ? C9 C10 C11 C12 164.7(2) . . . . ? N2 C11 C12 C13 -0.1(4) . . . . ? C10 C11 C12 C13 -178.1(2) . . . . ? C11 C12 C13 C14 -0.2(4) . . . . ? C12 C13 C14 C15 -0.7(3) . . . . ? C11 N2 C15 C14 -2.3(3) . . . . ? C11 N2 C15 C16 177.50(19) . . . . ? C13 C14 C15 N2 2.1(4) . . . . ? C13 C14 C15 C16 -177.8(2) . . . . ? C20 N3 C16 C17 0.5(3) . . . . ? C20 N3 C16 C15 -179.5(2) . . . . ? N2 C15 C16 N3 -178.1(2) . . . . ? C14 C15 C16 N3 1.7(3) . . . . ? N2 C15 C16 C17 1.9(3) . . . . ? C14 C15 C16 C17 -178.3(2) . . . . ? N3 C16 C17 C18 -0.8(4) . . . . ? C15 C16 C17 C18 179.2(2) . . . . ? C16 C17 C18 C19 1.3(4) . . . . ? C17 C18 C19 C20 -1.4(4) . . . . ? C16 N3 C20 C19 -0.6(3) . . . . ? C16 N3 C20 C21 178.9(2) . . . . ? C18 C19 C20 N3 1.1(4) . . . . ? C18 C19 C20 C21 -178.4(2) . . . . ? N3 C20 C21 C22 -79(7) . . . . ? C19 C20 C21 C22 101(7) . . . . ? C20 C21 C22 Si2 3(11) . . . . ? C23 Si2 C22 C21 121(5) . . . . ? C24 Si2 C22 C21 -118(5) . . . . ? C25 Si2 C22 C21 1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.256 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.056 ###END data_pr9922 _database_code_CSD 174649 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Compound 4a ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H31 N3 Si2' _chemical_formula_weight 501.77 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' _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 11.389(6) _cell_length_b 13.353(11) _cell_length_c 19.540(16) _cell_angle_alpha 94.69(3) _cell_angle_beta 99.71(5) _cell_angle_gamma 90.48(5) _cell_volume 2918(4) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 13311 _cell_measurement_theta_min 1.53 _cell_measurement_theta_max 22.47 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 0.145 _exptl_absorpt_correction_type SORTAV _exptl_absorpt_correction_T_min 0.9717 _exptl_absorpt_correction_T_max 0.9914 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'omega and psi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'not appliciable' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13311 _diffrn_reflns_av_R_equivalents 0.0639 _diffrn_reflns_av_sigmaI/netI 0.0913 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 22.47 _reflns_number_total 7470 _reflns_number_gt 4861 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius HKL Scalepack' _computing_data_reduction 'Nonius HKL Denzo & Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (J. Barbour, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1006P)^2^+1.8277P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7470 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1120 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.2086 _refine_ls_wR_factor_gt 0.1777 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si -0.13044(13) 0.66612(12) 0.86593(7) 0.0657(5) Uani 1 1 d . . . Si2 Si -0.32554(14) -0.09642(13) 0.11878(8) 0.0760(5) Uani 1 1 d . . . Si3 Si 0.38091(13) 0.60539(12) 0.88825(8) 0.0649(5) Uani 1 1 d . . . Si4 Si 0.16654(12) -0.15351(11) 0.13850(7) 0.0624(5) Uani 1 1 d . . . N1 N -0.0616(3) 0.4687(3) 0.62951(19) 0.0429(9) Uani 1 1 d . . . N2 N -0.0405(3) 0.3371(2) 0.46381(18) 0.0392(9) Uani 1 1 d . . . N3 N -0.1226(3) 0.1749(3) 0.30811(18) 0.0465(10) Uani 1 1 d . . . N4 N 0.4783(3) 0.3323(3) 0.70223(19) 0.0462(9) Uani 1 1 d . . . N5 N 0.4781(3) 0.1715(2) 0.54577(18) 0.0396(9) Uani 1 1 d . . . N6 N 0.3682(3) 0.0363(2) 0.37987(19) 0.0421(9) Uani 1 1 d . . . C1 C -0.0117(3) 0.4200(3) 0.5790(2) 0.0382(10) Uani 1 1 d . . . C5 C 0.0111(4) 0.4998(3) 0.6894(2) 0.0439(11) Uani 1 1 d . . . C6 C -0.0934(3) 0.3837(3) 0.5133(2) 0.0374(10) Uani 1 1 d . . . C8 C -0.2887(3) 0.3607(3) 0.4429(2) 0.0392(11) Uani 1 1 d . . . C10 C -0.1104(4) 0.2979(3) 0.4053(2) 0.0393(11) Uani 1 1 d . . . C11 C -0.4192(4) 0.3735(3) 0.4289(2) 0.0413(11) Uani 1 1 d . . . C17 C -0.0502(4) 0.2351(3) 0.3554(2) 0.0404(11) Uani 1 1 d . . . C21 C -0.0706(4) 0.1129(3) 0.2645(2) 0.0506(12) Uani 1 1 d . . . C22 C -0.0433(4) 0.5517(4) 0.7437(3) 0.0508(12) Uani 1 1 d . . . C23 C -0.0816(4) 0.5970(4) 0.7908(3) 0.0582(13) Uani 1 1 d . . . C24 C -0.1515(4) 0.0454(4) 0.2167(3) 0.0585(13) Uani 1 1 d . . . C25 C -0.2183(5) -0.0122(4) 0.1773(3) 0.0679(15) Uani 1 1 d . . . C32 C 0.5245(3) 0.2745(3) 0.6543(2) 0.0405(11) Uani 1 1 d . . . C36 C 0.5536(4) 0.3929(3) 0.7481(2) 0.0477(12) Uani 1 1 d . . . C39 C 0.2393(3) 0.1463(3) 0.5616(2) 0.0399(11) Uani 1 1 d . . . C37 C 0.4375(4) 0.2109(3) 0.6029(2) 0.0405(11) Uani 1 1 d . . . C41 C 0.3984(3) 0.1237(3) 0.4954(2) 0.0378(10) Uani 1 1 d . . . C42 C 0.1142(4) 0.1318(3) 0.5722(2) 0.0404(11) Uani 1 1 d . . . C48 C 0.4454(3) 0.0861(3) 0.4313(2) 0.0383(10) Uani 1 1 d . . . C52 C 0.4090(4) 0.0038(3) 0.3214(2) 0.0441(11) Uani 1 1 d . . . C53 C 0.4998(4) 0.4589(4) 0.7957(3) 0.0553(13) Uani 1 1 d . . . C54 C 0.4545(4) 0.5167(4) 0.8334(3) 0.0608(14) Uani 1 1 d . . . C55 C 0.3245(4) -0.0485(3) 0.2658(3) 0.0494(12) Uani 1 1 d . . . C56 C 0.2588(4) -0.0923(4) 0.2171(3) 0.0559(13) Uani 1 1 d . . . C2 C 0.1102(4) 0.4022(3) 0.5876(2) 0.0459(12) Uani 1 1 d . . . H2 H 0.1431 0.3679 0.5510 0.055 Uiso 1 1 calc R . . C3 C 0.1818(4) 0.4342(3) 0.6486(3) 0.0527(13) Uani 1 1 d . . . H3 H 0.2649 0.4222 0.6550 0.063 Uiso 1 1 calc R . . C4 C 0.1327(4) 0.4838(3) 0.7006(3) 0.0518(13) Uani 1 1 d . . . H4 H 0.1811 0.5068 0.7436 0.062 Uiso 1 1 calc R . . C7 C -0.2160(3) 0.3953(3) 0.5053(2) 0.0401(11) Uani 1 1 d . . . H7 H -0.2503 0.4267 0.5424 0.048 Uiso 1 1 calc R . . C9 C -0.2333(4) 0.3089(3) 0.3930(2) 0.0433(11) Uani 1 1 d . . . H9 H -0.2794 0.2810 0.3506 0.052 Uiso 1 1 calc R . . C12 C -0.4778(4) 0.3847(3) 0.3611(3) 0.0561(13) Uani 1 1 d . . . H12 H -0.4333 0.3847 0.3241 0.067 Uiso 1 1 calc R . . C13 C -0.5991(5) 0.3956(4) 0.3476(3) 0.0672(15) Uani 1 1 d . . . H13 H -0.6381 0.4024 0.3013 0.081 Uiso 1 1 calc R . . C14 C -0.6651(4) 0.3970(3) 0.4011(3) 0.0622(15) Uani 1 1 d . . . H14 H -0.7488 0.4053 0.3915 0.075 Uiso 1 1 calc R . . C15 C -0.6089(4) 0.3862(3) 0.4685(3) 0.0576(14) Uani 1 1 d . . . H15 H -0.6539 0.3857 0.5052 0.069 Uiso 1 1 calc R . . C16 C -0.4860(4) 0.3760(3) 0.4821(3) 0.0457(12) Uani 1 1 d . . . H16 H -0.4472 0.3707 0.5287 0.055 Uiso 1 1 calc R . . C18 C 0.0723(4) 0.2357(3) 0.3607(2) 0.0475(12) Uani 1 1 d . . . H18 H 0.1207 0.2786 0.3957 0.057 Uiso 1 1 calc R . . C19 C 0.1236(4) 0.1737(4) 0.3148(2) 0.0529(12) Uani 1 1 d . . . H19 H 0.2075 0.1745 0.3166 0.063 Uiso 1 1 calc R . . C20 C 0.0506(4) 0.1102(4) 0.2663(3) 0.0547(13) Uani 1 1 d . . . H20 H 0.0835 0.0654 0.2346 0.066 Uiso 1 1 calc R . . C33 C 0.6456(4) 0.2758(3) 0.6503(2) 0.0461(11) Uani 1 1 d . . . H33 H 0.6755 0.2347 0.6154 0.055 Uiso 1 1 calc R . . C34 C 0.7212(4) 0.3386(4) 0.6987(2) 0.0522(12) Uani 1 1 d . . . H34 H 0.8043 0.3405 0.6977 0.063 Uiso 1 1 calc R . . C35 C 0.6754(4) 0.3979(4) 0.7479(2) 0.0544(13) Uani 1 1 d . . . H35 H 0.7259 0.4416 0.7813 0.065 Uiso 1 1 calc R . . C38 C 0.3213(3) 0.1988(3) 0.6128(2) 0.0420(11) Uani 1 1 d . . . H38 H 0.2975 0.2263 0.6546 0.050 Uiso 1 1 calc R . . C40 C 0.2793(3) 0.1101(3) 0.5011(2) 0.0383(10) Uani 1 1 d . . . H40 H 0.2255 0.0763 0.4637 0.046 Uiso 1 1 calc R . . C43 C 0.0885(4) 0.1253(4) 0.6388(3) 0.0611(14) Uani 1 1 d . . . H43 H 0.1515 0.1288 0.6777 0.073 Uiso 1 1 calc R . . C44 C -0.0281(5) 0.1137(4) 0.6489(3) 0.0727(17) Uani 1 1 d . . . H44 H -0.0450 0.1092 0.6945 0.087 Uiso 1 1 calc R . . C45 C -0.1200(4) 0.1088(3) 0.5924(3) 0.0618(15) Uani 1 1 d . . . H45 H -0.2000 0.1015 0.5995 0.074 Uiso 1 1 calc R . . C46 C -0.0964(4) 0.1143(3) 0.5259(3) 0.0568(13) Uani 1 1 d . . . H46 H -0.1596 0.1107 0.4872 0.068 Uiso 1 1 calc R . . C47 C 0.0207(4) 0.1250(3) 0.5160(3) 0.0453(11) Uani 1 1 d . . . H47 H 0.0373 0.1278 0.4701 0.054 Uiso 1 1 calc R . . C49 C 0.5627(4) 0.1041(3) 0.4252(2) 0.0461(12) Uani 1 1 d . . . H49 H 0.6154 0.1393 0.4624 0.055 Uiso 1 1 calc R . . C50 C 0.6032(4) 0.0706(3) 0.3646(3) 0.0512(12) Uani 1 1 d . . . H50 H 0.6835 0.0828 0.3595 0.061 Uiso 1 1 calc R . . C51 C 0.5249(4) 0.0193(3) 0.3118(2) 0.0498(12) Uani 1 1 d . . . H51 H 0.5501 -0.0050 0.2697 0.060 Uiso 1 1 calc R . . C26 C -0.2681(5) 0.7341(5) 0.8374(3) 0.093(2) Uani 1 1 d . . . H26A H -0.2933 0.7704 0.8780 0.140 Uiso 1 1 calc R . . H26B H -0.3310 0.6860 0.8148 0.140 Uiso 1 1 calc R . . H26C H -0.2531 0.7821 0.8044 0.140 Uiso 1 1 calc R . . C27 C -0.1568(7) 0.5749(5) 0.9273(4) 0.115(3) Uani 1 1 d . . . H27A H -0.1829 0.6101 0.9679 0.173 Uiso 1 1 calc R . . H27B H -0.0828 0.5398 0.9424 0.173 Uiso 1 1 calc R . . H27C H -0.2186 0.5260 0.9043 0.173 Uiso 1 1 calc R . . C28 C -0.0098(5) 0.7556(4) 0.9067(3) 0.0807(18) Uani 1 1 d . . . H28A H -0.0334 0.7933 0.9471 0.121 Uiso 1 1 calc R . . H28B H 0.0054 0.8023 0.8728 0.121 Uiso 1 1 calc R . . H28C H 0.0627 0.7187 0.9217 0.121 Uiso 1 1 calc R . . C29 C -0.3479(6) -0.2100(5) 0.1636(4) 0.113(2) Uani 1 1 d . . . H29A H -0.4048 -0.2561 0.1329 0.169 Uiso 1 1 calc R . . H29B H -0.3789 -0.1908 0.2065 0.169 Uiso 1 1 calc R . . H29C H -0.2716 -0.2434 0.1751 0.169 Uiso 1 1 calc R . . C30 C -0.4669(5) -0.0265(6) 0.0987(3) 0.112(2) Uani 1 1 d . . . H30A H -0.5263 -0.0694 0.0672 0.169 Uiso 1 1 calc R . . H30B H -0.4516 0.0342 0.0764 0.169 Uiso 1 1 calc R . . H30C H -0.4969 -0.0077 0.1420 0.169 Uiso 1 1 calc R . . C31 C -0.2620(6) -0.1301(6) 0.0394(3) 0.114(3) Uani 1 1 d . . . H31A H -0.3178 -0.1752 0.0071 0.172 Uiso 1 1 calc R . . H31B H -0.1864 -0.1640 0.0519 0.172 Uiso 1 1 calc R . . H31C H -0.2481 -0.0690 0.0170 0.172 Uiso 1 1 calc R . . C57 C 0.3306(6) 0.7119(5) 0.8369(4) 0.105(2) Uani 1 1 d . . . H57A H 0.2908 0.7605 0.8651 0.158 Uiso 1 1 calc R . . H57B H 0.2747 0.6872 0.7950 0.158 Uiso 1 1 calc R . . H57C H 0.3995 0.7446 0.8233 0.158 Uiso 1 1 calc R . . C58 C 0.2544(5) 0.5382(5) 0.9131(3) 0.0826(18) Uani 1 1 d . . . H58A H 0.2137 0.5840 0.9427 0.124 Uiso 1 1 calc R . . H58B H 0.2838 0.4809 0.9387 0.124 Uiso 1 1 calc R . . H58C H 0.1986 0.5142 0.8710 0.124 Uiso 1 1 calc R . . C59 C 0.4916(5) 0.6496(5) 0.9663(3) 0.098(2) Uani 1 1 d . . . H59A H 0.4540 0.6969 0.9966 0.147 Uiso 1 1 calc R . . H59B H 0.5589 0.6832 0.9517 0.147 Uiso 1 1 calc R . . H59C H 0.5203 0.5920 0.9919 0.147 Uiso 1 1 calc R . . C60 C 0.0432(5) -0.2296(5) 0.1613(3) 0.0875(19) Uani 1 1 d . . . H60A H -0.0048 -0.2614 0.1186 0.131 Uiso 1 1 calc R . . H60B H -0.0071 -0.1859 0.1862 0.131 Uiso 1 1 calc R . . H60C H 0.0766 -0.2816 0.1910 0.131 Uiso 1 1 calc R . . C61 C 0.1028(6) -0.0521(4) 0.0855(3) 0.092(2) Uani 1 1 d . . . H61A H 0.0528 -0.0817 0.0428 0.138 Uiso 1 1 calc R . . H61B H 0.1674 -0.0117 0.0735 0.138 Uiso 1 1 calc R . . H61C H 0.0543 -0.0091 0.1123 0.138 Uiso 1 1 calc R . . C62 C 0.2629(5) -0.2353(5) 0.0916(3) 0.091(2) Uani 1 1 d . . . H62A H 0.2151 -0.2685 0.0492 0.136 Uiso 1 1 calc R . . H62B H 0.2979 -0.2863 0.1217 0.136 Uiso 1 1 calc R . . H62C H 0.3266 -0.1945 0.0789 0.136 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 Si1 0.0792(10) 0.0706(11) 0.0467(9) -0.0092(8) 0.0165(7) -0.0090(8) Si2 0.0860(11) 0.0870(12) 0.0520(10) -0.0126(9) 0.0130(8) -0.0234(9) Si3 0.0706(9) 0.0645(10) 0.0574(10) -0.0099(8) 0.0120(7) -0.0008(7) Si4 0.0706(9) 0.0626(10) 0.0490(9) -0.0098(7) 0.0032(7) -0.0002(7) N1 0.043(2) 0.038(2) 0.049(2) 0.0023(19) 0.0115(18) -0.0033(16) N2 0.041(2) 0.032(2) 0.045(2) 0.0035(18) 0.0091(18) -0.0027(16) N3 0.052(2) 0.046(2) 0.041(2) -0.003(2) 0.0107(18) 0.0046(18) N4 0.053(2) 0.040(2) 0.043(2) -0.0015(19) 0.0051(18) -0.0053(18) N5 0.0376(19) 0.036(2) 0.046(2) 0.0057(18) 0.0072(17) 0.0010(16) N6 0.042(2) 0.037(2) 0.047(2) 0.0010(18) 0.0084(18) 0.0022(16) C1 0.046(3) 0.027(2) 0.043(3) 0.007(2) 0.009(2) -0.0022(19) C5 0.047(3) 0.040(3) 0.043(3) -0.007(2) 0.007(2) -0.007(2) C6 0.040(3) 0.030(2) 0.043(3) 0.004(2) 0.008(2) 0.0013(18) C8 0.042(3) 0.034(2) 0.043(3) 0.007(2) 0.008(2) 0.0030(19) C10 0.047(3) 0.029(2) 0.043(3) 0.005(2) 0.010(2) 0.0028(19) C11 0.044(3) 0.028(2) 0.051(3) 0.003(2) 0.006(2) 0.0023(19) C17 0.047(3) 0.035(3) 0.039(3) 0.003(2) 0.008(2) -0.001(2) C21 0.059(3) 0.047(3) 0.046(3) 0.002(2) 0.013(2) 0.002(2) C22 0.048(3) 0.050(3) 0.050(3) 0.001(3) 0.001(2) -0.010(2) C23 0.063(3) 0.059(3) 0.051(3) -0.003(3) 0.009(3) -0.010(2) C24 0.066(3) 0.058(3) 0.053(3) -0.008(3) 0.018(3) 0.007(3) C25 0.080(4) 0.073(4) 0.051(3) -0.008(3) 0.016(3) -0.001(3) C32 0.046(3) 0.037(3) 0.038(3) 0.007(2) 0.007(2) -0.001(2) C36 0.048(3) 0.046(3) 0.048(3) -0.003(2) 0.009(2) -0.010(2) C39 0.049(3) 0.029(2) 0.042(3) 0.008(2) 0.009(2) -0.002(2) C37 0.047(3) 0.031(2) 0.044(3) 0.003(2) 0.006(2) 0.0015(19) C41 0.042(3) 0.028(2) 0.044(3) 0.006(2) 0.010(2) 0.0053(19) C42 0.046(3) 0.030(2) 0.048(3) 0.001(2) 0.014(2) -0.0037(19) C48 0.039(3) 0.030(2) 0.046(3) 0.005(2) 0.006(2) 0.0005(19) C52 0.048(3) 0.039(3) 0.047(3) 0.003(2) 0.012(2) 0.003(2) C53 0.061(3) 0.050(3) 0.052(3) -0.010(3) 0.010(3) -0.017(2) C54 0.067(3) 0.061(3) 0.052(3) -0.007(3) 0.009(3) -0.012(3) C55 0.051(3) 0.048(3) 0.052(3) 0.002(3) 0.019(2) 0.005(2) C56 0.056(3) 0.056(3) 0.057(3) -0.001(3) 0.014(3) 0.002(2) C2 0.041(3) 0.037(3) 0.060(3) 0.001(2) 0.012(2) 0.001(2) C3 0.040(3) 0.054(3) 0.061(3) -0.004(3) 0.003(2) -0.001(2) C4 0.048(3) 0.051(3) 0.052(3) -0.001(3) -0.004(2) -0.005(2) C7 0.048(3) 0.031(2) 0.042(3) 0.004(2) 0.008(2) 0.0000(19) C9 0.048(3) 0.036(3) 0.045(3) 0.007(2) 0.004(2) -0.003(2) C12 0.057(3) 0.055(3) 0.051(3) -0.002(3) -0.003(2) 0.008(2) C13 0.058(4) 0.056(3) 0.078(4) 0.000(3) -0.014(3) 0.011(3) C14 0.043(3) 0.035(3) 0.101(5) 0.002(3) -0.008(3) 0.004(2) C15 0.050(3) 0.038(3) 0.087(4) 0.008(3) 0.016(3) -0.001(2) C16 0.041(3) 0.031(3) 0.064(3) 0.011(2) 0.004(2) -0.0012(19) C18 0.051(3) 0.047(3) 0.045(3) 0.003(2) 0.011(2) -0.003(2) C19 0.051(3) 0.055(3) 0.056(3) 0.008(3) 0.017(2) 0.006(2) C20 0.064(3) 0.051(3) 0.051(3) 0.001(3) 0.017(2) 0.011(2) C33 0.048(3) 0.043(3) 0.047(3) 0.005(2) 0.005(2) 0.002(2) C34 0.043(3) 0.056(3) 0.056(3) 0.007(3) 0.002(2) -0.009(2) C35 0.060(3) 0.053(3) 0.047(3) -0.006(3) 0.004(2) -0.014(2) C38 0.046(3) 0.034(3) 0.046(3) 0.003(2) 0.011(2) -0.004(2) C40 0.043(3) 0.027(2) 0.045(3) 0.002(2) 0.007(2) -0.0037(18) C43 0.067(3) 0.065(3) 0.053(3) -0.004(3) 0.022(3) -0.021(3) C44 0.075(4) 0.073(4) 0.076(4) -0.015(3) 0.041(3) -0.028(3) C45 0.053(3) 0.033(3) 0.107(5) -0.005(3) 0.042(3) -0.006(2) C46 0.045(3) 0.042(3) 0.086(4) 0.007(3) 0.016(3) -0.003(2) C47 0.052(3) 0.030(3) 0.059(3) 0.011(2) 0.020(2) 0.003(2) C49 0.042(3) 0.042(3) 0.054(3) 0.005(2) 0.006(2) -0.001(2) C50 0.044(3) 0.054(3) 0.059(3) 0.006(3) 0.019(2) -0.002(2) C51 0.054(3) 0.049(3) 0.048(3) -0.001(2) 0.019(2) 0.001(2) C26 0.076(4) 0.120(6) 0.084(4) -0.029(4) 0.031(3) 0.006(3) C27 0.173(7) 0.097(5) 0.083(5) -0.007(4) 0.051(5) -0.028(5) C28 0.089(4) 0.078(4) 0.069(4) -0.020(3) 0.008(3) -0.005(3) C29 0.151(6) 0.097(5) 0.084(5) -0.001(4) 0.009(4) -0.045(5) C30 0.097(5) 0.162(7) 0.073(5) 0.007(5) 0.003(4) -0.006(4) C31 0.121(5) 0.151(7) 0.066(4) -0.042(5) 0.026(4) -0.039(5) C57 0.128(5) 0.083(5) 0.107(6) 0.002(4) 0.030(4) 0.032(4) C58 0.078(4) 0.101(5) 0.071(4) 0.003(4) 0.019(3) 0.005(3) C59 0.086(4) 0.109(5) 0.091(5) -0.037(4) 0.010(3) -0.005(4) C60 0.076(4) 0.103(5) 0.075(4) -0.002(4) -0.006(3) -0.021(3) C61 0.131(5) 0.074(4) 0.061(4) 0.003(3) -0.012(4) 0.002(4) C62 0.091(4) 0.098(5) 0.076(4) -0.034(4) 0.015(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C27 1.834(7) . ? Si1 C23 1.838(6) . ? Si1 C28 1.843(5) . ? Si1 C26 1.845(6) . ? Si2 C25 1.832(6) . ? Si2 C31 1.844(6) . ? Si2 C29 1.849(7) . ? Si2 C30 1.868(7) . ? Si3 C54 1.834(6) . ? Si3 C58 1.844(6) . ? Si3 C57 1.847(7) . ? Si3 C59 1.859(6) . ? Si4 C56 1.835(5) . ? Si4 C61 1.851(6) . ? Si4 C62 1.853(5) . ? Si4 C60 1.861(6) . ? N1 C1 1.344(5) . ? N1 C5 1.347(5) . ? N2 C6 1.338(5) . ? N2 C10 1.343(5) . ? N3 C17 1.338(5) . ? N3 C21 1.351(5) . ? N4 C36 1.343(5) . ? N4 C32 1.343(5) . ? N5 C41 1.337(5) . ? N5 C37 1.349(5) . ? N6 C48 1.344(5) . ? N6 C52 1.345(5) . ? C1 C2 1.395(5) . ? C1 C6 1.496(6) . ? C5 C4 1.387(6) . ? C5 C22 1.449(6) . ? C6 C7 1.390(5) . ? C8 C9 1.389(6) . ? C8 C7 1.395(6) . ? C8 C11 1.480(6) . ? C10 C9 1.391(6) . ? C10 C17 1.492(6) . ? C11 C16 1.387(6) . ? C11 C12 1.400(6) . ? C17 C18 1.382(6) . ? C21 C20 1.376(6) . ? C21 C24 1.447(7) . ? C22 C23 1.204(6) . ? C24 C25 1.208(6) . ? C32 C33 1.395(6) . ? C32 C37 1.491(6) . ? C36 C35 1.389(6) . ? C36 C53 1.445(7) . ? C39 C38 1.387(6) . ? C39 C40 1.390(6) . ? C39 C42 1.486(6) . ? C37 C38 1.380(6) . ? C41 C40 1.391(5) . ? C41 C48 1.495(6) . ? C42 C47 1.391(6) . ? C42 C43 1.392(6) . ? C48 C49 1.382(5) . ? C52 C51 1.380(6) . ? C52 C55 1.451(7) . ? C53 C54 1.203(6) . ? C55 C56 1.212(6) . ? C2 C3 1.361(6) . ? C3 C4 1.368(6) . ? C12 C13 1.374(6) . ? C13 C14 1.386(8) . ? C14 C15 1.383(7) . ? C15 C16 1.389(6) . ? C18 C19 1.377(6) . ? C19 C20 1.377(6) . ? C33 C34 1.386(6) . ? C34 C35 1.369(6) . ? C43 C44 1.384(6) . ? C44 C45 1.384(8) . ? C45 C46 1.379(7) . ? C46 C47 1.387(6) . ? C49 C50 1.384(6) . ? C50 C51 1.375(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C27 Si1 C23 108.0(3) . . ? C27 Si1 C28 110.3(3) . . ? C23 Si1 C28 107.8(2) . . ? C27 Si1 C26 110.3(3) . . ? C23 Si1 C26 110.3(3) . . ? C28 Si1 C26 110.2(3) . . ? C25 Si2 C31 107.8(3) . . ? C25 Si2 C29 108.4(3) . . ? C31 Si2 C29 110.3(4) . . ? C25 Si2 C30 107.3(3) . . ? C31 Si2 C30 111.4(3) . . ? C29 Si2 C30 111.5(3) . . ? C54 Si3 C58 107.8(3) . . ? C54 Si3 C57 107.8(3) . . ? C58 Si3 C57 111.5(3) . . ? C54 Si3 C59 108.1(2) . . ? C58 Si3 C59 111.1(3) . . ? C57 Si3 C59 110.3(3) . . ? C56 Si4 C61 106.8(3) . . ? C56 Si4 C62 108.3(2) . . ? C61 Si4 C62 111.5(3) . . ? C56 Si4 C60 110.9(3) . . ? C61 Si4 C60 109.2(3) . . ? C62 Si4 C60 110.0(3) . . ? C1 N1 C5 117.3(3) . . ? C6 N2 C10 117.8(3) . . ? C17 N3 C21 116.9(4) . . ? C36 N4 C32 117.6(4) . . ? C41 N5 C37 117.0(3) . . ? C48 N6 C52 117.6(3) . . ? N1 C1 C2 121.9(4) . . ? N1 C1 C6 117.0(3) . . ? C2 C1 C6 121.1(4) . . ? N1 C5 C4 123.1(4) . . ? N1 C5 C22 117.0(4) . . ? C4 C5 C22 119.9(4) . . ? N2 C6 C7 122.6(4) . . ? N2 C6 C1 115.3(3) . . ? C7 C6 C1 122.0(4) . . ? C9 C8 C7 116.7(4) . . ? C9 C8 C11 119.6(4) . . ? C7 C8 C11 123.6(4) . . ? N2 C10 C9 122.7(4) . . ? N2 C10 C17 116.3(3) . . ? C9 C10 C17 120.9(4) . . ? C16 C11 C12 118.5(4) . . ? C16 C11 C8 121.3(4) . . ? C12 C11 C8 120.1(4) . . ? N3 C17 C18 122.9(4) . . ? N3 C17 C10 115.3(4) . . ? C18 C17 C10 121.7(4) . . ? N3 C21 C20 123.4(4) . . ? N3 C21 C24 115.1(4) . . ? C20 C21 C24 121.5(4) . . ? C23 C22 C5 176.0(5) . . ? C22 C23 Si1 176.3(4) . . ? C25 C24 C21 178.9(6) . . ? C24 C25 Si2 177.3(5) . . ? N4 C32 C33 122.8(4) . . ? N4 C32 C37 115.9(4) . . ? C33 C32 C37 121.2(4) . . ? N4 C36 C35 123.0(4) . . ? N4 C36 C53 116.0(4) . . ? C35 C36 C53 120.8(4) . . ? C38 C39 C40 117.1(4) . . ? C38 C39 C42 120.2(4) . . ? C40 C39 C42 122.7(4) . . ? N5 C37 C38 123.2(4) . . ? N5 C37 C32 116.0(4) . . ? C38 C37 C32 120.8(4) . . ? N5 C41 C40 122.9(4) . . ? N5 C41 C48 115.4(3) . . ? C40 C41 C48 121.6(4) . . ? C47 C42 C43 118.7(4) . . ? C47 C42 C39 120.9(4) . . ? C43 C42 C39 120.4(4) . . ? N6 C48 C49 122.0(4) . . ? N6 C48 C41 117.1(3) . . ? C49 C48 C41 120.9(4) . . ? N6 C52 C51 123.5(4) . . ? N6 C52 C55 117.2(4) . . ? C51 C52 C55 119.3(4) . . ? C54 C53 C36 177.3(6) . . ? C53 C54 Si3 178.0(5) . . ? C56 C55 C52 176.4(5) . . ? C55 C56 Si4 175.1(5) . . ? C3 C2 C1 119.8(4) . . ? C2 C3 C4 119.2(4) . . ? C3 C4 C5 118.8(4) . . ? C6 C7 C8 120.1(4) . . ? C8 C9 C10 120.0(4) . . ? C13 C12 C11 120.5(5) . . ? C12 C13 C14 120.5(5) . . ? C15 C14 C13 119.9(5) . . ? C14 C15 C16 119.5(5) . . ? C11 C16 C15 121.0(5) . . ? C19 C18 C17 119.3(4) . . ? C18 C19 C20 118.6(4) . . ? C21 C20 C19 118.9(4) . . ? C34 C33 C32 118.2(4) . . ? C35 C34 C33 119.6(4) . . ? C34 C35 C36 118.7(4) . . ? C37 C38 C39 119.8(4) . . ? C39 C40 C41 119.7(4) . . ? C44 C43 C42 120.5(5) . . ? C45 C44 C43 119.9(5) . . ? C46 C45 C44 120.6(4) . . ? C45 C46 C47 119.3(5) . . ? C46 C47 C42 121.0(5) . . ? C48 C49 C50 119.8(4) . . ? C51 C50 C49 118.7(4) . . ? C50 C51 C52 118.5(4) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 22.47 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.469 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.058 ###END data_cam115 _database_code_CSD 174650 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Compound 2M ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H76 N2 P4 Pt2' _chemical_formula_weight 1219.19 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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.540(7) _cell_length_b 9.389(3) _cell_length_c 25.662(7) _cell_angle_alpha 90.00 _cell_angle_beta 116.005(14) _cell_angle_gamma 90.00 _cell_volume 5097(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25703 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 29.14 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2424 _exptl_absorpt_coefficient_mu 5.642 _exptl_absorpt_correction_type multiscans _exptl_absorpt_correction_T_min 0.6023 _exptl_absorpt_correction_T_max 0.9457 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.68980 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method 'Thin slice, \w-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 'not appliciable' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26831 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.0487 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9734 _reflns_number_gt 8910 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'LSCELL (CLEGG, 1997)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (J. Barbour, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0522P)^2^+57.0881P] 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 'methyls rigid, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9734 _refine_ls_number_parameters 535 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1508 _refine_ls_wR_factor_gt 0.1475 _refine_ls_goodness_of_fit_ref 1.286 _refine_ls_restrained_S_all 1.286 _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 Pt1 Pt 0.322443(14) 0.90256(4) 0.290904(15) 0.01678(11) Uani 1 1 d . . . Pt2 Pt 0.844654(16) -0.07364(4) 0.555259(16) 0.02143(12) Uani 1 1 d . . . C1 C 0.3937(4) 0.7639(10) 0.3060(4) 0.0223(19) Uani 1 1 d . . . C2 C 0.4328(4) 0.6729(10) 0.3157(4) 0.0208(19) Uani 1 1 d . . . N1 N 0.5094(3) 0.5109(8) 0.3782(3) 0.0216(16) Uani 1 1 d . . . C3 C 0.4791(4) 0.5652(10) 0.3241(4) 0.0228(19) Uani 1 1 d . . . C4 C 0.4913(5) 0.5204(12) 0.2785(5) 0.031(2) Uani 1 1 d . . . H4 H 0.4693 0.5620 0.2412 0.037 Uiso 1 1 calc R . . C5 C 0.5356(5) 0.4147(11) 0.2875(5) 0.029(2) Uani 1 1 d . . . H5 H 0.5436 0.3805 0.2565 0.035 Uiso 1 1 calc R . . C6 C 0.5684(5) 0.3598(11) 0.3435(5) 0.027(2) Uani 1 1 d . . . H6 H 0.5995 0.2879 0.3513 0.032 Uiso 1 1 calc R . . C7 C 0.5548(4) 0.4120(9) 0.3872(4) 0.0186(18) Uani 1 1 d . . . N2 N 0.6398(3) 0.2748(8) 0.4595(3) 0.0203(16) Uani 1 1 d . . . C8 C 0.5882(4) 0.3569(9) 0.4480(4) 0.0181(18) Uani 1 1 d . . . C9 C 0.5694(4) 0.3913(10) 0.4906(4) 0.0217(19) Uani 1 1 d . . . H9 H 0.5346 0.4535 0.4819 0.026 Uiso 1 1 calc R . . C10 C 0.6010(4) 0.3354(10) 0.5455(4) 0.0242(19) Uani 1 1 d . . . H10 H 0.5873 0.3562 0.5743 0.029 Uiso 1 1 calc R . . C11 C 0.6528(4) 0.2492(10) 0.5583(4) 0.025(2) Uani 1 1 d . . . H11 H 0.6753 0.2088 0.5957 0.030 Uiso 1 1 calc R . . C12 C 0.6711(4) 0.2234(10) 0.5141(4) 0.0213(19) Uani 1 1 d . . . C13 C 0.7263(4) 0.1365(10) 0.5254(4) 0.025(2) Uani 1 1 d . . . C14 C 0.7707(5) 0.0600(10) 0.5367(5) 0.026(2) Uani 1 1 d . . . C21 C 0.2470(4) 1.0373(10) 0.2756(4) 0.0222(19) Uani 1 1 d . . . C22 C 0.2226(4) 1.0466(10) 0.3158(4) 0.0231(19) Uani 1 1 d . . . H22 H 0.2412 0.9908 0.3501 0.028 Uiso 1 1 calc R . . C23 C 0.1716(5) 1.1350(11) 0.3078(5) 0.032(2) Uani 1 1 d . . . H23 H 0.1573 1.1426 0.3371 0.038 Uiso 1 1 calc R . . C24 C 0.1422(5) 1.2113(12) 0.2565(5) 0.035(3) Uani 1 1 d . . . H24 H 0.1065 1.2691 0.2499 0.042 Uiso 1 1 calc R . . C25 C 0.1649(5) 1.2035(12) 0.2145(5) 0.037(3) Uani 1 1 d . . . H25 H 0.1452 1.2565 0.1796 0.044 Uiso 1 1 calc R . . C26 C 0.2160(4) 1.1181(10) 0.2246(5) 0.027(2) Uani 1 1 d . . . H26 H 0.2311 1.1133 0.1959 0.032 Uiso 1 1 calc R . . C31 C 0.9187(4) -0.2184(12) 0.5761(5) 0.033(2) Uani 1 1 d . . . C32 C 0.9438(5) -0.2497(14) 0.5368(6) 0.042(3) Uani 1 1 d . . . H32 H 0.9291 -0.2002 0.5009 0.050 Uiso 1 1 calc R . . C33 C 0.9909(5) -0.3550(15) 0.5508(7) 0.049(3) Uani 1 1 d . . . H33 H 1.0073 -0.3764 0.5239 0.059 Uiso 1 1 calc R . . C34 C 1.0139(6) -0.4281(13) 0.6030(7) 0.052(4) Uani 1 1 d . . . H34 H 1.0445 -0.5013 0.6114 0.062 Uiso 1 1 calc R . . C35 C 0.9911(6) -0.3915(13) 0.6427(7) 0.051(4) Uani 1 1 d . . . H35 H 1.0079 -0.4365 0.6796 0.061 Uiso 1 1 calc R . . C36 C 0.9440(5) -0.2899(14) 0.6291(6) 0.042(3) Uani 1 1 d . . . H36 H 0.9285 -0.2684 0.6567 0.050 Uiso 1 1 calc R . . P1 P 0.38730(11) 1.0826(3) 0.34476(11) 0.0217(5) Uani 1 1 d . . . C41 C 0.4724(4) 1.0590(12) 0.3707(5) 0.030(2) Uani 1 1 d . . . H41A H 0.4804 1.0235 0.3382 0.036 Uiso 1 1 calc R . . H41B H 0.4931 1.1532 0.3821 0.036 Uiso 1 1 calc R . . C42 C 0.5037(5) 0.9564(14) 0.4222(6) 0.045(3) Uani 1 1 d . . . H42A H 0.4934 0.9858 0.4537 0.068 Uiso 1 1 calc R . . H42B H 0.5497 0.9585 0.4358 0.068 Uiso 1 1 calc R . . H42C H 0.4881 0.8595 0.4098 0.068 Uiso 1 1 calc R . . C43 C 0.3714(5) 1.2446(10) 0.3027(5) 0.031(2) Uani 1 1 d . . . H43A H 0.3283 1.2780 0.2941 0.037 Uiso 1 1 calc R . . H43B H 0.4016 1.3190 0.3262 0.037 Uiso 1 1 calc R . . C44 C 0.3766(6) 1.2270(12) 0.2450(5) 0.040(3) Uani 1 1 d . . . H44A H 0.4202 1.2026 0.2533 0.060 Uiso 1 1 calc R . . H44B H 0.3646 1.3164 0.2232 0.060 Uiso 1 1 calc R . . H44C H 0.3482 1.1507 0.2221 0.060 Uiso 1 1 calc R . . C45 C 0.3774(5) 1.1307(12) 0.4096(5) 0.031(2) Uani 1 1 d . . . H45A H 0.3321 1.1508 0.3976 0.037 Uiso 1 1 calc R . . H45B H 0.3888 1.0469 0.4357 0.037 Uiso 1 1 calc R . . C46 C 0.4155(6) 1.2578(13) 0.4444(6) 0.041(3) Uani 1 1 d . . . H46A H 0.4607 1.2362 0.4600 0.062 Uiso 1 1 calc R . . H46B H 0.4046 1.2774 0.4763 0.062 Uiso 1 1 calc R . . H46C H 0.4058 1.3414 0.4191 0.062 Uiso 1 1 calc R . . P2 P 0.25730(10) 0.7354(2) 0.22836(11) 0.0198(5) Uani 1 1 d . . . C51 C 0.2730(5) 0.7214(12) 0.1650(5) 0.032(2) Uani 1 1 d . . . H51A H 0.3158 0.6806 0.1773 0.038 Uiso 1 1 calc R . . H51B H 0.2423 0.6540 0.1372 0.038 Uiso 1 1 calc R . . C52 C 0.2693(5) 0.8610(12) 0.1340(5) 0.034(2) Uani 1 1 d . . . H52A H 0.2261 0.8985 0.1185 0.051 Uiso 1 1 calc R . . H52B H 0.2807 0.8450 0.1020 0.051 Uiso 1 1 calc R . . H52C H 0.2987 0.9297 0.1613 0.051 Uiso 1 1 calc R . . C53 C 0.1723(4) 0.7648(11) 0.2003(5) 0.030(2) Uani 1 1 d . . . H53A H 0.1620 0.7767 0.2335 0.036 Uiso 1 1 calc R . . H53B H 0.1614 0.8550 0.1781 0.036 Uiso 1 1 calc R . . C54 C 0.1307(5) 0.6467(12) 0.1614(6) 0.043(3) Uani 1 1 d . . . H54A H 0.1418 0.6305 0.1292 0.064 Uiso 1 1 calc R . . H54B H 0.0862 0.6748 0.1460 0.064 Uiso 1 1 calc R . . H54C H 0.1376 0.5589 0.1840 0.064 Uiso 1 1 calc R . . C55 C 0.2690(5) 0.5569(11) 0.2559(4) 0.026(2) Uani 1 1 d . . . H55A H 0.2427 0.4921 0.2239 0.031 Uiso 1 1 calc R . . H55B H 0.3137 0.5306 0.2681 0.031 Uiso 1 1 calc R . . C56 C 0.2531(6) 0.5318(12) 0.3065(5) 0.038(3) Uani 1 1 d . . . H56A H 0.2783 0.5962 0.3384 0.057 Uiso 1 1 calc R . . H56B H 0.2628 0.4329 0.3196 0.057 Uiso 1 1 calc R . . H56C H 0.2081 0.5502 0.2942 0.057 Uiso 1 1 calc R . . P3 P 0.77683(11) -0.2444(3) 0.49716(11) 0.0235(5) Uani 1 1 d . . . C61 C 0.6929(5) -0.2032(13) 0.4708(5) 0.038(3) Uani 1 1 d . . . H61A H 0.6833 -0.1967 0.5046 0.045 Uiso 1 1 calc R . . H61B H 0.6851 -0.1081 0.4522 0.045 Uiso 1 1 calc R . . C62 C 0.6471(6) -0.3082(16) 0.4278(7) 0.055(4) Uani 1 1 d . . . H62A H 0.6497 -0.3013 0.3908 0.082 Uiso 1 1 calc R . . H62B H 0.6040 -0.2859 0.4217 0.082 Uiso 1 1 calc R . . H62C H 0.6580 -0.4051 0.4431 0.082 Uiso 1 1 calc R . . C63 C 0.7847(6) -0.4216(12) 0.5261(6) 0.043(3) Uani 1 1 d . . . H63A H 0.7570 -0.4856 0.4945 0.051 Uiso 1 1 calc R . . H63B H 0.8288 -0.4533 0.5383 0.051 Uiso 1 1 calc R . . C64 C 0.7690(8) -0.4399(15) 0.5764(6) 0.055(4) Uani 1 1 d . . . H64A H 0.7940 -0.3729 0.6072 0.083 Uiso 1 1 calc R . . H64B H 0.7788 -0.5376 0.5910 0.083 Uiso 1 1 calc R . . H64C H 0.7239 -0.4212 0.5637 0.083 Uiso 1 1 calc R . . C65 C 0.7863(5) -0.2719(12) 0.4305(5) 0.032(2) Uani 1 1 d . . . H65A H 0.8279 -0.3166 0.4406 0.038 Uiso 1 1 calc R . . H65B H 0.7532 -0.3385 0.4049 0.038 Uiso 1 1 calc R . . C66 C 0.7818(7) -0.1350(15) 0.3979(5) 0.048(3) Uani 1 1 d . . . H66A H 0.7401 -0.0921 0.3864 0.073 Uiso 1 1 calc R . . H66B H 0.7879 -0.1555 0.3632 0.073 Uiso 1 1 calc R . . H66C H 0.8146 -0.0688 0.4229 0.073 Uiso 1 1 calc R . . P4 P 0.90927(12) 0.1118(3) 0.60344(13) 0.0321(6) Uani 1 1 d . . . C71 C 0.9957(6) 0.0951(16) 0.6330(7) 0.060(4) Uani 1 1 d . . . H71A H 1.0163 0.1736 0.6607 0.072 Uiso 1 1 calc R . . H71B H 1.0095 0.0037 0.6541 0.072 Uiso 1 1 calc R . . C72 C 1.0166(8) 0.101(2) 0.5805(9) 0.082(6) Uani 1 1 d . . . H72A H 0.9913 0.0331 0.5503 0.123 Uiso 1 1 calc R . . H72B H 1.0615 0.0767 0.5955 0.123 Uiso 1 1 calc R . . H72C H 1.0097 0.1975 0.5641 0.123 Uiso 1 1 calc R . . C73 C 0.8884(6) 0.2710(13) 0.5588(6) 0.042(3) Uani 1 1 d . . . H73A H 0.8516 0.3151 0.5614 0.051 Uiso 1 1 calc R . . H73B H 0.9240 0.3389 0.5762 0.051 Uiso 1 1 calc R . . C74 C 0.8729(8) 0.2573(18) 0.4960(7) 0.071(5) Uani 1 1 d . . . H74A H 0.9068 0.2054 0.4919 0.107 Uiso 1 1 calc R . . H74B H 0.8686 0.3523 0.4789 0.107 Uiso 1 1 calc R . . H74C H 0.8331 0.2051 0.4760 0.107 Uiso 1 1 calc R . . C75 C 0.8992(8) 0.1702(19) 0.6679(7) 0.067(4) Uani 1 1 d . . . H75A H 0.8532 0.1789 0.6561 0.080 Uiso 1 1 calc R . . H75B H 0.9150 0.0926 0.6969 0.080 Uiso 1 1 calc R . . C76 C 0.9296(9) 0.306(2) 0.6980(9) 0.085(6) Uani 1 1 d . . . H76A H 0.9745 0.2884 0.7231 0.128 Uiso 1 1 calc R . . H76B H 0.9089 0.3388 0.7216 0.128 Uiso 1 1 calc R . . H76C H 0.9254 0.3782 0.6691 0.128 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 Pt1 0.01205(17) 0.01514(18) 0.0235(2) 0.00177(13) 0.00812(13) 0.00237(12) Pt2 0.01797(18) 0.01872(19) 0.0268(2) 0.00162(14) 0.00905(15) 0.00585(13) C1 0.016(4) 0.023(5) 0.031(5) -0.004(4) 0.013(4) -0.003(4) C2 0.015(4) 0.027(5) 0.022(5) 0.002(4) 0.009(3) 0.003(4) N1 0.019(4) 0.019(4) 0.028(4) 0.007(3) 0.012(3) 0.003(3) C3 0.017(4) 0.017(4) 0.035(5) 0.004(4) 0.012(4) 0.000(3) C4 0.023(5) 0.031(5) 0.043(6) 0.002(5) 0.018(4) 0.008(4) C5 0.028(5) 0.034(6) 0.030(5) 0.005(4) 0.018(4) 0.010(4) C6 0.025(5) 0.025(5) 0.035(6) -0.002(4) 0.018(4) 0.000(4) C7 0.010(4) 0.018(4) 0.031(5) -0.003(4) 0.012(4) -0.001(3) N2 0.013(3) 0.018(4) 0.029(4) -0.001(3) 0.009(3) 0.006(3) C8 0.008(4) 0.020(4) 0.027(5) 0.001(4) 0.008(3) -0.001(3) C9 0.016(4) 0.020(4) 0.026(5) -0.003(4) 0.007(4) 0.003(3) C10 0.020(4) 0.027(5) 0.027(5) -0.003(4) 0.012(4) 0.002(4) C11 0.022(4) 0.019(4) 0.029(5) 0.001(4) 0.005(4) 0.004(4) C12 0.011(4) 0.020(4) 0.030(5) -0.005(4) 0.005(4) 0.004(3) C13 0.020(5) 0.020(5) 0.029(5) 0.002(4) 0.004(4) 0.003(4) C14 0.023(5) 0.022(5) 0.032(5) -0.002(4) 0.012(4) -0.001(4) C21 0.013(4) 0.022(5) 0.034(5) -0.005(4) 0.012(4) -0.006(3) C22 0.020(4) 0.021(4) 0.027(5) -0.001(4) 0.009(4) 0.001(4) C23 0.021(5) 0.028(5) 0.051(7) -0.001(5) 0.020(5) 0.006(4) C24 0.019(5) 0.036(6) 0.048(7) 0.004(5) 0.012(4) 0.013(4) C25 0.033(6) 0.032(6) 0.044(7) 0.010(5) 0.015(5) 0.010(5) C26 0.018(4) 0.023(5) 0.039(6) 0.010(4) 0.013(4) 0.012(4) C31 0.019(5) 0.029(6) 0.055(7) -0.001(5) 0.021(5) 0.006(4) C32 0.029(6) 0.042(7) 0.053(7) -0.004(6) 0.018(5) 0.004(5) C33 0.024(5) 0.055(8) 0.073(9) -0.017(7) 0.026(6) 0.006(5) C34 0.025(6) 0.032(6) 0.098(12) -0.014(7) 0.026(7) -0.001(5) C35 0.033(6) 0.033(6) 0.082(10) 0.021(7) 0.021(6) 0.011(5) C36 0.020(5) 0.049(7) 0.058(8) 0.016(6) 0.019(5) 0.014(5) P1 0.0156(10) 0.0202(11) 0.0286(13) -0.0006(10) 0.0090(9) -0.0002(9) C41 0.010(4) 0.036(6) 0.039(6) -0.005(5) 0.007(4) 0.000(4) C42 0.029(6) 0.049(7) 0.047(7) -0.005(6) 0.007(5) 0.008(5) C43 0.030(5) 0.019(5) 0.035(6) -0.001(4) 0.006(4) -0.004(4) C44 0.049(7) 0.028(6) 0.047(7) 0.008(5) 0.024(6) -0.008(5) C45 0.029(5) 0.037(6) 0.031(5) -0.010(5) 0.018(4) -0.008(4) C46 0.041(6) 0.032(6) 0.048(7) -0.010(5) 0.017(5) -0.012(5) P2 0.0128(10) 0.0165(11) 0.0291(12) 0.0018(10) 0.0083(9) 0.0013(8) C51 0.031(5) 0.036(6) 0.031(5) -0.001(5) 0.016(4) 0.004(4) C52 0.036(6) 0.037(6) 0.028(6) 0.005(5) 0.012(4) -0.001(5) C53 0.014(4) 0.026(5) 0.046(6) 0.002(5) 0.010(4) -0.003(4) C54 0.011(4) 0.033(6) 0.072(9) -0.007(6) 0.008(5) -0.003(4) C55 0.025(5) 0.026(5) 0.027(5) 0.002(4) 0.012(4) 0.008(4) C56 0.053(7) 0.031(6) 0.034(6) 0.002(5) 0.023(5) -0.013(5) P3 0.0235(12) 0.0197(11) 0.0300(13) 0.0012(10) 0.0142(10) 0.0018(9) C61 0.020(5) 0.041(6) 0.053(7) -0.018(6) 0.017(5) -0.004(4) C62 0.037(7) 0.054(8) 0.062(9) -0.008(7) 0.011(6) -0.015(6) C63 0.050(7) 0.027(6) 0.041(7) 0.001(5) 0.011(6) 0.007(5) C64 0.084(10) 0.041(7) 0.056(9) 0.003(6) 0.045(8) -0.018(7) C65 0.032(5) 0.032(6) 0.034(6) -0.004(5) 0.017(4) -0.005(4) C66 0.075(9) 0.049(8) 0.023(6) 0.005(5) 0.023(6) -0.012(7) P4 0.0217(12) 0.0259(13) 0.0366(15) 0.0009(12) 0.0019(11) 0.0000(10) C71 0.026(6) 0.052(8) 0.074(10) -0.009(7) -0.004(6) 0.015(6) C72 0.055(10) 0.093(14) 0.104(15) 0.019(12) 0.040(10) 0.018(9) C73 0.041(6) 0.038(6) 0.051(7) 0.005(6) 0.023(6) -0.004(5) C74 0.060(9) 0.069(10) 0.059(9) 0.013(8) 0.002(7) -0.033(8) C75 0.069(10) 0.074(11) 0.057(9) -0.025(8) 0.027(8) -0.028(9) C76 0.078(12) 0.087(13) 0.112(15) -0.054(12) 0.061(12) -0.041(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 2.022(9) . ? Pt1 C21 2.074(9) . ? Pt1 P2 2.287(2) . ? Pt1 P1 2.291(2) . ? Pt2 C14 2.026(10) . ? Pt2 C31 2.086(10) . ? Pt2 P4 2.286(3) . ? Pt2 P3 2.292(3) . ? C1 C2 1.199(13) . ? C2 C3 1.433(13) . ? N1 C3 1.352(13) . ? N1 C7 1.357(11) . ? C3 C4 1.387(15) . ? C4 C5 1.384(14) . ? C5 C6 1.396(15) . ? C6 C7 1.386(13) . ? C7 C8 1.498(13) . ? N2 C12 1.354(12) . ? N2 C8 1.356(11) . ? C8 C9 1.387(13) . ? C9 C10 1.375(14) . ? C10 C11 1.377(13) . ? C11 C12 1.398(14) . ? C12 C13 1.452(12) . ? C13 C14 1.195(14) . ? C21 C22 1.386(13) . ? C21 C26 1.408(14) . ? C22 C23 1.400(13) . ? C23 C24 1.388(16) . ? C24 C25 1.399(17) . ? C25 C26 1.373(14) . ? C31 C36 1.394(17) . ? C31 C32 1.407(16) . ? C32 C33 1.409(16) . ? C33 C34 1.39(2) . ? C34 C35 1.39(2) . ? C35 C36 1.385(16) . ? P1 C43 1.807(10) . ? P1 C41 1.827(9) . ? P1 C45 1.836(10) . ? C41 C42 1.537(17) . ? C43 C44 1.546(16) . ? C45 C46 1.524(15) . ? P2 C55 1.793(10) . ? P2 C51 1.825(11) . ? P2 C53 1.827(9) . ? C51 C52 1.515(15) . ? C53 C54 1.524(15) . ? C55 C56 1.518(14) . ? P3 C63 1.798(12) . ? P3 C61 1.826(10) . ? P3 C65 1.838(11) . ? C61 C62 1.519(17) . ? C63 C64 1.500(18) . ? C65 C66 1.511(16) . ? P4 C73 1.816(13) . ? P4 C71 1.841(13) . ? P4 C75 1.854(16) . ? C71 C72 1.63(3) . ? C73 C74 1.49(2) . ? C75 C76 1.50(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 C1 Pt1 C21 177.5(4) . . ? C1 Pt1 P2 86.4(3) . . ? C21 Pt1 P2 91.7(3) . . ? C1 Pt1 P1 94.7(3) . . ? C21 Pt1 P1 87.3(3) . . ? P2 Pt1 P1 173.70(9) . . ? C14 Pt2 C31 177.1(4) . . ? C14 Pt2 P4 87.4(3) . . ? C31 Pt2 P4 94.3(3) . . ? C14 Pt2 P3 89.9(3) . . ? C31 Pt2 P3 88.7(3) . . ? P4 Pt2 P3 173.24(10) . . ? C2 C1 Pt1 174.4(8) . . ? C1 C2 C3 176.8(10) . . ? C3 N1 C7 117.1(8) . . ? N1 C3 C4 122.8(9) . . ? N1 C3 C2 116.4(9) . . ? C4 C3 C2 120.9(9) . . ? C5 C4 C3 119.7(10) . . ? C4 C5 C6 118.3(10) . . ? C7 C6 C5 118.9(9) . . ? N1 C7 C6 123.2(9) . . ? N1 C7 C8 115.4(8) . . ? C6 C7 C8 121.3(8) . . ? C12 N2 C8 117.1(8) . . ? N2 C8 C9 121.7(8) . . ? N2 C8 C7 115.7(8) . . ? C9 C8 C7 122.5(8) . . ? C10 C9 C8 120.1(8) . . ? C9 C10 C11 119.6(9) . . ? C10 C11 C12 117.6(9) . . ? N2 C12 C11 123.8(8) . . ? N2 C12 C13 116.1(8) . . ? C11 C12 C13 120.1(9) . . ? C14 C13 C12 176.2(11) . . ? C13 C14 Pt2 178.7(9) . . ? C22 C21 C26 116.3(9) . . ? C22 C21 Pt1 119.8(7) . . ? C26 C21 Pt1 123.8(7) . . ? C21 C22 C23 122.5(10) . . ? C24 C23 C22 118.9(10) . . ? C23 C24 C25 120.2(9) . . ? C26 C25 C24 119.0(10) . . ? C25 C26 C21 122.9(10) . . ? C36 C31 C32 117.7(10) . . ? C36 C31 Pt2 121.1(8) . . ? C32 C31 Pt2 121.3(9) . . ? C31 C32 C33 119.6(12) . . ? C34 C33 C32 121.7(12) . . ? C33 C34 C35 118.3(11) . . ? C36 C35 C34 120.7(14) . . ? C35 C36 C31 122.0(12) . . ? C43 P1 C41 103.1(5) . . ? C43 P1 C45 105.0(5) . . ? C41 P1 C45 104.8(5) . . ? C43 P1 Pt1 110.6(3) . . ? C41 P1 Pt1 117.7(4) . . ? C45 P1 Pt1 114.4(3) . . ? C42 C41 P1 115.2(8) . . ? C44 C43 P1 113.5(7) . . ? C46 C45 P1 116.5(8) . . ? C55 P2 C51 103.2(5) . . ? C55 P2 C53 104.4(5) . . ? C51 P2 C53 105.9(5) . . ? C55 P2 Pt1 115.2(3) . . ? C51 P2 Pt1 109.8(4) . . ? C53 P2 Pt1 117.1(4) . . ? C52 C51 P2 114.7(8) . . ? C54 C53 P2 115.2(7) . . ? C56 C55 P2 115.4(7) . . ? C63 P3 C61 104.3(6) . . ? C63 P3 C65 102.8(6) . . ? C61 P3 C65 103.7(5) . . ? C63 P3 Pt2 117.5(4) . . ? C61 P3 Pt2 115.1(4) . . ? C65 P3 Pt2 111.7(4) . . ? C62 C61 P3 116.1(9) . . ? C64 C63 P3 116.2(9) . . ? C66 C65 P3 112.8(8) . . ? C73 P4 C71 105.9(7) . . ? C73 P4 C75 102.4(7) . . ? C71 P4 C75 102.0(8) . . ? C73 P4 Pt2 110.7(4) . . ? C71 P4 Pt2 120.7(5) . . ? C75 P4 Pt2 113.1(5) . . ? C72 C71 P4 109.7(10) . . ? C74 C73 P4 118.7(11) . . ? C76 C75 P4 119.5(13) . . ? 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 C21 Pt1 C1 C2 -6(16) . . . . ? P2 Pt1 C1 C2 -50(9) . . . . ? P1 Pt1 C1 C2 137(9) . . . . ? Pt1 C1 C2 C3 116(17) . . . . ? C7 N1 C3 C4 2.2(13) . . . . ? C7 N1 C3 C2 -178.0(8) . . . . ? C1 C2 C3 N1 175(100) . . . . ? C1 C2 C3 C4 -5(19) . . . . ? N1 C3 C4 C5 0.7(15) . . . . ? C2 C3 C4 C5 -179.1(9) . . . . ? C3 C4 C5 C6 -2.1(16) . . . . ? C4 C5 C6 C7 0.6(15) . . . . ? C3 N1 C7 C6 -3.8(13) . . . . ? C3 N1 C7 C8 178.7(7) . . . . ? C5 C6 C7 N1 2.4(14) . . . . ? C5 C6 C7 C8 179.7(9) . . . . ? C12 N2 C8 C9 2.2(13) . . . . ? C12 N2 C8 C7 179.9(8) . . . . ? N1 C7 C8 N2 -170.4(8) . . . . ? C6 C7 C8 N2 12.1(12) . . . . ? N1 C7 C8 C9 7.3(12) . . . . ? C6 C7 C8 C9 -170.2(9) . . . . ? N2 C8 C9 C10 -3.7(14) . . . . ? C7 C8 C9 C10 178.7(8) . . . . ? C8 C9 C10 C11 2.2(14) . . . . ? C9 C10 C11 C12 0.5(14) . . . . ? C8 N2 C12 C11 0.6(13) . . . . ? C8 N2 C12 C13 -179.7(8) . . . . ? C10 C11 C12 N2 -2.0(14) . . . . ? C10 C11 C12 C13 178.4(9) . . . . ? N2 C12 C13 C14 -141(16) . . . . ? C11 C12 C13 C14 39(17) . . . . ? C12 C13 C14 Pt2 52(51) . . . . ? C31 Pt2 C14 C13 -41(45) . . . . ? P4 Pt2 C14 C13 -166(100) . . . . ? P3 Pt2 C14 C13 20(40) . . . . ? C1 Pt1 C21 C22 59(9) . . . . ? P2 Pt1 C21 C22 102.1(7) . . . . ? P1 Pt1 C21 C22 -84.1(7) . . . . ? C1 Pt1 C21 C26 -118(9) . . . . ? P2 Pt1 C21 C26 -75.1(8) . . . . ? P1 Pt1 C21 C26 98.7(8) . . . . ? C26 C21 C22 C23 -2.4(14) . . . . ? Pt1 C21 C22 C23 -179.7(7) . . . . ? C21 C22 C23 C24 3.1(15) . . . . ? C22 C23 C24 C25 -2.3(17) . . . . ? C23 C24 C25 C26 0.8(17) . . . . ? C24 C25 C26 C21 0.0(17) . . . . ? C22 C21 C26 C25 0.8(15) . . . . ? Pt1 C21 C26 C25 178.0(8) . . . . ? C14 Pt2 C31 C36 -42(9) . . . . ? P4 Pt2 C31 C36 83.5(9) . . . . ? P3 Pt2 C31 C36 -102.6(9) . . . . ? C14 Pt2 C31 C32 136(8) . . . . ? P4 Pt2 C31 C32 -98.1(9) . . . . ? P3 Pt2 C31 C32 75.8(9) . . . . ? C36 C31 C32 C33 2.7(17) . . . . ? Pt2 C31 C32 C33 -175.8(9) . . . . ? C31 C32 C33 C34 -0.7(19) . . . . ? C32 C33 C34 C35 -2.4(19) . . . . ? C33 C34 C35 C36 3.5(19) . . . . ? C34 C35 C36 C31 -1(2) . . . . ? C32 C31 C36 C35 -1.7(18) . . . . ? Pt2 C31 C36 C35 176.8(10) . . . . ? C1 Pt1 P1 C43 127.3(5) . . . . ? C21 Pt1 P1 C43 -54.2(5) . . . . ? P2 Pt1 P1 C43 27.2(9) . . . . ? C1 Pt1 P1 C41 9.2(5) . . . . ? C21 Pt1 P1 C41 -172.3(5) . . . . ? P2 Pt1 P1 C41 -90.9(8) . . . . ? C1 Pt1 P1 C45 -114.4(5) . . . . ? C21 Pt1 P1 C45 64.1(5) . . . . ? P2 Pt1 P1 C45 145.5(8) . . . . ? C43 P1 C41 C42 162.4(8) . . . . ? C45 P1 C41 C42 52.7(10) . . . . ? Pt1 P1 C41 C42 -75.6(9) . . . . ? C41 P1 C43 C44 71.1(9) . . . . ? C45 P1 C43 C44 -179.4(8) . . . . ? Pt1 P1 C43 C44 -55.5(8) . . . . ? C43 P1 C45 C46 -53.8(10) . . . . ? C41 P1 C45 C46 54.5(10) . . . . ? Pt1 P1 C45 C46 -175.2(7) . . . . ? C1 Pt1 P2 C55 46.5(4) . . . . ? C21 Pt1 P2 C55 -131.8(4) . . . . ? P1 Pt1 P2 C55 147.0(8) . . . . ? C1 Pt1 P2 C51 -69.5(5) . . . . ? C21 Pt1 P2 C51 112.3(5) . . . . ? P1 Pt1 P2 C51 31.1(9) . . . . ? C1 Pt1 P2 C53 169.7(5) . . . . ? C21 Pt1 P2 C53 -8.5(5) . . . . ? P1 Pt1 P2 C53 -89.7(8) . . . . ? C55 P2 C51 C52 -177.5(8) . . . . ? C53 P2 C51 C52 73.1(9) . . . . ? Pt1 P2 C51 C52 -54.2(8) . . . . ? C55 P2 C53 C54 -48.2(10) . . . . ? C51 P2 C53 C54 60.4(10) . . . . ? Pt1 P2 C53 C54 -176.8(8) . . . . ? C51 P2 C55 C56 -174.6(8) . . . . ? C53 P2 C55 C56 -64.0(9) . . . . ? Pt1 P2 C55 C56 65.7(8) . . . . ? C14 Pt2 P3 C63 -132.0(6) . . . . ? C31 Pt2 P3 C63 45.5(6) . . . . ? P4 Pt2 P3 C63 161.4(9) . . . . ? C14 Pt2 P3 C61 -8.4(6) . . . . ? C31 Pt2 P3 C61 169.1(6) . . . . ? P4 Pt2 P3 C61 -75.0(10) . . . . ? C14 Pt2 P3 C65 109.6(5) . . . . ? C31 Pt2 P3 C65 -72.9(5) . . . . ? P4 Pt2 P3 C65 43.0(9) . . . . ? C63 P3 C61 C62 -55.0(12) . . . . ? C65 P3 C61 C62 52.3(12) . . . . ? Pt2 P3 C61 C62 174.6(9) . . . . ? C61 P3 C63 C64 -62.6(12) . . . . ? C65 P3 C63 C64 -170.6(11) . . . . ? Pt2 P3 C63 C64 66.3(12) . . . . ? C63 P3 C65 C66 -179.7(9) . . . . ? C61 P3 C65 C66 71.9(10) . . . . ? Pt2 P3 C65 C66 -52.7(9) . . . . ? C14 Pt2 P4 C73 -49.3(5) . . . . ? C31 Pt2 P4 C73 133.0(5) . . . . ? P3 Pt2 P4 C73 17.4(10) . . . . ? C14 Pt2 P4 C71 -173.9(7) . . . . ? C31 Pt2 P4 C71 8.5(8) . . . . ? P3 Pt2 P4 C71 -107.1(10) . . . . ? C14 Pt2 P4 C75 65.0(7) . . . . ? C31 Pt2 P4 C75 -112.7(8) . . . . ? P3 Pt2 P4 C75 131.7(10) . . . . ? C73 P4 C71 C72 -52.7(12) . . . . ? C75 P4 C71 C72 -159.5(12) . . . . ? Pt2 P4 C71 C72 74.0(12) . . . . ? C71 P4 C73 C74 90.6(12) . . . . ? C75 P4 C73 C74 -162.8(11) . . . . ? Pt2 P4 C73 C74 -42.0(11) . . . . ? C73 P4 C75 C76 -50.3(17) . . . . ? C71 P4 C75 C76 59.3(17) . . . . ? Pt2 P4 C75 C76 -169.5(14) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 5.267 _refine_diff_density_min -3.068 _refine_diff_density_rms 0.224 #END