# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H18 Ga3 P2 Pd2, 3(C10 H15)' _chemical_formula_sum 'C36 H63 Ga3 P2 Pd2' _chemical_formula_weight 979.76 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 18.0920(5) _cell_length_b 15.1214(4) _cell_length_c 18.3971(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.738(2) _cell_angle_gamma 90.00 _cell_volume 4889.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 200 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 2.438 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4507 _exptl_absorpt_correction_T_max 0.8326 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '560 images at 1.0 deg. in \w and 25 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44900 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8937 _reflns_number_gt 6445 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _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^)+(0.0692P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8937 _refine_ls_number_parameters 438 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1254 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.097 _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 Pd4 Pd 0.18001(3) 0.7500 0.01640(3) 0.02258(16) Uani 1 2 d S . . C4 C 0.6407(4) 0.5042(5) -0.5916(5) 0.060(2) Uani 1 1 d U . . P4 P 0.08984(12) 0.7500 -0.09299(11) 0.0271(5) Uani 1 2 d S . . Ga4 Ga 0.14418(5) 0.7500 0.13710(5) 0.0264(2) Uani 1 2 d S . . Pd3 Pd 0.28332(4) 0.7500 0.14345(3) 0.02720(17) Uani 1 2 d S . . C3 C 0.6649(4) 0.5140(4) -0.6584(4) 0.053(2) Uani 1 1 d U . . P3 P 0.37511(14) 0.7500 0.25168(12) 0.0443(7) Uani 1 2 d S . . Ga3 Ga 0.27134(4) 0.62616(5) 0.05246(4) 0.0406(2) Uani 1 1 d . . . Pd2 Pd 0.71149(3) 0.7500 -0.49117(3) 0.02518(17) Uani 1 2 d S . . C2 C 0.7436(4) 0.4970(4) -0.6434(3) 0.0330(15) Uani 1 1 d . . . P2 P 0.61844(13) 0.7500 -0.42689(11) 0.0331(6) Uani 1 2 d S . . Ga2 Ga 0.85055(5) 0.7500 -0.43172(4) 0.0258(2) Uani 1 2 d S . . Pd1 Pd 0.81547(3) 0.7500 -0.56927(3) 0.02330(16) Uani 1 2 d S . . C1 C 0.7675(4) 0.4784(6) -0.5674(3) 0.061(2) Uani 1 1 d . . . P1 P 0.90645(13) 0.7500 -0.63619(12) 0.0304(5) Uani 1 2 d S . . Ga1 Ga 0.72367(4) 0.62624(5) -0.57665(4) 0.0408(2) Uani 1 1 d . . . C9 C 0.5611(6) 0.5118(8) -0.5772(8) 0.130(4) Uani 1 1 d U . . H9A H 0.5255 0.5335 -0.6224 0.195 Uiso 1 1 calc R . . H9B H 0.5623 0.5531 -0.5359 0.195 Uiso 1 1 calc R . . H9C H 0.5444 0.4535 -0.5640 0.195 Uiso 1 1 calc R . . C10 C 0.7056(8) 0.4666(9) -0.4522(6) 0.146(5) Uani 1 1 d U . . H10A H 0.7375 0.4152 -0.4337 0.219 Uiso 1 1 calc R . . H10B H 0.6538 0.4560 -0.4467 0.219 Uiso 1 1 calc R . . H10C H 0.7266 0.5190 -0.4232 0.219 Uiso 1 1 calc R . . C11 C 0.8897(3) 0.7046(4) -0.3052(3) 0.0278(13) Uani 1 1 d . . . C12 C 0.9463(3) 0.6743(4) -0.3416(3) 0.0308(14) Uani 1 1 d . . . C8 C 0.6158(7) 0.5337(7) -0.7341(5) 0.130(4) Uani 1 1 d U . . H8A H 0.5624 0.5350 -0.7314 0.195 Uiso 1 1 calc R . . H8B H 0.6229 0.4877 -0.7693 0.195 Uiso 1 1 calc R . . H8C H 0.6300 0.5913 -0.7512 0.195 Uiso 1 1 calc R . . C7 C 0.7920(6) 0.4955(6) -0.6982(5) 0.093(4) Uani 1 1 d . . . H7A H 0.7620 0.5146 -0.7472 0.140 Uiso 1 1 calc R . . H7B H 0.8108 0.4352 -0.7020 0.140 Uiso 1 1 calc R . . H7C H 0.8353 0.5356 -0.6814 0.140 Uiso 1 1 calc R . . C6 C 0.8497(6) 0.4591(9) -0.5270(6) 0.125(4) Uani 1 1 d U . . H6A H 0.8804 0.4517 -0.5639 0.187 Uiso 1 1 calc R . . H6B H 0.8516 0.4047 -0.4977 0.187 Uiso 1 1 calc R . . H6C H 0.8698 0.5084 -0.4936 0.187 Uiso 1 1 calc R . . C5 C 0.7040(6) 0.4820(5) -0.5363(4) 0.074(3) Uani 1 1 d . . . C40 C 0.1214(6) 0.7500 -0.1794(5) 0.045(2) Uani 1 2 d S . . H40A H 0.0788 0.7656 -0.2212 0.068 Uiso 0.50 1 calc PR . . H40B H 0.1402 0.6910 -0.1879 0.068 Uiso 0.50 1 calc PR . . H40C H 0.1624 0.7933 -0.1759 0.068 Uiso 0.50 1 calc PR . . C15 C 0.9699(5) 0.5804(5) -0.3512(4) 0.059(2) Uani 1 1 d . . . H15A H 0.9280 0.5403 -0.3487 0.088 Uiso 1 1 calc R . . H15B H 1.0146 0.5656 -0.3114 0.088 Uiso 1 1 calc R . . H15C H 0.9824 0.5741 -0.4000 0.088 Uiso 1 1 calc R . . C14 C 0.8390(4) 0.6451(5) -0.2728(4) 0.056(2) Uani 1 1 d . . . H14A H 0.7965 0.6795 -0.2632 0.083 Uiso 1 1 calc R . . H14B H 0.8683 0.6195 -0.2258 0.083 Uiso 1 1 calc R . . H14C H 0.8194 0.5976 -0.3083 0.083 Uiso 1 1 calc R . . C13 C 0.9819(4) 0.7500 -0.3625(4) 0.0260(18) Uani 1 2 d S . . C22 C 0.2551(4) 0.4977(4) -0.0234(3) 0.0403(17) Uani 1 1 d . . . C21 C 0.2319(4) 0.4755(6) 0.0426(4) 0.054(2) Uani 1 1 d . . . C20 C 0.6127(4) 0.6564(6) -0.3649(4) 0.070(3) Uani 1 1 d . . . H20A H 0.6059 0.6014 -0.3939 0.105 Uiso 1 1 calc R . . H20B H 0.5694 0.6649 -0.3422 0.105 Uiso 1 1 calc R . . H20C H 0.6597 0.6530 -0.3255 0.105 Uiso 1 1 calc R . . C19 C 0.5218(5) 0.7500 -0.4835(5) 0.055(3) Uani 1 2 d S . . H19A H 0.5172 0.7932 -0.5241 0.082 Uiso 0.50 1 calc PR . . H19B H 0.4868 0.7659 -0.4524 0.082 Uiso 0.50 1 calc PR . . H19C H 0.5090 0.6910 -0.5048 0.082 Uiso 0.50 1 calc PR . . C18 C 0.8749(6) 0.7500 -0.7394(5) 0.060(3) Uani 1 2 d S . . H18A H 0.9180 0.7650 -0.7609 0.090 Uiso 0.50 1 calc PR . . H18B H 0.8344 0.7938 -0.7553 0.090 Uiso 0.50 1 calc PR . . H18C H 0.8557 0.6912 -0.7567 0.090 Uiso 0.50 1 calc PR . . C17 C 0.9735(4) 0.6572(5) -0.6213(4) 0.053(2) Uani 1 1 d . . . H17A H 0.9457 0.6020 -0.6363 0.080 Uiso 1 1 calc R . . H17B H 0.9997 0.6539 -0.5682 0.080 Uiso 1 1 calc R . . H17C H 1.0109 0.6659 -0.6514 0.080 Uiso 1 1 calc R . . C16 C 1.0470(5) 0.7500 -0.4006(5) 0.048(3) Uani 1 2 d S . . H16A H 1.0941 0.7334 -0.3645 0.073 Uiso 0.50 1 calc PR . . H16B H 1.0528 0.8092 -0.4202 0.073 Uiso 0.50 1 calc PR . . H16C H 1.0366 0.7074 -0.4419 0.073 Uiso 0.50 1 calc PR . . C23 C 0.3325(4) 0.5189(5) -0.0046(4) 0.0482(19) Uani 1 1 d . . . C31 C 0.0121(5) 0.7500 0.1453(4) 0.0297(19) Uani 1 2 d S . . C30 C 0.2965(8) 0.4646(9) 0.1840(5) 0.150(7) Uani 1 1 d . . . H30A H 0.2493 0.4338 0.1858 0.225 Uiso 1 1 calc R . . H30B H 0.2992 0.5207 0.2112 0.225 Uiso 1 1 calc R . . H30C H 0.3402 0.4276 0.2074 0.225 Uiso 1 1 calc R . . C29 C 0.4397(4) 0.5209(7) 0.1181(6) 0.090(3) Uani 1 1 d . . . H29A H 0.4657 0.4636 0.1239 0.136 Uiso 1 1 calc R . . H29B H 0.4397 0.5448 0.1676 0.136 Uiso 1 1 calc R . . H29C H 0.4662 0.5619 0.0918 0.136 Uiso 1 1 calc R . . C28 C 0.3792(6) 0.5446(8) -0.0585(6) 0.111(4) Uani 1 1 d U . . H28A H 0.4077 0.4931 -0.0692 0.166 Uiso 1 1 calc R . . H28B H 0.4149 0.5916 -0.0364 0.166 Uiso 1 1 calc R . . H28C H 0.3456 0.5661 -0.1050 0.166 Uiso 1 1 calc R . . C27 C 0.2022(5) 0.4959(6) -0.1007(4) 0.074(3) Uani 1 1 d . . . H27A H 0.2275 0.5234 -0.1365 0.112 Uiso 1 1 calc R . . H27B H 0.1556 0.5286 -0.1001 0.112 Uiso 1 1 calc R . . H27C H 0.1894 0.4345 -0.1155 0.112 Uiso 1 1 calc R . . C26 C 0.1545(6) 0.4497(9) 0.0500(5) 0.114(5) Uani 1 1 d . . . H26A H 0.1161 0.4748 0.0084 0.171 Uiso 1 1 calc R . . H26B H 0.1464 0.4724 0.0974 0.171 Uiso 1 1 calc R . . H26C H 0.1501 0.3851 0.0493 0.171 Uiso 1 1 calc R . . C25 C 0.2977(5) 0.4827(6) 0.1028(4) 0.061(2) Uani 1 1 d . . . C24 C 0.3592(4) 0.5090(5) 0.0740(4) 0.0481(18) Uani 1 1 d . . . C38 C 0.4735(5) 0.7500 0.2437(5) 0.044(2) Uani 1 2 d S . . H38A H 0.4797 0.7937 0.2062 0.067 Uiso 0.50 1 calc PR . . H38B H 0.4867 0.6912 0.2283 0.067 Uiso 0.50 1 calc PR . . H38C H 0.5071 0.7651 0.2922 0.067 Uiso 0.50 1 calc PR . . C37 C 0.3785(5) 0.6532(7) 0.3147(4) 0.093(3) Uani 1 1 d U . . H37A H 0.3822 0.5987 0.2869 0.140 Uiso 1 1 calc R . . H37B H 0.3322 0.6517 0.3335 0.140 Uiso 1 1 calc R . . H37C H 0.4231 0.6581 0.3569 0.140 Uiso 1 1 calc R . . C36 C 0.1565(4) 0.6446(5) 0.3011(4) 0.0510(19) Uani 1 1 d . . . H36A H 0.1775 0.5981 0.2749 0.077 Uiso 1 1 calc R . . H36B H 0.1274 0.6176 0.3340 0.077 Uiso 1 1 calc R . . H36C H 0.1981 0.6800 0.3312 0.077 Uiso 1 1 calc R . . C35 C 0.0269(5) 0.5796(5) 0.1620(4) 0.055(2) Uani 1 1 d . . . H35A H 0.0068 0.5755 0.1077 0.083 Uiso 1 1 calc R . . H35B H -0.0120 0.5597 0.1875 0.083 Uiso 1 1 calc R . . H35C H 0.0722 0.5422 0.1770 0.083 Uiso 1 1 calc R . . C34 C -0.0520(5) 0.7500 0.0771(5) 0.045(2) Uani 1 2 d S . . H34A H -0.0381 0.7858 0.0380 0.068 Uiso 0.50 1 calc PR . . H34B H -0.0975 0.7750 0.0894 0.068 Uiso 0.50 1 calc PR . . H34C H -0.0625 0.6892 0.0591 0.068 Uiso 0.50 1 calc PR . . C33 C 0.1058(3) 0.7022(4) 0.2459(3) 0.0337(14) Uani 1 1 d . . . C32 C 0.0479(3) 0.6746(4) 0.1832(3) 0.0296(14) Uani 1 1 d . . . C39 C 0.0236(4) 0.6582(5) -0.1098(4) 0.0480(18) Uani 1 1 d . . . H39A H -0.0137 0.6672 -0.1575 0.072 Uiso 1 1 calc R . . H39B H -0.0028 0.6547 -0.0692 0.072 Uiso 1 1 calc R . . H39C H 0.0514 0.6030 -0.1120 0.072 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 Pd4 0.0206(3) 0.0319(4) 0.0141(3) 0.000 0.0019(2) 0.000 C4 0.043(4) 0.027(4) 0.118(6) -0.009(4) 0.035(4) -0.008(3) P4 0.0273(12) 0.0318(13) 0.0188(10) 0.000 -0.0015(8) 0.000 Ga4 0.0263(5) 0.0329(6) 0.0229(4) 0.000 0.0113(4) 0.000 Pd3 0.0220(3) 0.0447(4) 0.0134(3) 0.000 0.0014(2) 0.000 C3 0.059(5) 0.024(4) 0.054(4) -0.014(3) -0.033(4) 0.006(3) P3 0.0306(14) 0.076(2) 0.0210(11) 0.000 -0.0039(9) 0.000 Ga3 0.0384(4) 0.0564(5) 0.0239(3) -0.0089(3) 0.0011(3) 0.0225(4) Pd2 0.0222(3) 0.0397(4) 0.0145(3) 0.000 0.0060(2) 0.000 C2 0.043(4) 0.032(4) 0.023(3) -0.007(3) 0.006(3) -0.013(3) P2 0.0223(12) 0.0594(16) 0.0184(10) 0.000 0.0068(9) 0.000 Ga2 0.0246(5) 0.0339(6) 0.0178(4) 0.000 0.0026(4) 0.000 Pd1 0.0244(3) 0.0299(4) 0.0177(3) 0.000 0.0093(2) 0.000 C1 0.064(5) 0.085(6) 0.031(4) 0.005(4) 0.007(3) 0.053(5) P1 0.0347(13) 0.0324(13) 0.0309(11) 0.000 0.0213(10) 0.000 Ga1 0.0425(4) 0.0532(5) 0.0313(4) -0.0206(3) 0.0177(3) -0.0222(4) C9 0.084(7) 0.101(7) 0.216(9) -0.054(7) 0.056(7) -0.020(6) C10 0.199(10) 0.150(9) 0.116(7) 0.051(6) 0.094(7) 0.061(8) C11 0.020(3) 0.042(3) 0.017(3) 0.013(2) -0.005(2) -0.002(3) C12 0.030(3) 0.028(3) 0.028(3) 0.003(2) -0.004(3) 0.002(3) C8 0.142(8) 0.111(7) 0.088(6) -0.045(5) -0.068(5) 0.061(6) C7 0.165(11) 0.068(6) 0.078(6) -0.042(5) 0.090(7) -0.051(7) C6 0.096(7) 0.170(9) 0.091(6) -0.045(6) -0.011(5) 0.067(6) C5 0.117(8) 0.057(6) 0.068(5) 0.041(4) 0.062(6) 0.050(5) C40 0.046(6) 0.057(7) 0.030(5) 0.000 0.002(4) 0.000 C15 0.060(5) 0.031(4) 0.078(5) 0.004(4) 0.001(4) 0.012(4) C14 0.042(4) 0.077(6) 0.046(4) 0.026(4) 0.006(3) -0.012(4) C13 0.021(4) 0.035(5) 0.020(4) 0.000 0.002(3) 0.000 C22 0.056(5) 0.035(4) 0.032(3) -0.001(3) 0.014(3) 0.018(3) C21 0.046(5) 0.082(6) 0.037(4) -0.002(4) 0.013(3) -0.017(4) C20 0.048(5) 0.113(7) 0.061(5) 0.042(5) 0.037(4) 0.009(5) C19 0.025(5) 0.093(9) 0.042(6) 0.000 -0.002(4) 0.000 C18 0.066(8) 0.089(9) 0.035(5) 0.000 0.031(5) 0.000 C17 0.054(5) 0.046(5) 0.070(5) 0.001(4) 0.037(4) 0.009(4) C16 0.036(6) 0.075(8) 0.036(5) 0.000 0.011(4) 0.000 C23 0.053(5) 0.034(4) 0.070(5) -0.018(3) 0.038(4) 0.006(3) C31 0.025(5) 0.033(5) 0.038(5) 0.000 0.020(4) 0.000 C30 0.201(15) 0.172(13) 0.056(6) 0.046(7) -0.012(7) -0.110(12) C29 0.036(5) 0.074(7) 0.146(9) -0.034(6) -0.009(5) 0.014(5) C28 0.115(7) 0.129(8) 0.120(7) -0.042(6) 0.092(6) -0.023(6) C27 0.112(8) 0.073(6) 0.031(4) -0.008(4) 0.002(4) 0.033(6) C26 0.074(7) 0.198(13) 0.074(6) -0.029(7) 0.026(5) -0.076(8) C25 0.069(6) 0.066(6) 0.036(4) 0.021(4) -0.012(4) -0.011(4) C24 0.025(4) 0.036(4) 0.076(5) -0.004(4) -0.003(3) 0.011(3) C38 0.037(6) 0.040(6) 0.048(6) 0.000 -0.008(4) 0.000 C37 0.062(5) 0.142(7) 0.059(5) 0.053(5) -0.018(4) -0.021(5) C36 0.046(4) 0.059(5) 0.051(4) 0.024(4) 0.015(3) 0.005(4) C35 0.057(5) 0.040(5) 0.069(5) -0.002(4) 0.015(4) -0.017(4) C34 0.038(6) 0.063(7) 0.030(5) 0.000 0.001(4) 0.000 C33 0.034(4) 0.038(3) 0.035(3) 0.010(3) 0.019(3) 0.002(3) C32 0.030(3) 0.027(3) 0.038(3) 0.000(3) 0.019(3) -0.002(3) C39 0.044(4) 0.050(5) 0.041(4) -0.004(3) -0.007(3) -0.013(4) _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 Pd4 P4 2.270(2) . ? Pd4 Ga4 2.4565(9) . ? Pd4 Ga3 2.4812(8) 4_575 ? Pd4 Ga3 2.4812(8) . ? Pd4 Pd3 2.6233(8) . ? C4 C5 1.380(12) . ? C4 C3 1.407(11) . ? C4 C9 1.530(12) . ? C4 Ga1 2.353(7) . ? P4 C39 1.812(7) . ? P4 C39 1.812(7) 4_575 ? P4 C40 1.813(9) . ? Ga4 C33 2.381(5) . ? Ga4 C33 2.381(5) 4_575 ? Ga4 C32 2.399(5) . ? Ga4 C32 2.399(5) 4_575 ? Ga4 C31 2.429(8) . ? Ga4 Pd3 2.4922(11) . ? Pd3 P3 2.270(2) . ? Pd3 Ga3 2.4866(8) 4_575 ? Pd3 Ga3 2.4866(8) . ? C3 C2 1.409(10) . ? C3 C8 1.492(10) . ? C3 Ga1 2.348(6) . ? P3 C38 1.821(10) . ? P3 C37 1.859(8) 4_575 ? P3 C37 1.859(8) . ? Ga3 C23 2.347(6) . ? Ga3 C24 2.350(7) . ? Ga3 C25 2.363(8) . ? Ga3 C22 2.369(6) . ? Ga3 C21 2.382(8) . ? Pd2 P2 2.275(2) . ? Pd2 Ga1 2.4877(7) 4_575 ? Pd2 Ga1 2.4877(7) . ? Pd2 Ga2 2.4938(11) . ? Pd2 Pd1 2.6245(8) . ? C2 C1 1.391(8) . ? C2 C7 1.484(9) . ? C2 Ga1 2.382(6) . ? P2 C19 1.811(9) . ? P2 C20 1.836(7) 4_575 ? P2 C20 1.836(7) . ? Ga2 C11 2.368(5) 4_575 ? Ga2 C11 2.368(5) . ? Ga2 C12 2.387(6) 4_575 ? Ga2 C12 2.387(6) . ? Ga2 C13 2.414(8) . ? Ga2 Pd1 2.4584(9) . ? Pd1 P1 2.278(2) . ? Pd1 Ga1 2.4843(8) . ? Pd1 Ga1 2.4843(8) 4_575 ? C1 C5 1.402(11) . ? C1 C6 1.524(12) . ? C1 Ga1 2.364(8) . ? P1 C17 1.833(7) 4_575 ? P1 C17 1.833(7) . ? P1 C18 1.848(9) . ? Ga1 C5 2.359(8) . ? C10 C5 1.557(12) . ? C11 C11 1.373(12) 4_575 ? C11 C12 1.424(8) . ? C11 C14 1.506(8) . ? C12 C13 1.411(7) . ? C12 C15 1.505(9) . ? C13 C12 1.411(7) 4_575 ? C13 C16 1.508(11) . ? C22 C23 1.397(10) . ? C22 C21 1.416(9) . ? C22 C27 1.513(9) . ? C21 C25 1.425(10) . ? C21 C26 1.492(11) . ? C23 C24 1.419(10) . ? C23 C28 1.499(10) . ? C31 C32 1.411(8) 4_575 ? C31 C32 1.411(8) . ? C31 C34 1.493(12) . ? C30 C25 1.525(11) . ? C29 C24 1.500(10) . ? C25 C24 1.400(10) . ? C36 C33 1.480(8) . ? C35 C32 1.513(9) . ? C33 C32 1.423(8) . ? C33 C33 1.446(13) 4_575 ? 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 P4 Pd4 Ga4 120.87(6) . . ? P4 Pd4 Ga3 121.99(3) . 4_575 ? Ga4 Pd4 Ga3 93.46(3) . 4_575 ? P4 Pd4 Ga3 121.99(3) . . ? Ga4 Pd4 Ga3 93.46(3) . . ? Ga3 Pd4 Ga3 98.00(4) 4_575 . ? P4 Pd4 Pd3 179.52(6) . . ? Ga4 Pd4 Pd3 58.65(3) . . ? Ga3 Pd4 Pd3 58.23(2) 4_575 . ? Ga3 Pd4 Pd3 58.23(2) . . ? C5 C4 C3 107.2(7) . . ? C5 C4 C9 122.7(9) . . ? C3 C4 C9 130.1(9) . . ? C5 C4 Ga1 73.2(5) . . ? C3 C4 Ga1 72.4(4) . . ? C9 C4 Ga1 121.5(6) . . ? C39 P4 C39 100.0(5) . 4_575 ? C39 P4 C40 100.6(3) . . ? C39 P4 C40 100.6(3) 4_575 . ? C39 P4 Pd4 117.3(2) . . ? C39 P4 Pd4 117.3(2) 4_575 . ? C40 P4 Pd4 117.9(3) . . ? C33 Ga4 C33 35.4(3) . 4_575 ? C33 Ga4 C32 34.6(2) . . ? C33 Ga4 C32 57.7(2) 4_575 . ? C33 Ga4 C32 57.7(2) . 4_575 ? C33 Ga4 C32 34.6(2) 4_575 4_575 ? C32 Ga4 C32 56.7(3) . 4_575 ? C33 Ga4 C31 57.4(2) . . ? C33 Ga4 C31 57.4(2) 4_575 . ? C32 Ga4 C31 33.98(17) . . ? C32 Ga4 C31 33.98(17) 4_575 . ? C33 Ga4 Pd4 162.16(15) . . ? C33 Ga4 Pd4 162.16(15) 4_575 . ? C32 Ga4 Pd4 133.58(14) . . ? C32 Ga4 Pd4 133.58(14) 4_575 . ? C31 Ga4 Pd4 122.04(19) . . ? C33 Ga4 Pd3 116.97(15) . . ? C33 Ga4 Pd3 116.97(15) 4_575 . ? C32 Ga4 Pd3 142.52(15) . . ? C32 Ga4 Pd3 142.52(15) 4_575 . ? C31 Ga4 Pd3 173.94(19) . . ? Pd4 Ga4 Pd3 64.02(3) . . ? P3 Pd3 Ga3 121.28(4) . 4_575 ? P3 Pd3 Ga3 121.28(4) . . ? Ga3 Pd3 Ga3 97.71(4) 4_575 . ? P3 Pd3 Ga4 124.16(7) . . ? Ga3 Pd3 Ga4 92.46(3) 4_575 . ? Ga3 Pd3 Ga4 92.46(3) . . ? P3 Pd3 Pd4 178.51(7) . . ? Ga3 Pd3 Pd4 58.03(2) 4_575 . ? Ga3 Pd3 Pd4 58.03(2) . . ? Ga4 Pd3 Pd4 57.33(3) . . ? C4 C3 C2 108.6(6) . . ? C4 C3 C8 126.6(9) . . ? C2 C3 C8 124.7(9) . . ? C4 C3 Ga1 72.8(4) . . ? C2 C3 Ga1 74.0(4) . . ? C8 C3 Ga1 122.2(6) . . ? C38 P3 C37 99.3(4) . 4_575 ? C38 P3 C37 99.3(4) . . ? C37 P3 C37 103.9(7) 4_575 . ? C38 P3 Pd3 117.0(3) . . ? C37 P3 Pd3 117.1(3) 4_575 . ? C37 P3 Pd3 117.1(3) . . ? C23 Ga3 C24 35.2(2) . . ? C23 Ga3 C25 57.8(3) . . ? C24 Ga3 C25 34.5(3) . . ? C23 Ga3 C22 34.5(2) . . ? C24 Ga3 C22 57.7(2) . . ? C25 Ga3 C22 57.5(2) . . ? C23 Ga3 C21 57.9(2) . . ? C24 Ga3 C21 58.0(3) . . ? C25 Ga3 C21 34.9(2) . . ? C22 Ga3 C21 34.7(2) . . ? C23 Ga3 Pd4 139.2(2) . . ? C24 Ga3 Pd4 174.1(2) . . ? C25 Ga3 Pd4 149.0(2) . . ? C22 Ga3 Pd4 118.67(16) . . ? C21 Ga3 Pd4 122.24(19) . . ? C23 Ga3 Pd3 147.8(2) . . ? C24 Ga3 Pd3 120.46(18) . . ? C25 Ga3 Pd3 116.77(18) . . ? C22 Ga3 Pd3 173.13(16) . . ? C21 Ga3 Pd3 138.47(16) . . ? Pd4 Ga3 Pd3 63.75(2) . . ? P2 Pd2 Ga1 121.07(3) . 4_575 ? P2 Pd2 Ga1 121.07(3) . . ? Ga1 Pd2 Ga1 97.57(4) 4_575 . ? P2 Pd2 Ga2 124.47(6) . . ? Ga1 Pd2 Ga2 92.61(3) 4_575 . ? Ga1 Pd2 Ga2 92.61(3) . . ? P2 Pd2 Pd1 178.19(6) . . ? Ga1 Pd2 Pd1 58.08(2) 4_575 . ? Ga1 Pd2 Pd1 58.08(2) . . ? Ga2 Pd2 Pd1 57.34(3) . . ? C1 C2 C3 107.0(6) . . ? C1 C2 C7 125.9(7) . . ? C3 C2 C7 127.1(7) . . ? C1 C2 Ga1 72.3(4) . . ? C3 C2 Ga1 71.4(4) . . ? C7 C2 Ga1 123.3(5) . . ? C19 P2 C20 99.7(3) . 4_575 ? C19 P2 C20 99.7(3) . . ? C20 P2 C20 100.9(6) 4_575 . ? C19 P2 Pd2 115.7(3) . . ? C20 P2 Pd2 118.7(2) 4_575 . ? C20 P2 Pd2 118.7(2) . . ? C11 Ga2 C11 33.7(3) 4_575 . ? C11 Ga2 C12 34.86(19) 4_575 4_575 ? C11 Ga2 C12 57.16(19) . 4_575 ? C11 Ga2 C12 57.16(19) 4_575 . ? C11 Ga2 C12 34.86(19) . . ? C12 Ga2 C12 57.3(3) 4_575 . ? C11 Ga2 C13 56.9(2) 4_575 . ? C11 Ga2 C13 56.9(2) . . ? C12 Ga2 C13 34.18(17) 4_575 . ? C12 Ga2 C13 34.18(17) . . ? C11 Ga2 Pd1 162.85(15) 4_575 . ? C11 Ga2 Pd1 162.85(15) . . ? C12 Ga2 Pd1 133.04(14) 4_575 . ? C12 Ga2 Pd1 133.04(14) . . ? C13 Ga2 Pd1 121.59(17) . . ? C11 Ga2 Pd2 117.81(14) 4_575 . ? C11 Ga2 Pd2 117.81(14) . . ? C12 Ga2 Pd2 142.64(15) 4_575 . ? C12 Ga2 Pd2 142.64(15) . . ? C13 Ga2 Pd2 174.41(17) . . ? Pd1 Ga2 Pd2 64.00(3) . . ? P1 Pd1 Ga2 120.89(7) . . ? P1 Pd1 Ga1 122.01(3) . . ? Ga2 Pd1 Ga1 93.56(3) . . ? P1 Pd1 Ga1 122.01(3) . 4_575 ? Ga2 Pd1 Ga1 93.56(3) . 4_575 ? Ga1 Pd1 Ga1 97.75(4) . 4_575 ? P1 Pd1 Pd2 179.54(7) . . ? Ga2 Pd1 Pd2 58.65(3) . . ? Ga1 Pd1 Pd2 58.20(2) . . ? Ga1 Pd1 Pd2 58.20(2) 4_575 . ? C2 C1 C5 108.3(6) . . ? C2 C1 C6 124.3(8) . . ? C5 C1 C6 127.4(7) . . ? C2 C1 Ga1 73.6(4) . . ? C5 C1 Ga1 72.5(4) . . ? C6 C1 Ga1 119.2(7) . . ? C17 P1 C17 100.0(5) 4_575 . ? C17 P1 C18 100.7(3) 4_575 . ? C17 P1 C18 100.7(3) . . ? C17 P1 Pd1 117.2(2) 4_575 . ? C17 P1 Pd1 117.2(2) . . ? C18 P1 Pd1 118.0(4) . . ? C3 Ga1 C4 34.8(3) . . ? C3 Ga1 C5 56.9(3) . . ? C4 Ga1 C5 34.1(3) . . ? C3 Ga1 C1 57.0(2) . . ? C4 Ga1 C1 57.4(3) . . ? C5 Ga1 C1 34.5(3) . . ? C3 Ga1 C2 34.6(2) . . ? C4 Ga1 C2 57.8(2) . . ? C5 Ga1 C2 57.1(2) . . ? C1 Ga1 C2 34.1(2) . . ? C3 Ga1 Pd1 140.8(2) . . ? C4 Ga1 Pd1 175.3(2) . . ? C5 Ga1 Pd1 146.0(3) . . ? C1 Ga1 Pd1 120.0(2) . . ? C2 Ga1 Pd1 117.74(15) . . ? C3 Ga1 Pd2 148.6(2) . . ? C4 Ga1 Pd2 120.9(2) . . ? C5 Ga1 Pd2 116.98(19) . . ? C1 Ga1 Pd2 138.10(16) . . ? C2 Ga1 Pd2 172.15(15) . . ? Pd1 Ga1 Pd2 63.72(2) . . ? C11 C11 C12 108.8(3) 4_575 . ? C11 C11 C14 126.7(4) 4_575 . ? C12 C11 C14 124.5(6) . . ? C11 C11 Ga2 73.14(15) 4_575 . ? C12 C11 Ga2 73.3(3) . . ? C14 C11 Ga2 119.6(4) . . ? C13 C12 C11 107.0(5) . . ? C13 C12 C15 124.9(6) . . ? C11 C12 C15 127.9(6) . . ? C13 C12 Ga2 74.0(4) . . ? C11 C12 Ga2 71.8(3) . . ? C15 C12 Ga2 123.3(4) . . ? C4 C5 C1 108.9(6) . . ? C4 C5 C10 125.9(9) . . ? C1 C5 C10 125.2(9) . . ? C4 C5 Ga1 72.7(4) . . ? C1 C5 Ga1 72.9(5) . . ? C10 C5 Ga1 118.8(7) . . ? C12 C13 C12 108.5(7) . 4_575 ? C12 C13 C16 125.8(4) . . ? C12 C13 C16 125.8(4) 4_575 . ? C12 C13 Ga2 71.9(4) . . ? C12 C13 Ga2 71.9(4) 4_575 . ? C16 C13 Ga2 122.4(5) . . ? C23 C22 C21 109.0(6) . . ? C23 C22 C27 127.5(7) . . ? C21 C22 C27 123.5(7) . . ? C23 C22 Ga3 71.9(4) . . ? C21 C22 Ga3 73.2(4) . . ? C27 C22 Ga3 122.1(5) . . ? C22 C21 C25 106.6(6) . . ? C22 C21 C26 128.1(7) . . ? C25 C21 C26 125.3(7) . . ? C22 C21 Ga3 72.2(4) . . ? C25 C21 Ga3 71.8(4) . . ? C26 C21 Ga3 120.9(7) . . ? C22 C23 C24 107.9(6) . . ? C22 C23 C28 125.8(8) . . ? C24 C23 C28 126.2(8) . . ? C22 C23 Ga3 73.6(4) . . ? C24 C23 Ga3 72.5(4) . . ? C28 C23 Ga3 121.1(6) . . ? C32 C31 C32 107.8(7) 4_575 . ? C32 C31 C34 126.1(4) 4_575 . ? C32 C31 C34 126.1(4) . . ? C32 C31 Ga4 71.9(4) 4_575 . ? C32 C31 Ga4 71.9(4) . . ? C34 C31 Ga4 121.8(5) . . ? C24 C25 C21 108.6(6) . . ? C24 C25 C30 128.4(8) . . ? C21 C25 C30 123.0(8) . . ? C24 C25 Ga3 72.2(4) . . ? C21 C25 Ga3 73.2(4) . . ? C30 C25 Ga3 120.0(7) . . ? C25 C24 C23 107.8(6) . . ? C25 C24 C29 125.8(8) . . ? C23 C24 C29 126.3(8) . . ? C25 C24 Ga3 73.2(4) . . ? C23 C24 Ga3 72.3(4) . . ? C29 C24 Ga3 122.2(5) . . ? C32 C33 C33 107.0(4) . 4_575 ? C32 C33 C36 126.9(6) . . ? C33 C33 C36 126.0(4) 4_575 . ? C32 C33 Ga4 73.4(3) . . ? C33 C33 Ga4 72.32(15) 4_575 . ? C36 C33 Ga4 120.0(4) . . ? C31 C32 C33 109.1(6) . . ? C31 C32 C35 125.6(6) . . ? C33 C32 C35 125.4(6) . . ? C31 C32 Ga4 74.2(4) . . ? C33 C32 Ga4 72.0(3) . . ? C35 C32 Ga4 121.2(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.304 _refine_diff_density_min -1.474 _refine_diff_density_rms 0.125 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.250 1.143 475.4 17.8 2 0.499 0.750 0.857 475.5 17.8 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 967769' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C6 H18 Ga3 P2 Pt2), 10(C10 H15), C20 H27 ' _chemical_formula_sum 'C144 H249 Ga12 P8 Pt8' _chemical_formula_weight 4625.55 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 17.9964(6) _cell_length_b 15.2155(4) _cell_length_c 18.3239(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.664(3) _cell_angle_gamma 90.00 _cell_volume 4875.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 200 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2229 _exptl_absorpt_coefficient_mu 7.439 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2977 _exptl_absorpt_correction_T_max 0.7307 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '560 images at 1.0 deg. in \w and 25 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36232 _diffrn_reflns_av_R_equivalents 0.0883 _diffrn_reflns_av_sigmaI/netI 0.0938 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8910 _reflns_number_gt 5999 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _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^)+(0.0471P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8910 _refine_ls_number_parameters 433 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1114 _refine_ls_wR_factor_gt 0.0990 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.965 _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 Pt1 Pt 0.17878(3) 0.2500 0.01728(3) 0.02706(15) Uani 1 2 d S . . C1 C 0.3338(9) 0.4742(8) -0.0061(7) 0.064(4) Uani 1 1 d . . . P1 P 0.0898(2) 0.2500 -0.09050(19) 0.0338(9) Uani 1 2 d S . . Ga1 Ga 0.27091(7) 0.37220(8) 0.05322(6) 0.0402(3) Uani 1 1 d . . . Pt3 Pt 0.71104(3) 0.2500 0.50987(3) 0.02825(15) Uani 1 2 d S . . C3 C 0.2337(8) 0.5241(8) 0.0433(7) 0.061(4) Uani 1 1 d . . . P3 P 0.9074(2) 0.2500 0.3683(2) 0.0346(9) Uani 1 2 d S . . Ga3 Ga 0.72512(7) 0.37270(7) 0.42488(6) 0.0362(3) Uani 1 1 d . . . Pt2 Pt 0.28295(3) 0.2500 0.14462(3) 0.03198(16) Uani 1 2 d S . . C2 C 0.2559(8) 0.4971(7) -0.0239(6) 0.048(3) Uani 1 1 d . . . P2 P 0.3731(3) 0.2500 0.2514(2) 0.0463(11) Uani 1 2 d S . . Ga2 Ga 0.14360(9) 0.2500 0.13863(8) 0.0297(4) Uani 1 2 d S . . Pt4 Pt 0.81717(3) 0.2500 0.43322(3) 0.02650(15) Uani 1 2 d S . . C4 C 0.2988(8) 0.5159(8) 0.1019(6) 0.059(4) Uani 1 1 d . . . P4 P 0.6189(2) 0.2500 0.57266(19) 0.0385(10) Uani 1 2 d S . . Ga4 Ga 0.84990(9) 0.2500 0.57113(7) 0.0286(4) Uani 1 2 d S . . C6 C 0.3765(11) 0.4443(11) -0.0596(9) 0.115(6) Uani 1 1 d U . . H6A H 0.3424 0.4114 -0.1000 0.172 Uiso 1 1 calc R . . H6B H 0.4185 0.4062 -0.0341 0.172 Uiso 1 1 calc R . . H6C H 0.3973 0.4952 -0.0809 0.172 Uiso 1 1 calc R . . C5 C 0.3594(7) 0.4874(8) 0.0731(7) 0.057(3) Uani 1 1 d U . . C7 C 0.2027(9) 0.4993(9) -0.1003(6) 0.082(5) Uani 1 1 d . . . H7A H 0.2010 0.5590 -0.1207 0.123 Uiso 1 1 calc R . . H7B H 0.1513 0.4819 -0.0964 0.123 Uiso 1 1 calc R . . H7C H 0.2209 0.4585 -0.1336 0.123 Uiso 1 1 calc R . . C19 C 0.3764(9) 0.3403(10) 0.3150(8) 0.097(5) Uani 1 1 d U . . H19A H 0.4076 0.3241 0.3646 0.145 Uiso 1 1 calc R . . H19B H 0.3244 0.3546 0.3191 0.145 Uiso 1 1 calc R . . H19C H 0.3990 0.3916 0.2962 0.145 Uiso 1 1 calc R . . C9 C 0.3009(13) 0.5389(12) 0.1827(8) 0.145(9) Uani 1 1 d . . . H9A H 0.2757 0.5956 0.1846 0.218 Uiso 1 1 calc R . . H9B H 0.3542 0.5426 0.2114 0.218 Uiso 1 1 calc R . . H9C H 0.2743 0.4933 0.2045 0.218 Uiso 1 1 calc R . . C8 C 0.1554(11) 0.5529(15) 0.0508(10) 0.146(9) Uani 1 1 d . . . H8A H 0.1610 0.5955 0.0919 0.219 Uiso 1 1 calc R . . H8B H 0.1268 0.5017 0.0616 0.219 Uiso 1 1 calc R . . H8C H 0.1278 0.5803 0.0038 0.219 Uiso 1 1 calc R . . C13 C 0.0121(9) 0.2500 0.1455(8) 0.038(4) Uani 1 2 d S . . C12 C 0.0463(6) 0.3251(6) 0.1825(6) 0.037(3) Uani 1 1 d . . . C11 C 0.1041(6) 0.2973(6) 0.2449(5) 0.034(2) Uani 1 1 d U . . C10 C 0.4393(10) 0.4744(11) 0.1178(9) 0.107(6) Uani 1 1 d U . . H10A H 0.4663 0.4349 0.0907 0.161 Uiso 1 1 calc R . . H10B H 0.4384 0.4487 0.1666 0.161 Uiso 1 1 calc R . . H10C H 0.4656 0.5313 0.1255 0.161 Uiso 1 1 calc R . . C18 C 0.1231(10) 0.2500 -0.1775(7) 0.052(5) Uani 1 2 d S . . H18A H 0.0789 0.2517 -0.2207 0.079 Uiso 1 2 calc SR . . H18B H 0.1528 0.1966 -0.1799 0.079 Uiso 0.50 1 calc PR . . H18C H 0.1552 0.3017 -0.1785 0.079 Uiso 0.50 1 calc PR . . C17 C 0.0243(7) 0.3419(7) -0.1080(6) 0.050(3) Uani 1 1 d . . . H17A H -0.0110 0.3348 -0.1573 0.076 Uiso 1 1 calc R . . H17B H 0.0532 0.3966 -0.1073 0.076 Uiso 1 1 calc R . . H17C H -0.0047 0.3440 -0.0691 0.076 Uiso 1 1 calc R . . C16 C -0.0542(8) 0.2500 0.0761(8) 0.051(4) Uani 1 2 d S . . H16A H -0.0447 0.2061 0.0402 0.076 Uiso 0.50 1 calc PR . . H16B H -0.0587 0.3083 0.0527 0.076 Uiso 0.50 1 calc PR . . H16C H -0.1017 0.2356 0.0907 0.076 Uiso 0.50 1 calc PR . . C15 C 0.0249(8) 0.4181(7) 0.1617(7) 0.067(4) Uani 1 1 d . . . H15A H 0.0158 0.4250 0.1071 0.100 Uiso 1 1 calc R . . H15B H 0.0665 0.4571 0.1865 0.100 Uiso 1 1 calc R . . H15C H -0.0217 0.4332 0.1778 0.100 Uiso 1 1 calc R . . C14 C 0.1543(7) 0.3558(8) 0.3003(6) 0.056(3) Uani 1 1 d . . . H14A H 0.1773 0.4002 0.2737 0.084 Uiso 1 1 calc R . . H14B H 0.1948 0.3209 0.3326 0.084 Uiso 1 1 calc R . . H14C H 0.1239 0.3850 0.3311 0.084 Uiso 1 1 calc R . . C21 C 0.7679(7) 0.5191(7) 0.4347(6) 0.047(3) Uani 1 1 d . . . C20 C 0.4715(10) 0.2500 0.2425(10) 0.062(5) Uani 1 2 d S . . H20A H 0.5057 0.2371 0.2914 0.094 Uiso 0.50 1 calc PR . . H20B H 0.4840 0.3078 0.2251 0.094 Uiso 0.50 1 calc PR . . H20C H 0.4778 0.2050 0.2061 0.094 Uiso 0.50 1 calc PR . . C24 C 0.6409(8) 0.4925(8) 0.4080(10) 0.070(4) Uani 1 1 d . . . C23 C 0.6666(8) 0.4832(7) 0.3418(7) 0.059(4) Uani 1 1 d . . . C22 C 0.7447(7) 0.5004(6) 0.3582(5) 0.034(3) Uani 1 1 d . . . C40 C 0.5202(9) 0.2500 0.5151(9) 0.062(5) Uani 1 2 d S . . H40A H 0.4845 0.2539 0.5479 0.093 Uiso 0.50 1 calc PR . . H40B H 0.5107 0.1956 0.4858 0.093 Uiso 0.50 1 calc PR . . H40C H 0.5128 0.3005 0.4810 0.093 Uiso 0.50 1 calc PR . . C39 C 0.6122(8) 0.3425(9) 0.6349(7) 0.076(4) Uani 1 1 d . . . H39A H 0.6078 0.3975 0.6063 0.114 Uiso 1 1 calc R . . H39B H 0.6582 0.3444 0.6761 0.114 Uiso 1 1 calc R . . H39C H 0.5670 0.3351 0.6554 0.114 Uiso 1 1 calc R . . C38 C 0.8750(11) 0.2500 0.2662(7) 0.057(5) Uani 1 2 d S . . H38A H 0.8596 0.1904 0.2487 0.086 Uiso 0.50 1 calc PR . . H38B H 0.9166 0.2699 0.2441 0.086 Uiso 0.50 1 calc PR . . H38C H 0.8312 0.2898 0.2510 0.086 Uiso 0.50 1 calc PR . . C37 C 0.9728(7) 0.1569(8) 0.3827(6) 0.059(3) Uani 1 1 d . . . H37A H 0.9439 0.1025 0.3685 0.088 Uiso 1 1 calc R . . H37B H 0.9999 0.1539 0.4358 0.088 Uiso 1 1 calc R . . H37C H 1.0099 0.1641 0.3517 0.088 Uiso 1 1 calc R . . C36 C 1.0485(10) 0.2500 0.6025(8) 0.057(5) Uani 1 2 d S . . H36A H 1.0553 0.1910 0.5837 0.086 Uiso 0.25 1 calc PR . . H36B H 1.0946 0.2671 0.6400 0.086 Uiso 0.25 1 calc PR . . H36C H 1.0393 0.2919 0.5607 0.086 Uiso 0.25 1 calc PR . . C35 C 0.9695(8) 0.4180(7) 0.6509(7) 0.066(4) Uani 1 1 d . . . H35A H 0.9780 0.4256 0.6004 0.100 Uiso 1 1 calc R . . H35B H 1.0166 0.4319 0.6884 0.100 Uiso 1 1 calc R . . H35C H 0.9286 0.4576 0.6575 0.100 Uiso 1 1 calc R . . C34 C 0.8384(7) 0.3543(9) 0.7287(6) 0.073(4) Uani 1 1 d . . . H34A H 0.8325 0.4110 0.7026 0.109 Uiso 1 1 calc R . . H34B H 0.8610 0.3636 0.7823 0.109 Uiso 1 1 calc R . . H34C H 0.7881 0.3265 0.7224 0.109 Uiso 1 1 calc R . . C33 C 0.9824(9) 0.2500 0.6374(7) 0.033(4) Uani 1 2 d S . . C32 C 0.9467(6) 0.3238(6) 0.6609(5) 0.034(3) Uani 1 1 d . . . C31 C 0.8890(6) 0.2965(6) 0.6967(5) 0.037(3) Uani 1 1 d U . . C30 C 0.7078(12) 0.5321(12) 0.5491(10) 0.131(7) Uani 1 1 d U . . H30A H 0.7137 0.5949 0.5609 0.196 Uiso 1 1 calc R . . H30B H 0.7515 0.4998 0.5793 0.196 Uiso 1 1 calc R . . H30C H 0.6605 0.5106 0.5605 0.196 Uiso 1 1 calc R . . C29 C 0.5598(12) 0.4838(12) 0.4187(10) 0.136(7) Uani 1 1 d U . . H29A H 0.5251 0.4684 0.3707 0.205 Uiso 1 1 calc R . . H29B H 0.5439 0.5398 0.4366 0.205 Uiso 1 1 calc R . . H29C H 0.5583 0.4377 0.4556 0.205 Uiso 1 1 calc R . . C28 C 0.6166(11) 0.4614(11) 0.2671(9) 0.118(6) Uani 1 1 d U . . H28A H 0.5950 0.5155 0.2418 0.176 Uiso 1 1 calc R . . H28B H 0.5750 0.4228 0.2738 0.176 Uiso 1 1 calc R . . H28C H 0.6468 0.4313 0.2366 0.176 Uiso 1 1 calc R . . C27 C 0.7954(10) 0.5018(9) 0.3039(7) 0.093(6) Uani 1 1 d . . . H27A H 0.7718 0.5379 0.2604 0.139 Uiso 1 1 calc R . . H27B H 0.8023 0.4417 0.2874 0.139 Uiso 1 1 calc R . . H27C H 0.8453 0.5266 0.3286 0.139 Uiso 1 1 calc R . . C26 C 0.8499(10) 0.5378(11) 0.4737(9) 0.110(6) Uani 1 1 d U . . H26A H 0.8806 0.4845 0.4739 0.165 Uiso 1 1 calc R . . H26B H 0.8527 0.5562 0.5256 0.165 Uiso 1 1 calc R . . H26C H 0.8699 0.5848 0.4471 0.165 Uiso 1 1 calc R . . C25 C 0.7042(10) 0.5180(8) 0.4654(8) 0.072(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0238(3) 0.0390(3) 0.0165(2) 0.000 0.0009(2) 0.000 C1 0.080(12) 0.054(8) 0.075(9) 0.019(6) 0.052(9) 0.003(8) P1 0.035(3) 0.040(2) 0.0224(17) 0.000 -0.0007(17) 0.000 Ga1 0.0372(8) 0.0562(8) 0.0256(5) 0.0044(5) 0.0042(5) -0.0159(6) Pt3 0.0259(4) 0.0426(3) 0.0167(2) 0.000 0.0060(2) 0.000 C3 0.057(10) 0.077(9) 0.049(7) 0.010(6) 0.013(7) 0.010(8) P3 0.036(3) 0.042(2) 0.0302(19) 0.000 0.0168(18) 0.000 Ga3 0.0384(8) 0.0450(7) 0.0265(5) 0.0099(5) 0.0102(5) 0.0113(6) Pt2 0.0246(4) 0.0535(4) 0.0165(3) 0.000 0.0022(2) 0.000 C2 0.055(9) 0.049(7) 0.042(6) 0.005(5) 0.013(6) -0.013(7) P2 0.026(3) 0.083(3) 0.0247(19) 0.000 -0.0055(17) 0.000 Ga2 0.0267(10) 0.0390(9) 0.0250(7) 0.000 0.0093(7) 0.000 Pt4 0.0276(4) 0.0342(3) 0.0193(3) 0.000 0.0089(2) 0.000 C4 0.067(10) 0.062(8) 0.041(7) -0.005(6) -0.001(7) 0.014(7) P4 0.027(2) 0.067(3) 0.0208(18) 0.000 0.0048(16) 0.000 Ga4 0.0282(10) 0.0360(9) 0.0197(7) 0.000 0.0022(6) 0.000 C6 0.116(8) 0.121(7) 0.115(7) 0.010(5) 0.043(5) 0.000(5) C5 0.035(7) 0.053(6) 0.075(7) 0.008(6) -0.003(6) -0.017(5) C7 0.118(15) 0.086(10) 0.034(7) 0.016(6) 0.004(8) -0.028(10) C19 0.078(9) 0.124(9) 0.077(7) -0.040(7) -0.005(7) 0.018(7) C9 0.22(3) 0.133(15) 0.054(10) -0.040(10) -0.016(12) 0.065(16) C8 0.110(18) 0.23(2) 0.117(15) 0.062(15) 0.062(13) 0.089(17) C13 0.038(10) 0.041(9) 0.045(9) 0.000 0.032(8) 0.000 C12 0.036(7) 0.037(7) 0.050(6) -0.003(5) 0.030(6) -0.005(5) C11 0.032(6) 0.050(5) 0.027(5) -0.014(4) 0.018(4) 0.002(4) C10 0.099(7) 0.104(7) 0.114(7) 0.009(5) 0.017(5) -0.008(5) C18 0.042(12) 0.085(13) 0.028(8) 0.000 0.004(8) 0.000 C17 0.043(8) 0.049(7) 0.047(7) 0.004(5) -0.014(6) 0.012(6) C16 0.017(9) 0.098(13) 0.040(9) 0.000 0.011(7) 0.000 C15 0.063(10) 0.049(8) 0.094(10) -0.005(7) 0.030(8) 0.011(7) C14 0.046(9) 0.072(8) 0.052(7) -0.020(6) 0.018(6) -0.005(7) C21 0.045(8) 0.056(7) 0.035(6) -0.005(5) -0.001(6) -0.027(6) C20 0.049(13) 0.060(12) 0.076(12) 0.000 0.008(10) 0.000 C24 0.037(9) 0.028(7) 0.151(15) 0.031(8) 0.034(10) 0.012(6) C23 0.061(10) 0.037(7) 0.057(8) 0.015(6) -0.028(7) -0.007(7) C22 0.046(8) 0.027(6) 0.029(5) 0.006(4) 0.006(5) 0.006(5) C40 0.030(11) 0.105(14) 0.053(10) 0.000 0.013(9) 0.000 C39 0.065(11) 0.106(11) 0.069(9) -0.018(8) 0.038(8) 0.000(9) C38 0.068(14) 0.083(12) 0.026(8) 0.000 0.022(8) 0.000 C37 0.049(9) 0.079(9) 0.059(8) -0.001(6) 0.034(7) 0.018(7) C36 0.049(13) 0.093(13) 0.031(8) 0.000 0.013(8) 0.000 C35 0.063(10) 0.047(8) 0.085(9) -0.016(6) 0.009(8) -0.002(7) C34 0.040(9) 0.127(12) 0.048(7) -0.054(8) 0.004(6) 0.001(8) C33 0.033(10) 0.039(9) 0.024(7) 0.000 -0.001(6) 0.000 C32 0.029(7) 0.035(6) 0.030(5) -0.006(4) -0.011(5) -0.007(5) C31 0.034(5) 0.047(4) 0.025(4) -0.010(3) -0.002(3) 0.004(4) C30 0.156(11) 0.128(10) 0.123(10) -0.032(8) 0.062(8) -0.024(8) C29 0.132(9) 0.130(8) 0.149(8) 0.012(5) 0.036(5) 0.003(5) C28 0.118(8) 0.113(7) 0.114(7) 0.014(5) 0.011(5) -0.013(5) C27 0.152(17) 0.075(9) 0.076(10) 0.030(8) 0.075(11) 0.014(11) C26 0.100(10) 0.125(9) 0.097(8) 0.023(7) 0.009(7) -0.037(8) C25 0.110(14) 0.047(8) 0.081(10) -0.032(7) 0.065(10) -0.025(8) _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 P1 2.230(4) . ? Pt1 Ga2 2.4515(15) . ? Pt1 Ga1 2.4747(12) . ? Pt1 Ga1 2.4747(12) 4_565 ? Pt1 Pt2 2.6255(7) . ? C1 C2 1.405(17) . ? C1 C5 1.430(17) . ? C1 C6 1.454(19) . ? C1 Ga1 2.335(11) . ? P1 C17 1.806(10) 4_565 ? P1 C17 1.806(10) . ? P1 C18 1.831(14) . ? Ga1 C5 2.338(11) . ? Ga1 C2 2.346(11) . ? Ga1 C4 2.370(12) . ? Ga1 C3 2.401(13) . ? Ga1 Pt2 2.4775(11) . ? Pt3 P4 2.230(4) . ? Pt3 Ga3 2.4823(11) 4_565 ? Pt3 Ga3 2.4823(11) . ? Pt3 Ga4 2.4859(17) . ? Pt3 Pt4 2.6246(8) . ? C3 C4 1.395(17) . ? C3 C2 1.442(15) . ? C3 C8 1.51(2) . ? P3 C37 1.822(11) . ? P3 C37 1.822(11) 4_565 ? P3 C38 1.823(14) . ? P3 Pt4 2.228(4) . ? Ga3 C24 2.343(12) . ? Ga3 C23 2.344(10) . ? Ga3 C21 2.350(10) . ? Ga3 C22 2.365(9) . ? Ga3 C25 2.390(12) . ? Ga3 Pt4 2.4767(12) . ? Pt2 P2 2.227(4) . ? Pt2 Ga1 2.4775(11) 4_565 ? Pt2 Ga2 2.4842(17) . ? C2 C7 1.497(15) . ? P2 C19 1.794(13) . ? P2 C19 1.794(13) 4_565 ? P2 C20 1.816(19) . ? Ga2 C11 2.338(8) . ? Ga2 C11 2.338(8) 4_565 ? Ga2 C12 2.385(10) 4_565 ? Ga2 C12 2.385(10) . ? Ga2 C13 2.400(15) . ? Pt4 Ga4 2.4554(14) . ? Pt4 Ga3 2.4767(12) 4_565 ? C4 C5 1.388(17) . ? C4 C9 1.514(17) . ? P4 C39 1.833(12) . ? P4 C39 1.833(12) 4_565 ? P4 C40 1.840(17) . ? Ga4 C31 2.350(9) . ? Ga4 C31 2.350(9) 4_565 ? Ga4 C32 2.377(9) . ? Ga4 C32 2.377(9) 4_565 ? Ga4 C33 2.407(15) . ? C5 C10 1.489(19) . ? C13 C12 1.396(13) . ? C13 C12 1.396(13) 4_565 ? C13 C16 1.52(2) . ? C12 C11 1.417(14) . ? C12 C15 1.491(14) . ? C11 C11 1.440(19) 4_565 ? C11 C14 1.485(14) . ? C21 C25 1.392(17) . ? C21 C22 1.393(13) . ? C21 C26 1.508(19) . ? C24 C23 1.404(18) . ? C24 C25 1.409(19) . ? C24 C29 1.52(2) . ? C23 C22 1.391(17) . ? C23 C28 1.487(18) . ? C22 C27 1.501(16) . ? C36 C33 1.48(2) . ? C35 C32 1.514(14) . ? C34 C31 1.484(14) . ? C33 C32 1.412(13) 4_565 ? C33 C32 1.412(13) . ? C32 C31 1.414(14) . ? C31 C31 1.416(19) 4_565 ? C30 C25 1.535(19) . ? 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 P1 Pt1 Ga2 121.19(11) . . ? P1 Pt1 Ga1 122.12(6) . . ? Ga2 Pt1 Ga1 93.38(4) . . ? P1 Pt1 Ga1 122.12(6) . 4_565 ? Ga2 Pt1 Ga1 93.38(4) . 4_565 ? Ga1 Pt1 Ga1 97.42(6) . 4_565 ? P1 Pt1 Pt2 179.66(11) . . ? Ga2 Pt1 Pt2 58.47(4) . . ? Ga1 Pt1 Pt2 58.04(3) . . ? Ga1 Pt1 Pt2 58.04(3) 4_565 . ? C2 C1 C5 105.4(11) . . ? C2 C1 C6 125.3(14) . . ? C5 C1 C6 129.3(15) . . ? C2 C1 Ga1 73.0(7) . . ? C5 C1 Ga1 72.3(6) . . ? C6 C1 Ga1 119.8(10) . . ? C17 P1 C17 101.4(8) 4_565 . ? C17 P1 C18 100.3(5) 4_565 . ? C17 P1 C18 100.3(5) . . ? C17 P1 Pt1 117.3(3) 4_565 . ? C17 P1 Pt1 117.3(3) . . ? C18 P1 Pt1 117.2(6) . . ? C1 Ga1 C5 35.6(4) . . ? C1 Ga1 C2 34.9(4) . . ? C5 Ga1 C2 57.6(4) . . ? C1 Ga1 C4 58.6(4) . . ? C5 Ga1 C4 34.3(4) . . ? C2 Ga1 C4 57.5(4) . . ? C1 Ga1 C3 58.8(4) . . ? C5 Ga1 C3 57.2(5) . . ? C2 Ga1 C3 35.3(4) . . ? C4 Ga1 C3 34.0(4) . . ? C1 Ga1 Pt1 138.0(4) . . ? C5 Ga1 Pt1 173.5(3) . . ? C2 Ga1 Pt1 118.3(3) . . ? C4 Ga1 Pt1 149.6(4) . . ? C3 Ga1 Pt1 123.1(3) . . ? C1 Ga1 Pt2 147.0(4) . . ? C5 Ga1 Pt2 120.6(3) . . ? C2 Ga1 Pt2 174.1(3) . . ? C4 Ga1 Pt2 117.5(3) . . ? C3 Ga1 Pt2 138.7(3) . . ? Pt1 Ga1 Pt2 64.03(3) . . ? P4 Pt3 Ga3 121.48(5) . 4_565 ? P4 Pt3 Ga3 121.48(5) . . ? Ga3 Pt3 Ga3 97.55(5) 4_565 . ? P4 Pt3 Ga4 123.89(10) . . ? Ga3 Pt3 Ga4 92.44(4) 4_565 . ? Ga3 Pt3 Ga4 92.44(4) . . ? P4 Pt3 Pt4 178.76(10) . . ? Ga3 Pt3 Pt4 57.94(3) 4_565 . ? Ga3 Pt3 Pt4 57.94(3) . . ? Ga4 Pt3 Pt4 57.36(4) . . ? C4 C3 C2 106.3(12) . . ? C4 C3 C8 125.9(13) . . ? C2 C3 C8 127.8(13) . . ? C4 C3 Ga1 71.8(7) . . ? C2 C3 Ga1 70.2(7) . . ? C8 C3 Ga1 121.4(12) . . ? C37 P3 C37 102.1(9) . 4_565 ? C37 P3 C38 100.9(5) . . ? C37 P3 C38 100.9(5) 4_565 . ? C37 P3 Pt4 116.8(4) . . ? C37 P3 Pt4 116.8(4) 4_565 . ? C38 P3 Pt4 116.8(6) . . ? C24 Ga3 C23 34.8(5) . . ? C24 Ga3 C21 57.5(5) . . ? C23 Ga3 C21 57.2(4) . . ? C24 Ga3 C22 57.6(4) . . ? C23 Ga3 C22 34.3(4) . . ? C21 Ga3 C22 34.4(3) . . ? C24 Ga3 C25 34.6(5) . . ? C23 Ga3 C25 57.2(5) . . ? C21 Ga3 C25 34.2(4) . . ? C22 Ga3 C25 56.9(4) . . ? C24 Ga3 Pt4 175.3(4) . . ? C23 Ga3 Pt4 140.5(4) . . ? C21 Ga3 Pt4 120.5(3) . . ? C22 Ga3 Pt4 118.2(3) . . ? C25 Ga3 Pt4 146.1(4) . . ? C24 Ga3 Pt3 120.6(4) . . ? C23 Ga3 Pt3 148.2(4) . . ? C21 Ga3 Pt3 138.2(2) . . ? C22 Ga3 Pt3 172.6(2) . . ? C25 Ga3 Pt3 117.0(3) . . ? Pt4 Ga3 Pt3 63.91(3) . . ? P2 Pt2 Ga1 121.55(6) . 4_565 ? P2 Pt2 Ga1 121.55(6) . . ? Ga1 Pt2 Ga1 97.27(5) 4_565 . ? P2 Pt2 Ga2 123.84(12) . . ? Ga1 Pt2 Ga2 92.52(4) 4_565 . ? Ga1 Pt2 Ga2 92.52(4) . . ? P2 Pt2 Pt1 178.90(12) . . ? Ga1 Pt2 Pt1 57.93(3) 4_565 . ? Ga1 Pt2 Pt1 57.93(3) . . ? Ga2 Pt2 Pt1 57.26(4) . . ? C1 C2 C3 109.5(11) . . ? C1 C2 C7 127.2(12) . . ? C3 C2 C7 123.1(13) . . ? C1 C2 Ga1 72.1(7) . . ? C3 C2 Ga1 74.4(7) . . ? C7 C2 Ga1 122.6(8) . . ? C19 P2 C19 100.0(11) . 4_565 ? C19 P2 C20 100.1(7) . . ? C19 P2 C20 100.1(7) 4_565 . ? C19 P2 Pt2 118.5(5) . . ? C19 P2 Pt2 118.5(5) 4_565 . ? C20 P2 Pt2 116.4(6) . . ? C11 Ga2 C11 35.9(5) . 4_565 ? C11 Ga2 C12 58.3(3) . 4_565 ? C11 Ga2 C12 34.9(3) 4_565 4_565 ? C11 Ga2 C12 34.9(3) . . ? C11 Ga2 C12 58.3(3) 4_565 . ? C12 Ga2 C12 57.3(5) 4_565 . ? C11 Ga2 C13 57.3(4) . . ? C11 Ga2 C13 57.3(4) 4_565 . ? C12 Ga2 C13 33.9(3) 4_565 . ? C12 Ga2 C13 33.9(3) . . ? C11 Ga2 Pt1 161.7(2) . . ? C11 Ga2 Pt1 161.7(2) 4_565 . ? C12 Ga2 Pt1 132.3(3) 4_565 . ? C12 Ga2 Pt1 132.3(3) . . ? C13 Ga2 Pt1 121.1(3) . . ? C11 Ga2 Pt2 117.7(3) . . ? C11 Ga2 Pt2 117.7(3) 4_565 . ? C12 Ga2 Pt2 143.1(3) 4_565 . ? C12 Ga2 Pt2 143.1(3) . . ? C13 Ga2 Pt2 174.6(3) . . ? Pt1 Ga2 Pt2 64.27(4) . . ? P3 Pt4 Ga4 121.45(11) . . ? P3 Pt4 Ga3 121.88(5) . 4_565 ? Ga4 Pt4 Ga3 93.32(4) . 4_565 ? P3 Pt4 Ga3 121.88(5) . . ? Ga4 Pt4 Ga3 93.32(4) . . ? Ga3 Pt4 Ga3 97.84(6) 4_565 . ? P3 Pt4 Pt3 179.93(10) . . ? Ga4 Pt4 Pt3 58.48(4) . . ? Ga3 Pt4 Pt3 58.15(3) 4_565 . ? Ga3 Pt4 Pt3 58.15(3) . . ? C5 C4 C3 109.2(11) . . ? C5 C4 C9 127.1(14) . . ? C3 C4 C9 123.7(14) . . ? C5 C4 Ga1 71.6(7) . . ? C3 C4 Ga1 74.2(7) . . ? C9 C4 Ga1 122.4(10) . . ? C39 P4 C39 100.4(9) . 4_565 ? C39 P4 C40 99.2(6) . . ? C39 P4 C40 99.2(6) 4_565 . ? C39 P4 Pt3 119.1(4) . . ? C39 P4 Pt3 119.1(4) 4_565 . ? C40 P4 Pt3 116.1(5) . . ? C31 Ga4 C31 35.1(5) . 4_565 ? C31 Ga4 C32 34.8(3) . . ? C31 Ga4 C32 57.6(3) 4_565 . ? C31 Ga4 C32 57.6(3) . 4_565 ? C31 Ga4 C32 34.8(3) 4_565 4_565 ? C32 Ga4 C32 56.4(5) . 4_565 ? C31 Ga4 C33 58.3(4) . . ? C31 Ga4 C33 58.3(4) 4_565 . ? C32 Ga4 C33 34.3(3) . . ? C32 Ga4 C33 34.3(3) 4_565 . ? C31 Ga4 Pt4 162.0(2) . . ? C31 Ga4 Pt4 162.0(2) 4_565 . ? C32 Ga4 Pt4 132.1(3) . . ? C32 Ga4 Pt4 132.1(3) 4_565 . ? C33 Ga4 Pt4 119.2(3) . . ? C31 Ga4 Pt3 118.6(3) . . ? C31 Ga4 Pt3 118.6(3) 4_565 . ? C32 Ga4 Pt3 143.8(3) . . ? C32 Ga4 Pt3 143.8(3) 4_565 . ? C33 Ga4 Pt3 176.7(3) . . ? Pt4 Ga4 Pt3 64.16(4) . . ? C4 C5 C1 109.6(11) . . ? C4 C5 C10 125.1(13) . . ? C1 C5 C10 125.3(14) . . ? C4 C5 Ga1 74.1(8) . . ? C1 C5 Ga1 72.1(7) . . ? C10 C5 Ga1 121.3(9) . . ? C12 C13 C12 109.9(14) . 4_565 ? C12 C13 C16 125.0(7) . . ? C12 C13 C16 125.0(7) 4_565 . ? C12 C13 Ga2 72.4(8) . . ? C12 C13 Ga2 72.4(8) 4_565 . ? C16 C13 Ga2 122.9(9) . . ? C13 C12 C11 107.7(10) . . ? C13 C12 C15 126.5(11) . . ? C11 C12 C15 125.8(10) . . ? C13 C12 Ga2 73.6(7) . . ? C11 C12 Ga2 70.7(6) . . ? C15 C12 Ga2 122.3(7) . . ? C12 C11 C11 107.4(6) . 4_565 ? C12 C11 C14 125.8(9) . . ? C11 C11 C14 126.8(6) 4_565 . ? C12 C11 Ga2 74.4(5) . . ? C11 C11 Ga2 72.1(2) 4_565 . ? C14 C11 Ga2 119.9(7) . . ? C25 C21 C22 108.9(11) . . ? C25 C21 C26 128.2(12) . . ? C22 C21 C26 122.9(12) . . ? C25 C21 Ga3 74.5(7) . . ? C22 C21 Ga3 73.4(6) . . ? C26 C21 Ga3 118.8(9) . . ? C23 C24 C25 107.4(12) . . ? C23 C24 C29 128.5(17) . . ? C25 C24 C29 123.9(16) . . ? C23 C24 Ga3 72.6(7) . . ? C25 C24 Ga3 74.5(8) . . ? C29 C24 Ga3 121.7(10) . . ? C22 C23 C24 108.4(11) . . ? C22 C23 C28 127.0(15) . . ? C24 C23 C28 124.5(16) . . ? C22 C23 Ga3 73.7(6) . . ? C24 C23 Ga3 72.5(7) . . ? C28 C23 Ga3 121.2(9) . . ? C23 C22 C21 107.7(10) . . ? C23 C22 C27 127.0(11) . . ? C21 C22 C27 125.3(12) . . ? C23 C22 Ga3 72.0(6) . . ? C21 C22 Ga3 72.2(6) . . ? C27 C22 Ga3 122.8(8) . . ? C32 C33 C32 105.5(13) 4_565 . ? C32 C33 C36 127.1(7) 4_565 . ? C32 C33 C36 127.1(7) . . ? C32 C33 Ga4 71.7(7) 4_565 . ? C32 C33 Ga4 71.7(7) . . ? C36 C33 Ga4 125.8(9) . . ? C33 C32 C31 110.2(9) . . ? C33 C32 C35 124.1(10) . . ? C31 C32 C35 125.7(10) . . ? C33 C32 Ga4 74.0(7) . . ? C31 C32 Ga4 71.6(5) . . ? C35 C32 Ga4 122.6(7) . . ? C32 C31 C31 107.1(6) . 4_565 ? C32 C31 C34 126.5(10) . . ? C31 C31 C34 126.4(7) 4_565 . ? C32 C31 Ga4 73.6(5) . . ? C31 C31 Ga4 72.5(2) 4_565 . ? C34 C31 Ga4 119.7(7) . . ? C21 C25 C24 107.4(11) . . ? C21 C25 C30 123.9(15) . . ? C24 C25 C30 128.3(15) . . ? C21 C25 Ga3 71.3(7) . . ? C24 C25 Ga3 70.9(6) . . ? C30 C25 Ga3 117.8(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.812 _refine_diff_density_min -2.718 _refine_diff_density_rms 0.194 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.494 0.250 0.849 476.5 36.4 2 0.506 0.750 0.151 476.5 38.0 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 967770' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H27 Ga3 P3 Pd3, 3(C10 H15) ' _chemical_formula_sum 'C39 H72 Ga3 P3 Pd3' _chemical_formula_weight 1162.24 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 23.3586(3) _cell_length_b 17.7180(2) _cell_length_c 23.6868(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.709(2) _cell_angle_gamma 90.00 _cell_volume 9599.2(2) _cell_formula_units_Z 8 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 200 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4656 _exptl_absorpt_coefficient_mu 2.884 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5361 _exptl_absorpt_correction_T_max 0.6492 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '560 images at 1.0 deg. in \w and 25 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 135402 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16877 _reflns_number_gt 13545 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _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^)+(0.0135P)^2^+80.4073P] 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 16877 _refine_ls_number_parameters 907 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1033 _refine_ls_wR_factor_gt 0.0964 _refine_ls_goodness_of_fit_ref 1.239 _refine_ls_restrained_S_all 1.239 _refine_ls_shift/su_max 0.004 _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 Pd1 Pd 0.18476(2) 0.27257(3) 0.65603(2) 0.01604(11) Uani 1 1 d . . . C1 C 0.2693(4) 0.3590(5) 0.7817(4) 0.046(2) Uani 1 1 d . . . H1A H 0.2862 0.3976 0.7603 0.069 Uiso 1 1 calc R . . H1B H 0.2969 0.3474 0.8177 0.069 Uiso 1 1 calc R . . H1C H 0.2327 0.3779 0.7906 0.069 Uiso 1 1 calc R . . P1 P 0.25470(8) 0.27408(11) 0.73829(8) 0.0253(4) Uani 1 1 d . . . Ga1 Ga 0.18183(3) 0.35181(4) 0.56684(3) 0.02092(17) Uani 1 1 d . . . Pd2 Pd 0.09370(2) 0.16399(3) 0.66029(2) 0.02409(13) Uani 1 1 d . . . C73 C 0.3973(3) 0.9265(4) 0.2747(3) 0.0220(15) Uani 1 1 d . . . C2 C 0.3288(4) 0.2469(8) 0.7350(5) 0.075(4) Uani 1 1 d . . . H2A H 0.3289 0.1953 0.7202 0.113 Uiso 1 1 calc R . . H2B H 0.3535 0.2494 0.7737 0.113 Uiso 1 1 calc R . . H2C H 0.3442 0.2814 0.7093 0.113 Uiso 1 1 calc R . . P2 P 0.05314(9) 0.06695(11) 0.69970(9) 0.0288(4) Uani 1 1 d . . . Ga2 Ga 0.08151(3) 0.30264(4) 0.66767(3) 0.01798(16) Uani 1 1 d . . . Pd3 Pd 0.09857(2) 0.26386(3) 0.56819(2) 0.01548(11) Uani 1 1 d . . . C3 C 0.2376(5) 0.2083(6) 0.7930(4) 0.061(3) Uani 1 1 d . . . H3A H 0.2025 0.2256 0.8058 0.092 Uiso 1 1 calc R . . H3B H 0.2705 0.2067 0.8261 0.092 Uiso 1 1 calc R . . H3C H 0.2308 0.1577 0.7763 0.092 Uiso 1 1 calc R . . P3 P 0.02025(8) 0.24729(11) 0.49539(8) 0.0233(4) Uani 1 1 d . . . Ga3 Ga 0.16485(3) 0.15000(4) 0.59667(3) 0.02113(17) Uani 1 1 d . . . Pd5 Pd 0.42134(2) 0.68325(3) 0.33310(2) 0.02357(13) Uani 1 1 d . . . C5 C 0.0156(5) -0.0026(7) 0.6499(5) 0.082(4) Uani 1 1 d . . . H5A H 0.0284 0.0016 0.6131 0.123 Uiso 1 1 calc R . . H5B H -0.0267 0.0060 0.6437 0.123 Uiso 1 1 calc R . . H5C H 0.0247 -0.0532 0.6660 0.123 Uiso 1 1 calc R . . P5 P 0.46673(8) 0.60891(10) 0.27823(8) 0.0242(4) Uani 1 1 d . . . Ga5 Ga 0.35871(3) 0.63707(4) 0.39839(3) 0.01941(16) Uani 1 1 d . . . Pd4 Pd 0.40147(2) 0.76511(3) 0.43079(2) 0.01458(11) Uani 1 1 d . . . C4 C 0.1033(6) 0.0053(6) 0.7461(6) 0.087(3) Uani 1 1 d . . . H4A H 0.1345 -0.0101 0.7264 0.130 Uiso 1 1 calc R . . H4B H 0.0823 -0.0394 0.7553 0.130 Uiso 1 1 calc R . . H4C H 0.1204 0.0321 0.7817 0.130 Uiso 1 1 calc R . . P4 P 0.47908(8) 0.77183(10) 0.50587(8) 0.0221(4) Uani 1 1 d . . . Ga4 Ga 0.30570(3) 0.82507(4) 0.43360(3) 0.02163(17) Uani 1 1 d . . . Pd6 Pd 0.31454(2) 0.75723(3) 0.34315(2) 0.01406(11) Uani 1 1 d . . . C6 C -0.0021(6) 0.0784(6) 0.7420(6) 0.087(3) Uani 1 1 d . . . H6A H -0.0331 0.1116 0.7216 0.130 Uiso 1 1 calc R . . H6B H 0.0154 0.1009 0.7793 0.130 Uiso 1 1 calc R . . H6C H -0.0187 0.0290 0.7482 0.130 Uiso 1 1 calc R . . P6 P 0.24309(8) 0.74900(10) 0.26246(8) 0.0205(4) Uani 1 1 d . . . Ga6 Ga 0.41086(3) 0.82175(4) 0.33547(3) 0.01704(16) Uani 1 1 d . . . C7 C -0.0311(4) 0.3236(5) 0.4728(4) 0.055(3) Uani 1 1 d . . . H7A H -0.0117 0.3640 0.4554 0.083 Uiso 1 1 calc R . . H7B H -0.0448 0.3434 0.5063 0.083 Uiso 1 1 calc R . . H7C H -0.0645 0.3047 0.4444 0.083 Uiso 1 1 calc R . . C10 C 0.1694(3) 0.4665(4) 0.5139(3) 0.0313(18) Uani 1 1 d . . . C9 C 0.0333(4) 0.2179(7) 0.4254(4) 0.064(3) Uani 1 1 d . . . H9A H -0.0040 0.2143 0.3978 0.097 Uiso 1 1 calc R . . H9B H 0.0527 0.1685 0.4290 0.097 Uiso 1 1 calc R . . H9C H 0.0584 0.2551 0.4116 0.097 Uiso 1 1 calc R . . C8 C -0.0284(4) 0.1721(6) 0.5087(5) 0.064(3) Uani 1 1 d . . . H8A H -0.0592 0.1647 0.4743 0.096 Uiso 1 1 calc R . . H8B H -0.0461 0.1858 0.5414 0.096 Uiso 1 1 calc R . . H8C H -0.0061 0.1252 0.5175 0.096 Uiso 1 1 calc R . . C11 C 0.2132(3) 0.4772(4) 0.5638(3) 0.0293(17) Uani 1 1 d . . . C14 C 0.1911(3) 0.4153(5) 0.4779(3) 0.0315(18) Uani 1 1 d . . . C13 C 0.2488(3) 0.3935(4) 0.5055(3) 0.0271(17) Uani 1 1 d . . . C12 C 0.2624(3) 0.4314(4) 0.5587(3) 0.0285(17) Uani 1 1 d . . . C16 C 0.2118(4) 0.5299(5) 0.6125(4) 0.050(2) Uani 1 1 d . . . H16A H 0.2333 0.5760 0.6073 0.075 Uiso 1 1 calc R . . H16B H 0.2301 0.5057 0.6489 0.075 Uiso 1 1 calc R . . H16C H 0.1712 0.5426 0.6134 0.075 Uiso 1 1 calc R . . C15 C 0.1117(4) 0.5053(6) 0.4991(4) 0.059(3) Uani 1 1 d . . . H15A H 0.1141 0.5470 0.4725 0.088 Uiso 1 1 calc R . . H15B H 0.1014 0.5252 0.5344 0.088 Uiso 1 1 calc R . . H15C H 0.0818 0.4694 0.4808 0.088 Uiso 1 1 calc R . . C17 C 0.3194(4) 0.4259(6) 0.6012(4) 0.050(2) Uani 1 1 d . . . H17A H 0.3420 0.3832 0.5910 0.075 Uiso 1 1 calc R . . H17B H 0.3118 0.4183 0.6400 0.075 Uiso 1 1 calc R . . H17C H 0.3417 0.4726 0.6003 0.075 Uiso 1 1 calc R . . C18 C 0.2898(4) 0.3482(5) 0.4783(4) 0.046(2) Uani 1 1 d . . . H18A H 0.2680 0.3092 0.4536 0.069 Uiso 1 1 calc R . . H18B H 0.3192 0.3243 0.5085 0.069 Uiso 1 1 calc R . . H18C H 0.3094 0.3814 0.4551 0.069 Uiso 1 1 calc R . . C19 C 0.1598(5) 0.3903(6) 0.4190(4) 0.058(3) Uani 1 1 d . . . H19A H 0.1597 0.4316 0.3914 0.086 Uiso 1 1 calc R . . H19B H 0.1195 0.3765 0.4203 0.086 Uiso 1 1 calc R . . H19C H 0.1800 0.3465 0.4069 0.086 Uiso 1 1 calc R . . C21 C 0.0807(3) 0.4217(4) 0.7151(3) 0.0213(15) Uani 1 1 d . . . C20 C 0.0344(3) 0.4210(4) 0.6653(3) 0.0217(15) Uani 1 1 d . . . C22 C 0.0677(3) 0.3673(4) 0.7548(3) 0.0207(15) Uani 1 1 d . . . C27 C 0.1044(3) 0.3501(5) 0.8125(3) 0.0325(18) Uani 1 1 d . . . H27A H 0.0993 0.2971 0.8221 0.049 Uiso 1 1 calc R . . H27B H 0.0925 0.3825 0.8416 0.049 Uiso 1 1 calc R . . H27C H 0.1456 0.3596 0.8118 0.049 Uiso 1 1 calc R . . C26 C 0.1323(3) 0.4735(4) 0.7234(3) 0.0303(17) Uani 1 1 d . . . H26A H 0.1628 0.4511 0.7058 0.045 Uiso 1 1 calc R . . H26B H 0.1475 0.4811 0.7647 0.045 Uiso 1 1 calc R . . H26C H 0.1203 0.5222 0.7051 0.045 Uiso 1 1 calc R . . C25 C 0.0281(4) 0.4711(5) 0.6137(3) 0.0355(19) Uani 1 1 d . . . H25A H 0.0042 0.4459 0.5803 0.053 Uiso 1 1 calc R . . H25B H 0.0669 0.4820 0.6058 0.053 Uiso 1 1 calc R . . H25C H 0.0093 0.5184 0.6213 0.053 Uiso 1 1 calc R . . C24 C -0.0073(3) 0.3660(4) 0.6757(3) 0.0177(14) Uani 1 1 d . . . C23 C 0.0141(3) 0.3340(4) 0.7302(3) 0.0229(15) Uani 1 1 d . . . C30 C 0.2087(3) 0.1157(4) 0.5185(3) 0.0264(17) Uani 1 1 d . . . C29 C -0.0639(3) 0.3476(5) 0.6359(3) 0.0343(19) Uani 1 1 d . . . H29A H -0.0578 0.3451 0.5962 0.051 Uiso 1 1 calc R . . H29B H -0.0927 0.3868 0.6387 0.051 Uiso 1 1 calc R . . H29C H -0.0782 0.2987 0.6466 0.051 Uiso 1 1 calc R . . C28 C -0.0179(3) 0.2754(4) 0.7583(3) 0.0323(18) Uani 1 1 d . . . H28A H -0.0418 0.2440 0.7285 0.048 Uiso 1 1 calc R . . H28B H -0.0431 0.3006 0.7809 0.048 Uiso 1 1 calc R . . H28C H 0.0105 0.2436 0.7838 0.048 Uiso 1 1 calc R . . C31 C 0.2535(3) 0.1213(4) 0.5678(3) 0.0257(16) Uani 1 1 d . . . C32 C 0.2440(3) 0.0628(4) 0.6064(3) 0.0303(18) Uani 1 1 d . . . C35 C 0.2027(4) 0.1659(5) 0.4657(3) 0.0343(18) Uani 1 1 d . . . H35A H 0.2389 0.1637 0.4507 0.051 Uiso 1 1 calc R . . H35B H 0.1955 0.2180 0.4762 0.051 Uiso 1 1 calc R . . H35C H 0.1700 0.1482 0.4359 0.051 Uiso 1 1 calc R . . C34 C 0.1712(3) 0.0533(4) 0.5256(3) 0.0254(16) Uani 1 1 d . . . C33 C 0.1935(4) 0.0222(4) 0.5797(3) 0.0307(18) Uani 1 1 d . . . C36 C 0.3028(3) 0.1770(5) 0.5765(4) 0.038(2) Uani 1 1 d . . . H36A H 0.3235 0.1731 0.5445 0.057 Uiso 1 1 calc R . . H36B H 0.3299 0.1661 0.6129 0.057 Uiso 1 1 calc R . . H36C H 0.2871 0.2281 0.5777 0.057 Uiso 1 1 calc R . . C46 C 0.1874(4) 0.6754(5) 0.2573(4) 0.044(2) Uani 1 1 d . . . H46A H 0.1637 0.6743 0.2181 0.066 Uiso 1 1 calc R . . H46B H 0.1622 0.6860 0.2848 0.066 Uiso 1 1 calc R . . H46C H 0.2064 0.6263 0.2663 0.066 Uiso 1 1 calc R . . C45 C 0.5285(4) 0.5551(6) 0.3160(4) 0.065(3) Uani 1 1 d . . . H45A H 0.5417 0.5204 0.2890 0.097 Uiso 1 1 calc R . . H45B H 0.5170 0.5262 0.3471 0.097 Uiso 1 1 calc R . . H45C H 0.5605 0.5896 0.3322 0.097 Uiso 1 1 calc R . . C44 C 0.4957(6) 0.6433(6) 0.2175(5) 0.071(4) Uani 1 1 d . . . H44A H 0.5077 0.6004 0.1965 0.107 Uiso 1 1 calc R . . H44B H 0.5295 0.6758 0.2315 0.107 Uiso 1 1 calc R . . H44C H 0.4654 0.6722 0.1916 0.107 Uiso 1 1 calc R . . C43 C 0.4204(4) 0.5358(5) 0.2400(4) 0.047(2) Uani 1 1 d . . . H43A H 0.3875 0.5590 0.2133 0.070 Uiso 1 1 calc R . . H43B H 0.4055 0.5040 0.2677 0.070 Uiso 1 1 calc R . . H43C H 0.4431 0.5047 0.2182 0.070 Uiso 1 1 calc R . . C42 C 0.5014(4) 0.8643(5) 0.5370(4) 0.051(2) Uani 1 1 d . . . H42A H 0.5085 0.8984 0.5066 0.077 Uiso 1 1 calc R . . H42B H 0.5373 0.8590 0.5664 0.077 Uiso 1 1 calc R . . H42C H 0.4703 0.8850 0.5547 0.077 Uiso 1 1 calc R . . C41 C 0.5480(3) 0.7359(5) 0.4921(4) 0.043(2) Uani 1 1 d . . . H41A H 0.5611 0.7678 0.4634 0.065 Uiso 1 1 calc R . . H41B H 0.5425 0.6841 0.4775 0.065 Uiso 1 1 calc R . . H41C H 0.5775 0.7364 0.5280 0.065 Uiso 1 1 calc R . . C40 C 0.4740(4) 0.7211(5) 0.5714(3) 0.041(2) Uani 1 1 d . . . H40A H 0.4388 0.7372 0.5846 0.062 Uiso 1 1 calc R . . H40B H 0.5085 0.7320 0.6013 0.062 Uiso 1 1 calc R . . H40C H 0.4719 0.6668 0.5635 0.062 Uiso 1 1 calc R . . C39 C 0.1201(4) 0.0254(5) 0.4833(4) 0.039(2) Uani 1 1 d . . . H39A H 0.1098 0.0621 0.4519 0.059 Uiso 1 1 calc R . . H39B H 0.0869 0.0188 0.5023 0.059 Uiso 1 1 calc R . . H39C H 0.1298 -0.0230 0.4676 0.059 Uiso 1 1 calc R . . C38 C 0.1696(4) -0.0474(5) 0.6037(4) 0.050(3) Uani 1 1 d . . . H38A H 0.1283 -0.0537 0.5855 0.076 Uiso 1 1 calc R . . H38B H 0.1733 -0.0419 0.6455 0.076 Uiso 1 1 calc R . . H38C H 0.1917 -0.0918 0.5957 0.076 Uiso 1 1 calc R . . C37 C 0.2814(4) 0.0455(5) 0.6641(4) 0.052(3) Uani 1 1 d . . . H37A H 0.2777 -0.0081 0.6729 0.078 Uiso 1 1 calc R . . H37B H 0.2687 0.0763 0.6936 0.078 Uiso 1 1 calc R . . H37C H 0.3223 0.0571 0.6634 0.078 Uiso 1 1 calc R . . C49 C 0.2450(3) 0.9325(4) 0.4325(3) 0.0270(17) Uani 1 1 d . . . C48 C 0.2708(4) 0.7298(6) 0.1980(3) 0.047(2) Uani 1 1 d . . . H48A H 0.2383 0.7290 0.1646 0.070 Uiso 1 1 calc R . . H48B H 0.2905 0.6807 0.2018 0.070 Uiso 1 1 calc R . . H48C H 0.2986 0.7693 0.1928 0.070 Uiso 1 1 calc R . . C47 C 0.1952(3) 0.8289(5) 0.2369(4) 0.041(2) Uani 1 1 d . . . H47A H 0.2189 0.8742 0.2355 0.062 Uiso 1 1 calc R . . H47B H 0.1685 0.8373 0.2632 0.062 Uiso 1 1 calc R . . H47C H 0.1726 0.8179 0.1982 0.062 Uiso 1 1 calc R . . C52 C 0.2339(3) 0.8343(4) 0.4922(3) 0.0312(18) Uani 1 1 d . . . C51 C 0.2832(3) 0.8763(4) 0.5192(3) 0.0289(17) Uani 1 1 d . . . C50 C 0.2901(3) 0.9376(4) 0.4826(3) 0.0259(16) Uani 1 1 d . . . C55 C 0.3355(4) 0.9981(5) 0.4968(3) 0.037(2) Uani 1 1 d . . . H55A H 0.3745 0.9753 0.5033 0.056 Uiso 1 1 calc R . . H55B H 0.3305 1.0248 0.5318 0.056 Uiso 1 1 calc R . . H55C H 0.3312 1.0339 0.4647 0.056 Uiso 1 1 calc R . . C54 C 0.2340(4) 0.9877(5) 0.3833(4) 0.038(2) Uani 1 1 d . . . H54A H 0.2373 0.9616 0.3475 0.057 Uiso 1 1 calc R . . H54B H 0.2630 1.0284 0.3909 0.057 Uiso 1 1 calc R . . H54C H 0.1947 1.0089 0.3793 0.057 Uiso 1 1 calc R . . C53 C 0.2099(3) 0.8694(4) 0.4386(3) 0.0273(17) Uani 1 1 d . . . C64 C 0.2210(3) 0.5970(5) 0.4078(4) 0.038(2) Uani 1 1 d . . . H64A H 0.2219 0.6514 0.4007 0.058 Uiso 1 1 calc R . . H64B H 0.2026 0.5876 0.4409 0.058 Uiso 1 1 calc R . . H64C H 0.1984 0.5717 0.3737 0.058 Uiso 1 1 calc R . . C63 C 0.3235(3) 0.5753(4) 0.4731(3) 0.0281(17) Uani 1 1 d . . . C62 C 0.3743(3) 0.5353(4) 0.4688(3) 0.0287(17) Uani 1 1 d . . . C61 C 0.3649(3) 0.5018(4) 0.4138(3) 0.0289(17) Uani 1 1 d . . . C60 C 0.3086(3) 0.5201(4) 0.3836(3) 0.0280(17) Uani 1 1 d . . . C59 C 0.2818(3) 0.5669(4) 0.4204(3) 0.0288(17) Uani 1 1 d . . . C58 C 0.1569(4) 0.8443(5) 0.3959(4) 0.045(2) Uani 1 1 d . . . H58A H 0.1539 0.8731 0.3601 0.068 Uiso 1 1 calc R . . H58B H 0.1219 0.8529 0.4119 0.068 Uiso 1 1 calc R . . H58C H 0.1602 0.7904 0.3879 0.068 Uiso 1 1 calc R . . C57 C 0.2067(4) 0.7691(5) 0.5183(4) 0.047(2) Uani 1 1 d . . . H57A H 0.1924 0.7316 0.4884 0.071 Uiso 1 1 calc R . . H57B H 0.1740 0.7876 0.5346 0.071 Uiso 1 1 calc R . . H57C H 0.2360 0.7460 0.5489 0.071 Uiso 1 1 calc R . . C56 C 0.3219(4) 0.8615(5) 0.5767(3) 0.045(2) Uani 1 1 d . . . H56A H 0.3210 0.8077 0.5858 0.068 Uiso 1 1 calc R . . H56B H 0.3081 0.8909 0.6063 0.068 Uiso 1 1 calc R . . H56C H 0.3621 0.8764 0.5755 0.068 Uiso 1 1 calc R . . C74 C 0.4246(4) 0.8427(5) 0.1943(3) 0.043(2) Uani 1 1 d . . . H74A H 0.3931 0.8694 0.1683 0.065 Uiso 1 1 calc R . . H74B H 0.4131 0.7901 0.1983 0.065 Uiso 1 1 calc R . . H74C H 0.4602 0.8442 0.1785 0.065 Uiso 1 1 calc R . . C72 C 0.4251(3) 0.9531(3) 0.3294(3) 0.0198(15) Uani 1 1 d . . . C71 C 0.4825(3) 0.9219(4) 0.3407(3) 0.0204(15) Uani 1 1 d . . . C70 C 0.4887(3) 0.8769(4) 0.2932(3) 0.0253(16) Uani 1 1 d . . . C69 C 0.4360(3) 0.8802(4) 0.2524(3) 0.0228(15) Uani 1 1 d . . . C68 C 0.3128(4) 0.6188(5) 0.5232(3) 0.038(2) Uani 1 1 d . . . H68A H 0.3215 0.6722 0.5182 0.058 Uiso 1 1 calc R . . H68B H 0.3381 0.5997 0.5585 0.058 Uiso 1 1 calc R . . H68C H 0.2718 0.6133 0.5262 0.058 Uiso 1 1 calc R . . C67 C 0.4274(3) 0.5255(5) 0.5157(4) 0.038(2) Uani 1 1 d . . . H67A H 0.4353 0.4715 0.5223 0.056 Uiso 1 1 calc R . . H67B H 0.4206 0.5489 0.5512 0.056 Uiso 1 1 calc R . . H67C H 0.4610 0.5496 0.5042 0.056 Uiso 1 1 calc R . . C66 C 0.4079(4) 0.4490(5) 0.3930(4) 0.041(2) Uani 1 1 d . . . H66A H 0.3924 0.4349 0.3528 0.061 Uiso 1 1 calc R . . H66B H 0.4134 0.4036 0.4170 0.061 Uiso 1 1 calc R . . H66C H 0.4455 0.4748 0.3957 0.061 Uiso 1 1 calc R . . C65 C 0.2810(4) 0.4960(5) 0.3237(4) 0.048(2) Uani 1 1 d . . . H65A H 0.2922 0.5311 0.2959 0.072 Uiso 1 1 calc R . . H65B H 0.2383 0.4959 0.3193 0.072 Uiso 1 1 calc R . . H65C H 0.2943 0.4450 0.3166 0.072 Uiso 1 1 calc R . . C75 C 0.5430(4) 0.8346(5) 0.2885(4) 0.046(2) Uani 1 1 d . . . H75A H 0.5453 0.8298 0.2478 0.069 Uiso 1 1 calc R . . H75B H 0.5419 0.7842 0.3053 0.069 Uiso 1 1 calc R . . H75C H 0.5773 0.8619 0.3092 0.069 Uiso 1 1 calc R . . C77 C 0.3991(3) 1.0057(4) 0.3661(4) 0.0334(18) Uani 1 1 d . . . H77A H 0.4013 1.0574 0.3520 0.050 Uiso 1 1 calc R . . H77B H 0.4208 1.0023 0.4060 0.050 Uiso 1 1 calc R . . H77C H 0.3581 0.9921 0.3644 0.050 Uiso 1 1 calc R . . C78 C 0.3360(3) 0.9488(4) 0.2447(4) 0.0369(19) Uani 1 1 d . . . H78A H 0.3368 0.9994 0.2282 0.055 Uiso 1 1 calc R . . H78B H 0.3103 0.9488 0.2726 0.055 Uiso 1 1 calc R . . H78C H 0.3213 0.9126 0.2139 0.055 Uiso 1 1 calc R . . C76 C 0.5296(3) 0.9377(5) 0.3929(3) 0.038(2) Uani 1 1 d . . . H76A H 0.5506 0.8908 0.4057 0.056 Uiso 1 1 calc R . . H76B H 0.5119 0.9577 0.4239 0.056 Uiso 1 1 calc R . . H76C H 0.5571 0.9748 0.3829 0.056 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 Pd1 0.0147(3) 0.0166(3) 0.0174(3) 0.0014(2) 0.0046(2) 0.0010(2) C1 0.045(5) 0.040(5) 0.047(5) -0.010(4) -0.007(4) -0.008(4) P1 0.0216(10) 0.0277(10) 0.0247(10) -0.0026(8) 0.0001(8) 0.0047(8) Ga1 0.0202(4) 0.0207(4) 0.0230(4) 0.0052(3) 0.0070(3) -0.0024(3) Pd2 0.0300(3) 0.0157(3) 0.0310(3) 0.0036(2) 0.0166(2) -0.0014(2) C73 0.021(4) 0.013(3) 0.031(4) 0.006(3) 0.005(3) 0.000(3) C2 0.034(5) 0.127(11) 0.058(7) -0.026(7) -0.006(5) 0.032(6) P2 0.0309(11) 0.0200(10) 0.0397(12) 0.0080(8) 0.0167(9) -0.0012(8) Ga2 0.0179(4) 0.0185(4) 0.0188(4) -0.0038(3) 0.0067(3) 0.0022(3) Pd3 0.0157(3) 0.0170(3) 0.0144(3) 0.0005(2) 0.0046(2) 0.0012(2) C3 0.083(8) 0.045(6) 0.047(6) 0.018(5) -0.010(5) -0.003(5) P3 0.0201(9) 0.0302(11) 0.0189(10) -0.0060(8) 0.0021(8) 0.0005(8) Ga3 0.0243(4) 0.0166(4) 0.0242(4) -0.0017(3) 0.0089(3) 0.0054(3) Pd5 0.0300(3) 0.0152(3) 0.0310(3) -0.0025(2) 0.0189(3) 0.0017(2) C5 0.081(9) 0.068(8) 0.090(9) 0.003(7) 0.003(7) -0.034(7) P5 0.0245(10) 0.0216(10) 0.0287(10) -0.0069(8) 0.0108(8) 0.0024(8) Ga5 0.0217(4) 0.0133(4) 0.0246(4) 0.0023(3) 0.0079(3) -0.0019(3) Pd4 0.0169(3) 0.0134(2) 0.0141(3) -0.00061(19) 0.0047(2) 0.0002(2) C4 0.111(7) 0.046(5) 0.122(8) 0.026(5) 0.068(6) 0.009(5) P4 0.0246(10) 0.0240(10) 0.0167(9) -0.0003(7) 0.0018(8) -0.0026(8) Ga4 0.0239(4) 0.0211(4) 0.0228(4) -0.0031(3) 0.0118(3) 0.0048(3) Pd6 0.0147(2) 0.0125(2) 0.0156(3) 0.00020(19) 0.0046(2) 0.00102(19) C6 0.111(7) 0.046(5) 0.122(8) 0.026(5) 0.068(6) 0.009(5) P6 0.0186(9) 0.0220(10) 0.0199(9) -0.0012(7) 0.0021(7) -0.0014(7) Ga6 0.0189(4) 0.0153(4) 0.0179(4) 0.0022(3) 0.0059(3) -0.0023(3) C7 0.054(6) 0.051(6) 0.049(6) -0.005(5) -0.015(5) 0.022(5) C10 0.030(4) 0.031(4) 0.036(5) 0.017(3) 0.015(4) -0.002(3) C9 0.054(6) 0.105(9) 0.030(5) -0.028(5) -0.001(5) 0.013(6) C8 0.043(6) 0.070(7) 0.072(7) 0.010(6) -0.004(5) -0.028(5) C11 0.040(5) 0.020(4) 0.034(4) 0.005(3) 0.020(4) -0.008(3) C14 0.035(4) 0.040(5) 0.021(4) 0.011(3) 0.010(3) -0.008(4) C13 0.029(4) 0.022(4) 0.035(4) 0.007(3) 0.019(3) -0.005(3) C12 0.023(4) 0.022(4) 0.042(5) 0.009(3) 0.010(3) -0.009(3) C16 0.066(6) 0.035(5) 0.057(6) -0.006(4) 0.035(5) -0.020(5) C15 0.041(5) 0.072(7) 0.066(7) 0.047(6) 0.019(5) 0.017(5) C17 0.036(5) 0.062(6) 0.050(6) 0.011(5) 0.001(4) -0.016(4) C18 0.050(5) 0.032(5) 0.067(6) 0.007(4) 0.039(5) -0.001(4) C19 0.076(7) 0.069(7) 0.027(5) 0.009(5) 0.010(5) -0.012(6) C21 0.022(4) 0.023(4) 0.020(4) -0.005(3) 0.010(3) 0.005(3) C20 0.023(4) 0.023(4) 0.021(4) -0.006(3) 0.009(3) 0.007(3) C22 0.024(4) 0.020(4) 0.020(4) -0.002(3) 0.009(3) 0.005(3) C27 0.033(4) 0.044(5) 0.022(4) 0.002(3) 0.010(3) 0.001(4) C26 0.031(4) 0.033(4) 0.027(4) -0.006(3) 0.007(3) -0.007(3) C25 0.035(5) 0.041(5) 0.032(4) 0.009(4) 0.009(4) 0.007(4) C24 0.019(3) 0.016(3) 0.021(4) -0.002(3) 0.010(3) 0.006(3) C23 0.023(4) 0.023(4) 0.027(4) 0.002(3) 0.015(3) 0.006(3) C30 0.034(4) 0.023(4) 0.029(4) -0.003(3) 0.021(3) 0.001(3) C29 0.024(4) 0.047(5) 0.032(4) 0.000(4) 0.008(3) -0.002(4) C28 0.034(4) 0.029(4) 0.036(5) 0.009(3) 0.014(4) -0.004(3) C31 0.029(4) 0.020(4) 0.029(4) -0.002(3) 0.010(3) 0.006(3) C32 0.034(4) 0.024(4) 0.033(4) -0.003(3) 0.007(4) 0.014(3) C35 0.039(5) 0.035(5) 0.031(4) -0.001(4) 0.013(4) 0.005(4) C34 0.025(4) 0.021(4) 0.032(4) -0.011(3) 0.012(3) 0.006(3) C33 0.043(5) 0.017(4) 0.037(5) -0.002(3) 0.021(4) 0.009(3) C36 0.026(4) 0.037(5) 0.053(5) -0.007(4) 0.009(4) 0.003(4) C46 0.032(5) 0.046(5) 0.048(5) 0.006(4) -0.006(4) -0.014(4) C45 0.049(6) 0.084(8) 0.055(6) -0.028(6) -0.003(5) 0.035(6) C44 0.124(10) 0.038(6) 0.077(8) 0.002(5) 0.079(8) 0.007(6) C43 0.039(5) 0.052(6) 0.049(6) -0.025(5) 0.012(4) -0.005(4) C42 0.070(7) 0.039(5) 0.039(5) -0.007(4) -0.003(5) -0.016(5) C41 0.031(5) 0.057(6) 0.039(5) 0.005(4) 0.002(4) 0.007(4) C40 0.039(5) 0.060(6) 0.024(4) 0.007(4) 0.002(4) -0.002(4) C39 0.038(5) 0.033(5) 0.049(5) -0.012(4) 0.014(4) -0.006(4) C38 0.073(7) 0.024(5) 0.064(6) 0.008(4) 0.036(5) 0.008(4) C37 0.060(6) 0.040(5) 0.048(6) 0.005(4) -0.008(5) 0.032(5) C49 0.026(4) 0.034(4) 0.023(4) -0.005(3) 0.010(3) 0.011(3) C48 0.040(5) 0.073(7) 0.026(5) -0.008(4) 0.003(4) 0.001(5) C47 0.031(4) 0.051(6) 0.036(5) 0.010(4) -0.009(4) 0.005(4) C52 0.038(4) 0.029(4) 0.035(4) -0.008(3) 0.025(4) 0.003(3) C51 0.032(4) 0.039(5) 0.021(4) -0.005(3) 0.019(3) 0.004(3) C50 0.028(4) 0.022(4) 0.033(4) -0.010(3) 0.017(3) 0.006(3) C55 0.043(5) 0.038(5) 0.033(5) -0.016(4) 0.013(4) -0.002(4) C54 0.038(5) 0.037(5) 0.042(5) 0.004(4) 0.016(4) 0.011(4) C53 0.026(4) 0.027(4) 0.034(4) -0.009(3) 0.019(3) 0.002(3) C64 0.027(4) 0.033(5) 0.056(6) 0.005(4) 0.011(4) -0.003(3) C63 0.035(4) 0.018(4) 0.037(5) 0.013(3) 0.021(4) 0.001(3) C62 0.024(4) 0.025(4) 0.037(5) 0.011(3) 0.007(3) -0.006(3) C61 0.032(4) 0.016(4) 0.041(5) 0.007(3) 0.011(4) -0.003(3) C60 0.035(4) 0.012(3) 0.037(4) 0.002(3) 0.009(4) -0.011(3) C59 0.027(4) 0.021(4) 0.040(5) 0.013(3) 0.012(4) -0.001(3) C58 0.034(5) 0.058(6) 0.049(5) -0.011(5) 0.018(4) -0.005(4) C57 0.058(6) 0.039(5) 0.060(6) -0.002(4) 0.046(5) 0.000(4) C56 0.058(6) 0.052(6) 0.030(5) 0.004(4) 0.021(4) 0.003(5) C74 0.070(6) 0.037(5) 0.029(5) -0.009(4) 0.024(4) -0.007(4) C72 0.025(4) 0.006(3) 0.030(4) 0.001(3) 0.010(3) -0.003(3) C71 0.024(4) 0.014(3) 0.024(4) 0.003(3) 0.005(3) -0.009(3) C70 0.027(4) 0.017(4) 0.037(4) 0.004(3) 0.018(3) -0.002(3) C69 0.034(4) 0.022(4) 0.014(3) 0.001(3) 0.007(3) -0.007(3) C68 0.045(5) 0.036(5) 0.039(5) 0.020(4) 0.018(4) 0.006(4) C67 0.034(5) 0.039(5) 0.039(5) 0.012(4) 0.004(4) 0.004(4) C66 0.043(5) 0.028(5) 0.054(6) 0.005(4) 0.015(4) 0.005(4) C65 0.047(6) 0.037(5) 0.051(6) -0.008(4) -0.011(4) -0.005(4) C75 0.035(5) 0.034(5) 0.078(7) -0.005(5) 0.033(5) -0.001(4) C77 0.028(4) 0.027(4) 0.046(5) -0.011(4) 0.012(4) 0.000(3) C78 0.035(5) 0.026(4) 0.045(5) 0.007(4) -0.002(4) 0.004(3) C76 0.035(5) 0.039(5) 0.037(5) 0.007(4) 0.002(4) -0.010(4) _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 Pd1 P1 2.2746(19) . ? Pd1 Ga1 2.5260(9) . ? Pd1 Ga2 2.5390(8) . ? Pd1 Ga3 2.5776(9) . ? Pd1 Pd3 2.5896(7) . ? Pd1 Pd2 2.8848(7) . ? C1 P1 1.816(8) . ? P1 C2 1.814(9) . ? P1 C3 1.846(9) . ? Ga1 C11 2.345(7) . ? Ga1 C10 2.374(7) . ? Ga1 C12 2.391(7) . ? Ga1 C14 2.437(7) . ? Ga1 C13 2.454(7) . ? Ga1 Pd3 2.4975(9) . ? Pd2 P2 2.2549(19) . ? Pd2 Ga3 2.4722(9) . ? Pd2 Ga2 2.4833(9) . ? Pd2 Pd3 2.8290(7) . ? C73 C69 1.400(10) . ? C73 C72 1.409(10) . ? C73 C78 1.516(10) . ? C73 Ga6 2.331(7) . ? P2 C6 1.799(11) . ? P2 C4 1.803(12) . ? P2 C5 1.805(11) . ? Ga2 C20 2.364(7) . ? Ga2 C21 2.392(7) . ? Ga2 C24 2.399(6) . ? Ga2 C23 2.434(6) . ? Ga2 C22 2.438(6) . ? Ga2 Pd3 2.5621(8) . ? Pd3 P3 2.2641(19) . ? Pd3 Ga3 2.5491(9) . ? P3 C7 1.815(9) . ? P3 C8 1.820(9) . ? P3 C9 1.823(9) . ? Ga3 C31 2.364(7) . ? Ga3 C30 2.369(7) . ? Ga3 C32 2.385(7) . ? Ga3 C33 2.417(7) . ? Ga3 C34 2.426(7) . ? Pd5 P5 2.2600(18) . ? Pd5 Ga6 2.4679(9) . ? Pd5 Ga5 2.4740(9) . ? Pd5 Pd4 2.8479(7) . ? Pd5 Pd6 2.8705(7) . ? P5 C45 1.808(9) . ? P5 C43 1.809(8) . ? P5 C44 1.815(9) . ? Ga5 C59 2.329(7) . ? Ga5 C63 2.365(7) . ? Ga5 C60 2.371(7) . ? Ga5 C61 2.425(7) . ? Ga5 C62 2.434(7) . ? Ga5 Pd4 2.5343(9) . ? Ga5 Pd6 2.6002(9) . ? Pd4 P4 2.2704(19) . ? Pd4 Ga4 2.4895(9) . ? Pd4 Ga6 2.5206(8) . ? Pd4 Pd6 2.5963(7) . ? P4 C40 1.817(8) . ? P4 C41 1.821(8) . ? P4 C42 1.828(9) . ? Ga4 C49 2.372(7) . ? Ga4 C50 2.373(7) . ? Ga4 C51 2.376(7) . ? Ga4 C52 2.390(7) . ? Ga4 C53 2.396(7) . ? Ga4 Pd6 2.5014(9) . ? Pd6 P6 2.2728(19) . ? Pd6 Ga6 2.5629(8) . ? P6 C48 1.806(8) . ? P6 C47 1.829(8) . ? P6 C46 1.830(8) . ? Ga6 C72 2.359(6) . ? Ga6 C69 2.400(6) . ? Ga6 C71 2.425(6) . ? Ga6 C70 2.449(7) . ? C10 C14 1.408(11) . ? C10 C11 1.411(11) . ? C10 C15 1.491(11) . ? C11 C12 1.432(10) . ? C11 C16 1.488(11) . ? C14 C13 1.426(11) . ? C14 C19 1.504(11) . ? C13 C12 1.406(11) . ? C13 C18 1.493(10) . ? C12 C17 1.500(11) . ? C21 C22 1.421(9) . ? C21 C20 1.431(10) . ? C21 C26 1.495(10) . ? C20 C24 1.433(9) . ? C20 C25 1.492(10) . ? C22 C23 1.399(10) . ? C22 C27 1.491(10) . ? C24 C23 1.406(9) . ? C24 C29 1.496(10) . ? C23 C28 1.511(9) . ? C30 C31 1.403(11) . ? C30 C34 1.442(10) . ? C30 C35 1.518(10) . ? C31 C32 1.430(10) . ? C31 C36 1.498(10) . ? C32 C33 1.417(11) . ? C32 C37 1.495(11) . ? C34 C33 1.396(11) . ? C34 C39 1.479(11) . ? C33 C38 1.511(11) . ? C49 C53 1.410(10) . ? C49 C50 1.421(10) . ? C49 C54 1.504(11) . ? C52 C51 1.410(11) . ? C52 C53 1.424(11) . ? C52 C57 1.509(11) . ? C51 C50 1.419(10) . ? C51 C56 1.497(11) . ? C50 C55 1.498(11) . ? C53 C58 1.499(11) . ? C64 C59 1.490(10) . ? C63 C62 1.404(10) . ? C63 C59 1.426(11) . ? C63 C68 1.478(11) . ? C62 C61 1.409(11) . ? C62 C67 1.497(10) . ? C61 C60 1.401(11) . ? C61 C66 1.524(11) . ? C60 C59 1.436(10) . ? C60 C65 1.499(11) . ? C74 C69 1.501(10) . ? C72 C71 1.424(9) . ? C72 C77 1.484(9) . ? C71 C70 1.410(10) . ? C71 C76 1.505(10) . ? C70 C69 1.404(10) . ? C70 C75 1.497(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 Ga1 127.07(6) . . ? P1 Pd1 Ga2 115.94(5) . . ? Ga1 Pd1 Ga2 96.26(3) . . ? P1 Pd1 Ga3 119.73(6) . . ? Ga1 Pd1 Ga3 92.34(3) . . ? Ga2 Pd1 Ga3 99.55(3) . . ? P1 Pd1 Pd3 174.30(6) . . ? Ga1 Pd1 Pd3 58.43(2) . . ? Ga2 Pd1 Pd3 59.93(2) . . ? Ga3 Pd1 Pd3 59.12(2) . . ? P1 Pd1 Pd2 112.60(6) . . ? Ga1 Pd1 Pd2 120.32(3) . . ? Ga2 Pd1 Pd2 54.04(2) . . ? Ga3 Pd1 Pd2 53.46(2) . . ? Pd3 Pd1 Pd2 61.955(19) . . ? C2 P1 C1 100.0(5) . . ? C2 P1 C3 102.0(6) . . ? C1 P1 C3 99.6(5) . . ? C2 P1 Pd1 119.1(3) . . ? C1 P1 Pd1 121.0(3) . . ? C3 P1 Pd1 112.0(3) . . ? C11 Ga1 C10 34.8(3) . . ? C11 Ga1 C12 35.2(3) . . ? C10 Ga1 C12 57.7(3) . . ? C11 Ga1 C14 56.9(3) . . ? C10 Ga1 C14 34.0(3) . . ? C12 Ga1 C14 56.5(3) . . ? C11 Ga1 C13 57.1(2) . . ? C10 Ga1 C13 56.9(2) . . ? C12 Ga1 C13 33.7(3) . . ? C14 Ga1 C13 33.9(3) . . ? C11 Ga1 Pd3 147.19(19) . . ? C10 Ga1 Pd3 121.93(19) . . ? C12 Ga1 Pd3 175.5(2) . . ? C14 Ga1 Pd3 120.35(19) . . ? C13 Ga1 Pd3 141.89(18) . . ? C11 Ga1 Pd1 126.61(19) . . ? C10 Ga1 Pd1 153.8(2) . . ? C12 Ga1 Pd1 120.49(19) . . ? C14 Ga1 Pd1 171.0(2) . . ? C13 Ga1 Pd1 138.59(18) . . ? Pd3 Ga1 Pd1 62.06(2) . . ? P2 Pd2 Ga3 124.53(6) . . ? P2 Pd2 Ga2 131.41(6) . . ? Ga3 Pd2 Ga2 104.06(3) . . ? P2 Pd2 Pd3 151.90(6) . . ? Ga3 Pd2 Pd3 57.00(2) . . ? Ga2 Pd2 Pd3 57.23(2) . . ? P2 Pd2 Pd1 153.86(6) . . ? Ga3 Pd2 Pd1 56.90(2) . . ? Ga2 Pd2 Pd1 55.85(2) . . ? Pd3 Pd2 Pd1 53.891(17) . . ? C69 C73 C72 109.3(6) . . ? C69 C73 C78 126.6(7) . . ? C72 C73 C78 124.0(6) . . ? C69 C73 Ga6 75.5(4) . . ? C72 C73 Ga6 73.6(4) . . ? C78 C73 Ga6 119.6(5) . . ? C6 P2 C4 100.4(6) . . ? C6 P2 C5 97.6(6) . . ? C4 P2 C5 98.9(6) . . ? C6 P2 Pd2 123.6(4) . . ? C4 P2 Pd2 116.0(4) . . ? C5 P2 Pd2 116.1(4) . . ? C20 Ga2 C21 35.0(2) . . ? C20 Ga2 C24 35.0(2) . . ? C21 Ga2 C24 57.4(2) . . ? C20 Ga2 C23 57.1(2) . . ? C21 Ga2 C23 56.3(2) . . ? C24 Ga2 C23 33.8(2) . . ? C20 Ga2 C22 57.5(2) . . ? C21 Ga2 C22 34.2(2) . . ? C24 Ga2 C22 56.5(2) . . ? C23 Ga2 C22 33.4(2) . . ? C20 Ga2 Pd2 159.29(18) . . ? C21 Ga2 Pd2 156.54(17) . . ? C24 Ga2 Pd2 125.58(16) . . ? C23 Ga2 Pd2 111.48(17) . . ? C22 Ga2 Pd2 124.13(16) . . ? C20 Ga2 Pd1 129.17(17) . . ? C21 Ga2 Pd1 109.54(16) . . ? C24 Ga2 Pd1 164.17(16) . . ? C23 Ga2 Pd1 149.27(17) . . ? C22 Ga2 Pd1 118.84(16) . . ? Pd2 Ga2 Pd1 70.11(2) . . ? C20 Ga2 Pd3 111.98(17) . . ? C21 Ga2 Pd3 133.34(17) . . ? C24 Ga2 Pd3 119.77(16) . . ? C23 Ga2 Pd3 149.46(18) . . ? C22 Ga2 Pd3 167.52(16) . . ? Pd2 Ga2 Pd3 68.19(2) . . ? Pd1 Ga2 Pd3 61.01(2) . . ? P3 Pd3 Ga1 125.60(6) . . ? P3 Pd3 Ga3 116.90(5) . . ? Ga1 Pd3 Ga3 93.69(3) . . ? P3 Pd3 Ga2 118.87(5) . . ? Ga1 Pd3 Ga2 96.39(3) . . ? Ga3 Pd3 Ga2 99.69(3) . . ? P3 Pd3 Pd1 174.84(6) . . ? Ga1 Pd3 Pd1 59.51(2) . . ? Ga3 Pd3 Pd1 60.21(2) . . ? Ga2 Pd3 Pd1 59.05(2) . . ? P3 Pd3 Pd2 110.70(5) . . ? Ga1 Pd3 Pd2 123.60(3) . . ? Ga3 Pd3 Pd2 54.43(2) . . ? Ga2 Pd3 Pd2 54.58(2) . . ? Pd1 Pd3 Pd2 64.15(2) . . ? C7 P3 C8 101.4(5) . . ? C7 P3 C9 99.6(5) . . ? C8 P3 C9 100.0(5) . . ? C7 P3 Pd3 120.8(3) . . ? C8 P3 Pd3 113.5(3) . . ? C9 P3 Pd3 118.1(3) . . ? C31 Ga3 C30 34.5(3) . . ? C31 Ga3 C32 35.0(3) . . ? C30 Ga3 C32 57.3(3) . . ? C31 Ga3 C33 57.5(3) . . ? C30 Ga3 C33 56.8(2) . . ? C32 Ga3 C33 34.3(3) . . ? C31 Ga3 C34 57.8(2) . . ? C30 Ga3 C34 35.0(2) . . ? C32 Ga3 C34 56.9(3) . . ? C33 Ga3 C34 33.5(3) . . ? C31 Ga3 Pd2 159.16(18) . . ? C30 Ga3 Pd2 162.31(19) . . ? C32 Ga3 Pd2 127.57(19) . . ? C33 Ga3 Pd2 115.95(18) . . ? C34 Ga3 Pd2 129.55(17) . . ? C31 Ga3 Pd3 127.92(18) . . ? C30 Ga3 Pd3 109.38(18) . . ? C32 Ga3 Pd3 162.9(2) . . ? C33 Ga3 Pd3 150.6(2) . . ? C34 Ga3 Pd3 119.63(18) . . ? Pd2 Ga3 Pd3 68.56(2) . . ? C31 Ga3 Pd1 105.53(18) . . ? C30 Ga3 Pd1 125.69(18) . . ? C32 Ga3 Pd1 116.27(19) . . ? C33 Ga3 Pd1 148.7(2) . . ? C34 Ga3 Pd1 160.62(18) . . ? Pd2 Ga3 Pd1 69.64(2) . . ? Pd3 Ga3 Pd1 60.68(2) . . ? P5 Pd5 Ga6 130.76(6) . . ? P5 Pd5 Ga5 124.94(6) . . ? Ga6 Pd5 Ga5 103.92(3) . . ? P5 Pd5 Pd4 159.55(6) . . ? Ga6 Pd5 Pd4 56.06(2) . . ? Ga5 Pd5 Pd4 56.35(2) . . ? P5 Pd5 Pd6 146.19(6) . . ? Ga6 Pd5 Pd6 56.78(2) . . ? Ga5 Pd5 Pd6 57.65(2) . . ? Pd4 Pd5 Pd6 54.003(17) . . ? C45 P5 C43 101.9(5) . . ? C45 P5 C44 100.4(6) . . ? C43 P5 C44 97.1(5) . . ? C45 P5 Pd5 116.3(3) . . ? C43 P5 Pd5 113.7(3) . . ? C44 P5 Pd5 123.6(3) . . ? C59 Ga5 C63 35.4(3) . . ? C59 Ga5 C60 35.6(3) . . ? C63 Ga5 C60 58.0(3) . . ? C59 Ga5 C61 57.6(3) . . ? C63 Ga5 C61 56.6(3) . . ? C60 Ga5 C61 34.0(3) . . ? C59 Ga5 C62 57.7(2) . . ? C63 Ga5 C62 34.0(2) . . ? C60 Ga5 C62 56.9(3) . . ? C61 Ga5 C62 33.7(3) . . ? C59 Ga5 Pd5 153.8(2) . . ? C63 Ga5 Pd5 163.76(19) . . ? C60 Ga5 Pd5 122.25(19) . . ? C61 Ga5 Pd5 113.32(18) . . ? C62 Ga5 Pd5 130.43(18) . . ? C59 Ga5 Pd4 133.2(2) . . ? C63 Ga5 Pd4 111.27(19) . . ? C60 Ga5 Pd4 168.42(19) . . ? C61 Ga5 Pd4 146.26(19) . . ? C62 Ga5 Pd4 117.45(19) . . ? Pd5 Ga5 Pd4 69.30(2) . . ? C59 Ga5 Pd6 107.73(18) . . ? C63 Ga5 Pd6 126.34(18) . . ? C60 Ga5 Pd6 120.55(19) . . ? C61 Ga5 Pd6 152.97(19) . . ? C62 Ga5 Pd6 160.16(18) . . ? Pd5 Ga5 Pd6 68.85(2) . . ? Pd4 Ga5 Pd6 60.73(2) . . ? P4 Pd4 Ga4 122.39(5) . . ? P4 Pd4 Ga6 118.68(5) . . ? Ga4 Pd4 Ga6 95.52(3) . . ? P4 Pd4 Ga5 119.15(5) . . ? Ga4 Pd4 Ga5 95.11(3) . . ? Ga6 Pd4 Ga5 100.70(3) . . ? P4 Pd4 Pd6 178.55(5) . . ? Ga4 Pd4 Pd6 58.88(2) . . ? Ga6 Pd4 Pd6 60.09(2) . . ? Ga5 Pd4 Pd6 60.89(2) . . ? P4 Pd4 Pd5 115.29(5) . . ? Ga4 Pd4 Pd5 122.32(3) . . ? Ga6 Pd4 Pd5 54.32(2) . . ? Ga5 Pd4 Pd5 54.35(2) . . ? Pd6 Pd4 Pd5 63.444(19) . . ? C40 P4 C41 101.1(4) . . ? C40 P4 C42 99.3(4) . . ? C41 P4 C42 101.3(5) . . ? C40 P4 Pd4 117.5(3) . . ? C41 P4 Pd4 115.8(3) . . ? C42 P4 Pd4 118.7(3) . . ? C49 Ga4 C50 34.8(3) . . ? C49 Ga4 C51 57.8(3) . . ? C50 Ga4 C51 34.8(3) . . ? C49 Ga4 C52 57.5(3) . . ? C50 Ga4 C52 57.5(3) . . ? C51 Ga4 C52 34.4(3) . . ? C49 Ga4 C53 34.4(3) . . ? C50 Ga4 C53 57.5(2) . . ? C51 Ga4 C53 57.5(3) . . ? C52 Ga4 C53 34.6(3) . . ? C49 Ga4 Pd4 151.79(19) . . ? C50 Ga4 Pd4 126.88(18) . . ? C51 Ga4 Pd4 122.79(19) . . ? C52 Ga4 Pd4 141.7(2) . . ? C53 Ga4 Pd4 173.77(18) . . ? C49 Ga4 Pd6 122.00(18) . . ? C50 Ga4 Pd6 150.54(19) . . ? C51 Ga4 Pd6 170.25(19) . . ? C52 Ga4 Pd6 136.1(2) . . ? C53 Ga4 Pd6 116.09(18) . . ? Pd4 Ga4 Pd6 62.69(2) . . ? P6 Pd6 Ga4 125.24(5) . . ? P6 Pd6 Ga6 118.31(5) . . ? Ga4 Pd6 Ga6 94.17(3) . . ? P6 Pd6 Pd4 175.98(5) . . ? Ga4 Pd6 Pd4 58.43(2) . . ? Ga6 Pd6 Pd4 58.49(2) . . ? P6 Pd6 Ga5 121.29(5) . . ? Ga4 Pd6 Ga5 93.20(3) . . ? Ga6 Pd6 Ga5 97.85(3) . . ? Pd4 Pd6 Ga5 58.38(2) . . ? P6 Pd6 Pd5 113.77(5) . . ? Ga4 Pd6 Pd5 120.98(3) . . ? Ga6 Pd6 Pd5 53.66(2) . . ? Pd4 Pd6 Pd5 62.553(19) . . ? Ga5 Pd6 Pd5 53.50(2) . . ? C48 P6 C47 99.5(4) . . ? C48 P6 C46 100.5(4) . . ? C47 P6 C46 98.7(4) . . ? C48 P6 Pd6 113.2(3) . . ? C47 P6 Pd6 121.6(3) . . ? C46 P6 Pd6 119.5(3) . . ? C73 Ga6 C72 35.0(2) . . ? C73 Ga6 C69 34.4(2) . . ? C72 Ga6 C69 57.6(2) . . ? C73 Ga6 C71 57.0(2) . . ? C72 Ga6 C71 34.6(2) . . ? C69 Ga6 C71 56.3(2) . . ? C73 Ga6 C70 56.6(2) . . ? C72 Ga6 C70 57.1(2) . . ? C69 Ga6 C70 33.7(2) . . ? C71 Ga6 C70 33.6(2) . . ? C73 Ga6 Pd5 141.19(18) . . ? C72 Ga6 Pd5 164.49(16) . . ? C69 Ga6 Pd5 111.62(17) . . ? C71 Ga6 Pd5 131.17(17) . . ? C70 Ga6 Pd5 107.57(16) . . ? C73 Ga6 Pd4 147.65(18) . . ? C72 Ga6 Pd4 119.07(17) . . ? C69 Ga6 Pd4 170.62(17) . . ? C71 Ga6 Pd4 115.47(16) . . ? C70 Ga6 Pd4 137.01(18) . . ? Pd5 Ga6 Pd4 69.62(2) . . ? C73 Ga6 Pd6 112.82(17) . . ? C72 Ga6 Pd6 125.51(16) . . ? C69 Ga6 Pd6 127.95(17) . . ? C71 Ga6 Pd6 158.34(17) . . ? C70 Ga6 Pd6 160.39(19) . . ? Pd5 Ga6 Pd6 69.55(2) . . ? Pd4 Ga6 Pd6 61.42(2) . . ? C14 C10 C11 107.8(7) . . ? C14 C10 C15 125.0(8) . . ? C11 C10 C15 127.0(8) . . ? C14 C10 Ga1 75.5(4) . . ? C11 C10 Ga1 71.5(4) . . ? C15 C10 Ga1 121.8(5) . . ? C10 C11 C12 108.1(7) . . ? C10 C11 C16 127.4(8) . . ? C12 C11 C16 124.4(8) . . ? C10 C11 Ga1 73.7(4) . . ? C12 C11 Ga1 74.2(4) . . ? C16 C11 Ga1 121.0(5) . . ? C10 C14 C13 108.6(7) . . ? C10 C14 C19 125.8(8) . . ? C13 C14 C19 125.6(8) . . ? C10 C14 Ga1 70.5(4) . . ? C13 C14 Ga1 73.7(4) . . ? C19 C14 Ga1 123.7(6) . . ? C12 C13 C14 107.7(7) . . ? C12 C13 C18 126.5(7) . . ? C14 C13 C18 125.3(8) . . ? C12 C13 Ga1 70.7(4) . . ? C14 C13 Ga1 72.4(4) . . ? C18 C13 Ga1 129.5(5) . . ? C13 C12 C11 107.9(7) . . ? C13 C12 C17 125.4(7) . . ? C11 C12 C17 126.7(8) . . ? C13 C12 Ga1 75.6(4) . . ? C11 C12 Ga1 70.6(4) . . ? C17 C12 Ga1 120.9(5) . . ? C22 C21 C20 108.2(6) . . ? C22 C21 C26 127.2(6) . . ? C20 C21 C26 124.6(6) . . ? C22 C21 Ga2 74.7(4) . . ? C20 C21 Ga2 71.4(4) . . ? C26 C21 Ga2 121.3(5) . . ? C21 C20 C24 106.8(6) . . ? C21 C20 C25 127.0(7) . . ? C24 C20 C25 126.1(7) . . ? C21 C20 Ga2 73.6(4) . . ? C24 C20 Ga2 73.8(4) . . ? C25 C20 Ga2 121.0(5) . . ? C23 C22 C21 107.7(6) . . ? C23 C22 C27 126.5(6) . . ? C21 C22 C27 125.7(6) . . ? C23 C22 Ga2 73.2(4) . . ? C21 C22 Ga2 71.1(4) . . ? C27 C22 Ga2 122.0(5) . . ? C23 C24 C20 107.8(6) . . ? C23 C24 C29 126.5(6) . . ? C20 C24 C29 125.7(6) . . ? C23 C24 Ga2 74.5(4) . . ? C20 C24 Ga2 71.2(4) . . ? C29 C24 Ga2 121.0(5) . . ? C22 C23 C24 109.4(6) . . ? C22 C23 C28 126.0(7) . . ? C24 C23 C28 124.5(6) . . ? C22 C23 Ga2 73.5(4) . . ? C24 C23 Ga2 71.7(4) . . ? C28 C23 Ga2 123.4(5) . . ? C31 C30 C34 109.0(6) . . ? C31 C30 C35 125.0(7) . . ? C34 C30 C35 126.0(7) . . ? C31 C30 Ga3 72.6(4) . . ? C34 C30 Ga3 74.7(4) . . ? C35 C30 Ga3 120.8(5) . . ? C30 C31 C32 107.2(7) . . ? C30 C31 C36 125.6(7) . . ? C32 C31 C36 127.2(7) . . ? C30 C31 Ga3 72.9(4) . . ? C32 C31 Ga3 73.3(4) . . ? C36 C31 Ga3 120.8(5) . . ? C33 C32 C31 107.8(7) . . ? C33 C32 C37 125.7(8) . . ? C31 C32 C37 126.5(8) . . ? C33 C32 Ga3 74.1(4) . . ? C31 C32 Ga3 71.7(4) . . ? C37 C32 Ga3 121.3(5) . . ? C33 C34 C30 106.8(7) . . ? C33 C34 C39 126.1(7) . . ? C30 C34 C39 127.1(7) . . ? C33 C34 Ga3 72.9(4) . . ? C30 C34 Ga3 70.3(4) . . ? C39 C34 Ga3 123.5(5) . . ? C34 C33 C32 109.3(7) . . ? C34 C33 C38 124.8(8) . . ? C32 C33 C38 125.8(8) . . ? C34 C33 Ga3 73.6(4) . . ? C32 C33 Ga3 71.6(4) . . ? C38 C33 Ga3 124.6(5) . . ? C53 C49 C50 108.2(7) . . ? C53 C49 C54 125.7(7) . . ? C50 C49 C54 126.0(7) . . ? C53 C49 Ga4 73.8(4) . . ? C50 C49 Ga4 72.6(4) . . ? C54 C49 Ga4 122.5(5) . . ? C51 C52 C53 108.1(7) . . ? C51 C52 C57 126.2(8) . . ? C53 C52 C57 125.3(8) . . ? C51 C52 Ga4 72.2(4) . . ? C53 C52 Ga4 72.9(4) . . ? C57 C52 Ga4 126.1(5) . . ? C52 C51 C50 108.1(7) . . ? C52 C51 C56 127.4(7) . . ? C50 C51 C56 124.5(7) . . ? C52 C51 Ga4 73.3(4) . . ? C50 C51 Ga4 72.5(4) . . ? C56 C51 Ga4 120.8(5) . . ? C51 C50 C49 107.7(7) . . ? C51 C50 C55 125.0(7) . . ? C49 C50 C55 127.2(7) . . ? C51 C50 Ga4 72.7(4) . . ? C49 C50 Ga4 72.5(4) . . ? C55 C50 Ga4 122.6(5) . . ? C49 C53 C52 107.8(7) . . ? C49 C53 C58 125.8(7) . . ? C52 C53 C58 126.4(7) . . ? C49 C53 Ga4 71.8(4) . . ? C52 C53 Ga4 72.4(4) . . ? C58 C53 Ga4 121.4(5) . . ? C62 C63 C59 108.7(7) . . ? C62 C63 C68 127.2(8) . . ? C59 C63 C68 124.1(7) . . ? C62 C63 Ga5 75.7(4) . . ? C59 C63 Ga5 70.9(4) . . ? C68 C63 Ga5 120.1(5) . . ? C63 C62 C61 107.8(7) . . ? C63 C62 C67 126.2(7) . . ? C61 C62 C67 125.9(7) . . ? C63 C62 Ga5 70.3(4) . . ? C61 C62 Ga5 72.8(4) . . ? C67 C62 Ga5 125.5(5) . . ? C60 C61 C62 109.1(7) . . ? C60 C61 C66 126.0(7) . . ? C62 C61 C66 124.7(7) . . ? C60 C61 Ga5 70.9(4) . . ? C62 C61 Ga5 73.5(4) . . ? C66 C61 Ga5 125.5(5) . . ? C61 C60 C59 107.7(7) . . ? C61 C60 C65 126.6(7) . . ? C59 C60 C65 125.7(7) . . ? C61 C60 Ga5 75.1(4) . . ? C59 C60 Ga5 70.6(4) . . ? C65 C60 Ga5 119.6(5) . . ? C63 C59 C60 106.7(6) . . ? C63 C59 C64 126.3(7) . . ? C60 C59 C64 126.9(7) . . ? C63 C59 Ga5 73.7(4) . . ? C60 C59 Ga5 73.8(4) . . ? C64 C59 Ga5 120.8(5) . . ? C73 C72 C71 106.5(6) . . ? C73 C72 C77 125.6(6) . . ? C71 C72 C77 127.9(7) . . ? C73 C72 Ga6 71.4(4) . . ? C71 C72 Ga6 75.2(4) . . ? C77 C72 Ga6 120.3(5) . . ? C70 C71 C72 108.3(6) . . ? C70 C71 C76 125.7(7) . . ? C72 C71 C76 125.9(7) . . ? C70 C71 Ga6 74.1(4) . . ? C72 C71 Ga6 70.2(3) . . ? C76 C71 Ga6 124.1(5) . . ? C69 C70 C71 108.0(6) . . ? C69 C70 C75 127.3(7) . . ? C71 C70 C75 124.7(7) . . ? C69 C70 Ga6 71.2(4) . . ? C71 C70 Ga6 72.2(4) . . ? C75 C70 Ga6 122.8(5) . . ? C73 C69 C70 107.9(6) . . ? C73 C69 C74 126.6(7) . . ? C70 C69 C74 125.4(7) . . ? C73 C69 Ga6 70.1(4) . . ? C70 C69 Ga6 75.1(4) . . ? C74 C69 Ga6 122.2(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.246 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.136 _database_code_depnum_ccdc_archive 'CCDC 967771' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H69 P5 Pd2 Zn4' _chemical_formula_sum 'C28 H69 P5 Pd2 Zn4' _chemical_formula_weight 1034.96 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 43 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+3/4' 'y, -x, z+1/4' _cell_length_a 12.44770(10) _cell_length_b 12.44770(10) _cell_length_c 27.5483(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4268.48(10) _cell_formula_units_Z 4 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 200 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.270 _exptl_crystal_size_mid 0.139 _exptl_crystal_size_min 0.113 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 3.240 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.556 _exptl_absorpt_correction_T_max 0.687 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '560 images at 1.0 deg. in \w and 25 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47546 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7495 _reflns_number_gt 6891 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _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^)+(0.0620P)^2^+21.9022P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.000(16) _refine_ls_number_reflns 7495 _refine_ls_number_parameters 375 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 Pd2 Pd 0.41792(5) 0.91271(5) 0.19340(2) 0.02100(15) Uani 1 1 d . . . C1 C 0.6612(7) 1.1779(7) 0.0392(4) 0.030(2) Uani 1 1 d . . . P1 P 0.56917(17) 0.72260(17) 0.05933(8) 0.0209(4) Uani 1 1 d . . . Zn1 Zn 0.67000(8) 1.01010(8) 0.08154(3) 0.0227(2) Uani 1 1 d . . . Zn3 Zn 0.44831(8) 0.93736(8) 0.10142(3) 0.0223(2) Uani 1 1 d . . . P3 P 0.4643(2) 0.8746(2) 0.27567(9) 0.0331(5) Uani 1 1 d . . . C3 C 0.8253(7) 1.1165(7) 0.0657(3) 0.0243(18) Uani 1 1 d . . . Pd1 Pd 0.61250(5) 0.84038(5) 0.12147(2) 0.01571(14) Uani 1 1 d . . . C2 C 0.7412(7) 1.1903(7) 0.0757(3) 0.0249(19) Uani 1 1 d . . . P2 P 0.77516(17) 0.77935(18) 0.15103(8) 0.0228(5) Uani 1 1 d . . . Zn2 Zn 0.60913(8) 0.98538(8) 0.18079(3) 0.0226(2) Uani 1 1 d . . . Zn4 Zn 0.49615(8) 0.73083(8) 0.17508(3) 0.0227(2) Uani 1 1 d . . . C4 C 0.7981(8) 1.0595(7) 0.0228(3) 0.028(2) Uani 1 1 d . . . P4 P 0.24688(19) 0.8334(2) 0.18723(10) 0.0345(6) Uani 1 1 d . . . P5 P 0.37394(19) 1.09735(19) 0.18582(10) 0.0320(5) Uani 1 1 d . . . C5 C 0.6982(8) 1.0973(7) 0.0070(3) 0.031(2) Uani 1 1 d . . . C6 C 0.5643(9) 1.2479(9) 0.0328(5) 0.050(3) Uani 1 1 d . . . H6A H 0.5753 1.2956 0.0049 0.074 Uiso 1 1 calc R . . H6B H 0.5533 1.2909 0.0621 0.074 Uiso 1 1 calc R . . H6C H 0.5010 1.2028 0.0270 0.074 Uiso 1 1 calc R . . C7 C 0.7429(9) 1.2749(8) 0.1150(4) 0.042(2) Uani 1 1 d . . . H7A H 0.7728 1.3417 0.1019 0.062 Uiso 1 1 calc R . . H7B H 0.7874 1.2501 0.1421 0.062 Uiso 1 1 calc R . . H7C H 0.6695 1.2879 0.1265 0.062 Uiso 1 1 calc R . . C10 C 0.6379(10) 1.0656(10) -0.0385(4) 0.053(3) Uani 1 1 d . . . H10A H 0.6389 1.1256 -0.0616 0.079 Uiso 1 1 calc R . . H10B H 0.5635 1.0480 -0.0302 0.079 Uiso 1 1 calc R . . H10C H 0.6725 1.0028 -0.0533 0.079 Uiso 1 1 calc R . . C9 C 0.8649(9) 0.9770(8) -0.0025(4) 0.039(2) Uani 1 1 d . . . H9A H 0.8881 1.0051 -0.0340 0.059 Uiso 1 1 calc R . . H9B H 0.8223 0.9117 -0.0074 0.059 Uiso 1 1 calc R . . H9C H 0.9281 0.9602 0.0173 0.059 Uiso 1 1 calc R . . C8 C 0.9269(7) 1.1058(8) 0.0949(4) 0.037(2) Uani 1 1 d . . . H8A H 0.9622 1.0377 0.0869 0.055 Uiso 1 1 calc R . . H8B H 0.9095 1.1070 0.1296 0.055 Uiso 1 1 calc R . . H8C H 0.9752 1.1656 0.0872 0.055 Uiso 1 1 calc R . . C12 C 0.3557(8) 0.9918(8) 0.0475(3) 0.033(2) Uani 1 1 d . . . H12A H 0.3862 0.9697 0.0163 0.049 Uiso 1 1 calc R . . H12B H 0.3522 1.0704 0.0490 0.049 Uiso 1 1 calc R . . H12C H 0.2832 0.9620 0.0508 0.049 Uiso 1 1 calc R . . C11 C 0.6798(8) 1.0931(8) 0.2238(4) 0.038(2) Uani 1 1 d . . . H11A H 0.7100 1.1511 0.2040 0.056 Uiso 1 1 calc R . . H11B H 0.7376 1.0583 0.2422 0.056 Uiso 1 1 calc R . . H11C H 0.6268 1.1228 0.2464 0.056 Uiso 1 1 calc R . . C15 C 0.4288(7) 0.6809(8) 0.0522(3) 0.031(2) Uani 1 1 d . . . H15A H 0.3842 0.7441 0.0454 0.046 Uiso 1 1 calc R . . H15B H 0.4041 0.6464 0.0822 0.046 Uiso 1 1 calc R . . H15C H 0.4231 0.6300 0.0252 0.046 Uiso 1 1 calc R . . C14 C 0.6010(7) 0.7647(8) -0.0022(3) 0.030(2) Uani 1 1 d . . . H14A H 0.5800 0.7080 -0.0251 0.045 Uiso 1 1 calc R . . H14B H 0.6783 0.7779 -0.0050 0.045 Uiso 1 1 calc R . . H14C H 0.5616 0.8308 -0.0099 0.045 Uiso 1 1 calc R . . C13 C 0.4813(8) 0.5728(7) 0.1888(4) 0.033(2) Uani 1 1 d . . . H13A H 0.4315 0.5407 0.1654 0.049 Uiso 1 1 calc R . . H13B H 0.4534 0.5627 0.2218 0.049 Uiso 1 1 calc R . . H13C H 0.5517 0.5382 0.1860 0.049 Uiso 1 1 calc R . . C16 C 0.6324(9) 0.5905(8) 0.0595(4) 0.036(2) Uani 1 1 d . . . H16A H 0.6083 0.5497 0.0311 0.054 Uiso 1 1 calc R . . H16B H 0.6123 0.5519 0.0891 0.054 Uiso 1 1 calc R . . H16C H 0.7107 0.5989 0.0583 0.054 Uiso 1 1 calc R . . C19 C 0.7835(8) 0.6434(8) 0.1752(4) 0.038(2) Uani 1 1 d . . . H19A H 0.7584 0.5923 0.1507 0.057 Uiso 1 1 calc R . . H19B H 0.7384 0.6377 0.2043 0.057 Uiso 1 1 calc R . . H19C H 0.8582 0.6272 0.1837 0.057 Uiso 1 1 calc R . . C18 C 0.8505(8) 0.8510(9) 0.1981(4) 0.041(2) Uani 1 1 d . . . H18A H 0.8761 0.9198 0.1851 0.061 Uiso 1 1 calc R . . H18B H 0.9121 0.8075 0.2083 0.061 Uiso 1 1 calc R . . H18C H 0.8037 0.8642 0.2261 0.061 Uiso 1 1 calc R . . C17 C 0.8774(7) 0.7713(8) 0.1033(4) 0.035(2) Uani 1 1 d . . . H17A H 0.8479 0.7332 0.0752 0.052 Uiso 1 1 calc R . . H17B H 0.9402 0.7325 0.1157 0.052 Uiso 1 1 calc R . . H17C H 0.8987 0.8440 0.0937 0.052 Uiso 1 1 calc R . . C20 C 0.6032(9) 0.8479(9) 0.2911(4) 0.047(3) Uani 1 1 d . . . H20A H 0.6293 0.7868 0.2720 0.071 Uiso 1 1 calc R . . H20B H 0.6086 0.8309 0.3257 0.071 Uiso 1 1 calc R . . H20C H 0.6468 0.9114 0.2839 0.071 Uiso 1 1 calc R . . C22 C 0.4030(11) 0.7558(11) 0.3037(4) 0.061(4) Uani 1 1 d . . . H22A H 0.3249 0.7651 0.3051 0.092 Uiso 1 1 calc R . . H22B H 0.4313 0.7468 0.3367 0.092 Uiso 1 1 calc R . . H22C H 0.4202 0.6920 0.2844 0.092 Uiso 1 1 calc R . . C21 C 0.4373(11) 0.9748(12) 0.3229(4) 0.066(4) Uani 1 1 d . . . H21A H 0.4793 1.0398 0.3163 0.099 Uiso 1 1 calc R . . H21B H 0.4575 0.9455 0.3546 0.099 Uiso 1 1 calc R . . H21C H 0.3606 0.9926 0.3229 0.099 Uiso 1 1 calc R . . C23 C 0.1589(9) 0.8821(10) 0.2357(5) 0.054(3) Uani 1 1 d . . . H23A H 0.1546 0.9607 0.2342 0.081 Uiso 1 1 calc R . . H23B H 0.1880 0.8603 0.2672 0.081 Uiso 1 1 calc R . . H23C H 0.0869 0.8515 0.2316 0.081 Uiso 1 1 calc R . . C25 C 0.1653(8) 0.8585(10) 0.1329(5) 0.052(3) Uani 1 1 d . . . H25A H 0.2025 0.8300 0.1043 0.078 Uiso 1 1 calc R . . H25B H 0.1545 0.9360 0.1289 0.078 Uiso 1 1 calc R . . H25C H 0.0955 0.8229 0.1363 0.078 Uiso 1 1 calc R . . C24 C 0.2225(9) 0.6888(8) 0.1926(5) 0.049(3) Uani 1 1 d . . . H24A H 0.1450 0.6749 0.1913 0.073 Uiso 1 1 calc R . . H24B H 0.2512 0.6629 0.2236 0.073 Uiso 1 1 calc R . . H24C H 0.2581 0.6512 0.1659 0.073 Uiso 1 1 calc R . . C27 C 0.2419(9) 1.1334(9) 0.1604(5) 0.050(3) Uani 1 1 d . . . H27A H 0.2336 1.2117 0.1607 0.075 Uiso 1 1 calc R . . H27B H 0.1850 1.1006 0.1801 0.075 Uiso 1 1 calc R . . H27C H 0.2368 1.1070 0.1270 0.075 Uiso 1 1 calc R . . C26 C 0.4555(9) 1.1890(8) 0.1493(5) 0.046(3) Uani 1 1 d . . . H26A H 0.4590 1.1626 0.1158 0.069 Uiso 1 1 calc R . . H26B H 0.5282 1.1928 0.1628 0.069 Uiso 1 1 calc R . . H26C H 0.4231 1.2607 0.1496 0.069 Uiso 1 1 calc R . . C28 C 0.3691(11) 1.1738(10) 0.2420(4) 0.055(3) Uani 1 1 d . . . H28A H 0.4408 1.1756 0.2567 0.083 Uiso 1 1 calc R . . H28B H 0.3185 1.1397 0.2645 0.083 Uiso 1 1 calc R . . H28C H 0.3454 1.2473 0.2351 0.083 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd2 0.0173(3) 0.0253(3) 0.0204(3) -0.0015(3) 0.0049(2) -0.0024(2) C1 0.026(5) 0.029(5) 0.036(5) 0.013(4) 0.003(4) -0.005(4) P1 0.0219(11) 0.0227(11) 0.0182(10) -0.0031(8) 0.0001(8) -0.0034(8) Zn1 0.0241(5) 0.0239(5) 0.0201(5) 0.0048(4) 0.0020(4) -0.0050(4) Zn3 0.0205(5) 0.0259(5) 0.0203(5) -0.0008(4) -0.0032(4) 0.0028(4) P3 0.0363(14) 0.0435(15) 0.0194(11) 0.0000(10) 0.0072(10) 0.0021(11) C3 0.028(5) 0.022(4) 0.023(4) 0.002(3) -0.001(3) -0.007(4) Pd1 0.0153(3) 0.0193(3) 0.0125(3) 0.0005(2) -0.0001(2) -0.0023(2) C2 0.026(4) 0.022(4) 0.026(5) 0.004(4) 0.010(4) -0.008(3) P2 0.0172(11) 0.0328(12) 0.0185(10) 0.0039(9) -0.0011(8) 0.0006(9) Zn2 0.0208(5) 0.0278(5) 0.0192(5) -0.0065(4) 0.0012(4) -0.0058(4) Zn4 0.0224(5) 0.0244(5) 0.0213(5) 0.0037(4) 0.0038(4) -0.0031(4) C4 0.039(5) 0.025(5) 0.020(4) 0.006(4) 0.011(4) -0.004(4) P4 0.0196(11) 0.0366(14) 0.0474(15) 0.0022(12) 0.0057(11) -0.0059(10) P5 0.0309(12) 0.0262(12) 0.0390(14) -0.0046(10) 0.0128(11) 0.0033(10) C5 0.041(5) 0.033(5) 0.019(4) 0.006(4) -0.001(4) -0.017(4) C6 0.037(6) 0.044(6) 0.068(8) 0.032(6) 0.001(5) 0.002(5) C7 0.053(6) 0.030(5) 0.042(6) -0.008(4) 0.019(5) -0.011(4) C10 0.063(8) 0.064(8) 0.031(5) 0.014(5) -0.013(5) -0.035(6) C9 0.061(7) 0.027(5) 0.031(5) -0.003(4) 0.013(5) -0.009(5) C8 0.031(5) 0.043(6) 0.036(5) 0.009(4) -0.004(4) -0.014(4) C12 0.031(5) 0.036(5) 0.032(5) 0.001(4) -0.010(4) 0.008(4) C11 0.039(6) 0.040(6) 0.034(5) -0.012(4) -0.001(4) -0.017(4) C15 0.029(5) 0.039(5) 0.025(5) -0.007(4) 0.000(4) -0.006(4) C14 0.032(5) 0.037(5) 0.021(4) -0.006(4) 0.003(4) -0.007(4) C13 0.039(5) 0.023(5) 0.037(5) 0.009(4) -0.001(4) -0.006(4) C16 0.046(6) 0.026(5) 0.035(5) -0.012(4) 0.000(4) 0.006(4) C19 0.027(5) 0.042(6) 0.046(6) 0.012(5) -0.005(4) 0.009(4) C18 0.023(5) 0.065(7) 0.034(5) -0.014(5) -0.007(4) -0.001(4) C17 0.025(5) 0.045(6) 0.034(5) 0.006(4) 0.002(4) 0.002(4) C20 0.059(7) 0.046(7) 0.036(6) 0.009(5) -0.007(5) 0.005(5) C22 0.064(8) 0.084(9) 0.036(6) 0.029(6) 0.007(6) -0.013(7) C21 0.076(9) 0.087(10) 0.034(6) -0.017(6) 0.000(6) 0.028(8) C23 0.032(6) 0.063(8) 0.067(8) -0.005(6) 0.018(6) -0.007(5) C25 0.028(5) 0.057(7) 0.071(8) 0.011(6) -0.016(5) -0.013(5) C24 0.039(6) 0.039(6) 0.068(8) 0.001(5) 0.009(6) -0.021(5) C27 0.038(6) 0.039(6) 0.073(8) 0.006(6) 0.007(6) 0.008(5) C26 0.048(7) 0.027(5) 0.063(7) 0.005(5) 0.020(6) 0.008(5) C28 0.070(8) 0.049(7) 0.046(7) -0.016(5) 0.027(6) 0.008(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 Pd2 P4 2.353(2) . ? Pd2 P5 2.372(2) . ? Pd2 P3 2.386(3) . ? Pd2 Zn4 2.5157(11) . ? Pd2 Zn2 2.5698(11) . ? Pd2 Zn3 2.5803(11) . ? Pd2 Pd1 3.2563(8) . ? C1 C5 1.417(14) . ? C1 C2 1.425(13) . ? C1 C6 1.497(14) . ? C1 Zn1 2.395(9) . ? P1 C14 1.819(9) . ? P1 C16 1.823(9) . ? P1 C15 1.833(9) . ? P1 Pd1 2.318(2) . ? Zn1 C5 2.349(8) . ? Zn1 C4 2.353(8) . ? Zn1 C3 2.384(8) . ? Zn1 C2 2.417(8) . ? Zn1 Pd1 2.4870(11) . ? Zn1 Zn2 2.8539(13) . ? Zn1 Zn3 2.9555(13) . ? Zn3 C12 1.999(9) . ? Zn3 Pd1 2.4372(11) . ? Zn3 Zn2 3.0243(13) . ? P3 C20 1.811(12) . ? P3 C21 1.832(12) . ? P3 C22 1.834(12) . ? C3 C4 1.420(12) . ? C3 C2 1.419(13) . ? C3 C8 1.504(13) . ? Pd1 P2 2.311(2) . ? Pd1 Zn2 2.4352(11) . ? Pd1 Zn4 2.4776(11) . ? C2 C7 1.511(13) . ? P2 C19 1.821(10) . ? P2 C17 1.832(9) . ? P2 C18 1.832(10) . ? Zn2 C11 1.994(9) . ? Zn4 C13 2.011(8) . ? C4 C5 1.399(14) . ? C4 C9 1.495(13) . ? P4 C24 1.831(10) . ? P4 C23 1.830(11) . ? P4 C25 1.836(11) . ? P5 C28 1.818(11) . ? P5 C26 1.830(11) . ? P5 C27 1.842(11) . ? C5 C10 1.513(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P4 Pd2 P5 101.04(9) . . ? P4 Pd2 P3 101.77(9) . . ? P5 Pd2 P3 109.39(9) . . ? P4 Pd2 Zn4 87.59(7) . . ? P5 Pd2 Zn4 160.69(7) . . ? P3 Pd2 Zn4 85.30(7) . . ? P4 Pd2 Zn2 167.42(8) . . ? P5 Pd2 Zn2 82.00(6) . . ? P3 Pd2 Zn2 88.53(7) . . ? Zn4 Pd2 Zn2 86.05(4) . . ? P4 Pd2 Zn3 96.41(7) . . ? P5 Pd2 Zn3 80.34(7) . . ? P3 Pd2 Zn3 157.05(7) . . ? Zn4 Pd2 Zn3 81.56(3) . . ? Zn2 Pd2 Zn3 71.92(3) . . ? P4 Pd2 Pd1 120.86(7) . . ? P5 Pd2 Pd1 112.71(6) . . ? P3 Pd2 Pd1 110.07(6) . . ? Zn4 Pd2 Pd1 48.79(3) . . ? Zn2 Pd2 Pd1 47.64(2) . . ? Zn3 Pd2 Pd1 47.65(3) . . ? C5 C1 C2 106.9(8) . . ? C5 C1 C6 126.9(10) . . ? C2 C1 C6 125.7(10) . . ? C5 C1 Zn1 70.8(5) . . ? C2 C1 Zn1 73.6(5) . . ? C6 C1 Zn1 127.0(6) . . ? C14 P1 C16 99.7(5) . . ? C14 P1 C15 100.9(4) . . ? C16 P1 C15 99.0(5) . . ? C14 P1 Pd1 117.1(3) . . ? C16 P1 Pd1 117.9(3) . . ? C15 P1 Pd1 118.7(3) . . ? C5 Zn1 C4 34.6(3) . . ? C5 Zn1 C3 57.5(3) . . ? C4 Zn1 C3 34.9(3) . . ? C5 Zn1 C1 34.7(3) . . ? C4 Zn1 C1 57.9(3) . . ? C3 Zn1 C1 57.6(3) . . ? C5 Zn1 C2 57.2(3) . . ? C4 Zn1 C2 57.5(3) . . ? C3 Zn1 C2 34.4(3) . . ? C1 Zn1 C2 34.4(3) . . ? C5 Zn1 Pd1 145.3(2) . . ? C4 Zn1 Pd1 136.2(2) . . ? C3 Zn1 Pd1 141.8(2) . . ? C1 Zn1 Pd1 160.6(2) . . ? C2 Zn1 Pd1 157.4(2) . . ? C5 Zn1 Zn2 158.0(3) . . ? C4 Zn1 Zn2 150.1(2) . . ? C3 Zn1 Zn2 116.8(2) . . ? C1 Zn1 Zn2 123.3(2) . . ? C2 Zn1 Zn2 105.1(2) . . ? Pd1 Zn1 Zn2 53.72(3) . . ? C5 Zn1 Zn3 116.3(2) . . ? C4 Zn1 Zn3 147.2(2) . . ? C3 Zn1 Zn3 164.0(2) . . ? C1 Zn1 Zn3 108.3(2) . . ? C2 Zn1 Zn3 129.7(2) . . ? Pd1 Zn1 Zn3 52.35(3) . . ? Zn2 Zn1 Zn3 62.71(3) . . ? C12 Zn3 Pd1 145.1(3) . . ? C12 Zn3 Pd2 133.3(3) . . ? Pd1 Zn3 Pd2 80.88(3) . . ? C12 Zn3 Zn1 107.3(3) . . ? Pd1 Zn3 Zn1 53.89(3) . . ? Pd2 Zn3 Zn1 110.81(4) . . ? C12 Zn3 Zn2 148.5(3) . . ? Pd1 Zn3 Zn2 51.60(3) . . ? Pd2 Zn3 Zn2 53.88(3) . . ? Zn1 Zn3 Zn2 57.00(3) . . ? C20 P3 C21 97.7(6) . . ? C20 P3 C22 98.6(6) . . ? C21 P3 C22 100.0(7) . . ? C20 P3 Pd2 119.3(4) . . ? C21 P3 Pd2 119.6(4) . . ? C22 P3 Pd2 117.4(4) . . ? C4 C3 C2 108.0(8) . . ? C4 C3 C8 126.9(9) . . ? C2 C3 C8 125.0(8) . . ? C4 C3 Zn1 71.4(5) . . ? C2 C3 Zn1 74.1(5) . . ? C8 C3 Zn1 122.3(6) . . ? P2 Pd1 P1 104.85(8) . . ? P2 Pd1 Zn2 91.27(6) . . ? P1 Pd1 Zn2 163.86(6) . . ? P2 Pd1 Zn3 167.82(7) . . ? P1 Pd1 Zn3 87.18(6) . . ? Zn2 Pd1 Zn3 76.73(4) . . ? P2 Pd1 Zn4 96.96(6) . . ? P1 Pd1 Zn4 87.48(6) . . ? Zn2 Pd1 Zn4 89.88(4) . . ? Zn3 Pd1 Zn4 85.27(4) . . ? P2 Pd1 Zn1 100.54(7) . . ? P1 Pd1 Zn1 106.12(6) . . ? Zn2 Pd1 Zn1 70.86(4) . . ? Zn3 Pd1 Zn1 73.76(4) . . ? Zn4 Pd1 Zn1 154.08(4) . . ? P2 Pd1 Pd2 121.88(6) . . ? P1 Pd1 Pd2 116.83(6) . . ? Zn2 Pd1 Pd2 51.24(3) . . ? Zn3 Pd1 Pd2 51.48(3) . . ? Zn4 Pd1 Pd2 49.81(3) . . ? Zn1 Pd1 Pd2 104.38(3) . . ? C3 C2 C1 108.0(8) . . ? C3 C2 C7 125.4(9) . . ? C1 C2 C7 126.2(9) . . ? C3 C2 Zn1 71.5(5) . . ? C1 C2 Zn1 72.0(5) . . ? C7 C2 Zn1 127.3(6) . . ? C19 P2 C17 99.9(5) . . ? C19 P2 C18 99.5(5) . . ? C17 P2 C18 100.3(5) . . ? C19 P2 Pd1 119.0(3) . . ? C17 P2 Pd1 112.0(3) . . ? C18 P2 Pd1 122.5(3) . . ? C11 Zn2 Pd1 152.8(3) . . ? C11 Zn2 Pd2 124.4(3) . . ? Pd1 Zn2 Pd2 81.13(3) . . ? C11 Zn2 Zn1 112.3(3) . . ? Pd1 Zn2 Zn1 55.42(3) . . ? Pd2 Zn2 Zn1 114.41(4) . . ? C11 Zn2 Zn3 148.7(3) . . ? Pd1 Zn2 Zn3 51.66(3) . . ? Pd2 Zn2 Zn3 54.20(3) . . ? Zn1 Zn2 Zn3 60.29(3) . . ? C13 Zn4 Pd1 134.8(3) . . ? C13 Zn4 Pd2 143.8(3) . . ? Pd1 Zn4 Pd2 81.40(3) . . ? C5 C4 C3 107.7(8) . . ? C5 C4 C9 125.4(9) . . ? C3 C4 C9 126.8(9) . . ? C5 C4 Zn1 72.5(5) . . ? C3 C4 Zn1 73.8(5) . . ? C9 C4 Zn1 121.2(6) . . ? C24 P4 C23 99.6(6) . . ? C24 P4 C25 98.2(6) . . ? C23 P4 C25 102.0(6) . . ? C24 P4 Pd2 123.8(4) . . ? C23 P4 Pd2 110.5(4) . . ? C25 P4 Pd2 119.2(4) . . ? C28 P5 C26 99.3(6) . . ? C28 P5 C27 99.6(6) . . ? C26 P5 C27 97.7(5) . . ? C28 P5 Pd2 116.1(4) . . ? C26 P5 Pd2 121.6(3) . . ? C27 P5 Pd2 118.4(4) . . ? C4 C5 C1 109.4(8) . . ? C4 C5 C10 127.7(10) . . ? C1 C5 C10 122.8(10) . . ? C4 C5 Zn1 72.8(5) . . ? C1 C5 Zn1 74.4(5) . . ? C10 C5 Zn1 122.0(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.453 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.078 _database_code_depnum_ccdc_archive 'CCDC 967772' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H54 P2 Pt Zn4 ' _chemical_formula_sum 'C28 H54 P2 Pt Zn4' _chemical_formula_weight 909.22 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' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -4.5932 6.9264 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.7556(4) _cell_length_b 18.4752(7) _cell_length_c 16.4826(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.654(3) _cell_angle_gamma 90.00 _cell_volume 3578.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 200 _cell_measurement_theta_min 3.59 _cell_measurement_theta_max 70.00 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 11.052 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3655 _exptl_absorpt_correction_T_max 0.6361 _exptl_absorpt_process_details abspack _exptl_special_details ; Since only twinned crystals could be obtained the data was not merged. ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12040 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 70.00 _reflns_number_total 12040 _reflns_number_gt 10492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _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^)+(0.1010P)^2^+4.1233P] 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 12040 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1398 _refine_ls_wR_factor_gt 0.1317 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.007 _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 0.028916(16) 0.165510(10) 0.239571(11) 0.02285(9) Uani 1 1 d . . . C1 C -0.2478(4) -0.0005(3) 0.2480(3) 0.0301(10) Uani 1 1 d . . . P1 P 0.10161(11) 0.10811(8) 0.12914(7) 0.0287(3) Uani 1 1 d . . . Zn1 Zn -0.15749(5) 0.10985(4) 0.24681(4) 0.02907(16) Uani 1 1 d . . . Zn2 Zn 0.13100(6) 0.27931(4) 0.23333(4) 0.03227(16) Uani 1 1 d . . . C2 C -0.2928(4) 0.0396(3) 0.1811(3) 0.0329(11) Uani 1 1 d . . . P2 P 0.11723(11) 0.10725(7) 0.34675(8) 0.0289(3) Uani 1 1 d . . . C22 C -0.1326(7) 0.3027(4) 0.4176(4) 0.0512(17) Uani 1 1 d . . . H22A H -0.2100 0.2855 0.4270 0.077 Uiso 1 1 calc R . . H22B H -0.1355 0.3535 0.4003 0.077 Uiso 1 1 calc R . . H22C H -0.0866 0.2987 0.4679 0.077 Uiso 1 1 calc R . . C21 C -0.1844(8) 0.2915(4) 0.0718(5) 0.060(2) Uani 1 1 d . . . H21A H -0.1373 0.3284 0.0465 0.090 Uiso 1 1 calc R . . H21B H -0.2479 0.3148 0.0987 0.090 Uiso 1 1 calc R . . H21C H -0.2142 0.2582 0.0300 0.090 Uiso 1 1 calc R . . Zn4 Zn -0.06435(7) 0.24396(4) 0.33290(4) 0.03278(17) Uani 1 1 d . . . C4 C -0.3371(5) 0.0995(3) 0.2977(3) 0.0344(12) Uani 1 1 d . . . C26 C 0.1084(7) 0.0092(4) 0.3456(4) 0.0511(17) Uani 1 1 d . . . H26A H 0.0283 -0.0056 0.3435 0.077 Uiso 1 1 calc R . . H26B H 0.1457 -0.0103 0.3949 0.077 Uiso 1 1 calc R . . H26C H 0.1464 -0.0095 0.2978 0.077 Uiso 1 1 calc R . . C27 C 0.0668(6) 0.1267(4) 0.4486(3) 0.0465(16) Uani 1 1 d . . . H27A H -0.0144 0.1150 0.4509 0.070 Uiso 1 1 calc R . . H27B H 0.0782 0.1781 0.4609 0.070 Uiso 1 1 calc R . . H27C H 0.1095 0.0973 0.4885 0.070 Uiso 1 1 calc R . . C28 C 0.2696(5) 0.1204(4) 0.3633(4) 0.0471(15) Uani 1 1 d . . . H28A H 0.3104 0.0981 0.3187 0.071 Uiso 1 1 calc R . . H28B H 0.2939 0.0979 0.4147 0.071 Uiso 1 1 calc R . . H28C H 0.2865 0.1724 0.3652 0.071 Uiso 1 1 calc R . . C25 C 0.2550(5) 0.0970(4) 0.1279(4) 0.0473(15) Uani 1 1 d . . . H25A H 0.2762 0.0753 0.0762 0.071 Uiso 1 1 calc R . . H25B H 0.2799 0.0655 0.1727 0.071 Uiso 1 1 calc R . . H25C H 0.2918 0.1444 0.1340 0.071 Uiso 1 1 calc R . . C24 C 0.0736(7) 0.1480(5) 0.0289(4) 0.0527(17) Uani 1 1 d . . . H24A H 0.1151 0.1208 -0.0119 0.079 Uiso 1 1 calc R . . H24B H 0.0989 0.1985 0.0291 0.079 Uiso 1 1 calc R . . H24C H -0.0081 0.1459 0.0157 0.079 Uiso 1 1 calc R . . C23 C 0.0535(6) 0.0151(4) 0.1107(4) 0.0449(15) Uani 1 1 d . . . H23A H -0.0294 0.0145 0.1028 0.067 Uiso 1 1 calc R . . H23B H 0.0752 -0.0153 0.1574 0.067 Uiso 1 1 calc R . . H23C H 0.0890 -0.0038 0.0619 0.067 Uiso 1 1 calc R . . C7 C -0.2905(6) 0.0184(4) 0.0934(4) 0.0459(15) Uani 1 1 d . . . H7A H -0.2797 0.0617 0.0601 0.069 Uiso 1 1 calc R . . H7B H -0.3626 -0.0048 0.0774 0.069 Uiso 1 1 calc R . . H7C H -0.2277 -0.0154 0.0852 0.069 Uiso 1 1 calc R . . Zn3 Zn -0.09204(7) 0.23738(4) 0.15194(4) 0.03436(17) Uani 1 1 d . . . C3 C -0.3487(5) 0.1014(3) 0.2112(3) 0.0347(11) Uani 1 1 d . . . C5 C -0.2752(5) 0.0368(3) 0.3200(3) 0.0339(12) Uani 1 1 d . . . C6 C -0.1906(6) -0.0733(3) 0.2433(4) 0.0412(13) Uani 1 1 d . . . H6A H -0.2485 -0.1114 0.2404 0.062 Uiso 1 1 calc R . . H6B H -0.1415 -0.0806 0.2917 0.062 Uiso 1 1 calc R . . H6C H -0.1445 -0.0753 0.1947 0.062 Uiso 1 1 calc R . . C9 C -0.3859(6) 0.1542(4) 0.3556(4) 0.0513(17) Uani 1 1 d . . . H9A H -0.3908 0.2016 0.3291 0.077 Uiso 1 1 calc R . . H9B H -0.3365 0.1576 0.4044 0.077 Uiso 1 1 calc R . . H9C H -0.4621 0.1387 0.3709 0.077 Uiso 1 1 calc R . . C8 C -0.4127(6) 0.1561(4) 0.1617(5) 0.0505(17) Uani 1 1 d . . . H8A H -0.3937 0.1508 0.1045 0.076 Uiso 1 1 calc R . . H8B H -0.3919 0.2048 0.1804 0.076 Uiso 1 1 calc R . . H8C H -0.4946 0.1487 0.1676 0.076 Uiso 1 1 calc R . . C10 C -0.2489(6) 0.0116(4) 0.4051(4) 0.0456(15) Uani 1 1 d . . . H10A H -0.1797 -0.0180 0.4058 0.068 Uiso 1 1 calc R . . H10B H -0.3126 -0.0173 0.4243 0.068 Uiso 1 1 calc R . . H10C H -0.2372 0.0536 0.4406 0.068 Uiso 1 1 calc R . . C11 C 0.2967(5) 0.3404(3) 0.2605(4) 0.0396(13) Uani 1 1 d . . . C12 C 0.2665(6) 0.3476(3) 0.1774(4) 0.0408(14) Uani 1 1 d . . . C13 C 0.1652(6) 0.3883(4) 0.1708(4) 0.0399(13) Uani 1 1 d . . . C16 C 0.4034(6) 0.3060(4) 0.2946(7) 0.070(3) Uani 1 1 d . . . H16A H 0.4147 0.2589 0.2685 0.105 Uiso 1 1 calc R . . H16B H 0.3967 0.2991 0.3532 0.105 Uiso 1 1 calc R . . H16C H 0.4686 0.3374 0.2843 0.105 Uiso 1 1 calc R . . C15 C 0.2121(5) 0.3760(3) 0.3061(3) 0.0327(11) Uani 1 1 d . . . C14 C 0.1310(5) 0.4057(3) 0.2502(4) 0.0343(11) Uani 1 1 d . . . C17 C 0.3368(9) 0.3225(4) 0.1077(6) 0.068(3) Uani 1 1 d . . . H17A H 0.2873 0.3154 0.0595 0.102 Uiso 1 1 calc R . . H17B H 0.3743 0.2767 0.1221 0.102 Uiso 1 1 calc R . . H17C H 0.3945 0.3591 0.0962 0.102 Uiso 1 1 calc R . . C18 C 0.1028(9) 0.4130(5) 0.0943(4) 0.065(2) Uani 1 1 d . . . H18A H 0.1172 0.3788 0.0503 0.098 Uiso 1 1 calc R . . H18B H 0.1299 0.4612 0.0792 0.098 Uiso 1 1 calc R . . H18C H 0.0210 0.4151 0.1038 0.098 Uiso 1 1 calc R . . C20 C 0.2093(8) 0.3802(4) 0.3970(4) 0.0564(19) Uani 1 1 d . . . H20A H 0.2104 0.4311 0.4139 0.085 Uiso 1 1 calc R . . H20B H 0.2758 0.3552 0.4207 0.085 Uiso 1 1 calc R . . H20C H 0.1397 0.3571 0.4156 0.085 Uiso 1 1 calc R . . C19 C 0.0285(6) 0.4490(4) 0.2730(5) 0.0547(18) Uani 1 1 d . . . H19A H 0.0352 0.4983 0.2518 0.082 Uiso 1 1 calc R . . H19B H 0.0239 0.4506 0.3322 0.082 Uiso 1 1 calc R . . H19C H -0.0403 0.4262 0.2497 0.082 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 0.02736(12) 0.01576(13) 0.02534(12) -0.00094(7) -0.00069(7) -0.00124(7) C1 0.032(2) 0.025(3) 0.033(2) 0.004(2) 0.0007(18) -0.008(2) P1 0.0320(6) 0.0253(7) 0.0289(6) -0.0052(5) 0.0029(4) -0.0016(5) Zn1 0.0281(3) 0.0245(4) 0.0346(3) 0.0023(3) 0.0001(2) -0.0027(3) Zn2 0.0392(4) 0.0206(4) 0.0371(4) -0.0024(3) 0.0033(3) -0.0081(3) C2 0.030(3) 0.034(3) 0.035(3) 0.004(2) -0.0022(19) -0.009(2) P2 0.0335(6) 0.0218(7) 0.0309(6) 0.0012(5) -0.0058(5) 0.0030(5) C22 0.076(5) 0.035(4) 0.044(3) -0.001(3) 0.019(3) 0.011(3) C21 0.078(5) 0.044(4) 0.057(4) 0.010(3) -0.025(4) 0.007(4) Zn4 0.0439(4) 0.0244(4) 0.0303(3) -0.0003(3) 0.0054(3) 0.0074(3) C4 0.032(3) 0.033(3) 0.038(3) 0.005(2) 0.006(2) -0.003(2) C26 0.062(4) 0.028(3) 0.063(4) 0.008(3) -0.020(3) 0.008(3) C27 0.057(4) 0.058(4) 0.023(3) 0.008(3) -0.005(2) 0.017(3) C28 0.038(3) 0.055(4) 0.047(3) 0.000(3) -0.010(2) 0.000(3) C25 0.034(3) 0.049(4) 0.059(4) -0.015(3) 0.007(2) 0.000(3) C24 0.068(5) 0.061(5) 0.029(3) -0.006(3) 0.009(3) 0.009(4) C23 0.059(4) 0.033(3) 0.043(3) -0.020(3) 0.011(3) -0.005(3) C7 0.049(4) 0.054(4) 0.034(3) 0.000(3) -0.004(2) -0.014(3) Zn3 0.0448(4) 0.0259(4) 0.0320(4) 0.0037(3) -0.0059(3) 0.0044(3) C3 0.029(2) 0.035(3) 0.040(3) 0.008(2) -0.001(2) -0.005(2) C5 0.032(3) 0.034(3) 0.036(3) 0.003(2) 0.002(2) -0.005(2) C6 0.049(3) 0.025(3) 0.049(3) 0.005(2) 0.001(2) -0.004(2) C9 0.040(3) 0.055(5) 0.059(4) -0.001(3) 0.008(3) 0.014(3) C8 0.036(3) 0.051(4) 0.064(4) 0.016(3) -0.011(3) -0.003(3) C10 0.050(4) 0.049(4) 0.037(3) 0.006(3) 0.001(2) -0.001(3) C11 0.033(3) 0.017(3) 0.068(4) -0.003(2) 0.001(3) -0.003(2) C12 0.049(3) 0.022(3) 0.053(3) -0.007(2) 0.018(3) -0.010(3) C13 0.048(3) 0.032(3) 0.040(3) -0.001(2) 0.002(2) -0.016(3) C16 0.035(3) 0.035(4) 0.139(8) 0.013(4) -0.005(4) 0.000(3) C15 0.037(3) 0.020(3) 0.041(3) -0.003(2) 0.002(2) -0.006(2) C14 0.038(3) 0.017(3) 0.048(3) -0.002(2) 0.006(2) -0.002(2) C17 0.092(6) 0.030(4) 0.084(6) -0.021(4) 0.053(5) -0.015(4) C18 0.096(6) 0.054(5) 0.044(4) 0.018(3) -0.013(4) -0.031(5) C20 0.077(5) 0.052(5) 0.040(3) -0.002(3) -0.003(3) -0.019(4) C19 0.040(3) 0.043(4) 0.081(5) 0.021(4) 0.015(3) 0.010(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 Pt1 P2 2.2916(13) . ? Pt1 P1 2.2930(13) . ? Pt1 Zn3 2.3985(7) . ? Pt1 Zn4 2.4013(7) . ? Pt1 Zn2 2.4245(7) . ? Pt1 Zn1 2.4266(7) . ? C1 C5 1.418(8) . ? C1 C2 1.418(8) . ? C1 C6 1.507(8) . ? C1 Zn1 2.299(5) . ? P1 C25 1.816(6) . ? P1 C24 1.831(7) . ? P1 C23 1.833(6) . ? Zn1 C5 2.299(5) . ? Zn1 C2 2.300(5) . ? Zn1 C4 2.302(5) . ? Zn1 C3 2.313(5) . ? Zn1 Zn3 2.9424(10) . ? Zn1 Zn4 3.0432(10) . ? Zn2 C12 2.250(6) . ? Zn2 C11 2.284(6) . ? Zn2 C13 2.303(6) . ? Zn2 C15 2.340(5) . ? Zn2 C14 2.352(5) . ? Zn2 Zn4 2.9345(10) . ? Zn2 Zn3 3.0120(11) . ? C2 C3 1.414(9) . ? C2 C7 1.499(8) . ? P2 C26 1.815(7) . ? P2 C28 1.820(6) . ? P2 C27 1.832(6) . ? C22 Zn4 1.959(6) . ? C21 Zn3 1.960(7) . ? Zn4 Zn3 2.9934(10) . ? C4 C5 1.411(9) . ? C4 C3 1.429(8) . ? C4 C9 1.514(9) . ? C3 C8 1.488(9) . ? C5 C10 1.502(8) . ? C11 C12 1.411(10) . ? C11 C15 1.425(8) . ? C11 C16 1.502(10) . ? C12 C13 1.410(10) . ? C12 C17 1.507(9) . ? C13 C14 1.417(8) . ? C13 C18 1.511(10) . ? C15 C14 1.417(8) . ? C15 C20 1.501(8) . ? C14 C19 1.502(8) . ? 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 P2 Pt1 P1 102.93(5) . . ? P2 Pt1 Zn3 166.36(4) . . ? P1 Pt1 Zn3 90.35(4) . . ? P2 Pt1 Zn4 89.70(4) . . ? P1 Pt1 Zn4 167.20(4) . . ? Zn3 Pt1 Zn4 77.17(3) . . ? P2 Pt1 Zn2 103.07(4) . . ? P1 Pt1 Zn2 99.85(4) . . ? Zn3 Pt1 Zn2 77.29(3) . . ? Zn4 Pt1 Zn2 74.90(3) . . ? P2 Pt1 Zn1 98.78(4) . . ? P1 Pt1 Zn1 101.59(4) . . ? Zn3 Pt1 Zn1 75.15(3) . . ? Zn4 Pt1 Zn1 78.15(3) . . ? Zn2 Pt1 Zn1 144.92(3) . . ? C5 C1 C2 107.9(5) . . ? C5 C1 C6 126.1(5) . . ? C2 C1 C6 125.8(5) . . ? C5 C1 Zn1 72.0(3) . . ? C2 C1 Zn1 72.1(3) . . ? C6 C1 Zn1 125.8(4) . . ? C25 P1 C24 100.8(4) . . ? C25 P1 C23 101.2(3) . . ? C24 P1 C23 100.4(3) . . ? C25 P1 Pt1 117.0(2) . . ? C24 P1 Pt1 118.0(2) . . ? C23 P1 Pt1 116.5(2) . . ? C5 Zn1 C1 35.9(2) . . ? C5 Zn1 C2 59.81(19) . . ? C1 Zn1 C2 35.92(19) . . ? C5 Zn1 C4 35.7(2) . . ? C1 Zn1 C4 59.7(2) . . ? C2 Zn1 C4 59.7(2) . . ? C5 Zn1 C3 59.87(19) . . ? C1 Zn1 C3 59.8(2) . . ? C2 Zn1 C3 35.7(2) . . ? C4 Zn1 C3 36.1(2) . . ? C5 Zn1 Pt1 146.36(14) . . ? C1 Zn1 Pt1 142.56(14) . . ? C2 Zn1 Pt1 146.04(14) . . ? C4 Zn1 Pt1 153.12(15) . . ? C3 Zn1 Pt1 152.72(14) . . ? C5 Zn1 Zn3 156.81(15) . . ? C1 Zn1 Zn3 147.39(13) . . ? C2 Zn1 Zn3 112.92(14) . . ? C4 Zn1 Zn3 121.10(15) . . ? C3 Zn1 Zn3 100.73(14) . . ? Pt1 Zn1 Zn3 51.99(2) . . ? C5 Zn1 Zn4 116.56(15) . . ? C1 Zn1 Zn4 151.43(13) . . ? C2 Zn1 Zn4 156.01(16) . . ? C4 Zn1 Zn4 102.65(15) . . ? C3 Zn1 Zn4 120.48(16) . . ? Pt1 Zn1 Zn4 50.557(19) . . ? Zn3 Zn1 Zn4 59.99(2) . . ? C12 Zn2 C11 36.3(3) . . ? C12 Zn2 C13 36.1(2) . . ? C11 Zn2 C13 59.8(2) . . ? C12 Zn2 C15 59.9(2) . . ? C11 Zn2 C15 35.9(2) . . ? C13 Zn2 C15 59.2(2) . . ? C12 Zn2 C14 59.6(2) . . ? C11 Zn2 C14 59.27(19) . . ? C13 Zn2 C14 35.4(2) . . ? C15 Zn2 C14 35.1(2) . . ? C12 Zn2 Pt1 149.41(15) . . ? C11 Zn2 Pt1 147.18(15) . . ? C13 Zn2 Pt1 150.51(15) . . ? C15 Zn2 Pt1 146.65(14) . . ? C14 Zn2 Pt1 148.70(14) . . ? C12 Zn2 Zn4 158.19(16) . . ? C11 Zn2 Zn4 132.59(18) . . ? C13 Zn2 Zn4 126.46(17) . . ? C15 Zn2 Zn4 101.37(14) . . ? C14 Zn2 Zn4 98.76(14) . . ? Pt1 Zn2 Zn4 52.19(2) . . ? C12 Zn2 Zn3 125.41(19) . . ? C11 Zn2 Zn3 160.21(17) . . ? C13 Zn2 Zn3 100.76(16) . . ? C15 Zn2 Zn3 139.58(15) . . ? C14 Zn2 Zn3 107.78(15) . . ? Pt1 Zn2 Zn3 50.97(2) . . ? Zn4 Zn2 Zn3 60.43(2) . . ? C3 C2 C1 108.5(5) . . ? C3 C2 C7 124.8(5) . . ? C1 C2 C7 126.6(6) . . ? C3 C2 Zn1 72.6(3) . . ? C1 C2 Zn1 72.0(3) . . ? C7 C2 Zn1 124.7(4) . . ? C26 P2 C28 101.0(3) . . ? C26 P2 C27 100.7(4) . . ? C28 P2 C27 100.4(3) . . ? C26 P2 Pt1 115.9(2) . . ? C28 P2 Pt1 118.3(2) . . ? C27 P2 Pt1 117.6(2) . . ? C22 Zn4 Pt1 174.4(2) . . ? C22 Zn4 Zn2 128.2(2) . . ? Pt1 Zn4 Zn2 52.91(2) . . ? C22 Zn4 Zn3 134.2(2) . . ? Pt1 Zn4 Zn3 51.37(2) . . ? Zn2 Zn4 Zn3 61.06(3) . . ? C22 Zn4 Zn1 129.4(3) . . ? Pt1 Zn4 Zn1 51.297(19) . . ? Zn2 Zn4 Zn1 101.38(3) . . ? Zn3 Zn4 Zn1 58.34(2) . . ? C5 C4 C3 108.3(5) . . ? C5 C4 C9 125.8(5) . . ? C3 C4 C9 125.8(6) . . ? C5 C4 Zn1 72.0(3) . . ? C3 C4 Zn1 72.4(3) . . ? C9 C4 Zn1 122.9(4) . . ? C21 Zn3 Pt1 174.6(3) . . ? C21 Zn3 Zn1 128.2(3) . . ? Pt1 Zn3 Zn1 52.86(2) . . ? C21 Zn3 Zn4 133.9(3) . . ? Pt1 Zn3 Zn4 51.46(2) . . ? Zn1 Zn3 Zn4 61.68(2) . . ? C21 Zn3 Zn2 128.9(3) . . ? Pt1 Zn3 Zn2 51.74(2) . . ? Zn1 Zn3 Zn2 101.94(3) . . ? Zn4 Zn3 Zn2 58.50(2) . . ? C2 C3 C4 107.3(5) . . ? C2 C3 C8 126.0(6) . . ? C4 C3 C8 126.6(6) . . ? C2 C3 Zn1 71.6(3) . . ? C4 C3 Zn1 71.6(3) . . ? C8 C3 Zn1 124.4(4) . . ? C4 C5 C1 108.0(5) . . ? C4 C5 C10 126.1(6) . . ? C1 C5 C10 125.8(6) . . ? C4 C5 Zn1 72.3(3) . . ? C1 C5 Zn1 72.0(3) . . ? C10 C5 Zn1 124.1(4) . . ? C12 C11 C15 108.0(5) . . ? C12 C11 C16 125.9(7) . . ? C15 C11 C16 125.9(7) . . ? C12 C11 Zn2 70.6(3) . . ? C15 C11 Zn2 74.2(3) . . ? C16 C11 Zn2 124.3(4) . . ? C13 C12 C11 108.3(5) . . ? C13 C12 C17 125.8(7) . . ? C11 C12 C17 125.7(7) . . ? C13 C12 Zn2 74.0(3) . . ? C11 C12 Zn2 73.2(3) . . ? C17 C12 Zn2 123.3(4) . . ? C12 C13 C14 108.1(5) . . ? C12 C13 C18 127.8(7) . . ? C14 C13 C18 124.0(7) . . ? C12 C13 Zn2 70.0(4) . . ? C14 C13 Zn2 74.2(3) . . ? C18 C13 Zn2 123.4(4) . . ? C14 C15 C11 107.6(5) . . ? C14 C15 C20 126.5(6) . . ? C11 C15 C20 125.9(6) . . ? C14 C15 Zn2 72.9(3) . . ? C11 C15 Zn2 69.9(3) . . ? C20 C15 Zn2 122.0(4) . . ? C13 C14 C15 108.0(5) . . ? C13 C14 C19 127.0(6) . . ? C15 C14 C19 125.0(6) . . ? C13 C14 Zn2 70.4(3) . . ? C15 C14 Zn2 72.0(3) . . ? C19 C14 Zn2 124.1(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 70.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.138 _refine_diff_density_min -1.800 _refine_diff_density_rms 0.182 _database_code_depnum_ccdc_archive 'CCDC 967773'