Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Cameron Jones' 'David P. Mills' 'Richard P. Rose' 'Andreas Stasch' _publ_contact_author_name 'Cameron Jones' _publ_contact_author_address ; School of Chemistry Monash University PO Box 23 Victoria 3800 AUSTRALIA ; _publ_contact_author_email CAMERON.JONES@SCI.MONASH.EDU.AU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and Structural Characterisation of Group 10 Metal(II) Gallyl Complexes: Analogies with Platinum Diboration Catalysts? ; data_compound5 _database_code_depnum_ccdc_archive 'CCDC 664045' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H110 Ga2 N4 P2 Pt' _chemical_formula_weight 1416.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.658(4) _cell_length_b 14.530(3) _cell_length_c 25.189(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.38(3) _cell_angle_gamma 90.00 _cell_volume 6937(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2936 _exptl_absorpt_coefficient_mu 2.871 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.533 _exptl_absorpt_correction_T_max 0.658 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29111 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.00 _reflns_number_total 15109 _reflns_number_gt 11826 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One molecule of toluene was located in the asymmetric unit and found to be disordered over 2 sites in a 50:50 ratio. This disorder was successfully modelled and refined with the isotropic carbon atoms. The largest residual electron density peak (1.616 e-/ang.3) in the final difference map is located close to Pt(1). ; _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^)+(0.0239P)^2^+9.8572P] 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 15109 _refine_ls_number_parameters 739 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0831 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.048 _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 0.258126(7) 0.073068(10) 0.779845(6) 0.01675(5) Uani 1 1 d . . . Ga1 Ga 0.20380(2) -0.05930(3) 0.812823(17) 0.01823(10) Uani 1 1 d . . . Ga2 Ga 0.31206(2) 0.20604(3) 0.748791(17) 0.01941(10) Uani 1 1 d . . . P1 P 0.29989(5) -0.02437(8) 0.72399(5) 0.0256(2) Uani 1 1 d . . . P2 P 0.21333(5) 0.16711(7) 0.83554(4) 0.0203(2) Uani 1 1 d . . . N1 N 0.14738(17) -0.1631(2) 0.78150(13) 0.0221(7) Uani 1 1 d . . . N2 N 0.20401(17) -0.1086(2) 0.88291(13) 0.0214(7) Uani 1 1 d . . . N3 N 0.37798(17) 0.2995(2) 0.78207(13) 0.0228(7) Uani 1 1 d . . . N4 N 0.29732(18) 0.2730(2) 0.68219(13) 0.0286(8) Uani 1 1 d . . . C1 C 0.1361(2) -0.2176(3) 0.82434(17) 0.0257(9) Uani 1 1 d . . . H1 H 0.1089 -0.2724 0.8168 0.031 Uiso 1 1 calc R . . C2 C 0.1647(2) -0.1901(3) 0.87596(17) 0.0240(9) Uani 1 1 d . . . H2 H 0.1587 -0.2242 0.9066 0.029 Uiso 1 1 calc R . . C3 C 0.1133(2) -0.1925(3) 0.72701(17) 0.0229(9) Uani 1 1 d . . . C4 C 0.1342(2) -0.2759(3) 0.70760(18) 0.0285(10) Uani 1 1 d . . . C5 C 0.0960(2) -0.3073(3) 0.65568(19) 0.0353(11) Uani 1 1 d . . . H5 H 0.1081 -0.3647 0.6426 0.042 Uiso 1 1 calc R . . C6 C 0.0413(2) -0.2568(3) 0.62314(19) 0.0373(12) Uani 1 1 d . . . H6 H 0.0155 -0.2796 0.5883 0.045 Uiso 1 1 calc R . . C7 C 0.0242(2) -0.1724(3) 0.64170(18) 0.0323(10) Uani 1 1 d . . . H7 H -0.0116 -0.1360 0.6183 0.039 Uiso 1 1 calc R . . C8 C 0.0582(2) -0.1397(3) 0.69372(17) 0.0265(9) Uani 1 1 d . . . C9 C 0.1974(2) -0.3321(3) 0.73924(19) 0.0323(10) Uani 1 1 d . . . H9 H 0.2240 -0.2938 0.7710 0.039 Uiso 1 1 calc R . . C10 C 0.1758(3) -0.4216(3) 0.7628(2) 0.0435(12) Uani 1 1 d . . . H10A H 0.1488 -0.4068 0.7893 0.065 Uiso 1 1 calc R . . H10B H 0.2181 -0.4563 0.7814 0.065 Uiso 1 1 calc R . . H10C H 0.1466 -0.4587 0.7328 0.065 Uiso 1 1 calc R . . C11 C 0.2477(2) -0.3543(4) 0.7036(2) 0.0481(13) Uani 1 1 d . . . H11A H 0.2247 -0.3971 0.6742 0.072 Uiso 1 1 calc R . . H11B H 0.2908 -0.3825 0.7265 0.072 Uiso 1 1 calc R . . H11C H 0.2597 -0.2974 0.6872 0.072 Uiso 1 1 calc R . . C12 C 0.0364(2) -0.0486(3) 0.71401(17) 0.0265(10) Uani 1 1 d . . . H12 H 0.0807 -0.0141 0.7314 0.032 Uiso 1 1 calc R . . C13 C -0.0022(2) -0.0645(3) 0.75917(18) 0.0327(10) Uani 1 1 d . . . H13A H -0.0478 -0.0941 0.7430 0.049 Uiso 1 1 calc R . . H13B H -0.0098 -0.0053 0.7753 0.049 Uiso 1 1 calc R . . H13C H 0.0265 -0.1044 0.7879 0.049 Uiso 1 1 calc R . . C14 C -0.0079(2) 0.0127(3) 0.66890(19) 0.0357(11) Uani 1 1 d . . . H14A H -0.0537 -0.0167 0.6529 0.053 Uiso 1 1 calc R . . H14B H 0.0167 0.0219 0.6402 0.053 Uiso 1 1 calc R . . H14C H -0.0154 0.0724 0.6846 0.053 Uiso 1 1 calc R . . C15 C 0.2319(2) -0.0764(3) 0.93794(16) 0.0240(9) Uani 1 1 d . . . C16 C 0.1862(2) -0.0465(3) 0.96937(18) 0.0278(10) Uani 1 1 d . . . C17 C 0.2158(3) -0.0167(4) 1.02288(19) 0.0429(12) Uani 1 1 d . . . H17 H 0.1856 0.0027 1.0446 0.051 Uiso 1 1 calc R . . C18 C 0.2877(3) -0.0144(4) 1.0455(2) 0.0518(14) Uani 1 1 d . . . H18 H 0.3067 0.0067 1.0821 0.062 Uiso 1 1 calc R . . C19 C 0.3319(3) -0.0430(3) 1.01440(19) 0.0421(12) Uani 1 1 d . . . H19 H 0.3814 -0.0415 1.0301 0.050 Uiso 1 1 calc R . . C20 C 0.3057(2) -0.0741(3) 0.96054(18) 0.0284(10) Uani 1 1 d . . . C21 C 0.1067(2) -0.0444(3) 0.94692(19) 0.0329(10) Uani 1 1 d . . . H21 H 0.0951 -0.0573 0.9065 0.039 Uiso 1 1 calc R . . C22 C 0.0713(2) -0.1182(3) 0.9735(2) 0.0424(12) Uani 1 1 d . . . H22A H 0.0839 -0.1087 1.0135 0.064 Uiso 1 1 calc R . . H22B H 0.0874 -0.1791 0.9654 0.064 Uiso 1 1 calc R . . H22C H 0.0200 -0.1140 0.9588 0.064 Uiso 1 1 calc R . . C23 C 0.0756(3) 0.0491(3) 0.9548(2) 0.0471(13) Uani 1 1 d . . . H23A H 0.0781 0.0580 0.9939 0.071 Uiso 1 1 calc R . . H23B H 0.0262 0.0517 0.9331 0.071 Uiso 1 1 calc R . . H23C H 0.1025 0.0977 0.9426 0.071 Uiso 1 1 calc R . . C24 C 0.3555(2) -0.1081(3) 0.92781(18) 0.0273(10) Uani 1 1 d . . . H24 H 0.3389 -0.0814 0.8900 0.033 Uiso 1 1 calc R . . C25 C 0.4322(2) -0.0774(3) 0.95129(19) 0.0390(12) Uani 1 1 d . . . H25A H 0.4337 -0.0106 0.9569 0.059 Uiso 1 1 calc R . . H25B H 0.4597 -0.0936 0.9254 0.059 Uiso 1 1 calc R . . H25C H 0.4522 -0.1084 0.9866 0.059 Uiso 1 1 calc R . . C26 C 0.3522(2) -0.2132(3) 0.9216(2) 0.0400(12) Uani 1 1 d . . . H26A H 0.3668 -0.2418 0.9581 0.060 Uiso 1 1 calc R . . H26B H 0.3840 -0.2330 0.8997 0.060 Uiso 1 1 calc R . . H26C H 0.3039 -0.2319 0.9031 0.060 Uiso 1 1 calc R . . C27 C 0.3803(2) 0.3661(3) 0.74235(18) 0.0338(11) Uani 1 1 d . . . H27 H 0.4099 0.4187 0.7510 0.041 Uiso 1 1 calc R . . C28 C 0.3389(2) 0.3519(3) 0.69196(18) 0.0373(11) Uani 1 1 d . . . H28 H 0.3378 0.3948 0.6632 0.045 Uiso 1 1 calc R . . C29 C 0.4252(2) 0.3097(3) 0.83544(16) 0.0242(9) Uani 1 1 d . . . C30 C 0.4777(2) 0.2415(3) 0.85525(17) 0.0269(9) Uani 1 1 d . . . C31 C 0.5228(2) 0.2510(3) 0.90774(19) 0.0380(12) Uani 1 1 d . . . H31 H 0.5568 0.2044 0.9217 0.046 Uiso 1 1 calc R . . C32 C 0.5193(3) 0.3267(4) 0.9400(2) 0.0452(13) Uani 1 1 d . . . H32 H 0.5514 0.3328 0.9754 0.054 Uiso 1 1 calc R . . C33 C 0.4694(2) 0.3932(3) 0.92070(19) 0.0385(12) Uani 1 1 d . . . H33 H 0.4673 0.4450 0.9432 0.046 Uiso 1 1 calc R . . C34 C 0.4215(2) 0.3865(3) 0.86877(17) 0.0286(10) Uani 1 1 d . . . C35 C 0.3667(2) 0.4624(3) 0.8518(2) 0.0342(11) Uani 1 1 d . . . H35 H 0.3304 0.4417 0.8181 0.041 Uiso 1 1 calc R . . C36 C 0.3990(3) 0.5522(3) 0.8381(2) 0.0484(14) Uani 1 1 d . . . H36A H 0.4335 0.5750 0.8711 0.073 Uiso 1 1 calc R . . H36B H 0.3617 0.5982 0.8257 0.073 Uiso 1 1 calc R . . H36C H 0.4225 0.5410 0.8090 0.073 Uiso 1 1 calc R . . C37 C 0.3294(3) 0.4817(4) 0.8973(2) 0.0499(14) Uani 1 1 d . . . H37A H 0.3626 0.5112 0.9286 0.075 Uiso 1 1 calc R . . H37B H 0.3129 0.4236 0.9092 0.075 Uiso 1 1 calc R . . H37C H 0.2891 0.5225 0.8829 0.075 Uiso 1 1 calc R . . C38 C 0.4857(2) 0.1598(3) 0.81905(19) 0.0323(10) Uani 1 1 d . . . H38 H 0.4374 0.1348 0.8024 0.039 Uiso 1 1 calc R . . C39 C 0.5303(3) 0.0811(3) 0.8501(2) 0.0531(15) Uani 1 1 d . . . H39A H 0.5791 0.1020 0.8649 0.080 Uiso 1 1 calc R . . H39B H 0.5293 0.0294 0.8250 0.080 Uiso 1 1 calc R . . H39C H 0.5112 0.0613 0.8805 0.080 Uiso 1 1 calc R . . C40 C 0.5152(3) 0.1919(3) 0.7716(2) 0.0475(13) Uani 1 1 d . . . H40A H 0.4867 0.2432 0.7523 0.071 Uiso 1 1 calc R . . H40B H 0.5136 0.1409 0.7458 0.071 Uiso 1 1 calc R . . H40C H 0.5641 0.2122 0.7863 0.071 Uiso 1 1 calc R . . C41 C 0.2592(2) 0.2537(3) 0.62661(16) 0.0251(9) Uani 1 1 d . . . C42 C 0.1850(2) 0.2588(3) 0.61125(18) 0.0304(10) Uani 1 1 d . . . C43 C 0.1489(2) 0.2422(3) 0.55671(19) 0.0385(12) Uani 1 1 d . . . H43 H 0.0988 0.2455 0.5461 0.046 Uiso 1 1 calc R . . C44 C 0.1837(2) 0.2214(3) 0.51805(18) 0.0417(12) Uani 1 1 d . . . H44 H 0.1580 0.2118 0.4808 0.050 Uiso 1 1 calc R . . C45 C 0.2560(2) 0.2143(3) 0.53302(17) 0.0383(12) Uani 1 1 d . . . H45 H 0.2798 0.1990 0.5060 0.046 Uiso 1 1 calc R . . C46 C 0.2948(2) 0.2292(3) 0.58713(17) 0.0300(10) Uani 1 1 d . . . C47 C 0.1443(2) 0.2859(4) 0.65239(19) 0.0433(13) Uani 1 1 d . . . H47 H 0.1709 0.2615 0.6892 0.052 Uiso 1 1 calc R . . C48 C 0.0700(3) 0.2480(4) 0.6402(2) 0.0488(14) Uani 1 1 d . . . H48A H 0.0488 0.2654 0.6699 0.073 Uiso 1 1 calc R . . H48B H 0.0714 0.1807 0.6376 0.073 Uiso 1 1 calc R . . H48C H 0.0417 0.2733 0.6053 0.073 Uiso 1 1 calc R . . C49 C 0.1421(4) 0.3885(4) 0.6571(3) 0.084(2) Uani 1 1 d U . . H49A H 0.1903 0.4127 0.6678 0.126 Uiso 1 1 calc R . . H49B H 0.1177 0.4052 0.6849 0.126 Uiso 1 1 calc R . . H49C H 0.1168 0.4147 0.6214 0.126 Uiso 1 1 calc R . . C50 C 0.3751(2) 0.2164(4) 0.6013(2) 0.0405(12) Uani 1 1 d . . . H50 H 0.3925 0.2061 0.6419 0.049 Uiso 1 1 calc R . . C51 C 0.4140(3) 0.3000(4) 0.5867(2) 0.0591(16) Uani 1 1 d . . . H51A H 0.4648 0.2879 0.5969 0.089 Uiso 1 1 calc R . . H51B H 0.4043 0.3541 0.6068 0.089 Uiso 1 1 calc R . . H51C H 0.3977 0.3117 0.5470 0.089 Uiso 1 1 calc R . . C52 C 0.3944(3) 0.1315(4) 0.5723(2) 0.0606(17) Uani 1 1 d . . . H52A H 0.3860 0.1444 0.5329 0.091 Uiso 1 1 calc R . . H52B H 0.3653 0.0793 0.5775 0.091 Uiso 1 1 calc R . . H52C H 0.4443 0.1166 0.5881 0.091 Uiso 1 1 calc R . . C53 C 0.3389(2) -0.1368(3) 0.7584(2) 0.0474(14) Uani 1 1 d . . . H53A H 0.3057 -0.1650 0.7771 0.057 Uiso 1 1 calc R . . H53B H 0.3457 -0.1804 0.7300 0.057 Uiso 1 1 calc R . . C54 C 0.4098(3) -0.1188(4) 0.8004(2) 0.0619(16) Uani 1 1 d . . . H54A H 0.4446 -0.0994 0.7811 0.093 Uiso 1 1 calc R . . H54B H 0.4260 -0.1754 0.8211 0.093 Uiso 1 1 calc R . . H54C H 0.4040 -0.0703 0.8259 0.093 Uiso 1 1 calc R . . C55 C 0.2295(3) -0.0647(4) 0.6669(2) 0.0488(14) Uani 1 1 d . . . H55A H 0.2503 -0.0961 0.6400 0.059 Uiso 1 1 calc R . . H55B H 0.2008 -0.1103 0.6806 0.059 Uiso 1 1 calc R . . C56 C 0.1818(3) 0.0127(3) 0.6379(2) 0.0497(14) Uani 1 1 d . . . H56A H 0.1620 0.0450 0.6645 0.075 Uiso 1 1 calc R . . H56B H 0.1434 -0.0131 0.6086 0.075 Uiso 1 1 calc R . . H56C H 0.2092 0.0559 0.6220 0.075 Uiso 1 1 calc R . . C57 C 0.3703(3) 0.0144(3) 0.6958(2) 0.0400(12) Uani 1 1 d . . . H57A H 0.3524 0.0668 0.6709 0.048 Uiso 1 1 calc R . . H57B H 0.4088 0.0382 0.7265 0.048 Uiso 1 1 calc R . . C58 C 0.4017(3) -0.0562(3) 0.6642(2) 0.0467(14) Uani 1 1 d . . . H58A H 0.4249 -0.1051 0.6894 0.070 Uiso 1 1 calc R . . H58B H 0.4365 -0.0260 0.6484 0.070 Uiso 1 1 calc R . . H58C H 0.3641 -0.0828 0.6346 0.070 Uiso 1 1 calc R . . C59 C 0.2614(2) 0.1541(3) 0.90741(16) 0.0289(10) Uani 1 1 d . . . H59A H 0.2442 0.2007 0.9295 0.035 Uiso 1 1 calc R . . H59B H 0.2512 0.0926 0.9203 0.035 Uiso 1 1 calc R . . C60 C 0.3411(2) 0.1647(3) 0.91773(19) 0.0414(12) Uani 1 1 d . . . H60A H 0.3581 0.1226 0.8937 0.062 Uiso 1 1 calc R . . H60B H 0.3643 0.1501 0.9563 0.062 Uiso 1 1 calc R . . H60C H 0.3522 0.2282 0.9099 0.062 Uiso 1 1 calc R . . C61 C 0.2140(2) 0.2920(3) 0.82375(18) 0.0267(9) Uani 1 1 d . . . H61A H 0.2637 0.3124 0.8315 0.032 Uiso 1 1 calc R . . H61B H 0.1916 0.3039 0.7843 0.032 Uiso 1 1 calc R . . C62 C 0.1771(2) 0.3511(3) 0.85767(19) 0.0314(10) Uani 1 1 d . . . H62A H 0.1270 0.3342 0.8490 0.047 Uiso 1 1 calc R . . H62B H 0.1814 0.4162 0.8489 0.047 Uiso 1 1 calc R . . H62C H 0.1990 0.3409 0.8970 0.047 Uiso 1 1 calc R . . C63 C 0.1216(2) 0.1473(3) 0.83541(18) 0.0294(10) Uani 1 1 d . . . H63A H 0.1152 0.0814 0.8428 0.035 Uiso 1 1 calc R . . H63B H 0.1108 0.1835 0.8655 0.035 Uiso 1 1 calc R . . C64 C 0.0699(2) 0.1739(3) 0.7809(2) 0.0379(12) Uani 1 1 d . . . H64A H 0.0736 0.2401 0.7746 0.057 Uiso 1 1 calc R . . H64B H 0.0217 0.1593 0.7822 0.057 Uiso 1 1 calc R . . H64C H 0.0811 0.1395 0.7508 0.057 Uiso 1 1 calc R . . C65 C 0.1561(5) -0.0847(7) 0.5035(4) 0.062(3) Uiso 0.593(10) 1 d PD A 1 C66 C 0.1506(8) -0.1628(12) 0.5289(8) 0.076(8) Uiso 0.593(10) 1 d PD A 1 H66 H 0.1064 -0.1807 0.5342 0.092 Uiso 0.593(10) 1 calc PR A 1 C67 C 0.2077(5) -0.2176(9) 0.5475(5) 0.070(3) Uiso 0.593(10) 1 d PD A 1 H67 H 0.2034 -0.2730 0.5663 0.084 Uiso 0.593(10) 1 calc PR A 1 C78 C 0.2647(9) -0.2398(12) 0.5561(7) 0.083(6) Uiso 0.407(10) 1 d PD A 2 H78A H 0.2474 -0.2677 0.5854 0.124 Uiso 0.407(10) 1 calc PR A 2 H78B H 0.3104 -0.2102 0.5722 0.124 Uiso 0.407(10) 1 calc PR A 2 H78C H 0.2704 -0.2876 0.5302 0.124 Uiso 0.407(10) 1 calc PR A 2 C69 C 0.2779(7) -0.1148(8) 0.5150(5) 0.072(4) Uiso 0.593(10) 1 d PD A 1 H69 H 0.3227 -0.0982 0.5102 0.087 Uiso 0.593(10) 1 calc PR A 1 C70 C 0.2218(7) -0.0560(10) 0.4964(6) 0.081(4) Uiso 0.593(10) 1 d PD A 1 H70 H 0.2270 0.0012 0.4796 0.097 Uiso 0.593(10) 1 calc PR A 1 C71 C 0.0893(9) -0.0299(12) 0.4855(8) 0.131(8) Uiso 0.593(10) 1 d PD A 1 H71A H 0.0820 -0.0111 0.4470 0.197 Uiso 0.593(10) 1 calc PR A 1 H71B H 0.0928 0.0249 0.5088 0.197 Uiso 0.593(10) 1 calc PR A 1 H71C H 0.0494 -0.0677 0.4889 0.197 Uiso 0.593(10) 1 calc PR A 1 C72 C 0.2145(7) -0.1715(11) 0.5272(7) 0.069(5) Uiso 0.407(10) 1 d PD A 2 C73 C 0.2365(11) -0.1000(14) 0.4981(9) 0.101(8) Uiso 0.407(10) 1 d PD A 2 H73 H 0.2832 -0.0945 0.4944 0.121 Uiso 0.407(10) 1 calc PR A 2 C74 C 0.1842(13) -0.0399(14) 0.4758(10) 0.113(8) Uiso 0.407(10) 1 d PD A 2 H74 H 0.1969 0.0066 0.4537 0.136 Uiso 0.407(10) 1 calc PR A 2 C75 C 0.1194(13) -0.0350(16) 0.4794(11) 0.119(10) Uiso 0.407(10) 1 d PD A 2 H75 H 0.0886 0.0142 0.4643 0.142 Uiso 0.407(10) 1 calc PR A 2 C76 C 0.0991(9) -0.1104(12) 0.5083(8) 0.093(7) Uiso 0.407(10) 1 d PD A 2 H76 H 0.0512 -0.1187 0.5082 0.111 Uiso 0.407(10) 1 calc PR A 2 C77 C 0.1507(8) -0.1717(14) 0.5365(10) 0.052(8) Uiso 0.407(10) 1 d PD A 2 H77 H 0.1405 -0.2135 0.5623 0.062 Uiso 0.407(10) 1 calc PR A 2 C68 C 0.2715(6) -0.1939(8) 0.5394(5) 0.069(3) Uiso 0.593(10) 1 d PD A 1 H68 H 0.3109 -0.2338 0.5512 0.083 Uiso 0.593(10) 1 calc PR A 1 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 0.01835(8) 0.01765(8) 0.01564(8) -0.00110(6) 0.00695(6) -0.00171(6) Ga1 0.0192(2) 0.0177(2) 0.0188(2) -0.00113(18) 0.00676(17) -0.00292(17) Ga2 0.0213(2) 0.0212(2) 0.0171(2) 0.00130(18) 0.00758(17) -0.00265(18) P1 0.0219(6) 0.0294(6) 0.0279(6) -0.0116(5) 0.0109(5) -0.0034(5) P2 0.0244(5) 0.0190(5) 0.0204(5) -0.0011(4) 0.0111(4) -0.0001(4) N1 0.0271(18) 0.0184(17) 0.0214(18) -0.0038(15) 0.0074(14) -0.0073(14) N2 0.0250(18) 0.0197(17) 0.0203(18) 0.0001(15) 0.0074(14) -0.0016(14) N3 0.0274(18) 0.0218(17) 0.0192(17) 0.0032(15) 0.0060(14) -0.0051(14) N4 0.034(2) 0.033(2) 0.0173(18) 0.0028(16) 0.0034(15) -0.0102(16) C1 0.027(2) 0.022(2) 0.029(2) 0.0007(19) 0.0094(18) -0.0061(18) C2 0.029(2) 0.018(2) 0.027(2) 0.0015(18) 0.0115(18) -0.0052(17) C3 0.020(2) 0.025(2) 0.025(2) -0.0034(18) 0.0094(17) -0.0095(17) C4 0.028(2) 0.028(2) 0.030(2) -0.010(2) 0.0091(19) -0.0107(18) C5 0.041(3) 0.027(2) 0.042(3) -0.014(2) 0.018(2) -0.006(2) C6 0.038(3) 0.045(3) 0.028(3) -0.015(2) 0.008(2) -0.015(2) C7 0.029(2) 0.045(3) 0.024(2) -0.004(2) 0.0084(19) -0.007(2) C8 0.026(2) 0.028(2) 0.029(2) -0.0008(19) 0.0126(19) -0.0074(18) C9 0.029(2) 0.029(2) 0.037(3) -0.010(2) 0.007(2) -0.0049(19) C10 0.048(3) 0.027(2) 0.055(3) 0.001(2) 0.014(3) 0.000(2) C11 0.044(3) 0.047(3) 0.055(3) -0.010(3) 0.016(3) 0.003(2) C12 0.021(2) 0.029(2) 0.028(2) -0.0010(19) 0.0037(18) -0.0051(17) C13 0.032(2) 0.031(2) 0.036(3) -0.005(2) 0.010(2) -0.001(2) C14 0.027(2) 0.036(3) 0.040(3) 0.005(2) 0.003(2) -0.001(2) C15 0.031(2) 0.020(2) 0.022(2) 0.0023(18) 0.0076(17) -0.0045(17) C16 0.031(2) 0.029(2) 0.027(2) 0.0000(19) 0.0122(19) -0.0008(18) C17 0.045(3) 0.057(3) 0.031(3) -0.014(2) 0.019(2) -0.003(2) C18 0.054(3) 0.067(4) 0.030(3) -0.019(3) 0.003(2) -0.007(3) C19 0.039(3) 0.057(3) 0.025(2) -0.005(2) 0.000(2) -0.006(2) C20 0.030(2) 0.027(2) 0.028(2) 0.001(2) 0.0078(19) -0.0045(19) C21 0.034(3) 0.035(3) 0.033(3) 0.000(2) 0.015(2) 0.004(2) C22 0.035(3) 0.050(3) 0.045(3) 0.007(3) 0.016(2) -0.003(2) C23 0.052(3) 0.051(3) 0.045(3) 0.005(3) 0.026(3) 0.018(3) C24 0.026(2) 0.031(2) 0.024(2) -0.0002(19) 0.0048(18) 0.0029(18) C25 0.025(2) 0.056(3) 0.035(3) 0.000(2) 0.004(2) -0.001(2) C26 0.042(3) 0.033(3) 0.045(3) 0.000(2) 0.012(2) 0.009(2) C27 0.039(3) 0.031(2) 0.031(3) 0.005(2) 0.008(2) -0.018(2) C28 0.048(3) 0.038(3) 0.026(2) 0.011(2) 0.009(2) -0.012(2) C29 0.026(2) 0.025(2) 0.023(2) 0.0019(18) 0.0083(17) -0.0077(17) C30 0.030(2) 0.027(2) 0.025(2) -0.0007(19) 0.0095(18) -0.0062(18) C31 0.038(3) 0.038(3) 0.032(3) 0.003(2) -0.002(2) 0.001(2) C32 0.045(3) 0.053(3) 0.029(3) -0.001(2) -0.005(2) -0.005(3) C33 0.042(3) 0.040(3) 0.034(3) -0.010(2) 0.009(2) -0.005(2) C34 0.027(2) 0.033(2) 0.025(2) 0.002(2) 0.0060(19) -0.0095(19) C35 0.031(2) 0.029(2) 0.040(3) -0.003(2) 0.005(2) -0.0053(19) C36 0.042(3) 0.029(3) 0.070(4) 0.004(3) 0.006(3) -0.001(2) C37 0.038(3) 0.061(4) 0.049(3) -0.026(3) 0.008(2) -0.002(3) C38 0.024(2) 0.032(2) 0.040(3) -0.002(2) 0.007(2) -0.0031(19) C39 0.042(3) 0.035(3) 0.071(4) -0.008(3) -0.005(3) 0.004(2) C40 0.048(3) 0.046(3) 0.058(3) -0.014(3) 0.030(3) -0.004(2) C41 0.030(2) 0.029(2) 0.015(2) 0.0081(18) 0.0051(17) -0.0019(18) C42 0.035(3) 0.033(2) 0.025(2) 0.005(2) 0.011(2) 0.0009(19) C43 0.028(2) 0.056(3) 0.029(3) 0.007(2) 0.003(2) 0.003(2) C44 0.045(3) 0.058(3) 0.019(2) 0.004(2) 0.003(2) 0.004(2) C45 0.047(3) 0.052(3) 0.018(2) 0.009(2) 0.013(2) 0.009(2) C46 0.033(2) 0.036(3) 0.022(2) 0.010(2) 0.0096(19) 0.002(2) C47 0.038(3) 0.068(4) 0.024(2) 0.000(3) 0.009(2) 0.007(3) C48 0.049(3) 0.045(3) 0.059(4) 0.005(3) 0.028(3) 0.008(2) C49 0.092(4) 0.075(4) 0.113(5) -0.045(4) 0.073(4) -0.024(3) C50 0.033(3) 0.059(3) 0.031(3) 0.011(3) 0.012(2) 0.001(2) C51 0.043(3) 0.077(4) 0.059(4) 0.023(3) 0.015(3) -0.008(3) C52 0.037(3) 0.090(5) 0.058(4) 0.013(3) 0.019(3) 0.023(3) C53 0.040(3) 0.050(3) 0.063(4) -0.022(3) 0.034(3) -0.002(2) C54 0.057(4) 0.078(4) 0.052(4) 0.007(3) 0.015(3) 0.016(3) C55 0.048(3) 0.055(3) 0.043(3) -0.016(3) 0.011(2) 0.001(3) C56 0.071(4) 0.041(3) 0.028(3) -0.009(2) -0.002(3) 0.003(3) C57 0.047(3) 0.028(2) 0.058(3) -0.003(2) 0.038(3) -0.002(2) C58 0.054(3) 0.039(3) 0.064(4) -0.005(3) 0.045(3) 0.002(2) C59 0.039(3) 0.028(2) 0.021(2) 0.0007(19) 0.0117(19) 0.0043(19) C60 0.042(3) 0.051(3) 0.026(2) -0.004(2) 0.000(2) -0.001(2) C61 0.034(2) 0.018(2) 0.032(2) -0.0017(19) 0.0142(19) -0.0026(18) C62 0.034(2) 0.023(2) 0.039(3) -0.001(2) 0.014(2) 0.0017(19) C63 0.034(2) 0.021(2) 0.041(3) -0.001(2) 0.022(2) 0.0011(18) C64 0.031(3) 0.029(2) 0.053(3) -0.006(2) 0.009(2) -0.0009(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.2947(11) . ? Pt1 P1 2.2956(11) . ? Pt1 Ga2 2.4308(6) . ? Pt1 Ga1 2.4495(6) . ? Ga1 N2 1.904(3) . ? Ga1 N1 1.914(3) . ? Ga2 N4 1.894(3) . ? Ga2 N3 1.910(3) . ? P1 C57 1.805(4) . ? P1 C55 1.808(5) . ? P1 C53 1.911(5) . ? P2 C59 1.816(4) . ? P2 C63 1.825(4) . ? P2 C61 1.839(4) . ? N1 C1 1.403(5) . ? N1 C3 1.424(5) . ? N2 C2 1.399(5) . ? N2 C15 1.428(5) . ? N3 C27 1.401(5) . ? N3 C29 1.424(5) . ? N4 C28 1.393(5) . ? N4 C41 1.429(5) . ? C1 C2 1.334(5) . ? C3 C8 1.408(6) . ? C3 C4 1.408(6) . ? C4 C5 1.400(6) . ? C4 C9 1.522(6) . ? C5 C6 1.379(6) . ? C6 C7 1.385(6) . ? C7 C8 1.387(6) . ? C8 C12 1.521(6) . ? C9 C11 1.537(6) . ? C9 C10 1.536(6) . ? C12 C14 1.523(6) . ? C12 C13 1.543(6) . ? C15 C20 1.411(6) . ? C15 C16 1.414(6) . ? C16 C17 1.388(6) . ? C16 C21 1.515(6) . ? C17 C18 1.378(7) . ? C18 C19 1.378(7) . ? C19 C20 1.393(6) . ? C20 C24 1.521(6) . ? C21 C23 1.524(6) . ? C21 C22 1.526(6) . ? C24 C25 1.532(6) . ? C24 C26 1.534(6) . ? C27 C28 1.329(6) . ? C29 C34 1.410(6) . ? C29 C30 1.422(6) . ? C30 C31 1.390(6) . ? C30 C38 1.530(6) . ? C31 C32 1.381(7) . ? C32 C33 1.371(6) . ? C33 C34 1.398(6) . ? C34 C35 1.522(6) . ? C35 C36 1.529(6) . ? C35 C37 1.540(6) . ? C38 C39 1.525(6) . ? C38 C40 1.533(6) . ? C41 C46 1.405(6) . ? C41 C42 1.409(6) . ? C42 C43 1.390(6) . ? C42 C47 1.519(6) . ? C43 C44 1.365(6) . ? C44 C45 1.374(6) . ? C45 C46 1.391(6) . ? C46 C50 1.534(6) . ? C47 C49 1.497(8) . ? C47 C48 1.514(6) . ? C50 C52 1.531(7) . ? C50 C51 1.532(7) . ? C53 C54 1.532(7) . ? C55 C56 1.521(7) . ? C57 C58 1.526(6) . ? C59 C60 1.527(6) . ? C61 C62 1.525(5) . ? C63 C64 1.526(6) . ? C65 C66 1.321(14) . ? C65 C70 1.414(13) . ? C65 C71 1.499(14) . ? C66 C67 1.353(13) . ? C67 C68 1.366(12) . ? C78 C72 1.452(15) . ? C69 C68 1.325(12) . ? C69 C70 1.376(14) . ? C72 C77 1.335(16) . ? C72 C73 1.404(15) . ? C73 C74 1.352(16) . ? C74 C75 1.303(16) . ? C75 C76 1.428(17) . ? C76 C77 1.395(16) . ? 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 178.08(4) . . ? P2 Pt1 Ga2 89.67(3) . . ? P1 Pt1 Ga2 92.04(4) . . ? P2 Pt1 Ga1 89.29(3) . . ? P1 Pt1 Ga1 89.00(4) . . ? Ga2 Pt1 Ga1 178.865(16) . . ? N2 Ga1 N1 86.80(14) . . ? N2 Ga1 Pt1 135.72(10) . . ? N1 Ga1 Pt1 137.39(10) . . ? N4 Ga2 N3 87.17(14) . . ? N4 Ga2 Pt1 135.71(10) . . ? N3 Ga2 Pt1 136.61(10) . . ? C57 P1 C55 107.0(3) . . ? C57 P1 C53 100.8(2) . . ? C55 P1 C53 102.4(2) . . ? C57 P1 Pt1 118.97(16) . . ? C55 P1 Pt1 111.40(17) . . ? C53 P1 Pt1 114.50(16) . . ? C59 P2 C63 103.8(2) . . ? C59 P2 C61 103.8(2) . . ? C63 P2 C61 101.81(19) . . ? C59 P2 Pt1 111.39(14) . . ? C63 P2 Pt1 116.37(14) . . ? C61 P2 Pt1 117.93(14) . . ? C1 N1 C3 116.3(3) . . ? C1 N1 Ga1 108.7(2) . . ? C3 N1 Ga1 135.0(3) . . ? C2 N2 C15 117.2(3) . . ? C2 N2 Ga1 109.7(3) . . ? C15 N2 Ga1 133.0(3) . . ? C27 N3 C29 117.7(3) . . ? C27 N3 Ga2 108.9(3) . . ? C29 N3 Ga2 133.2(3) . . ? C28 N4 C41 117.7(3) . . ? C28 N4 Ga2 108.8(3) . . ? C41 N4 Ga2 133.2(3) . . ? C2 C1 N1 118.0(4) . . ? C1 C2 N2 116.9(4) . . ? C8 C3 C4 120.7(4) . . ? C8 C3 N1 120.1(4) . . ? C4 C3 N1 119.2(4) . . ? C5 C4 C3 118.1(4) . . ? C5 C4 C9 118.4(4) . . ? C3 C4 C9 123.5(4) . . ? C6 C5 C4 121.5(4) . . ? C5 C6 C7 119.5(4) . . ? C6 C7 C8 121.5(4) . . ? C7 C8 C3 118.6(4) . . ? C7 C8 C12 120.4(4) . . ? C3 C8 C12 121.0(4) . . ? C4 C9 C11 111.6(4) . . ? C4 C9 C10 112.7(4) . . ? C11 C9 C10 109.6(4) . . ? C8 C12 C14 114.5(4) . . ? C8 C12 C13 110.8(3) . . ? C14 C12 C13 110.0(4) . . ? C20 C15 C16 120.3(4) . . ? C20 C15 N2 119.2(4) . . ? C16 C15 N2 120.5(4) . . ? C17 C16 C15 118.3(4) . . ? C17 C16 C21 118.8(4) . . ? C15 C16 C21 122.9(4) . . ? C18 C17 C16 122.0(5) . . ? C17 C18 C19 119.3(5) . . ? C18 C19 C20 121.7(4) . . ? C19 C20 C15 118.4(4) . . ? C19 C20 C24 120.6(4) . . ? C15 C20 C24 121.0(4) . . ? C16 C21 C23 112.3(4) . . ? C16 C21 C22 111.5(4) . . ? C23 C21 C22 108.9(4) . . ? C20 C24 C25 113.9(4) . . ? C20 C24 C26 111.2(4) . . ? C25 C24 C26 109.8(4) . . ? C28 C27 N3 116.6(4) . . ? C27 C28 N4 118.5(4) . . ? C34 C29 C30 119.3(4) . . ? C34 C29 N3 121.4(4) . . ? C30 C29 N3 119.3(4) . . ? C31 C30 C29 119.1(4) . . ? C31 C30 C38 120.2(4) . . ? C29 C30 C38 120.7(4) . . ? C32 C31 C30 121.3(4) . . ? C33 C32 C31 119.7(4) . . ? C32 C33 C34 121.7(4) . . ? C33 C34 C29 118.9(4) . . ? C33 C34 C35 117.7(4) . . ? C29 C34 C35 123.4(4) . . ? C34 C35 C36 112.1(4) . . ? C34 C35 C37 111.3(4) . . ? C36 C35 C37 108.6(4) . . ? C39 C38 C30 114.3(4) . . ? C39 C38 C40 110.1(4) . . ? C30 C38 C40 110.4(4) . . ? C46 C41 C42 119.6(4) . . ? C46 C41 N4 120.8(4) . . ? C42 C41 N4 119.6(4) . . ? C43 C42 C41 118.8(4) . . ? C43 C42 C47 119.8(4) . . ? C41 C42 C47 121.4(4) . . ? C44 C43 C42 121.5(4) . . ? C43 C44 C45 119.9(4) . . ? C44 C45 C46 121.1(4) . . ? C45 C46 C41 119.1(4) . . ? C45 C46 C50 118.2(4) . . ? C41 C46 C50 122.7(4) . . ? C49 C47 C48 109.4(4) . . ? C49 C47 C42 110.0(5) . . ? C48 C47 C42 114.9(4) . . ? C52 C50 C51 108.8(4) . . ? C52 C50 C46 110.9(4) . . ? C51 C50 C46 113.3(4) . . ? C54 C53 P1 110.5(4) . . ? C56 C55 P1 112.8(3) . . ? C58 C57 P1 117.0(3) . . ? C60 C59 P2 113.5(3) . . ? C62 C61 P2 116.1(3) . . ? C64 C63 P2 112.5(3) . . ? C66 C65 C70 120.6(12) . . ? C66 C65 C71 115.2(12) . . ? C70 C65 C71 124.1(13) . . ? C65 C66 C67 120.4(15) . . ? C66 C67 C68 120.6(15) . . ? C68 C69 C70 122.0(12) . . ? C69 C70 C65 116.8(12) . . ? C77 C72 C73 121.8(15) . . ? C77 C72 C78 117.2(16) . . ? C73 C72 C78 120.3(16) . . ? C74 C73 C72 112.9(16) . . ? C75 C74 C73 131.0(19) . . ? C74 C75 C76 113.8(19) . . ? C77 C76 C75 119.0(17) . . ? C72 C77 C76 120.0(17) . . ? C69 C68 C67 119.5(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.616 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.114 # Attachment 'compound6.cif' data_compound6 _database_code_depnum_ccdc_archive 'CCDC 664046' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H102 Ga2 N4 P2 Pt' _chemical_formula_weight 1323.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.646(3) _cell_length_b 19.976(4) _cell_length_c 21.147(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.28(3) _cell_angle_gamma 90.00 _cell_volume 6239(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 3.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.728 _exptl_absorpt_correction_T_max 0.920 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10556 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5450 _reflns_number_gt 4639 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The largest residual electron density peak (2.780 e-/ang.3) in the final difference map is located close to Pt(1). ; _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^)+(0.0221P)^2^+44.4146P] 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 5450 _refine_ls_number_parameters 341 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.5000 0.480507(15) 0.7500 0.02359(10) Uani 1 2 d S . . Ga1 Ga 0.40229(4) 0.38415(3) 0.74278(3) 0.02350(16) Uani 1 1 d . . . P1 P 0.61713(10) 0.55295(8) 0.75341(8) 0.0316(4) Uani 1 1 d . . . N1 N 0.3080(3) 0.3552(2) 0.6646(2) 0.0264(10) Uani 1 1 d . . . N2 N 0.3807(3) 0.3063(2) 0.7871(2) 0.0250(10) Uani 1 1 d . . . C1 C 0.2751(4) 0.2935(3) 0.6784(3) 0.0277(13) Uani 1 1 d . . . H1 H 0.2284 0.2702 0.6453 0.033 Uiso 1 1 calc R . . C2 C 0.3122(4) 0.2691(3) 0.7402(3) 0.0280(13) Uani 1 1 d . . . H2 H 0.2929 0.2274 0.7523 0.034 Uiso 1 1 calc R . . C3 C 0.2550(3) 0.3932(3) 0.6085(3) 0.0254(12) Uani 1 1 d . . . C4 C 0.1655(4) 0.4131(3) 0.6031(3) 0.0296(13) Uani 1 1 d . . . C5 C 0.1159(4) 0.4509(3) 0.5486(3) 0.0381(15) Uani 1 1 d . . . H5 H 0.0552 0.4625 0.5440 0.046 Uiso 1 1 calc R . . C6 C 0.1520(4) 0.4721(3) 0.5008(3) 0.0409(16) Uani 1 1 d . . . H6 H 0.1175 0.4993 0.4645 0.049 Uiso 1 1 calc R . . C7 C 0.2395(4) 0.4532(3) 0.5065(3) 0.0351(14) Uani 1 1 d . . . H7 H 0.2645 0.4680 0.4736 0.042 Uiso 1 1 calc R . . C8 C 0.2914(4) 0.4134(3) 0.5587(3) 0.0291(13) Uani 1 1 d . . . C9 C 0.1232(4) 0.3961(3) 0.6563(3) 0.0324(14) Uani 1 1 d . . . H9 H 0.1717 0.3772 0.6958 0.039 Uiso 1 1 calc R . . C10 C 0.0497(4) 0.3431(3) 0.6312(3) 0.0426(16) Uani 1 1 d . . . H10A H 0.0277 0.3300 0.6678 0.064 Uiso 1 1 calc R . . H10B H 0.0747 0.3038 0.6158 0.064 Uiso 1 1 calc R . . H10C H -0.0006 0.3614 0.5941 0.064 Uiso 1 1 calc R . . C11 C 0.0836(4) 0.4575(3) 0.6798(3) 0.0441(17) Uani 1 1 d . . . H11A H 0.0282 0.4715 0.6446 0.066 Uiso 1 1 calc R . . H11B H 0.1279 0.4940 0.6896 0.066 Uiso 1 1 calc R . . H11C H 0.0695 0.4462 0.7204 0.066 Uiso 1 1 calc R . . C12 C 0.3853(4) 0.3926(3) 0.5596(3) 0.0310(14) Uani 1 1 d . . . H12 H 0.4098 0.3590 0.5961 0.037 Uiso 1 1 calc R . . C13 C 0.3819(5) 0.3604(4) 0.4931(3) 0.0497(18) Uani 1 1 d . . . H13A H 0.3382 0.3234 0.4827 0.075 Uiso 1 1 calc R . . H13B H 0.4420 0.3432 0.4967 0.075 Uiso 1 1 calc R . . H13C H 0.3632 0.3939 0.4573 0.075 Uiso 1 1 calc R . . C14 C 0.4505(4) 0.4520(3) 0.5733(3) 0.0441(16) Uani 1 1 d . . . H14A H 0.4284 0.4851 0.5373 0.066 Uiso 1 1 calc R . . H14B H 0.5107 0.4365 0.5751 0.066 Uiso 1 1 calc R . . H14C H 0.4542 0.4726 0.6161 0.066 Uiso 1 1 calc R . . C15 C 0.3935(4) 0.2878(3) 0.8561(3) 0.0272(13) Uani 1 1 d . . . C16 C 0.3296(4) 0.3108(3) 0.8861(3) 0.0280(13) Uani 1 1 d . . . C17 C 0.3387(4) 0.2896(3) 0.9504(3) 0.0362(15) Uani 1 1 d . . . H17 H 0.2973 0.3055 0.9712 0.043 Uiso 1 1 calc R . . C18 C 0.4063(4) 0.2459(3) 0.9849(3) 0.0381(15) Uani 1 1 d . . . H18 H 0.4111 0.2317 1.0288 0.046 Uiso 1 1 calc R . . C19 C 0.4666(4) 0.2233(3) 0.9551(3) 0.0360(15) Uani 1 1 d . . . H19 H 0.5130 0.1931 0.9789 0.043 Uiso 1 1 calc R . . C20 C 0.4618(4) 0.2432(3) 0.8910(3) 0.0312(14) Uani 1 1 d . . . C21 C 0.2490(4) 0.3547(3) 0.8491(3) 0.0346(14) Uani 1 1 d . . . H21 H 0.2608 0.3742 0.8092 0.042 Uiso 1 1 calc R . . C22 C 0.1629(4) 0.3128(3) 0.8238(3) 0.0435(17) Uani 1 1 d . . . H22A H 0.1715 0.2769 0.7950 0.065 Uiso 1 1 calc R . . H22B H 0.1123 0.3413 0.7982 0.065 Uiso 1 1 calc R . . H22C H 0.1496 0.2933 0.8621 0.065 Uiso 1 1 calc R . . C23 C 0.2363(5) 0.4125(3) 0.8921(4) 0.0493(18) Uani 1 1 d . . . H23A H 0.2190 0.3948 0.9294 0.074 Uiso 1 1 calc R . . H23B H 0.1887 0.4424 0.8648 0.074 Uiso 1 1 calc R . . H23C H 0.2932 0.4375 0.9099 0.074 Uiso 1 1 calc R . . C24 C 0.5275(4) 0.2115(3) 0.8596(3) 0.0382(15) Uani 1 1 d . . . H24 H 0.5302 0.2407 0.8219 0.046 Uiso 1 1 calc R . . C25 C 0.6231(4) 0.2027(3) 0.9081(3) 0.0422(16) Uani 1 1 d . . . H25A H 0.6218 0.1735 0.9451 0.063 Uiso 1 1 calc R . . H25B H 0.6479 0.2464 0.9259 0.063 Uiso 1 1 calc R . . H25C H 0.6611 0.1824 0.8846 0.063 Uiso 1 1 calc R . . C26 C 0.4907(5) 0.1435(4) 0.8312(4) 0.066(2) Uani 1 1 d . . . H26A H 0.5336 0.1217 0.8130 0.099 Uiso 1 1 calc R . . H26B H 0.4324 0.1494 0.7955 0.099 Uiso 1 1 calc R . . H26C H 0.4823 0.1157 0.8668 0.099 Uiso 1 1 calc R . . C27 C 0.5929(4) 0.6394(3) 0.7260(3) 0.0419(16) Uani 1 1 d . . . H27A H 0.5661 0.6627 0.7564 0.050 Uiso 1 1 calc R . . H27B H 0.6503 0.6623 0.7293 0.050 Uiso 1 1 calc R . . C28 C 0.5277(5) 0.6449(4) 0.6539(3) 0.0512(18) Uani 1 1 d . . . H28A H 0.5549 0.6237 0.6234 0.077 Uiso 1 1 calc R . . H28B H 0.5158 0.6922 0.6419 0.077 Uiso 1 1 calc R . . H28C H 0.4706 0.6224 0.6504 0.077 Uiso 1 1 calc R . . C29 C 0.6839(4) 0.5261(3) 0.7015(3) 0.0404(15) Uani 1 1 d . . . H29A H 0.7158 0.4843 0.7210 0.048 Uiso 1 1 calc R . . H29B H 0.6412 0.5148 0.6566 0.048 Uiso 1 1 calc R . . C30 C 0.7546(4) 0.5750(3) 0.6918(3) 0.0429(16) Uani 1 1 d . . . H30A H 0.7243 0.6159 0.6702 0.064 Uiso 1 1 calc R . . H30B H 0.7857 0.5540 0.6636 0.064 Uiso 1 1 calc R . . H30C H 0.7989 0.5861 0.7355 0.064 Uiso 1 1 calc R . . C31 C 0.6992(4) 0.5609(3) 0.8397(4) 0.0487(18) Uani 1 1 d . . . H31A H 0.6656 0.5503 0.8707 0.058 Uiso 1 1 calc R . . H31B H 0.7445 0.5248 0.8450 0.058 Uiso 1 1 calc R . . C32 C 0.7498(7) 0.6220(4) 0.8644(5) 0.092(3) Uani 1 1 d . . . H32A H 0.7894 0.6318 0.8380 0.138 Uiso 1 1 calc R . . H32B H 0.7866 0.6162 0.9116 0.138 Uiso 1 1 calc R . . H32C H 0.7075 0.6593 0.8603 0.138 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 0.02091(16) 0.01779(17) 0.03294(19) 0.000 0.01008(13) 0.000 Ga1 0.0206(3) 0.0193(3) 0.0311(4) 0.0008(3) 0.0092(3) -0.0004(2) P1 0.0276(8) 0.0209(8) 0.0482(10) -0.0001(7) 0.0152(7) -0.0009(6) N1 0.025(2) 0.023(3) 0.030(3) 0.000(2) 0.008(2) 0.001(2) N2 0.027(2) 0.021(2) 0.027(3) 0.002(2) 0.010(2) -0.001(2) C1 0.026(3) 0.023(3) 0.036(4) -0.006(3) 0.011(3) -0.002(2) C2 0.028(3) 0.022(3) 0.035(3) -0.003(3) 0.013(3) -0.006(2) C3 0.023(3) 0.021(3) 0.027(3) -0.005(2) 0.001(2) -0.004(2) C4 0.023(3) 0.030(3) 0.032(3) -0.001(3) 0.005(3) -0.005(2) C5 0.023(3) 0.039(4) 0.048(4) 0.002(3) 0.006(3) 0.000(3) C6 0.032(3) 0.040(4) 0.043(4) 0.012(3) 0.003(3) 0.012(3) C7 0.037(3) 0.038(4) 0.031(3) 0.007(3) 0.012(3) -0.001(3) C8 0.026(3) 0.029(3) 0.032(3) 0.000(3) 0.010(3) -0.001(3) C9 0.022(3) 0.035(4) 0.040(4) 0.000(3) 0.010(3) 0.003(3) C10 0.034(3) 0.048(4) 0.053(4) -0.007(3) 0.023(3) -0.009(3) C11 0.035(3) 0.046(4) 0.052(4) -0.005(3) 0.017(3) 0.007(3) C12 0.031(3) 0.031(3) 0.034(4) 0.004(3) 0.016(3) 0.002(3) C13 0.049(4) 0.059(5) 0.043(4) 0.004(4) 0.019(3) 0.016(4) C14 0.034(3) 0.054(4) 0.045(4) 0.009(3) 0.015(3) 0.000(3) C15 0.028(3) 0.024(3) 0.029(3) -0.001(3) 0.010(3) -0.008(2) C16 0.031(3) 0.022(3) 0.033(3) -0.002(3) 0.013(3) -0.007(2) C17 0.038(3) 0.038(4) 0.038(4) 0.000(3) 0.020(3) -0.003(3) C18 0.036(3) 0.050(4) 0.031(4) 0.008(3) 0.015(3) 0.001(3) C19 0.028(3) 0.039(4) 0.042(4) 0.005(3) 0.013(3) 0.001(3) C20 0.029(3) 0.030(3) 0.034(3) 0.004(3) 0.010(3) 0.004(3) C21 0.041(3) 0.028(3) 0.040(4) 0.003(3) 0.020(3) 0.008(3) C22 0.033(3) 0.045(4) 0.059(5) 0.004(3) 0.024(3) 0.004(3) C23 0.067(5) 0.028(4) 0.065(5) 0.004(3) 0.038(4) 0.011(3) C24 0.035(3) 0.040(4) 0.042(4) 0.009(3) 0.017(3) 0.009(3) C25 0.036(3) 0.036(4) 0.058(4) 0.006(3) 0.019(3) 0.004(3) C26 0.044(4) 0.073(6) 0.079(6) -0.040(5) 0.017(4) 0.000(4) C27 0.043(4) 0.028(4) 0.059(5) 0.003(3) 0.022(3) 0.005(3) C28 0.047(4) 0.059(5) 0.050(4) 0.010(4) 0.018(3) 0.005(4) C29 0.034(3) 0.032(4) 0.062(4) -0.008(3) 0.025(3) -0.008(3) C30 0.040(4) 0.036(4) 0.060(5) 0.003(3) 0.028(3) -0.008(3) C31 0.046(4) 0.028(4) 0.058(5) 0.007(3) -0.001(3) 0.004(3) C32 0.096(7) 0.063(6) 0.087(7) 0.000(5) -0.010(6) -0.014(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.3173(15) . ? Pt1 P1 2.3173(15) 2_656 ? Pt1 Ga1 2.4313(7) . ? Pt1 Ga1 2.4313(7) 2_656 ? Ga1 N2 1.903(4) . ? Ga1 N1 1.906(4) . ? P1 C27 1.822(6) . ? P1 C29 1.829(6) . ? P1 C31 1.859(7) . ? N1 C1 1.402(7) . ? N1 C3 1.423(7) . ? N2 C2 1.406(7) . ? N2 C15 1.453(7) . ? C1 C2 1.333(8) . ? C3 C8 1.412(8) . ? C3 C4 1.423(7) . ? C4 C5 1.381(8) . ? C4 C9 1.521(8) . ? C5 C6 1.378(9) . ? C6 C7 1.386(8) . ? C7 C8 1.386(8) . ? C8 C12 1.520(8) . ? C9 C10 1.523(8) . ? C9 C11 1.529(8) . ? C12 C14 1.528(8) . ? C12 C13 1.531(8) . ? C15 C20 1.401(8) . ? C15 C16 1.426(8) . ? C16 C17 1.385(8) . ? C16 C21 1.523(8) . ? C17 C18 1.380(8) . ? C18 C19 1.373(8) . ? C19 C20 1.390(8) . ? C20 C24 1.533(8) . ? C21 C23 1.522(8) . ? C21 C22 1.526(9) . ? C24 C25 1.518(8) . ? C24 C26 1.519(9) . ? C27 C28 1.533(9) . ? C29 C30 1.539(8) . ? C31 C32 1.455(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 Pt1 P1 102.71(8) . 2_656 ? P1 Pt1 Ga1 166.10(4) . . ? P1 Pt1 Ga1 91.04(4) 2_656 . ? P1 Pt1 Ga1 91.04(4) . 2_656 ? P1 Pt1 Ga1 166.10(4) 2_656 2_656 ? Ga1 Pt1 Ga1 75.31(3) . 2_656 ? N2 Ga1 N1 88.03(19) . . ? N2 Ga1 Pt1 145.77(14) . . ? N1 Ga1 Pt1 125.84(14) . . ? C27 P1 C29 100.8(3) . . ? C27 P1 C31 103.6(3) . . ? C29 P1 C31 105.5(3) . . ? C27 P1 Pt1 120.2(2) . . ? C29 P1 Pt1 113.6(2) . . ? C31 P1 Pt1 111.5(2) . . ? C1 N1 C3 119.3(4) . . ? C1 N1 Ga1 108.6(4) . . ? C3 N1 Ga1 129.2(4) . . ? C2 N2 C15 113.3(4) . . ? C2 N2 Ga1 107.6(3) . . ? C15 N2 Ga1 135.5(4) . . ? C2 C1 N1 116.9(5) . . ? C1 C2 N2 118.8(5) . . ? C8 C3 C4 119.3(5) . . ? C8 C3 N1 120.5(5) . . ? C4 C3 N1 120.2(5) . . ? C5 C4 C3 119.2(5) . . ? C5 C4 C9 118.4(5) . . ? C3 C4 C9 122.4(5) . . ? C6 C5 C4 121.7(5) . . ? C5 C6 C7 119.0(6) . . ? C8 C7 C6 121.9(6) . . ? C7 C8 C3 118.9(5) . . ? C7 C8 C12 118.5(5) . . ? C3 C8 C12 122.6(5) . . ? C4 C9 C10 111.2(5) . . ? C4 C9 C11 112.5(5) . . ? C10 C9 C11 109.3(5) . . ? C8 C12 C14 111.8(5) . . ? C8 C12 C13 111.2(5) . . ? C14 C12 C13 108.7(5) . . ? C20 C15 C16 119.6(5) . . ? C20 C15 N2 121.3(5) . . ? C16 C15 N2 118.8(5) . . ? C17 C16 C15 118.6(5) . . ? C17 C16 C21 118.7(5) . . ? C15 C16 C21 122.6(5) . . ? C18 C17 C16 121.6(6) . . ? C19 C18 C17 119.3(6) . . ? C18 C19 C20 121.9(6) . . ? C19 C20 C15 118.9(5) . . ? C19 C20 C24 118.4(5) . . ? C15 C20 C24 122.6(5) . . ? C23 C21 C16 112.2(5) . . ? C23 C21 C22 110.6(5) . . ? C16 C21 C22 110.4(5) . . ? C25 C24 C26 108.9(5) . . ? C25 C24 C20 114.0(5) . . ? C26 C24 C20 108.7(5) . . ? C28 C27 P1 112.6(5) . . ? C30 C29 P1 118.2(4) . . ? C32 C31 P1 122.8(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.780 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.115 # Attachment 'compound7.CIF' data_compound7 _database_code_depnum_ccdc_archive 'CCDC 664047' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H102 Ga2 N4 Ni P2' _chemical_formula_weight 1187.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.788(2) _cell_length_b 12.518(3) _cell_length_c 13.824(3) _cell_angle_alpha 101.19(3) _cell_angle_beta 103.22(3) _cell_angle_gamma 113.31(3) _cell_volume 1582.2(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 634 _exptl_absorpt_coefficient_mu 1.230 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.704 _exptl_absorpt_correction_T_max 0.908 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11700 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0700 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 26.50 _reflns_number_total 6451 _reflns_number_gt 4982 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+0.9960P] 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 6451 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Ga1 Ga 0.56745(3) 0.51972(2) 0.68005(2) 0.01469(9) Uani 1 1 d . . . Ni1 Ni 0.5000 0.5000 0.5000 0.01424(12) Uani 1 2 d S . . P1 P 0.40269(7) 0.62218(6) 0.52584(6) 0.01758(16) Uani 1 1 d . . . N1 N 0.5248(2) 0.41563(18) 0.76477(17) 0.0180(5) Uani 1 1 d . . . N2 N 0.6700(2) 0.65329(18) 0.80842(16) 0.0154(5) Uani 1 1 d . . . C1 C 0.5863(3) 0.4868(2) 0.8705(2) 0.0229(6) Uani 1 1 d . . . H1 H 0.5768 0.4503 0.9243 0.027 Uiso 1 1 calc R . . C2 C 0.6592(3) 0.6084(2) 0.8929(2) 0.0206(6) Uani 1 1 d . . . H2 H 0.7019 0.6619 0.9631 0.025 Uiso 1 1 calc R . . C3 C 0.4742(3) 0.2864(2) 0.7414(2) 0.0169(6) Uani 1 1 d . . . C4 C 0.3260(3) 0.2062(2) 0.6907(2) 0.0201(6) Uani 1 1 d . . . C5 C 0.2791(3) 0.0800(2) 0.6639(2) 0.0261(7) Uani 1 1 d . . . H5 H 0.1800 0.0252 0.6288 0.031 Uiso 1 1 calc R . . C6 C 0.3756(3) 0.0336(3) 0.6880(2) 0.0301(7) Uani 1 1 d . . . H6 H 0.3424 -0.0526 0.6682 0.036 Uiso 1 1 calc R . . C7 C 0.5186(3) 0.1117(3) 0.7400(2) 0.0280(7) Uani 1 1 d . . . H7 H 0.5828 0.0784 0.7575 0.034 Uiso 1 1 calc R . . C8 C 0.5720(3) 0.2388(2) 0.7681(2) 0.0217(6) Uani 1 1 d . . . C9 C 0.2199(3) 0.2578(2) 0.6696(2) 0.0238(6) Uani 1 1 d . . . H9 H 0.2612 0.3267 0.6415 0.029 Uiso 1 1 calc R . . C10 C 0.2011(4) 0.3105(3) 0.7718(3) 0.0370(8) Uani 1 1 d . . . H10A H 0.1592 0.2445 0.8007 0.056 Uiso 1 1 calc R . . H10B H 0.1372 0.3479 0.7577 0.056 Uiso 1 1 calc R . . H10C H 0.2947 0.3729 0.8225 0.056 Uiso 1 1 calc R . . C11 C 0.0736(3) 0.1643(3) 0.5890(3) 0.0435(9) Uani 1 1 d . . . H11A H 0.0865 0.1264 0.5256 0.065 Uiso 1 1 calc R . . H11B H 0.0152 0.2056 0.5715 0.065 Uiso 1 1 calc R . . H11C H 0.0252 0.1008 0.6183 0.065 Uiso 1 1 calc R . . C12 C 0.7315(3) 0.3216(3) 0.8252(3) 0.0352(8) Uani 1 1 d . . . H12 H 0.7529 0.4061 0.8225 0.042 Uiso 1 1 calc R . . C13 C 0.7742(4) 0.3283(3) 0.9404(3) 0.0524(10) Uani 1 1 d . . . H13A H 0.7224 0.3625 0.9752 0.079 Uiso 1 1 calc R . . H13B H 0.8777 0.3810 0.9746 0.079 Uiso 1 1 calc R . . H13C H 0.7499 0.2458 0.9451 0.079 Uiso 1 1 calc R . . C14 C 0.8232(4) 0.2803(4) 0.7738(4) 0.0603(12) Uani 1 1 d . . . H14A H 0.8152 0.2031 0.7848 0.091 Uiso 1 1 calc R . . H14B H 0.9237 0.3433 0.8051 0.091 Uiso 1 1 calc R . . H14C H 0.7896 0.2679 0.6984 0.091 Uiso 1 1 calc R . . C15 C 0.7546(3) 0.7831(2) 0.8331(2) 0.0173(6) Uani 1 1 d . . . C16 C 0.7155(3) 0.8665(2) 0.8865(2) 0.0201(6) Uani 1 1 d . . . C17 C 0.8026(3) 0.9919(2) 0.9091(2) 0.0259(7) Uani 1 1 d . . . H17 H 0.7781 1.0489 0.9456 0.031 Uiso 1 1 calc R . . C18 C 0.9216(3) 1.0354(3) 0.8805(2) 0.0293(7) Uani 1 1 d . . . H18 H 0.9783 1.1212 0.8967 0.035 Uiso 1 1 calc R . . C19 C 0.9590(3) 0.9533(2) 0.8277(2) 0.0260(7) Uani 1 1 d . . . H19 H 1.0416 0.9838 0.8075 0.031 Uiso 1 1 calc R . . C20 C 0.8779(3) 0.8269(2) 0.8036(2) 0.0196(6) Uani 1 1 d . . . C21 C 0.5865(3) 0.8264(3) 0.9236(2) 0.0226(6) Uani 1 1 d . . . H21 H 0.5283 0.7354 0.8919 0.027 Uiso 1 1 calc R . . C22 C 0.6339(3) 0.8575(3) 1.0428(2) 0.0316(7) Uani 1 1 d . . . H22A H 0.6935 0.8187 1.0651 0.047 Uiso 1 1 calc R . . H22B H 0.5491 0.8272 1.0642 0.047 Uiso 1 1 calc R . . H22C H 0.6894 0.9467 1.0756 0.047 Uiso 1 1 calc R . . C23 C 0.4896(3) 0.8850(3) 0.8899(2) 0.0321(7) Uani 1 1 d . . . H23A H 0.5406 0.9734 0.9274 0.048 Uiso 1 1 calc R . . H23B H 0.4018 0.8478 0.9065 0.048 Uiso 1 1 calc R . . H23C H 0.4648 0.8713 0.8142 0.048 Uiso 1 1 calc R . . C24 C 0.9258(3) 0.7385(2) 0.7521(2) 0.0239(6) Uani 1 1 d . . . H24 H 0.8383 0.6675 0.6976 0.029 Uiso 1 1 calc R . . C25 C 0.9883(3) 0.6881(3) 0.8319(3) 0.0376(8) Uani 1 1 d . . . H25A H 1.0761 0.7551 0.8856 0.056 Uiso 1 1 calc R . . H25B H 1.0108 0.6260 0.7962 0.056 Uiso 1 1 calc R . . H25C H 0.9181 0.6508 0.8649 0.056 Uiso 1 1 calc R . . C26 C 1.0318(3) 0.7930(3) 0.6971(3) 0.0417(9) Uani 1 1 d . . . H26A H 0.9913 0.8261 0.6469 0.063 Uiso 1 1 calc R . . H26B H 1.0501 0.7288 0.6599 0.063 Uiso 1 1 calc R . . H26C H 1.1220 0.8589 0.7492 0.063 Uiso 1 1 calc R . . C27 C 0.3840(3) 0.6759(2) 0.6524(2) 0.0212(6) Uani 1 1 d . . . H27A H 0.4807 0.7194 0.7065 0.025 Uiso 1 1 calc R . . H27B H 0.3473 0.7366 0.6484 0.025 Uiso 1 1 calc R . . C28 C 0.2866(3) 0.5785(3) 0.6888(3) 0.0324(7) Uani 1 1 d . . . H28A H 0.1970 0.5231 0.6306 0.049 Uiso 1 1 calc R . . H28B H 0.2654 0.6180 0.7469 0.049 Uiso 1 1 calc R . . H28C H 0.3348 0.5315 0.7125 0.049 Uiso 1 1 calc R . . C29 C 0.2191(3) 0.5641(3) 0.4354(2) 0.0280(7) Uani 1 1 d . . . H29A H 0.2235 0.5603 0.3642 0.034 Uiso 1 1 calc R . . H29B H 0.1619 0.4789 0.4338 0.034 Uiso 1 1 calc R . . C30 C 0.1385(3) 0.6368(3) 0.4596(3) 0.0377(8) Uani 1 1 d . . . H30A H 0.1139 0.6263 0.5224 0.057 Uiso 1 1 calc R . . H30B H 0.0504 0.6067 0.4001 0.057 Uiso 1 1 calc R . . H30C H 0.1994 0.7240 0.4720 0.057 Uiso 1 1 calc R . . C31 C 0.5012(3) 0.7697(2) 0.5080(2) 0.0246(7) Uani 1 1 d . . . H31A H 0.4928 0.7559 0.4333 0.029 Uiso 1 1 calc R . . H31B H 0.4562 0.8227 0.5254 0.029 Uiso 1 1 calc R . . C32 C 0.6588(3) 0.8363(3) 0.5747(3) 0.0412(9) Uani 1 1 d . . . H32A H 0.6682 0.8527 0.6490 0.062 Uiso 1 1 calc R . . H32B H 0.7054 0.9140 0.5613 0.062 Uiso 1 1 calc R . . H32C H 0.7047 0.7851 0.5571 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.01676(16) 0.01357(15) 0.01401(16) 0.00472(12) 0.00500(13) 0.00724(12) Ni1 0.0159(3) 0.0144(2) 0.0131(3) 0.0038(2) 0.0044(2) 0.0081(2) P1 0.0192(4) 0.0171(4) 0.0167(4) 0.0027(3) 0.0047(3) 0.0107(3) N1 0.0208(12) 0.0139(11) 0.0165(13) 0.0070(10) 0.0040(10) 0.0055(9) N2 0.0185(12) 0.0131(11) 0.0104(12) 0.0015(9) 0.0042(10) 0.0046(9) C1 0.0301(16) 0.0237(15) 0.0190(16) 0.0106(13) 0.0083(13) 0.0145(13) C2 0.0259(16) 0.0217(14) 0.0123(14) 0.0047(12) 0.0050(12) 0.0104(12) C3 0.0235(15) 0.0155(13) 0.0149(14) 0.0093(12) 0.0087(12) 0.0089(11) C4 0.0246(15) 0.0202(14) 0.0195(15) 0.0105(13) 0.0098(13) 0.0108(12) C5 0.0255(16) 0.0187(14) 0.0270(17) 0.0085(13) 0.0056(14) 0.0046(12) C6 0.042(2) 0.0178(14) 0.0335(19) 0.0110(14) 0.0133(16) 0.0152(14) C7 0.0356(18) 0.0284(16) 0.0362(19) 0.0195(15) 0.0186(16) 0.0225(15) C8 0.0217(15) 0.0261(15) 0.0276(17) 0.0189(14) 0.0135(13) 0.0133(12) C9 0.0202(15) 0.0198(14) 0.0300(18) 0.0098(13) 0.0078(13) 0.0075(12) C10 0.0348(19) 0.0429(19) 0.049(2) 0.0214(18) 0.0233(17) 0.0248(16) C11 0.0287(19) 0.0355(19) 0.058(3) 0.0157(18) 0.0041(17) 0.0128(15) C12 0.0248(17) 0.0328(17) 0.055(2) 0.0266(17) 0.0134(16) 0.0137(14) C13 0.039(2) 0.046(2) 0.058(3) 0.026(2) -0.0058(19) 0.0136(17) C14 0.039(2) 0.074(3) 0.106(4) 0.058(3) 0.042(2) 0.040(2) C15 0.0215(15) 0.0128(13) 0.0098(14) 0.0013(11) -0.0006(11) 0.0048(11) C16 0.0244(15) 0.0196(14) 0.0133(14) 0.0042(12) 0.0021(12) 0.0101(12) C17 0.0359(18) 0.0149(14) 0.0242(17) 0.0020(13) 0.0081(14) 0.0122(13) C18 0.0321(18) 0.0156(14) 0.0316(18) 0.0071(14) 0.0061(15) 0.0057(13) C19 0.0242(16) 0.0225(15) 0.0224(16) 0.0081(13) 0.0059(13) 0.0030(13) C20 0.0208(15) 0.0194(14) 0.0116(14) 0.0023(12) 0.0013(12) 0.0061(12) C21 0.0271(16) 0.0222(15) 0.0187(16) 0.0032(13) 0.0071(13) 0.0134(13) C22 0.0382(19) 0.0344(17) 0.0230(18) 0.0076(15) 0.0119(15) 0.0173(15) C23 0.0375(19) 0.0359(18) 0.0264(18) 0.0048(15) 0.0085(15) 0.0236(15) C24 0.0195(15) 0.0201(14) 0.0230(16) -0.0001(13) 0.0059(13) 0.0044(12) C25 0.0321(19) 0.0368(18) 0.043(2) 0.0084(17) 0.0071(16) 0.0202(15) C26 0.036(2) 0.0353(19) 0.047(2) 0.0047(17) 0.0243(18) 0.0079(15) C27 0.0251(16) 0.0218(14) 0.0202(16) 0.0039(13) 0.0085(13) 0.0151(12) C28 0.0344(18) 0.0302(17) 0.036(2) 0.0090(15) 0.0186(16) 0.0147(14) C29 0.0240(16) 0.0306(16) 0.0257(17) 0.0008(14) 0.0026(14) 0.0160(13) C30 0.0281(18) 0.048(2) 0.035(2) 0.0024(16) 0.0048(15) 0.0234(16) C31 0.0308(17) 0.0231(15) 0.0252(17) 0.0101(13) 0.0108(14) 0.0158(13) C32 0.0342(19) 0.0395(19) 0.038(2) 0.0199(17) 0.0067(16) 0.0054(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N1 1.909(2) . ? Ga1 N2 1.912(2) . ? Ga1 Ni1 2.3614(7) . ? Ni1 P1 2.1908(8) 2_666 ? Ni1 P1 2.1908(8) . ? Ni1 Ga1 2.3614(7) 2_666 ? P1 C31 1.829(3) . ? P1 C27 1.835(3) . ? P1 C29 1.841(3) . ? N1 C1 1.398(4) . ? N1 C3 1.427(3) . ? N2 C2 1.399(3) . ? N2 C15 1.434(3) . ? C1 C2 1.337(4) . ? C3 C4 1.414(4) . ? C3 C8 1.417(4) . ? C4 C5 1.394(4) . ? C4 C9 1.522(4) . ? C5 C6 1.388(4) . ? C6 C7 1.370(4) . ? C7 C8 1.396(4) . ? C8 C12 1.519(4) . ? C9 C11 1.526(4) . ? C9 C10 1.533(4) . ? C12 C13 1.528(5) . ? C12 C14 1.528(5) . ? C15 C20 1.413(4) . ? C15 C16 1.416(4) . ? C16 C17 1.398(4) . ? C16 C21 1.525(4) . ? C17 C18 1.365(4) . ? C18 C19 1.388(4) . ? C19 C20 1.395(4) . ? C20 C24 1.520(4) . ? C21 C22 1.528(4) . ? C21 C23 1.538(4) . ? C24 C26 1.528(4) . ? C24 C25 1.528(4) . ? C27 C28 1.520(4) . ? C29 C30 1.530(4) . ? C31 C32 1.516(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ga1 N2 86.47(9) . . ? N1 Ga1 Ni1 137.40(7) . . ? N2 Ga1 Ni1 135.63(6) . . ? P1 Ni1 P1 180.0 2_666 . ? P1 Ni1 Ga1 89.41(3) 2_666 . ? P1 Ni1 Ga1 90.59(3) . . ? P1 Ni1 Ga1 90.59(3) 2_666 2_666 ? P1 Ni1 Ga1 89.41(3) . 2_666 ? Ga1 Ni1 Ga1 180.0 . 2_666 ? C31 P1 C27 99.79(13) . . ? C31 P1 C29 103.41(14) . . ? C27 P1 C29 101.30(14) . . ? C31 P1 Ni1 112.68(10) . . ? C27 P1 Ni1 122.14(9) . . ? C29 P1 Ni1 114.93(10) . . ? C1 N1 C3 117.2(2) . . ? C1 N1 Ga1 109.56(16) . . ? C3 N1 Ga1 131.40(18) . . ? C2 N2 C15 116.9(2) . . ? C2 N2 Ga1 109.50(16) . . ? C15 N2 Ga1 133.53(17) . . ? C2 C1 N1 117.3(2) . . ? C1 C2 N2 117.1(3) . . ? C4 C3 C8 120.3(2) . . ? C4 C3 N1 119.5(2) . . ? C8 C3 N1 120.2(2) . . ? C5 C4 C3 118.8(2) . . ? C5 C4 C9 121.0(2) . . ? C3 C4 C9 120.2(2) . . ? C6 C5 C4 120.7(3) . . ? C7 C6 C5 120.3(3) . . ? C6 C7 C8 121.6(3) . . ? C7 C8 C3 118.3(3) . . ? C7 C8 C12 119.6(2) . . ? C3 C8 C12 122.1(2) . . ? C4 C9 C11 113.5(2) . . ? C4 C9 C10 110.4(2) . . ? C11 C9 C10 109.6(3) . . ? C8 C12 C13 111.4(3) . . ? C8 C12 C14 112.2(3) . . ? C13 C12 C14 109.3(3) . . ? C20 C15 C16 120.3(2) . . ? C20 C15 N2 119.1(2) . . ? C16 C15 N2 120.6(2) . . ? C17 C16 C15 118.1(3) . . ? C17 C16 C21 118.6(2) . . ? C15 C16 C21 123.3(2) . . ? C18 C17 C16 122.2(3) . . ? C17 C18 C19 119.5(3) . . ? C18 C19 C20 121.3(3) . . ? C19 C20 C15 118.6(3) . . ? C19 C20 C24 120.7(2) . . ? C15 C20 C24 120.6(2) . . ? C16 C21 C22 111.1(2) . . ? C16 C21 C23 112.6(2) . . ? C22 C21 C23 108.7(2) . . ? C20 C24 C26 114.0(2) . . ? C20 C24 C25 110.6(2) . . ? C26 C24 C25 110.1(3) . . ? C28 C27 P1 116.6(2) . . ? C30 C29 P1 117.0(2) . . ? C32 C31 P1 113.48(19) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.461 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.080 # Attachment 'compound8.CIF' data_compound8 _database_code_depnum_ccdc_archive 'CCDC 664048' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H102 Ga2 N4 P2 Pd' _chemical_formula_weight 1235.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.783(2) _cell_length_b 12.571(3) _cell_length_c 13.913(3) _cell_angle_alpha 101.17(3) _cell_angle_beta 103.06(3) _cell_angle_gamma 113.84(3) _cell_volume 1592.2(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 1.210 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.739 _exptl_absorpt_correction_T_max 0.884 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10379 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_sigmaI/netI 0.0919 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 24.98 _reflns_number_total 5553 _reflns_number_gt 4044 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0111P)^2^+1.8925P] 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 5553 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.5000 0.5000 0.5000 0.01731(14) Uani 1 2 d S . . Ga1 Ga 0.56857(4) 0.52095(4) 0.68573(3) 0.01829(14) Uani 1 1 d . . . P1 P 0.40137(11) 0.63053(10) 0.52582(9) 0.0207(3) Uani 1 1 d . . . N1 N 0.6704(3) 0.6549(3) 0.8122(3) 0.0195(8) Uani 1 1 d . . . N2 N 0.5281(3) 0.4176(3) 0.7703(3) 0.0211(8) Uani 1 1 d . . . C1 C 0.6618(4) 0.6106(4) 0.8971(3) 0.0250(10) Uani 1 1 d . . . H1 H 0.7056 0.6646 0.9667 0.030 Uiso 1 1 calc R . . C2 C 0.5896(4) 0.4894(4) 0.8755(3) 0.0259(11) Uani 1 1 d . . . H2 H 0.5801 0.4533 0.9291 0.031 Uiso 1 1 calc R . . C3 C 0.7553(4) 0.7847(4) 0.8349(3) 0.0196(10) Uani 1 1 d . . . C4 C 0.7172(4) 0.8681(4) 0.8878(3) 0.0232(10) Uani 1 1 d . . . C5 C 0.8051(5) 0.9938(4) 0.9095(3) 0.0298(11) Uani 1 1 d . . . H5 H 0.7819 1.0511 0.9461 0.036 Uiso 1 1 calc R . . C6 C 0.9238(5) 1.0361(4) 0.8792(3) 0.0306(11) Uani 1 1 d . . . H6 H 0.9820 1.1218 0.8951 0.037 Uiso 1 1 calc R . . C7 C 0.9589(4) 0.9539(4) 0.8255(3) 0.0263(11) Uani 1 1 d . . . H7 H 1.0393 0.9840 0.8026 0.032 Uiso 1 1 calc R . . C8 C 0.8788(4) 0.8280(4) 0.8044(3) 0.0219(10) Uani 1 1 d . . . C9 C 0.5884(4) 0.8282(4) 0.9247(3) 0.0262(11) Uani 1 1 d . . . H9 H 0.5298 0.7370 0.8937 0.031 Uiso 1 1 calc R . . C10 C 0.6351(5) 0.8607(4) 1.0433(3) 0.0360(12) Uani 1 1 d . . . H10A H 0.6957 0.8235 1.0664 0.054 Uiso 1 1 calc R . . H10B H 0.5496 0.8294 1.0642 0.054 Uiso 1 1 calc R . . H10C H 0.6899 0.9501 1.0754 0.054 Uiso 1 1 calc R . . C11 C 0.4918(5) 0.8850(4) 0.8906(4) 0.0362(12) Uani 1 1 d . . . H11A H 0.5424 0.9734 0.9281 0.054 Uiso 1 1 calc R . . H11B H 0.4029 0.8467 0.9063 0.054 Uiso 1 1 calc R . . H11C H 0.4679 0.8715 0.8155 0.054 Uiso 1 1 calc R . . C12 C 0.9237(4) 0.7392(4) 0.7517(3) 0.0264(11) Uani 1 1 d . . . H12 H 0.8347 0.6677 0.6986 0.032 Uiso 1 1 calc R . . C13 C 0.9892(5) 0.6905(5) 0.8310(4) 0.0398(13) Uani 1 1 d . . . H13A H 1.0778 0.7585 0.8836 0.060 Uiso 1 1 calc R . . H13B H 1.0116 0.6290 0.7952 0.060 Uiso 1 1 calc R . . H13C H 0.9201 0.6530 0.8649 0.060 Uiso 1 1 calc R . . C14 C 1.0290(5) 0.7922(4) 0.6957(4) 0.0446(14) Uani 1 1 d . . . H14A H 0.9885 0.8251 0.6460 0.067 Uiso 1 1 calc R . . H14B H 1.0455 0.7274 0.6584 0.067 Uiso 1 1 calc R . . H14C H 1.1206 0.8582 0.7468 0.067 Uiso 1 1 calc R . . C15 C 0.4783(4) 0.2883(4) 0.7464(3) 0.0212(10) Uani 1 1 d . . . C16 C 0.3299(4) 0.2075(4) 0.6935(3) 0.0222(10) Uani 1 1 d . . . C17 C 0.2836(5) 0.0816(4) 0.6648(4) 0.0305(11) Uani 1 1 d . . . H17 H 0.1846 0.0264 0.6273 0.037 Uiso 1 1 calc R . . C18 C 0.3789(5) 0.0353(4) 0.6897(4) 0.0329(12) Uani 1 1 d . . . H18 H 0.3451 -0.0509 0.6701 0.040 Uiso 1 1 calc R . . C19 C 0.5232(5) 0.1149(4) 0.7431(4) 0.0340(12) Uani 1 1 d . . . H19 H 0.5881 0.0826 0.7599 0.041 Uiso 1 1 calc R . . C20 C 0.5756(4) 0.2422(4) 0.7731(3) 0.0267(11) Uani 1 1 d . . . C21 C 0.2230(4) 0.2567(4) 0.6706(3) 0.0269(11) Uani 1 1 d . . . H21 H 0.2652 0.3253 0.6424 0.032 Uiso 1 1 calc R . . C22 C 0.2030(5) 0.3107(5) 0.7711(4) 0.0443(14) Uani 1 1 d . . . H22A H 0.1601 0.2453 0.8003 0.066 Uiso 1 1 calc R . . H22B H 0.1393 0.3475 0.7558 0.066 Uiso 1 1 calc R . . H22C H 0.2969 0.3737 0.8216 0.066 Uiso 1 1 calc R . . C23 C 0.0767(5) 0.1634(5) 0.5905(4) 0.0515(15) Uani 1 1 d . . . H23A H 0.0898 0.1251 0.5278 0.077 Uiso 1 1 calc R . . H23B H 0.0190 0.2048 0.5724 0.077 Uiso 1 1 calc R . . H23C H 0.0269 0.1003 0.6196 0.077 Uiso 1 1 calc R . . C24 C 0.7362(5) 0.3263(5) 0.8330(4) 0.0403(13) Uani 1 1 d . . . H24 H 0.7585 0.4111 0.8316 0.048 Uiso 1 1 calc R . . C25 C 0.7739(5) 0.3303(5) 0.9473(4) 0.0532(16) Uani 1 1 d . . . H25A H 0.7194 0.3622 0.9804 0.080 Uiso 1 1 calc R . . H25B H 0.8774 0.3840 0.9837 0.080 Uiso 1 1 calc R . . H25C H 0.7491 0.2473 0.9506 0.080 Uiso 1 1 calc R . . C26 C 0.8312(6) 0.2876(6) 0.7840(6) 0.069(2) Uani 1 1 d . . . H26A H 0.8214 0.2097 0.7933 0.104 Uiso 1 1 calc R . . H26B H 0.9320 0.3509 0.8176 0.104 Uiso 1 1 calc R . . H26C H 0.8010 0.2776 0.7094 0.104 Uiso 1 1 calc R . . C27 C 0.3814(5) 0.6806(4) 0.6507(3) 0.0284(11) Uani 1 1 d . . . H27A H 0.4780 0.7231 0.7050 0.034 Uiso 1 1 calc R . . H27B H 0.3456 0.7415 0.6481 0.034 Uiso 1 1 calc R . . C28 C 0.2814(5) 0.5806(4) 0.6841(4) 0.0411(13) Uani 1 1 d . . . H28A H 0.1900 0.5286 0.6265 0.062 Uiso 1 1 calc R . . H28B H 0.2632 0.6183 0.7443 0.062 Uiso 1 1 calc R . . H28C H 0.3266 0.5304 0.7031 0.062 Uiso 1 1 calc R . . C29 C 0.5032(5) 0.7777(4) 0.5102(4) 0.0306(11) Uani 1 1 d . . . H29A H 0.4971 0.7642 0.4364 0.037 Uiso 1 1 calc R . . H29B H 0.4576 0.8301 0.5262 0.037 Uiso 1 1 calc R . . C30 C 0.6604(5) 0.8457(4) 0.5780(4) 0.0447(14) Uani 1 1 d . . . H30A H 0.6680 0.8624 0.6514 0.067 Uiso 1 1 calc R . . H30B H 0.7077 0.9234 0.5645 0.067 Uiso 1 1 calc R . . H30C H 0.7073 0.7954 0.5619 0.067 Uiso 1 1 calc R . . C31 C 0.2191(4) 0.5717(4) 0.4336(4) 0.0332(12) Uani 1 1 d . . . H31A H 0.2254 0.5682 0.3633 0.040 Uiso 1 1 calc R . . H31B H 0.1600 0.4866 0.4316 0.040 Uiso 1 1 calc R . . C32 C 0.1396(5) 0.6463(5) 0.4574(4) 0.0477(15) Uani 1 1 d . . . H32A H 0.1120 0.6348 0.5185 0.072 Uiso 1 1 calc R . . H32B H 0.0529 0.6180 0.3974 0.072 Uiso 1 1 calc R . . H32C H 0.2033 0.7335 0.4713 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 Pd1 0.0198(3) 0.0162(3) 0.0182(3) 0.0047(2) 0.0069(2) 0.0107(2) Ga1 0.0209(3) 0.0164(3) 0.0189(3) 0.0059(2) 0.0065(2) 0.0099(2) P1 0.0226(6) 0.0198(6) 0.0220(6) 0.0041(5) 0.0074(5) 0.0132(5) N1 0.0243(19) 0.0166(18) 0.0175(19) 0.0051(15) 0.0073(15) 0.0094(15) N2 0.0278(19) 0.0152(18) 0.021(2) 0.0101(16) 0.0090(16) 0.0085(16) C1 0.029(2) 0.024(3) 0.016(2) 0.003(2) 0.004(2) 0.011(2) C2 0.030(2) 0.026(3) 0.025(3) 0.013(2) 0.010(2) 0.014(2) C3 0.020(2) 0.016(2) 0.013(2) 0.0035(18) -0.0008(18) 0.0044(18) C4 0.027(2) 0.019(2) 0.020(2) 0.0050(19) 0.0043(19) 0.0090(19) C5 0.037(3) 0.027(3) 0.024(3) 0.002(2) 0.007(2) 0.018(2) C6 0.037(3) 0.014(2) 0.027(3) 0.004(2) 0.002(2) 0.004(2) C7 0.025(2) 0.023(2) 0.026(3) 0.010(2) 0.006(2) 0.006(2) C8 0.021(2) 0.022(2) 0.015(2) 0.0058(18) -0.0012(18) 0.0058(19) C9 0.032(3) 0.025(2) 0.023(3) 0.005(2) 0.012(2) 0.015(2) C10 0.041(3) 0.045(3) 0.030(3) 0.012(2) 0.015(2) 0.025(2) C11 0.047(3) 0.038(3) 0.032(3) 0.008(2) 0.017(2) 0.028(2) C12 0.024(2) 0.027(2) 0.026(3) 0.006(2) 0.010(2) 0.010(2) C13 0.039(3) 0.041(3) 0.042(3) 0.010(3) 0.012(2) 0.024(2) C14 0.035(3) 0.038(3) 0.050(3) 0.004(3) 0.021(3) 0.009(2) C15 0.025(2) 0.020(2) 0.023(2) 0.0112(19) 0.011(2) 0.0112(19) C16 0.029(2) 0.020(2) 0.022(2) 0.0105(19) 0.013(2) 0.012(2) C17 0.034(3) 0.020(2) 0.034(3) 0.010(2) 0.011(2) 0.009(2) C18 0.044(3) 0.019(2) 0.037(3) 0.008(2) 0.012(2) 0.016(2) C19 0.046(3) 0.032(3) 0.044(3) 0.022(2) 0.022(3) 0.027(2) C20 0.031(3) 0.033(3) 0.032(3) 0.021(2) 0.021(2) 0.020(2) C21 0.025(2) 0.022(2) 0.034(3) 0.012(2) 0.009(2) 0.010(2) C22 0.039(3) 0.047(3) 0.058(4) 0.023(3) 0.023(3) 0.026(3) C23 0.035(3) 0.044(3) 0.070(4) 0.018(3) 0.005(3) 0.021(3) C24 0.027(3) 0.039(3) 0.065(4) 0.030(3) 0.017(3) 0.018(2) C25 0.035(3) 0.049(3) 0.063(4) 0.025(3) -0.005(3) 0.016(3) C26 0.046(3) 0.079(5) 0.127(6) 0.068(4) 0.048(4) 0.044(3) C27 0.032(3) 0.027(3) 0.034(3) 0.013(2) 0.014(2) 0.019(2) C28 0.043(3) 0.038(3) 0.054(4) 0.019(3) 0.029(3) 0.021(3) C29 0.037(3) 0.029(3) 0.034(3) 0.011(2) 0.014(2) 0.022(2) C30 0.033(3) 0.036(3) 0.047(3) 0.019(3) 0.004(2) 0.003(2) C31 0.027(3) 0.038(3) 0.033(3) 0.007(2) 0.008(2) 0.018(2) C32 0.036(3) 0.059(4) 0.049(3) 0.004(3) 0.005(3) 0.034(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 Pd1 P1 2.3038(12) 2_666 ? Pd1 P1 2.3038(12) . ? Pd1 Ga1 2.4514(8) . ? Pd1 Ga1 2.4514(8) 2_666 ? Ga1 N1 1.903(3) . ? Ga1 N2 1.905(3) . ? P1 C29 1.816(5) . ? P1 C27 1.820(5) . ? P1 C31 1.837(4) . ? N1 C1 1.406(5) . ? N1 C3 1.436(5) . ? N2 C2 1.401(5) . ? N2 C15 1.430(5) . ? C1 C2 1.332(6) . ? C3 C4 1.414(6) . ? C3 C8 1.417(6) . ? C4 C5 1.400(6) . ? C4 C9 1.517(6) . ? C5 C6 1.371(6) . ? C6 C7 1.383(6) . ? C7 C8 1.392(6) . ? C8 C12 1.515(6) . ? C9 C11 1.526(6) . ? C9 C10 1.531(6) . ? C12 C14 1.527(6) . ? C12 C13 1.533(6) . ? C15 C20 1.405(6) . ? C15 C16 1.414(6) . ? C16 C17 1.392(6) . ? C16 C21 1.517(6) . ? C17 C18 1.384(6) . ? C18 C19 1.380(6) . ? C19 C20 1.400(6) . ? C20 C24 1.529(6) . ? C21 C23 1.520(6) . ? C21 C22 1.533(6) . ? C24 C26 1.530(7) . ? C24 C25 1.534(7) . ? C27 C28 1.522(6) . ? C29 C30 1.512(6) . ? C31 C32 1.543(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 P1 180.000(1) 2_666 . ? P1 Pd1 Ga1 89.17(4) 2_666 . ? P1 Pd1 Ga1 90.83(4) . . ? P1 Pd1 Ga1 90.83(4) 2_666 2_666 ? P1 Pd1 Ga1 89.17(4) . 2_666 ? Ga1 Pd1 Ga1 180.0 . 2_666 ? N1 Ga1 N2 86.57(14) . . ? N1 Ga1 Pd1 135.27(10) . . ? N2 Ga1 Pd1 137.79(10) . . ? C29 P1 C27 100.6(2) . . ? C29 P1 C31 103.9(2) . . ? C27 P1 C31 102.4(2) . . ? C29 P1 Pd1 113.30(15) . . ? C27 P1 Pd1 120.63(15) . . ? C31 P1 Pd1 113.89(15) . . ? C1 N1 C3 117.4(3) . . ? C1 N1 Ga1 109.6(3) . . ? C3 N1 Ga1 132.9(3) . . ? C2 N2 C15 117.7(3) . . ? C2 N2 Ga1 109.7(3) . . ? C15 N2 Ga1 130.9(3) . . ? C2 C1 N1 117.0(4) . . ? C1 C2 N2 117.1(4) . . ? C4 C3 C8 120.4(4) . . ? C4 C3 N1 120.5(4) . . ? C8 C3 N1 119.1(4) . . ? C5 C4 C3 118.2(4) . . ? C5 C4 C9 118.6(4) . . ? C3 C4 C9 123.2(4) . . ? C6 C5 C4 121.6(4) . . ? C5 C6 C7 120.0(4) . . ? C6 C7 C8 121.3(4) . . ? C7 C8 C3 118.4(4) . . ? C7 C8 C12 121.0(4) . . ? C3 C8 C12 120.6(4) . . ? C4 C9 C11 112.6(4) . . ? C4 C9 C10 111.6(4) . . ? C11 C9 C10 108.4(4) . . ? C8 C12 C14 114.5(4) . . ? C8 C12 C13 110.2(4) . . ? C14 C12 C13 109.2(4) . . ? C20 C15 C16 120.5(4) . . ? C20 C15 N2 120.6(4) . . ? C16 C15 N2 118.9(4) . . ? C17 C16 C15 118.6(4) . . ? C17 C16 C21 120.7(4) . . ? C15 C16 C21 120.7(4) . . ? C18 C17 C16 121.3(4) . . ? C19 C18 C17 119.7(4) . . ? C18 C19 C20 121.3(4) . . ? C19 C20 C15 118.6(4) . . ? C19 C20 C24 119.2(4) . . ? C15 C20 C24 122.3(4) . . ? C16 C21 C23 114.4(4) . . ? C16 C21 C22 110.5(4) . . ? C23 C21 C22 109.4(4) . . ? C20 C24 C26 112.2(5) . . ? C20 C24 C25 111.0(4) . . ? C26 C24 C25 109.5(4) . . ? C28 C27 P1 116.3(3) . . ? C30 C29 P1 114.5(3) . . ? C32 C31 P1 115.9(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.512 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.092 # Attachment 'compound9.CIF' data_compound9 _database_code_depnum_ccdc_archive 'CCDC 664049' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H66 Cl Ga N2 P2 Pd' _chemical_formula_weight 824.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.731(3) _cell_length_b 19.200(4) _cell_length_c 16.947(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.90(3) _cell_angle_gamma 90.00 _cell_volume 4103.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 1.265 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_T_max 0.952 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15565 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.1057 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 26.50 _reflns_number_total 8447 _reflns_number_gt 5418 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+0.0109P] 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 8447 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1001 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Pd1 Pd 0.72664(2) 0.007471(14) 0.208902(18) 0.01999(10) Uani 1 1 d . . . Ga1 Ga 0.67458(3) 0.11428(2) 0.25982(3) 0.01937(12) Uani 1 1 d . . . Cl1 Cl 0.77295(9) -0.10118(5) 0.15279(7) 0.0370(3) Uani 1 1 d . . . P1 P 0.85000(8) 0.06826(5) 0.14744(6) 0.0233(3) Uani 1 1 d . . . P2 P 0.61156(9) -0.05450(5) 0.27721(6) 0.0239(3) Uani 1 1 d . . . N1 N 0.7432(2) 0.18605(15) 0.32391(19) 0.0219(8) Uani 1 1 d . . . N2 N 0.5481(2) 0.16777(14) 0.25118(18) 0.0178(7) Uani 1 1 d . . . C1 C 0.6694(3) 0.2381(2) 0.3321(3) 0.0274(11) Uani 1 1 d . . . H1 H 0.6885 0.2788 0.3626 0.033 Uiso 1 1 calc R . . C2 C 0.5713(3) 0.22867(19) 0.2956(2) 0.0257(10) Uani 1 1 d . . . H2 H 0.5179 0.2626 0.2996 0.031 Uiso 1 1 calc R . . C3 C 0.8498(3) 0.19296(19) 0.3641(2) 0.0215(10) Uani 1 1 d . . . C4 C 0.8860(3) 0.1462(2) 0.4259(2) 0.0240(10) Uani 1 1 d . . . C5 C 0.9885(3) 0.1539(2) 0.4634(2) 0.0278(10) Uani 1 1 d . . . H5 H 1.0143 0.1227 0.5051 0.033 Uiso 1 1 calc R . . C6 C 1.0548(3) 0.2055(2) 0.4424(3) 0.0323(11) Uani 1 1 d . . . H6 H 1.1255 0.2090 0.4686 0.039 Uiso 1 1 calc R . . C7 C 1.0176(3) 0.2521(2) 0.3831(2) 0.0299(11) Uani 1 1 d . . . H7 H 1.0624 0.2887 0.3702 0.036 Uiso 1 1 calc R . . C8 C 0.9158(3) 0.24651(19) 0.3420(2) 0.0235(10) Uani 1 1 d . . . C9 C 0.8098(3) 0.0934(2) 0.4539(3) 0.0319(11) Uani 1 1 d . . . H9 H 0.7679 0.0727 0.4052 0.038 Uiso 1 1 calc R . . C10 C 0.8641(4) 0.0342(2) 0.5018(3) 0.0529(14) Uani 1 1 d . . . H10A H 0.9161 0.0125 0.4719 0.079 Uiso 1 1 calc R . . H10B H 0.8112 -0.0006 0.5120 0.079 Uiso 1 1 calc R . . H10C H 0.9002 0.0520 0.5525 0.079 Uiso 1 1 calc R . . C11 C 0.7324(4) 0.1293(3) 0.5001(3) 0.0603(16) Uani 1 1 d . . . H11A H 0.7706 0.1489 0.5492 0.090 Uiso 1 1 calc R . . H11B H 0.6799 0.0955 0.5135 0.090 Uiso 1 1 calc R . . H11C H 0.6963 0.1667 0.4677 0.090 Uiso 1 1 calc R . . C12 C 0.8801(3) 0.2982(2) 0.2759(2) 0.0305(11) Uani 1 1 d . . . H12 H 0.8133 0.2800 0.2447 0.037 Uiso 1 1 calc R . . C13 C 0.9632(4) 0.3061(2) 0.2186(2) 0.0415(13) Uani 1 1 d . . . H13A H 1.0250 0.3311 0.2455 0.062 Uiso 1 1 calc R . . H13B H 0.9324 0.3323 0.1714 0.062 Uiso 1 1 calc R . . H13C H 0.9850 0.2599 0.2024 0.062 Uiso 1 1 calc R . . C14 C 0.8562(4) 0.3698(2) 0.3086(3) 0.0451(13) Uani 1 1 d . . . H14A H 0.8004 0.3655 0.3427 0.068 Uiso 1 1 calc R . . H14B H 0.8325 0.4013 0.2642 0.068 Uiso 1 1 calc R . . H14C H 0.9206 0.3886 0.3397 0.068 Uiso 1 1 calc R . . C15 C 0.4441(3) 0.16022(18) 0.2107(2) 0.0206(9) Uani 1 1 d . . . C16 C 0.3564(3) 0.15841(19) 0.2538(2) 0.0251(10) Uani 1 1 d . . . C17 C 0.2550(3) 0.1583(2) 0.2115(3) 0.0352(12) Uani 1 1 d . . . H17 H 0.1956 0.1590 0.2399 0.042 Uiso 1 1 calc R . . C18 C 0.2382(3) 0.1571(2) 0.1296(3) 0.0394(12) Uani 1 1 d . . . H18 H 0.1681 0.1570 0.1019 0.047 Uiso 1 1 calc R . . C19 C 0.3250(3) 0.1560(2) 0.0877(3) 0.0311(11) Uani 1 1 d . . . H19 H 0.3134 0.1542 0.0311 0.037 Uiso 1 1 calc R . . C20 C 0.4269(3) 0.15761(19) 0.1268(3) 0.0239(10) Uani 1 1 d . . . C21 C 0.3679(3) 0.1545(2) 0.3440(2) 0.0312(11) Uani 1 1 d . . . H21 H 0.4449 0.1494 0.3650 0.037 Uiso 1 1 calc R . . C22 C 0.3265(3) 0.2215(2) 0.3792(2) 0.0379(12) Uani 1 1 d . . . H22A H 0.3670 0.2616 0.3641 0.057 Uiso 1 1 calc R . . H22B H 0.3347 0.2178 0.4374 0.057 Uiso 1 1 calc R . . H22C H 0.2513 0.2277 0.3585 0.057 Uiso 1 1 calc R . . C23 C 0.3086(4) 0.0925(2) 0.3721(3) 0.0436(13) Uani 1 1 d . . . H23A H 0.2320 0.1005 0.3598 0.065 Uiso 1 1 calc R . . H23B H 0.3277 0.0868 0.4297 0.065 Uiso 1 1 calc R . . H23C H 0.3277 0.0503 0.3449 0.065 Uiso 1 1 calc R . . C24 C 0.5218(3) 0.1607(2) 0.0799(2) 0.0271(10) Uani 1 1 d . . . H24 H 0.5823 0.1361 0.1123 0.032 Uiso 1 1 calc R . . C25 C 0.5551(4) 0.2364(2) 0.0714(3) 0.0447(13) Uani 1 1 d . . . H25A H 0.4965 0.2624 0.0414 0.067 Uiso 1 1 calc R . . H25B H 0.6171 0.2382 0.0431 0.067 Uiso 1 1 calc R . . H25C H 0.5730 0.2571 0.1244 0.067 Uiso 1 1 calc R . . C26 C 0.5013(4) 0.1244(2) -0.0006(2) 0.0429(12) Uani 1 1 d . . . H26A H 0.4793 0.0762 0.0069 0.064 Uiso 1 1 calc R . . H26B H 0.5663 0.1246 -0.0256 0.064 Uiso 1 1 calc R . . H26C H 0.4449 0.1489 -0.0350 0.064 Uiso 1 1 calc R . . C27 C 0.9678(3) 0.0847(2) 0.2180(2) 0.0318(11) Uani 1 1 d . . . H27A H 1.0283 0.0931 0.1883 0.038 Uiso 1 1 calc R . . H27B H 0.9568 0.1276 0.2483 0.038 Uiso 1 1 calc R . . C28 C 0.9958(4) 0.0251(2) 0.2765(3) 0.0477(13) Uani 1 1 d . . . H28A H 0.9396 0.0197 0.3102 0.071 Uiso 1 1 calc R . . H28B H 1.0631 0.0354 0.3100 0.071 Uiso 1 1 calc R . . H28C H 1.0028 -0.0182 0.2470 0.071 Uiso 1 1 calc R . . C29 C 0.8166(3) 0.1528(2) 0.1013(2) 0.0339(11) Uani 1 1 d . . . H29A H 0.7481 0.1483 0.0661 0.041 Uiso 1 1 calc R . . H29B H 0.8059 0.1864 0.1439 0.041 Uiso 1 1 calc R . . C30 C 0.8979(4) 0.1835(2) 0.0527(3) 0.0404(13) Uani 1 1 d . . . H30A H 0.9665 0.1878 0.0865 0.061 Uiso 1 1 calc R . . H30B H 0.8741 0.2296 0.0328 0.061 Uiso 1 1 calc R . . H30C H 0.9052 0.1527 0.0076 0.061 Uiso 1 1 calc R . . C31 C 0.8968(3) 0.0196(2) 0.0677(2) 0.0330(11) Uani 1 1 d . . . H31A H 0.9583 0.0441 0.0508 0.040 Uiso 1 1 calc R . . H31B H 0.9211 -0.0268 0.0880 0.040 Uiso 1 1 calc R . . C32 C 0.8122(4) 0.0104(2) -0.0041(3) 0.0457(13) Uani 1 1 d . . . H32A H 0.7510 -0.0141 0.0121 0.068 Uiso 1 1 calc R . . H32B H 0.8412 -0.0170 -0.0449 0.068 Uiso 1 1 calc R . . H32C H 0.7898 0.0561 -0.0258 0.068 Uiso 1 1 calc R . . C33 C 0.6683(3) -0.1369(2) 0.3164(3) 0.0326(11) Uani 1 1 d . . . H33A H 0.6150 -0.1617 0.3434 0.039 Uiso 1 1 calc R . . H33B H 0.6835 -0.1663 0.2713 0.039 Uiso 1 1 calc R . . C34 C 0.7691(4) -0.1290(2) 0.3745(3) 0.0521(14) Uani 1 1 d . . . H34A H 0.8194 -0.0997 0.3506 0.078 Uiso 1 1 calc R . . H34B H 0.8005 -0.1750 0.3868 0.078 Uiso 1 1 calc R . . H34C H 0.7526 -0.1072 0.4236 0.078 Uiso 1 1 calc R . . C35 C 0.5604(3) -0.0153(2) 0.3630(2) 0.0339(11) Uani 1 1 d . . . H35A H 0.6216 -0.0011 0.4023 0.041 Uiso 1 1 calc R . . H35B H 0.5210 0.0275 0.3448 0.041 Uiso 1 1 calc R . . C36 C 0.4883(4) -0.0610(2) 0.4053(3) 0.0427(13) Uani 1 1 d . . . H36A H 0.4261 -0.0745 0.3678 0.064 Uiso 1 1 calc R . . H36B H 0.4653 -0.0351 0.4498 0.064 Uiso 1 1 calc R . . H36C H 0.5269 -0.1029 0.4257 0.064 Uiso 1 1 calc R . . C37 C 0.4953(3) -0.0821(2) 0.2110(2) 0.0308(11) Uani 1 1 d . . . H37A H 0.5181 -0.1114 0.1684 0.037 Uiso 1 1 calc R . . H37B H 0.4508 -0.1113 0.2413 0.037 Uiso 1 1 calc R . . C38 C 0.4287(4) -0.0223(2) 0.1730(3) 0.0424(12) Uani 1 1 d . . . H38A H 0.4019 0.0053 0.2146 0.064 Uiso 1 1 calc R . . H38B H 0.3688 -0.0409 0.1365 0.064 Uiso 1 1 calc R . . H38C H 0.4723 0.0073 0.1433 0.064 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 0.01768(17) 0.01896(17) 0.02396(18) -0.00019(14) 0.00512(14) -0.00005(14) Ga1 0.0159(2) 0.0187(2) 0.0238(3) -0.00156(19) 0.0035(2) -0.00118(19) Cl1 0.0453(8) 0.0230(6) 0.0465(7) -0.0046(5) 0.0201(6) 0.0017(5) P1 0.0184(6) 0.0251(6) 0.0272(7) 0.0001(5) 0.0067(5) -0.0012(5) P2 0.0259(7) 0.0213(6) 0.0253(7) 0.0011(5) 0.0069(5) -0.0041(5) N1 0.0163(19) 0.0185(17) 0.030(2) -0.0058(15) -0.0014(16) 0.0020(15) N2 0.0149(18) 0.0150(17) 0.0228(19) -0.0020(15) 0.0000(15) 0.0018(14) C1 0.021(3) 0.022(2) 0.040(3) -0.011(2) 0.008(2) -0.0039(19) C2 0.023(3) 0.020(2) 0.035(3) -0.004(2) 0.006(2) 0.0046(19) C3 0.015(2) 0.020(2) 0.030(3) -0.0079(19) 0.001(2) -0.0007(17) C4 0.020(2) 0.023(2) 0.030(3) -0.002(2) 0.009(2) -0.0005(19) C5 0.022(3) 0.029(2) 0.032(3) 0.000(2) 0.001(2) 0.003(2) C6 0.021(3) 0.042(3) 0.034(3) -0.003(2) 0.007(2) -0.002(2) C7 0.025(3) 0.032(2) 0.034(3) -0.004(2) 0.010(2) -0.008(2) C8 0.022(2) 0.025(2) 0.025(2) -0.0048(19) 0.006(2) -0.0024(19) C9 0.031(3) 0.034(3) 0.030(3) 0.003(2) 0.000(2) -0.006(2) C10 0.050(4) 0.047(3) 0.059(4) 0.013(3) 0.000(3) -0.012(3) C11 0.059(4) 0.064(4) 0.066(4) -0.007(3) 0.036(3) -0.019(3) C12 0.023(3) 0.037(3) 0.030(3) 0.004(2) -0.001(2) -0.014(2) C13 0.051(3) 0.046(3) 0.027(3) 0.006(2) 0.003(2) -0.017(2) C14 0.055(4) 0.025(2) 0.056(3) 0.010(2) 0.010(3) -0.003(2) C15 0.014(2) 0.014(2) 0.033(3) -0.0033(19) -0.001(2) -0.0010(17) C16 0.021(2) 0.022(2) 0.031(3) -0.0012(19) 0.000(2) -0.0025(19) C17 0.022(3) 0.041(3) 0.043(3) -0.010(2) 0.004(2) -0.002(2) C18 0.019(3) 0.044(3) 0.052(3) -0.008(3) -0.006(2) -0.002(2) C19 0.035(3) 0.030(2) 0.027(3) -0.004(2) -0.001(2) 0.000(2) C20 0.021(2) 0.015(2) 0.034(3) -0.003(2) -0.002(2) -0.0002(18) C21 0.025(3) 0.038(3) 0.031(3) 0.001(2) 0.005(2) -0.005(2) C22 0.034(3) 0.046(3) 0.034(3) -0.011(2) 0.007(2) 0.000(2) C23 0.041(3) 0.050(3) 0.041(3) 0.001(2) 0.011(3) -0.007(3) C24 0.025(3) 0.029(2) 0.027(3) -0.007(2) 0.003(2) 0.003(2) C25 0.035(3) 0.042(3) 0.060(4) 0.016(3) 0.016(3) 0.006(2) C26 0.042(3) 0.058(3) 0.027(3) -0.001(2) 0.000(2) 0.009(3) C27 0.022(3) 0.038(3) 0.036(3) -0.002(2) 0.010(2) -0.001(2) C28 0.037(3) 0.058(3) 0.044(3) -0.002(3) -0.009(3) 0.008(3) C29 0.029(3) 0.038(3) 0.037(3) 0.008(2) 0.013(2) -0.002(2) C30 0.044(3) 0.037(3) 0.043(3) 0.008(2) 0.015(3) -0.002(2) C31 0.030(3) 0.034(3) 0.037(3) -0.007(2) 0.012(2) -0.005(2) C32 0.059(4) 0.049(3) 0.030(3) -0.006(2) 0.007(3) -0.016(3) C33 0.041(3) 0.028(2) 0.029(3) 0.005(2) 0.003(2) 0.000(2) C34 0.060(4) 0.048(3) 0.044(3) 0.011(3) -0.009(3) 0.013(3) C35 0.037(3) 0.032(2) 0.036(3) -0.003(2) 0.013(2) -0.010(2) C36 0.058(3) 0.036(3) 0.040(3) -0.004(2) 0.028(3) -0.014(2) C37 0.034(3) 0.028(2) 0.030(3) -0.004(2) 0.004(2) -0.005(2) C38 0.032(3) 0.043(3) 0.047(3) -0.006(2) -0.011(2) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.3160(11) . ? Pd1 P2 2.3171(11) . ? Pd1 Ga1 2.3551(6) . ? Pd1 Cl1 2.3996(11) . ? Ga1 N1 1.892(3) . ? Ga1 N2 1.898(3) . ? P1 C31 1.809(4) . ? P1 C27 1.812(4) . ? P1 C29 1.827(4) . ? P2 C37 1.809(4) . ? P2 C33 1.827(4) . ? P2 C35 1.835(4) . ? N1 C1 1.391(4) . ? N1 C3 1.438(5) . ? N2 C2 1.400(5) . ? N2 C15 1.413(5) . ? C1 C2 1.328(5) . ? C3 C4 1.407(5) . ? C3 C8 1.411(5) . ? C4 C5 1.379(5) . ? C4 C9 1.524(5) . ? C5 C6 1.379(5) . ? C6 C7 1.380(5) . ? C7 C8 1.388(5) . ? C8 C12 1.519(5) . ? C9 C11 1.508(6) . ? C9 C10 1.508(6) . ? C12 C14 1.528(6) . ? C12 C13 1.538(5) . ? C15 C20 1.409(5) . ? C15 C16 1.416(5) . ? C16 C17 1.388(5) . ? C16 C21 1.518(5) . ? C17 C18 1.375(6) . ? C18 C19 1.393(5) . ? C19 C20 1.374(5) . ? C20 C24 1.536(5) . ? C21 C23 1.521(5) . ? C21 C22 1.541(5) . ? C24 C26 1.524(5) . ? C24 C25 1.524(5) . ? C27 C28 1.525(5) . ? C29 C30 1.527(5) . ? C31 C32 1.521(6) . ? C33 C34 1.513(6) . ? C35 C36 1.519(5) . ? C37 C38 1.517(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 P2 176.35(4) . . ? P1 Pd1 Ga1 88.19(3) . . ? P2 Pd1 Ga1 92.01(3) . . ? P1 Pd1 Cl1 92.35(4) . . ? P2 Pd1 Cl1 87.61(4) . . ? Ga1 Pd1 Cl1 177.52(4) . . ? N1 Ga1 N2 88.28(13) . . ? N1 Ga1 Pd1 135.52(10) . . ? N2 Ga1 Pd1 136.16(10) . . ? C31 P1 C27 104.78(19) . . ? C31 P1 C29 102.75(19) . . ? C27 P1 C29 104.5(2) . . ? C31 P1 Pd1 112.89(14) . . ? C27 P1 Pd1 110.00(13) . . ? C29 P1 Pd1 120.51(13) . . ? C37 P2 C33 102.8(2) . . ? C37 P2 C35 105.21(19) . . ? C33 P2 C35 103.46(19) . . ? C37 P2 Pd1 111.11(13) . . ? C33 P2 Pd1 112.39(14) . . ? C35 P2 Pd1 120.22(13) . . ? C1 N1 C3 119.5(3) . . ? C1 N1 Ga1 108.4(3) . . ? C3 N1 Ga1 132.1(2) . . ? C2 N2 C15 117.5(3) . . ? C2 N2 Ga1 107.2(2) . . ? C15 N2 Ga1 135.3(2) . . ? C2 C1 N1 117.4(4) . . ? C1 C2 N2 118.7(4) . . ? C4 C3 C8 121.0(4) . . ? C4 C3 N1 119.0(3) . . ? C8 C3 N1 120.0(4) . . ? C5 C4 C3 117.8(4) . . ? C5 C4 C9 122.0(4) . . ? C3 C4 C9 119.9(4) . . ? C4 C5 C6 122.1(4) . . ? C5 C6 C7 119.5(4) . . ? C6 C7 C8 121.2(4) . . ? C7 C8 C3 118.2(4) . . ? C7 C8 C12 118.9(3) . . ? C3 C8 C12 122.8(4) . . ? C11 C9 C10 110.4(4) . . ? C11 C9 C4 110.3(3) . . ? C10 C9 C4 113.9(4) . . ? C8 C12 C14 112.0(3) . . ? C8 C12 C13 111.6(3) . . ? C14 C12 C13 109.1(3) . . ? C20 C15 N2 120.0(3) . . ? C20 C15 C16 119.7(4) . . ? N2 C15 C16 120.3(4) . . ? C17 C16 C15 118.5(4) . . ? C17 C16 C21 118.3(4) . . ? C15 C16 C21 123.2(4) . . ? C18 C17 C16 121.7(4) . . ? C17 C18 C19 119.5(4) . . ? C20 C19 C18 121.0(4) . . ? C19 C20 C15 119.6(4) . . ? C19 C20 C24 120.6(4) . . ? C15 C20 C24 119.7(4) . . ? C16 C21 C23 111.7(3) . . ? C16 C21 C22 111.0(3) . . ? C23 C21 C22 108.7(3) . . ? C26 C24 C25 111.6(4) . . ? C26 C24 C20 113.2(4) . . ? C25 C24 C20 109.5(3) . . ? C28 C27 P1 113.4(3) . . ? C30 C29 P1 116.0(3) . . ? C32 C31 P1 112.9(3) . . ? C34 C33 P2 114.0(3) . . ? C36 C35 P2 116.2(3) . . ? C38 C37 P2 113.8(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.483 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.110 # Attachment 'compound10.CIF' data_compound10 _database_code_depnum_ccdc_archive 'CCDC 664050' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H66 Cl Ga N2 Ni P2' _chemical_formula_weight 776.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.626(3) _cell_length_b 19.042(4) _cell_length_c 17.100(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.89(3) _cell_angle_gamma 90.00 _cell_volume 4072.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 1.295 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.525 _exptl_absorpt_correction_T_max 0.781 _exptl_absorpt_process_details 'Sortav Blessing(1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14205 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 26.50 _reflns_number_total 8395 _reflns_number_gt 6668 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+2.0740P] 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 8395 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.673312(17) 0.114000(12) 0.258035(13) 0.01546(7) Uani 1 1 d . . . Ni1 Ni 0.72381(2) 0.009098(14) 0.209390(16) 0.01704(8) Uani 1 1 d . . . Cl1 Cl 0.76411(5) -0.09231(3) 0.15744(4) 0.03410(15) Uani 1 1 d . . . P1 P 0.61380(5) -0.04909(3) 0.27604(3) 0.02045(14) Uani 1 1 d . . . N1 N 0.74168(14) 0.18683(9) 0.32213(10) 0.0188(4) Uani 1 1 d . . . C1 C 0.66728(18) 0.23988(12) 0.32910(14) 0.0236(5) Uani 1 1 d . . . H1 H 0.6868 0.2811 0.3588 0.028 Uiso 1 1 calc R . . P2 P 0.84269(4) 0.06711(3) 0.15075(3) 0.02036(13) Uani 1 1 d . . . N2 N 0.54620(13) 0.16881(9) 0.24902(10) 0.0174(4) Uani 1 1 d . . . C2 C 0.56773(17) 0.23067(11) 0.29255(13) 0.0216(5) Uani 1 1 d . . . H2 H 0.5137 0.2648 0.2960 0.026 Uiso 1 1 calc R . . C3 C 0.84765(16) 0.19522(11) 0.36269(12) 0.0181(5) Uani 1 1 d . . . C4 C 0.88393(17) 0.14861(12) 0.42543(12) 0.0190(5) Uani 1 1 d . . . C5 C 0.98793(17) 0.15672(12) 0.46358(13) 0.0237(5) Uani 1 1 d . . . H5 H 1.0146 0.1249 0.5044 0.028 Uiso 1 1 calc R . . C6 C 1.05312(18) 0.20995(13) 0.44350(14) 0.0272(6) Uani 1 1 d . . . H6 H 1.1235 0.2148 0.4708 0.033 Uiso 1 1 calc R . . C7 C 1.01626(17) 0.25612(13) 0.38384(13) 0.0251(5) Uani 1 1 d . . . H7 H 1.0614 0.2931 0.3711 0.030 Uiso 1 1 calc R . . C8 C 0.91379(17) 0.24949(12) 0.34171(13) 0.0203(5) Uani 1 1 d . . . C9 C 0.80891(18) 0.09476(12) 0.45307(14) 0.0245(5) Uani 1 1 d . . . H9 H 0.7698 0.0720 0.4048 0.029 Uiso 1 1 calc R . . C10 C 0.8635(2) 0.03648(14) 0.50469(16) 0.0404(7) Uani 1 1 d . . . H10A H 0.9152 0.0123 0.4763 0.061 Uiso 1 1 calc R . . H10B H 0.8097 0.0028 0.5175 0.061 Uiso 1 1 calc R . . H10C H 0.9007 0.0567 0.5536 0.061 Uiso 1 1 calc R . . C11 C 0.7254(2) 0.13150(15) 0.49542(16) 0.0399(7) Uani 1 1 d . . . H11A H 0.7605 0.1529 0.5443 0.060 Uiso 1 1 calc R . . H11B H 0.6725 0.0971 0.5080 0.060 Uiso 1 1 calc R . . H11C H 0.6895 0.1680 0.4611 0.060 Uiso 1 1 calc R . . C12 C 0.87883(19) 0.30114(13) 0.27525(14) 0.0285(6) Uani 1 1 d . . . H12 H 0.8118 0.2827 0.2441 0.034 Uiso 1 1 calc R . . C13 C 0.9634(2) 0.30821(15) 0.21926(15) 0.0408(7) Uani 1 1 d . . . H13A H 1.0268 0.3318 0.2468 0.061 Uiso 1 1 calc R . . H13B H 0.9341 0.3359 0.1730 0.061 Uiso 1 1 calc R . . H13C H 0.9832 0.2614 0.2022 0.061 Uiso 1 1 calc R . . C14 C 0.8542(2) 0.37355(14) 0.30758(17) 0.0423(7) Uani 1 1 d . . . H14A H 0.7985 0.3689 0.3420 0.063 Uiso 1 1 calc R . . H14B H 0.8291 0.4050 0.2636 0.063 Uiso 1 1 calc R . . H14C H 0.9191 0.3930 0.3379 0.063 Uiso 1 1 calc R . . C15 C 0.44050(17) 0.16173(11) 0.20848(13) 0.0183(5) Uani 1 1 d . . . C16 C 0.35228(17) 0.16025(12) 0.25085(13) 0.0222(5) Uani 1 1 d . . . C17 C 0.24938(18) 0.16012(13) 0.20863(15) 0.0322(6) Uani 1 1 d . . . H17 H 0.1893 0.1611 0.2365 0.039 Uiso 1 1 calc R . . C18 C 0.2335(2) 0.15863(14) 0.12737(16) 0.0374(7) Uani 1 1 d . . . H18 H 0.1629 0.1588 0.0997 0.045 Uiso 1 1 calc R . . C19 C 0.32029(19) 0.15689(13) 0.08572(15) 0.0300(6) Uani 1 1 d . . . H19 H 0.3086 0.1544 0.0297 0.036 Uiso 1 1 calc R . . C20 C 0.42381(18) 0.15881(12) 0.12493(13) 0.0216(5) Uani 1 1 d . . . C21 C 0.36354(19) 0.15775(13) 0.34053(14) 0.0268(5) Uani 1 1 d . . . H21 H 0.4411 0.1519 0.3612 0.032 Uiso 1 1 calc R . . C22 C 0.3026(2) 0.09549(14) 0.36934(17) 0.0410(7) Uani 1 1 d . . . H22A H 0.3213 0.0906 0.4266 0.062 Uiso 1 1 calc R . . H22B H 0.3221 0.0524 0.3433 0.062 Uiso 1 1 calc R . . H22C H 0.2256 0.1036 0.3565 0.062 Uiso 1 1 calc R . . C23 C 0.3245(2) 0.22576(14) 0.37472(15) 0.0349(6) Uani 1 1 d . . . H23A H 0.2488 0.2328 0.3548 0.052 Uiso 1 1 calc R . . H23B H 0.3662 0.2654 0.3588 0.052 Uiso 1 1 calc R . . H23C H 0.3336 0.2226 0.4324 0.052 Uiso 1 1 calc R . . C24 C 0.51761(19) 0.16166(12) 0.07869(13) 0.0251(5) Uani 1 1 d . . . H24 H 0.5784 0.1368 0.1108 0.030 Uiso 1 1 calc R . . C25 C 0.4985(2) 0.12509(16) -0.00139(15) 0.0402(7) Uani 1 1 d . . . H25A H 0.4760 0.0765 0.0057 0.060 Uiso 1 1 calc R . . H25B H 0.5647 0.1253 -0.0253 0.060 Uiso 1 1 calc R . . H25C H 0.4423 0.1500 -0.0360 0.060 Uiso 1 1 calc R . . C26 C 0.5524(2) 0.23788(14) 0.06999(17) 0.0399(7) Uani 1 1 d . . . H26A H 0.4933 0.2646 0.0410 0.060 Uiso 1 1 calc R . . H26B H 0.6141 0.2392 0.0409 0.060 Uiso 1 1 calc R . . H26C H 0.5722 0.2586 0.1224 0.060 Uiso 1 1 calc R . . C27 C 0.5567(2) -0.00834(13) 0.35822(14) 0.0295(6) Uani 1 1 d . . . H27A H 0.6164 0.0089 0.3971 0.035 Uiso 1 1 calc R . . H27B H 0.5146 0.0331 0.3375 0.035 Uiso 1 1 calc R . . C28 C 0.4852(2) -0.05471(15) 0.40173(16) 0.0411(7) Uani 1 1 d . . . H28A H 0.4269 -0.0738 0.3639 0.062 Uiso 1 1 calc R . . H28B H 0.4553 -0.0267 0.4415 0.062 Uiso 1 1 calc R . . H28C H 0.5275 -0.0934 0.4277 0.062 Uiso 1 1 calc R . . C29 C 0.49719(18) -0.07922(12) 0.20924(14) 0.0254(5) Uani 1 1 d . . . H29A H 0.5218 -0.1096 0.1683 0.031 Uiso 1 1 calc R . . H29B H 0.4521 -0.1083 0.2395 0.031 Uiso 1 1 calc R . . C30 C 0.4292(2) -0.02040(14) 0.16875(16) 0.0378(7) Uani 1 1 d . . . H30A H 0.4010 0.0085 0.2086 0.057 Uiso 1 1 calc R . . H30B H 0.3696 -0.0405 0.1330 0.057 Uiso 1 1 calc R . . H30C H 0.4730 0.0088 0.1385 0.057 Uiso 1 1 calc R . . C31 C 0.6692(2) -0.13194(13) 0.31817(14) 0.0300(6) Uani 1 1 d . . . H31A H 0.6143 -0.1558 0.3448 0.036 Uiso 1 1 calc R . . H31B H 0.6854 -0.1627 0.2747 0.036 Uiso 1 1 calc R . . C32 C 0.7702(2) -0.12321(15) 0.37714(16) 0.0467(8) Uani 1 1 d . . . H32A H 0.8243 -0.0981 0.3520 0.070 Uiso 1 1 calc R . . H32B H 0.7977 -0.1696 0.3946 0.070 Uiso 1 1 calc R . . H32C H 0.7536 -0.0963 0.4228 0.070 Uiso 1 1 calc R . . C33 C 0.81218(19) 0.15310(13) 0.10509(15) 0.0288(6) Uani 1 1 d . . . H33A H 0.7434 0.1493 0.0697 0.035 Uiso 1 1 calc R . . H33B H 0.8015 0.1869 0.1474 0.035 Uiso 1 1 calc R . . C34 C 0.8951(2) 0.18392(14) 0.05756(16) 0.0365(6) Uani 1 1 d . . . H34A H 0.9650 0.1854 0.0905 0.055 Uiso 1 1 calc R . . H34B H 0.8738 0.2316 0.0405 0.055 Uiso 1 1 calc R . . H34C H 0.8998 0.1545 0.0111 0.055 Uiso 1 1 calc R . . C35 C 0.96203(18) 0.08411(14) 0.22259(14) 0.0297(6) Uani 1 1 d . . . H35A H 1.0242 0.0910 0.1939 0.036 Uiso 1 1 calc R . . H35B H 0.9513 0.1281 0.2513 0.036 Uiso 1 1 calc R . . C36 C 0.9866(2) 0.02465(15) 0.28218(16) 0.0402(7) Uani 1 1 d . . . H36A H 0.9272 0.0196 0.3132 0.060 Uiso 1 1 calc R . . H36B H 1.0524 0.0355 0.3175 0.060 Uiso 1 1 calc R . . H36C H 0.9959 -0.0193 0.2541 0.060 Uiso 1 1 calc R . . C37 C 0.8955(2) 0.01924(14) 0.07168(14) 0.0316(6) Uani 1 1 d . . . H37A H 0.9578 0.0450 0.0567 0.038 Uiso 1 1 calc R . . H37B H 0.9206 -0.0275 0.0915 0.038 Uiso 1 1 calc R . . C38 C 0.8125(2) 0.00986(16) -0.00143(15) 0.0432(7) Uani 1 1 d . . . H38A H 0.7511 -0.0164 0.0128 0.065 Uiso 1 1 calc R . . H38B H 0.8444 -0.0161 -0.0418 0.065 Uiso 1 1 calc R . . H38C H 0.7886 0.0560 -0.0222 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.01434(12) 0.01391(13) 0.01855(13) -0.00050(10) 0.00376(9) -0.00074(10) Ni1 0.01774(15) 0.01373(15) 0.02051(15) -0.00050(11) 0.00568(11) -0.00020(11) Cl1 0.0444(4) 0.0180(3) 0.0444(4) -0.0061(3) 0.0220(3) -0.0004(3) P1 0.0241(3) 0.0167(3) 0.0214(3) -0.0001(2) 0.0060(2) -0.0039(2) N1 0.0153(9) 0.0146(10) 0.0262(10) -0.0036(8) 0.0018(8) 0.0006(8) C1 0.0221(12) 0.0164(12) 0.0325(13) -0.0071(10) 0.0044(10) -0.0017(10) P2 0.0187(3) 0.0203(3) 0.0233(3) 0.0008(2) 0.0075(2) 0.0005(2) N2 0.0150(9) 0.0136(9) 0.0236(10) -0.0015(8) 0.0025(7) 0.0003(8) C2 0.0185(11) 0.0136(12) 0.0330(13) -0.0031(10) 0.0048(10) 0.0019(9) C3 0.0139(10) 0.0184(12) 0.0221(11) -0.0051(9) 0.0022(9) -0.0003(9) C4 0.0186(11) 0.0193(12) 0.0200(11) -0.0034(9) 0.0062(9) -0.0018(9) C5 0.0195(11) 0.0265(13) 0.0246(12) 0.0008(10) 0.0014(10) 0.0041(10) C6 0.0167(11) 0.0380(15) 0.0265(13) -0.0025(11) 0.0015(10) -0.0015(11) C7 0.0181(11) 0.0281(14) 0.0303(13) -0.0048(11) 0.0082(10) -0.0062(10) C8 0.0207(11) 0.0191(12) 0.0215(11) -0.0036(9) 0.0043(9) -0.0016(10) C9 0.0256(12) 0.0230(13) 0.0251(12) 0.0029(10) 0.0046(10) -0.0064(10) C10 0.0504(17) 0.0316(16) 0.0379(16) 0.0090(12) 0.0013(13) -0.0069(13) C11 0.0397(15) 0.0397(17) 0.0455(17) -0.0009(13) 0.0244(13) -0.0094(13) C12 0.0290(13) 0.0261(14) 0.0291(13) 0.0025(11) -0.0006(11) -0.0092(11) C13 0.0478(17) 0.0431(17) 0.0326(15) 0.0037(13) 0.0089(13) -0.0144(14) C14 0.0478(17) 0.0263(15) 0.0530(18) 0.0041(13) 0.0073(14) -0.0043(13) C15 0.0170(11) 0.0130(11) 0.0250(12) -0.0013(9) 0.0029(9) -0.0005(9) C16 0.0184(11) 0.0194(13) 0.0294(13) -0.0056(10) 0.0052(10) -0.0029(10) C17 0.0167(12) 0.0379(16) 0.0426(16) -0.0087(12) 0.0067(11) -0.0029(11) C18 0.0170(12) 0.0457(17) 0.0467(17) -0.0084(14) -0.0054(11) -0.0020(12) C19 0.0253(13) 0.0326(15) 0.0302(13) -0.0053(11) -0.0028(11) -0.0001(11) C20 0.0220(12) 0.0157(12) 0.0270(12) 0.0000(10) 0.0025(10) 0.0006(10) C21 0.0200(12) 0.0291(14) 0.0328(14) -0.0043(11) 0.0090(10) -0.0018(10) C22 0.0408(16) 0.0385(17) 0.0473(17) 0.0009(13) 0.0187(13) -0.0083(13) C23 0.0291(13) 0.0402(16) 0.0375(15) -0.0115(12) 0.0129(11) -0.0002(12) C24 0.0244(12) 0.0275(14) 0.0236(12) 0.0048(10) 0.0041(10) 0.0032(11) C25 0.0411(15) 0.0536(19) 0.0260(13) -0.0022(13) 0.0047(12) 0.0112(14) C26 0.0372(15) 0.0366(16) 0.0480(17) 0.0119(13) 0.0127(13) 0.0003(13) C27 0.0336(14) 0.0287(14) 0.0290(13) -0.0054(11) 0.0149(11) -0.0113(11) C28 0.0528(17) 0.0400(17) 0.0354(15) -0.0049(13) 0.0236(13) -0.0135(14) C29 0.0267(12) 0.0204(13) 0.0291(13) -0.0026(10) 0.0032(10) -0.0046(10) C30 0.0346(15) 0.0303(15) 0.0459(16) -0.0040(13) -0.0042(12) 0.0018(12) C31 0.0376(14) 0.0222(13) 0.0298(13) 0.0050(11) 0.0032(11) -0.0026(11) C32 0.0558(19) 0.0406(18) 0.0386(16) 0.0084(13) -0.0119(14) 0.0042(15) C33 0.0284(13) 0.0251(14) 0.0352(14) 0.0081(11) 0.0125(11) 0.0031(11) C34 0.0398(15) 0.0310(15) 0.0420(16) 0.0115(12) 0.0177(12) -0.0016(12) C35 0.0226(12) 0.0359(15) 0.0312(14) -0.0039(12) 0.0057(10) -0.0062(11) C36 0.0336(15) 0.0435(17) 0.0405(16) -0.0034(13) -0.0061(12) 0.0048(13) C37 0.0317(14) 0.0325(15) 0.0331(14) -0.0049(12) 0.0139(11) -0.0025(12) C38 0.0515(18) 0.0501(19) 0.0284(14) -0.0077(13) 0.0069(13) -0.0124(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N1 1.8999(17) . ? Ga1 N2 1.9029(17) . ? Ga1 Ni1 2.2878(5) . ? Ni1 P1 2.2115(8) . ? Ni1 P2 2.2118(8) . ? Ni1 Cl1 2.2138(7) . ? P1 C29 1.828(2) . ? P1 C31 1.833(2) . ? P1 C27 1.837(2) . ? N1 C1 1.396(3) . ? N1 C3 1.429(3) . ? C1 C2 1.336(3) . ? P2 C37 1.830(2) . ? P2 C33 1.832(2) . ? P2 C35 1.837(2) . ? N2 C2 1.400(3) . ? N2 C15 1.423(3) . ? C3 C8 1.406(3) . ? C3 C4 1.419(3) . ? C4 C5 1.392(3) . ? C4 C9 1.515(3) . ? C5 C6 1.379(3) . ? C6 C7 1.378(3) . ? C7 C8 1.397(3) . ? C8 C12 1.522(3) . ? C9 C10 1.523(3) . ? C9 C11 1.528(3) . ? C12 C14 1.533(4) . ? C12 C13 1.534(4) . ? C15 C16 1.410(3) . ? C15 C20 1.416(3) . ? C16 C17 1.397(3) . ? C16 C21 1.521(3) . ? C17 C18 1.377(4) . ? C18 C19 1.386(4) . ? C19 C20 1.385(3) . ? C20 C24 1.513(3) . ? C21 C23 1.530(3) . ? C21 C22 1.531(3) . ? C24 C25 1.526(3) . ? C24 C26 1.530(3) . ? C27 C28 1.527(3) . ? C29 C30 1.519(3) . ? C31 C32 1.522(3) . ? C33 C34 1.528(3) . ? C35 C36 1.526(4) . ? C37 C38 1.528(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ga1 N2 87.58(8) . . ? N1 Ga1 Ni1 136.04(5) . . ? N2 Ga1 Ni1 136.35(5) . . ? P1 Ni1 P2 175.74(2) . . ? P1 Ni1 Cl1 87.99(3) . . ? P2 Ni1 Cl1 92.64(3) . . ? P1 Ni1 Ga1 91.37(3) . . ? P2 Ni1 Ga1 88.23(3) . . ? Cl1 Ni1 Ga1 176.71(2) . . ? C29 P1 C31 101.93(11) . . ? C29 P1 C27 104.11(11) . . ? C31 P1 C27 103.40(12) . . ? C29 P1 Ni1 110.13(8) . . ? C31 P1 Ni1 113.64(9) . . ? C27 P1 Ni1 121.52(8) . . ? C1 N1 C3 118.29(17) . . ? C1 N1 Ga1 108.65(14) . . ? C3 N1 Ga1 133.05(14) . . ? C2 C1 N1 117.8(2) . . ? C37 P2 C33 101.94(12) . . ? C37 P2 C35 103.50(11) . . ? C33 P2 C35 103.46(12) . . ? C37 P2 Ni1 115.13(9) . . ? C33 P2 Ni1 121.57(8) . . ? C35 P2 Ni1 109.27(8) . . ? C2 N2 C15 116.06(17) . . ? C2 N2 Ga1 108.57(13) . . ? C15 N2 Ga1 135.35(14) . . ? C1 C2 N2 117.4(2) . . ? C8 C3 C4 120.75(19) . . ? C8 C3 N1 120.52(19) . . ? C4 C3 N1 118.72(19) . . ? C5 C4 C3 118.1(2) . . ? C5 C4 C9 121.2(2) . . ? C3 C4 C9 120.56(19) . . ? C6 C5 C4 121.4(2) . . ? C7 C6 C5 120.1(2) . . ? C6 C7 C8 121.2(2) . . ? C7 C8 C3 118.4(2) . . ? C7 C8 C12 118.7(2) . . ? C3 C8 C12 122.96(19) . . ? C4 C9 C10 114.9(2) . . ? C4 C9 C11 109.9(2) . . ? C10 C9 C11 110.2(2) . . ? C8 C12 C14 111.4(2) . . ? C8 C12 C13 111.6(2) . . ? C14 C12 C13 109.8(2) . . ? C16 C15 C20 119.9(2) . . ? C16 C15 N2 120.38(19) . . ? C20 C15 N2 119.65(19) . . ? C17 C16 C15 118.6(2) . . ? C17 C16 C21 118.2(2) . . ? C15 C16 C21 123.2(2) . . ? C18 C17 C16 121.2(2) . . ? C17 C18 C19 120.2(2) . . ? C20 C19 C18 120.7(2) . . ? C19 C20 C15 119.3(2) . . ? C19 C20 C24 120.2(2) . . ? C15 C20 C24 120.5(2) . . ? C16 C21 C23 111.6(2) . . ? C16 C21 C22 111.5(2) . . ? C23 C21 C22 109.3(2) . . ? C20 C24 C25 114.4(2) . . ? C20 C24 C26 109.9(2) . . ? C25 C24 C26 111.0(2) . . ? C28 C27 P1 116.66(18) . . ? C30 C29 P1 114.19(17) . . ? C32 C31 P1 113.97(18) . . ? C34 C33 P2 116.77(17) . . ? C36 C35 P2 112.87(17) . . ? C38 C37 P2 112.61(18) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.357 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.067 # Attachment 'compound11.CIF' data_compound11 _database_code_depnum_ccdc_archive 'CCDC 664051' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H94 Cl Ga N2 O P2 Pt' _chemical_formula_weight 1173.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.893(3) _cell_length_b 21.811(4) _cell_length_c 20.656(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.11(3) _cell_angle_gamma 90.00 _cell_volume 5633(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 3.101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.409 _exptl_absorpt_correction_T_max 0.550 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22427 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 26.50 _reflns_number_total 11617 _reflns_number_gt 9916 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One molecule of diethyl ether was located in the asymmetric unit. The non hydrogen atoms of this molecule were refined isotropically. The largest residual electron density peak (1.450 e-/ang.3) in the final difference map is located close to Pt(1). ; _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^)+(0.0240P)^2^+12.5707P] 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 11617 _refine_ls_number_parameters 562 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0669 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.605679(10) 0.188700(6) 0.438073(6) 0.01300(4) Uani 1 1 d . . . Ga1 Ga 0.76830(3) 0.240094(16) 0.494977(18) 0.01458(8) Uani 1 1 d . . . Cl1 Cl 0.66422(7) 0.11582(4) 0.52452(4) 0.02327(19) Uani 1 1 d . . . P1 P 0.55906(7) 0.25703(4) 0.35767(4) 0.01602(18) Uani 1 1 d . . . P2 P 0.45395(7) 0.13380(4) 0.38809(4) 0.01493(18) Uani 1 1 d . . . O1 O 0.5173(3) 0.46877(16) 0.27053(18) 0.0553(9) Uiso 1 1 d . . . N1 N 0.8092(2) 0.28397(13) 0.57653(14) 0.0172(6) Uani 1 1 d . . . N2 N 0.9158(2) 0.22920(13) 0.49889(14) 0.0172(6) Uani 1 1 d . . . C1 C 0.9208(3) 0.27861(16) 0.60044(17) 0.0190(7) Uani 1 1 d . . . H1 H 0.9568 0.2943 0.6429 0.023 Uiso 1 1 calc R . . C2 C 0.9739(3) 0.25041(15) 0.56074(17) 0.0180(7) Uani 1 1 d . . . H2 H 1.0492 0.2450 0.5744 0.022 Uiso 1 1 calc R . . C3 C 0.7593(3) 0.33244(16) 0.60361(17) 0.0196(7) Uani 1 1 d . . . C4 C 0.6711(3) 0.31994(17) 0.63127(18) 0.0216(8) Uani 1 1 d . . . C5 C 0.6279(3) 0.36808(18) 0.66084(19) 0.0280(9) Uani 1 1 d . . . H5 H 0.5691 0.3601 0.6798 0.034 Uiso 1 1 calc R . . C6 C 0.6683(3) 0.42678(19) 0.6633(2) 0.0320(9) Uani 1 1 d . . . H6 H 0.6398 0.4584 0.6855 0.038 Uiso 1 1 calc R . . C7 C 0.7508(3) 0.43941(17) 0.6330(2) 0.0277(9) Uani 1 1 d . . . H7 H 0.7772 0.4801 0.6337 0.033 Uiso 1 1 calc R . . C8 C 0.7957(3) 0.39342(16) 0.60173(19) 0.0233(8) Uani 1 1 d . . . C9 C 0.6265(3) 0.25546(17) 0.6296(2) 0.0256(8) Uani 1 1 d . . . H9 H 0.6278 0.2375 0.5852 0.031 Uiso 1 1 calc R . . C10 C 0.6971(4) 0.2155(2) 0.6825(2) 0.0460(12) Uani 1 1 d . . . H10A H 0.7704 0.2161 0.6768 0.069 Uiso 1 1 calc R . . H10B H 0.6700 0.1733 0.6780 0.069 Uiso 1 1 calc R . . H10C H 0.6966 0.2312 0.7268 0.069 Uiso 1 1 calc R . . C11 C 0.5111(3) 0.2534(2) 0.6352(2) 0.0420(12) Uani 1 1 d . . . H11A H 0.5079 0.2657 0.6803 0.063 Uiso 1 1 calc R . . H11B H 0.4832 0.2117 0.6263 0.063 Uiso 1 1 calc R . . H11C H 0.4678 0.2817 0.6026 0.063 Uiso 1 1 calc R . . C12 C 0.8760(3) 0.41120(17) 0.5616(2) 0.0271(9) Uani 1 1 d . . . H12 H 0.8879 0.3741 0.5358 0.033 Uiso 1 1 calc R . . C13 C 0.9845(3) 0.4306(2) 0.6045(2) 0.0402(11) Uani 1 1 d . . . H13A H 0.9761 0.4675 0.6298 0.060 Uiso 1 1 calc R . . H13B H 1.0330 0.4394 0.5757 0.060 Uiso 1 1 calc R . . H13C H 1.0143 0.3975 0.6355 0.060 Uiso 1 1 calc R . . C14 C 0.8304(4) 0.4617(2) 0.5106(2) 0.0419(11) Uani 1 1 d . . . H14A H 0.8204 0.4994 0.5342 0.063 Uiso 1 1 calc R . . H14B H 0.7615 0.4484 0.4824 0.063 Uiso 1 1 calc R . . H14C H 0.8803 0.4696 0.4825 0.063 Uiso 1 1 calc R . . C15 C 0.9712(3) 0.21589(16) 0.44862(17) 0.0170(7) Uani 1 1 d . . . C16 C 0.9616(3) 0.15646(16) 0.41996(18) 0.0188(7) Uani 1 1 d . . . C17 C 1.0159(3) 0.14380(18) 0.37089(19) 0.0258(8) Uani 1 1 d . . . H17 H 1.0086 0.1045 0.3505 0.031 Uiso 1 1 calc R . . C18 C 1.0806(3) 0.18752(18) 0.35096(19) 0.0262(8) Uani 1 1 d . . . H18 H 1.1181 0.1778 0.3180 0.031 Uiso 1 1 calc R . . C19 C 1.0898(3) 0.24505(17) 0.37947(19) 0.0241(8) Uani 1 1 d . . . H19 H 1.1339 0.2748 0.3658 0.029 Uiso 1 1 calc R . . C20 C 1.0356(3) 0.26045(16) 0.42795(18) 0.0200(8) Uani 1 1 d . . . C21 C 0.8962(3) 0.10758(16) 0.44458(19) 0.0223(8) Uani 1 1 d . . . H21 H 0.8288 0.1274 0.4499 0.027 Uiso 1 1 calc R . . C22 C 0.9561(3) 0.08428(18) 0.5130(2) 0.0325(10) Uani 1 1 d . . . H22A H 1.0212 0.0630 0.5091 0.049 Uiso 1 1 calc R . . H22B H 0.9104 0.0559 0.5302 0.049 Uiso 1 1 calc R . . H22C H 0.9753 0.1190 0.5437 0.049 Uiso 1 1 calc R . . C23 C 0.8643(3) 0.05439(18) 0.3956(2) 0.0357(10) Uani 1 1 d . . . H23A H 0.8301 0.0705 0.3512 0.054 Uiso 1 1 calc R . . H23B H 0.8141 0.0275 0.4108 0.054 Uiso 1 1 calc R . . H23C H 0.9282 0.0310 0.3933 0.054 Uiso 1 1 calc R . . C24 C 1.0453(3) 0.32530(17) 0.4549(2) 0.0270(9) Uani 1 1 d . . . H24 H 0.9947 0.3294 0.4845 0.032 Uiso 1 1 calc R . . C25 C 1.1583(3) 0.3383(2) 0.4977(2) 0.0383(11) Uani 1 1 d . . . H25A H 1.1731 0.3116 0.5371 0.057 Uiso 1 1 calc R . . H25B H 1.1632 0.3813 0.5120 0.057 Uiso 1 1 calc R . . H25C H 1.2106 0.3304 0.4714 0.057 Uiso 1 1 calc R . . C26 C 1.0133(4) 0.3730(2) 0.3992(3) 0.0460(12) Uani 1 1 d . . . H26A H 1.0629 0.3710 0.3701 0.069 Uiso 1 1 calc R . . H26B H 1.0159 0.4141 0.4188 0.069 Uiso 1 1 calc R . . H26C H 0.9405 0.3645 0.3729 0.069 Uiso 1 1 calc R . . C27 C 0.4540(3) 0.22232(16) 0.29085(17) 0.0208(8) Uani 1 1 d . . . H27A H 0.4113 0.2554 0.2641 0.025 Uiso 1 1 calc R . . H27B H 0.4881 0.1984 0.2609 0.025 Uiso 1 1 calc R . . C28 C 0.3793(3) 0.18028(16) 0.31767(18) 0.0197(8) Uani 1 1 d . . . H28A H 0.3410 0.1528 0.2815 0.024 Uiso 1 1 calc R . . H28B H 0.3254 0.2054 0.3325 0.024 Uiso 1 1 calc R . . C29 C 0.5065(3) 0.33110(16) 0.37963(19) 0.0205(8) Uani 1 1 d . . . H29 H 0.5182 0.3621 0.3464 0.025 Uiso 1 1 calc R . . C30 C 0.5682(3) 0.35315(17) 0.4488(2) 0.0280(9) Uani 1 1 d . . . H30A H 0.5599 0.3227 0.4827 0.034 Uiso 1 1 calc R . . H30B H 0.6453 0.3559 0.4498 0.034 Uiso 1 1 calc R . . C31 C 0.5291(3) 0.41577(18) 0.4666(2) 0.0342(10) Uani 1 1 d . . . H31A H 0.5678 0.4270 0.5126 0.041 Uiso 1 1 calc R . . H31B H 0.5450 0.4473 0.4358 0.041 Uiso 1 1 calc R . . C32 C 0.4095(3) 0.41459(18) 0.4617(2) 0.0339(10) Uani 1 1 d . . . H32A H 0.3851 0.4561 0.4706 0.041 Uiso 1 1 calc R . . H32B H 0.3944 0.3863 0.4958 0.041 Uiso 1 1 calc R . . C33 C 0.3487(3) 0.39361(17) 0.3925(2) 0.0304(9) Uani 1 1 d . . . H33A H 0.3600 0.4235 0.3587 0.036 Uiso 1 1 calc R . . H33B H 0.2712 0.3923 0.3904 0.036 Uiso 1 1 calc R . . C34 C 0.3861(3) 0.33013(16) 0.3763(2) 0.0245(8) Uani 1 1 d . . . H34A H 0.3461 0.3177 0.3310 0.029 Uiso 1 1 calc R . . H34B H 0.3714 0.2998 0.4085 0.029 Uiso 1 1 calc R . . C35 C 0.6624(3) 0.27861(18) 0.3136(2) 0.0287(9) Uani 1 1 d . . . H35 H 0.7169 0.3031 0.3461 0.034 Uiso 1 1 calc R . . C36 C 0.6254(4) 0.3180(2) 0.2541(2) 0.0452(12) Uani 1 1 d . . . H36A H 0.5916 0.3554 0.2668 0.054 Uiso 1 1 calc R . . H36B H 0.5707 0.2957 0.2203 0.054 Uiso 1 1 calc R . . C37 C 0.7188(5) 0.3364(3) 0.2235(3) 0.075(2) Uani 1 1 d . . . H37A H 0.6917 0.3618 0.1831 0.090 Uiso 1 1 calc R . . H37B H 0.7718 0.3609 0.2560 0.090 Uiso 1 1 calc R . . C38 C 0.7720(5) 0.2780(3) 0.2049(3) 0.074(2) Uani 1 1 d . . . H38A H 0.7196 0.2549 0.1706 0.089 Uiso 1 1 calc R . . H38B H 0.8326 0.2895 0.1857 0.089 Uiso 1 1 calc R . . C39 C 0.8110(4) 0.2391(3) 0.2634(3) 0.0584(15) Uani 1 1 d . . . H39A H 0.8678 0.2610 0.2960 0.070 Uiso 1 1 calc R . . H39B H 0.8426 0.2013 0.2497 0.070 Uiso 1 1 calc R . . C40 C 0.7211(3) 0.2214(2) 0.2969(2) 0.0333(10) Uani 1 1 d . . . H40A H 0.7518 0.1984 0.3384 0.040 Uiso 1 1 calc R . . H40B H 0.6694 0.1944 0.2667 0.040 Uiso 1 1 calc R . . C41 C 0.3561(3) 0.11762(15) 0.43778(17) 0.0174(7) Uani 1 1 d . . . H41 H 0.2857 0.1087 0.4061 0.021 Uiso 1 1 calc R . . C42 C 0.3422(3) 0.17440(16) 0.47896(19) 0.0218(8) Uani 1 1 d . . . H42A H 0.4119 0.1853 0.5091 0.026 Uiso 1 1 calc R . . H42B H 0.3184 0.2094 0.4485 0.026 Uiso 1 1 calc R . . C43 C 0.2602(3) 0.16316(17) 0.5206(2) 0.0256(8) Uani 1 1 d . . . H43A H 0.2585 0.1992 0.5495 0.031 Uiso 1 1 calc R . . H43B H 0.1882 0.1585 0.4902 0.031 Uiso 1 1 calc R . . C44 C 0.2867(3) 0.10605(17) 0.56386(19) 0.0258(8) Uani 1 1 d . . . H44A H 0.2285 0.0981 0.5864 0.031 Uiso 1 1 calc R . . H44B H 0.3535 0.1129 0.5987 0.031 Uiso 1 1 calc R . . C45 C 0.3002(3) 0.05052(17) 0.52183(19) 0.0244(8) Uani 1 1 d . . . H45A H 0.2315 0.0415 0.4895 0.029 Uiso 1 1 calc R . . H45B H 0.3202 0.0143 0.5512 0.029 Uiso 1 1 calc R . . C46 C 0.3867(3) 0.06228(16) 0.48409(18) 0.0213(8) Uani 1 1 d . . . H46A H 0.3948 0.0256 0.4575 0.026 Uiso 1 1 calc R . . H46B H 0.4559 0.0701 0.5163 0.026 Uiso 1 1 calc R . . C47 C 0.4826(3) 0.05926(16) 0.35477(18) 0.0197(7) Uani 1 1 d . . . H47 H 0.5231 0.0349 0.3938 0.024 Uiso 1 1 calc R . . C48 C 0.5566(3) 0.06537(17) 0.30714(19) 0.0256(8) Uani 1 1 d . . . H48A H 0.5185 0.0871 0.2662 0.031 Uiso 1 1 calc R . . H48B H 0.6201 0.0900 0.3288 0.031 Uiso 1 1 calc R . . C49 C 0.5929(3) 0.00234(18) 0.2885(2) 0.0297(9) Uani 1 1 d . . . H49A H 0.6355 0.0075 0.2549 0.036 Uiso 1 1 calc R . . H49B H 0.6394 -0.0169 0.3286 0.036 Uiso 1 1 calc R . . C50 C 0.4980(4) -0.03986(19) 0.2602(2) 0.0386(11) Uani 1 1 d . . . H50A H 0.4590 -0.0245 0.2158 0.046 Uiso 1 1 calc R . . H50B H 0.5248 -0.0815 0.2542 0.046 Uiso 1 1 calc R . . C51 C 0.4219(3) -0.04336(18) 0.3054(2) 0.0339(10) Uani 1 1 d . . . H51A H 0.4578 -0.0642 0.3475 0.041 Uiso 1 1 calc R . . H51B H 0.3586 -0.0680 0.2835 0.041 Uiso 1 1 calc R . . C52 C 0.3851(3) 0.02079(17) 0.3216(2) 0.0274(9) Uani 1 1 d . . . H52A H 0.3455 0.0410 0.2800 0.033 Uiso 1 1 calc R . . H52B H 0.3367 0.0171 0.3519 0.033 Uiso 1 1 calc R . . C53 C 0.6021(6) 0.5111(3) 0.2762(4) 0.087(2) Uiso 1 1 d . . . H53A H 0.5726 0.5513 0.2583 0.105 Uiso 1 1 calc R . . H53B H 0.6507 0.4967 0.2489 0.105 Uiso 1 1 calc R . . C54 C 0.6613(8) 0.5187(5) 0.3431(5) 0.145(4) Uiso 1 1 d . . . H54A H 0.6123 0.5283 0.3713 0.217 Uiso 1 1 calc R . . H54B H 0.7125 0.5524 0.3455 0.217 Uiso 1 1 calc R . . H54C H 0.6999 0.4808 0.3588 0.217 Uiso 1 1 calc R . . C55 C 0.4572(5) 0.4634(3) 0.2043(3) 0.0642(15) Uiso 1 1 d . . . H55A H 0.5048 0.4509 0.1756 0.077 Uiso 1 1 calc R . . H55B H 0.4260 0.5038 0.1885 0.077 Uiso 1 1 calc R . . C56 C 0.3720(5) 0.4187(3) 0.1984(3) 0.0696(17) Uiso 1 1 d . . . H56A H 0.4030 0.3775 0.2068 0.104 Uiso 1 1 calc R . . H56B H 0.3251 0.4203 0.1533 0.104 Uiso 1 1 calc R . . H56C H 0.3305 0.4279 0.2311 0.104 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 0.01280(7) 0.01316(7) 0.01320(7) -0.00039(5) 0.00344(5) -0.00087(5) Ga1 0.01365(18) 0.01445(18) 0.01621(19) -0.00229(14) 0.00475(15) -0.00210(14) Cl1 0.0239(5) 0.0215(4) 0.0224(5) 0.0070(4) 0.0017(4) 0.0000(3) P1 0.0175(4) 0.0160(4) 0.0159(5) 0.0025(3) 0.0066(4) 0.0002(3) P2 0.0139(4) 0.0150(4) 0.0155(4) -0.0012(3) 0.0027(3) -0.0020(3) N1 0.0170(15) 0.0162(14) 0.0185(16) -0.0051(12) 0.0048(12) -0.0015(11) N2 0.0146(14) 0.0197(15) 0.0188(16) -0.0018(12) 0.0067(12) -0.0004(11) C1 0.0212(19) 0.0206(18) 0.0136(18) 0.0031(14) 0.0016(14) -0.0035(14) C2 0.0178(18) 0.0185(17) 0.0168(18) 0.0042(14) 0.0024(14) -0.0010(13) C3 0.0227(19) 0.0206(18) 0.0154(18) -0.0072(14) 0.0047(15) -0.0040(14) C4 0.0197(19) 0.026(2) 0.0198(19) -0.0050(15) 0.0060(15) -0.0033(14) C5 0.023(2) 0.037(2) 0.026(2) -0.0087(18) 0.0112(17) -0.0012(17) C6 0.035(2) 0.031(2) 0.033(2) -0.0134(18) 0.0153(19) 0.0014(18) C7 0.033(2) 0.0197(19) 0.030(2) -0.0082(16) 0.0073(18) -0.0033(16) C8 0.025(2) 0.0211(19) 0.025(2) -0.0074(15) 0.0084(16) -0.0024(15) C9 0.026(2) 0.028(2) 0.026(2) -0.0090(16) 0.0134(17) -0.0096(16) C10 0.052(3) 0.033(2) 0.047(3) 0.006(2) 0.000(2) -0.015(2) C11 0.036(3) 0.048(3) 0.048(3) -0.018(2) 0.022(2) -0.019(2) C12 0.034(2) 0.0186(18) 0.033(2) -0.0027(16) 0.0176(18) -0.0040(16) C13 0.036(2) 0.032(2) 0.057(3) -0.005(2) 0.020(2) -0.0114(19) C14 0.050(3) 0.032(2) 0.048(3) 0.009(2) 0.022(2) -0.004(2) C15 0.0116(16) 0.0194(17) 0.0201(19) 0.0025(14) 0.0042(14) 0.0041(13) C16 0.0151(17) 0.0223(19) 0.0196(19) -0.0011(15) 0.0051(14) 0.0007(14) C17 0.0218(19) 0.030(2) 0.027(2) -0.0075(17) 0.0082(16) -0.0013(16) C18 0.0202(19) 0.040(2) 0.020(2) 0.0002(17) 0.0093(16) 0.0022(16) C19 0.0185(19) 0.029(2) 0.027(2) 0.0059(16) 0.0085(16) -0.0003(15) C20 0.0164(18) 0.0213(18) 0.022(2) 0.0041(15) 0.0052(15) 0.0002(14) C21 0.0206(19) 0.0198(18) 0.030(2) -0.0055(16) 0.0126(16) -0.0023(14) C22 0.041(2) 0.021(2) 0.039(3) 0.0027(18) 0.016(2) -0.0022(17) C23 0.038(2) 0.026(2) 0.050(3) -0.013(2) 0.023(2) -0.0109(18) C24 0.030(2) 0.0203(19) 0.034(2) 0.0052(16) 0.0147(18) -0.0002(15) C25 0.041(3) 0.031(2) 0.045(3) -0.008(2) 0.014(2) -0.0149(19) C26 0.054(3) 0.028(2) 0.059(3) 0.015(2) 0.020(3) 0.006(2) C27 0.0249(19) 0.0221(19) 0.0140(18) 0.0009(14) 0.0020(15) 0.0007(15) C28 0.0152(18) 0.0232(19) 0.0190(19) -0.0001(15) 0.0013(14) 0.0023(14) C29 0.0222(19) 0.0160(17) 0.026(2) 0.0033(15) 0.0108(16) 0.0008(14) C30 0.027(2) 0.0214(19) 0.034(2) -0.0051(17) 0.0047(17) -0.0001(16) C31 0.035(2) 0.021(2) 0.045(3) -0.0067(18) 0.008(2) -0.0018(17) C32 0.039(2) 0.021(2) 0.046(3) -0.0057(18) 0.020(2) 0.0039(17) C33 0.029(2) 0.023(2) 0.042(3) 0.0001(18) 0.0159(19) 0.0034(16) C34 0.025(2) 0.0190(18) 0.031(2) -0.0004(16) 0.0093(17) 0.0018(15) C35 0.029(2) 0.031(2) 0.033(2) 0.0050(18) 0.0197(18) -0.0007(17) C36 0.040(3) 0.059(3) 0.042(3) 0.018(2) 0.019(2) 0.006(2) C37 0.062(4) 0.094(5) 0.089(5) 0.057(4) 0.055(4) 0.024(3) C38 0.056(4) 0.121(6) 0.058(4) 0.027(4) 0.039(3) 0.036(4) C39 0.051(3) 0.082(4) 0.055(3) 0.011(3) 0.037(3) 0.019(3) C40 0.030(2) 0.039(2) 0.036(2) 0.0034(19) 0.0180(19) 0.0067(18) C41 0.0142(17) 0.0195(17) 0.0188(18) 0.0004(14) 0.0044(14) -0.0011(13) C42 0.0228(19) 0.0194(18) 0.025(2) 0.0006(15) 0.0085(16) 0.0004(14) C43 0.027(2) 0.025(2) 0.027(2) 0.0005(16) 0.0114(17) 0.0050(16) C44 0.026(2) 0.030(2) 0.026(2) 0.0045(17) 0.0156(17) 0.0008(16) C45 0.024(2) 0.0222(19) 0.029(2) 0.0063(16) 0.0097(16) -0.0009(15) C46 0.0211(19) 0.0187(18) 0.025(2) 0.0029(15) 0.0079(15) 0.0027(14) C47 0.0201(18) 0.0207(18) 0.0179(18) -0.0025(15) 0.0041(14) 0.0008(14) C48 0.029(2) 0.0226(19) 0.027(2) -0.0042(16) 0.0106(17) -0.0011(16) C49 0.036(2) 0.030(2) 0.026(2) -0.0034(17) 0.0145(18) 0.0045(17) C50 0.054(3) 0.025(2) 0.035(3) -0.0127(19) 0.010(2) 0.003(2) C51 0.039(2) 0.025(2) 0.037(3) -0.0106(18) 0.006(2) -0.0071(18) C52 0.025(2) 0.024(2) 0.031(2) -0.0099(17) 0.0028(17) -0.0051(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.2031(10) . ? Pt1 P2 2.3112(10) . ? Pt1 Cl1 2.3723(10) . ? Pt1 Ga1 2.4151(7) . ? Ga1 N1 1.897(3) . ? Ga1 N2 1.898(3) . ? P1 C27 1.844(4) . ? P1 C35 1.848(4) . ? P1 C29 1.850(4) . ? P2 C47 1.838(4) . ? P2 C28 1.840(4) . ? P2 C41 1.844(3) . ? O1 C55 1.403(6) . ? O1 C53 1.414(7) . ? N1 C1 1.408(4) . ? N1 C3 1.421(4) . ? N2 C2 1.393(4) . ? N2 C15 1.427(4) . ? C1 C2 1.340(5) . ? C3 C8 1.414(5) . ? C3 C4 1.417(5) . ? C4 C5 1.397(5) . ? C4 C9 1.516(5) . ? C5 C6 1.379(6) . ? C6 C7 1.386(5) . ? C7 C8 1.394(5) . ? C8 C12 1.525(5) . ? C9 C10 1.516(6) . ? C9 C11 1.522(5) . ? C12 C13 1.522(6) . ? C12 C14 1.540(6) . ? C15 C20 1.410(5) . ? C15 C16 1.418(5) . ? C16 C17 1.392(5) . ? C16 C21 1.522(5) . ? C17 C18 1.394(5) . ? C18 C19 1.379(5) . ? C19 C20 1.395(5) . ? C20 C24 1.515(5) . ? C21 C22 1.523(5) . ? C21 C23 1.529(5) . ? C24 C26 1.533(6) . ? C24 C25 1.535(6) . ? C27 C28 1.528(5) . ? C29 C30 1.533(5) . ? C29 C34 1.537(5) . ? C30 C31 1.531(5) . ? C31 C32 1.522(6) . ? C32 C33 1.523(6) . ? C33 C34 1.530(5) . ? C35 C36 1.479(6) . ? C35 C40 1.541(5) . ? C36 C37 1.545(6) . ? C37 C38 1.540(8) . ? C38 C39 1.462(7) . ? C39 C40 1.536(6) . ? C41 C46 1.531(5) . ? C41 C42 1.538(5) . ? C42 C43 1.536(5) . ? C43 C44 1.523(5) . ? C44 C45 1.525(5) . ? C45 C46 1.529(5) . ? C47 C52 1.528(5) . ? C47 C48 1.534(5) . ? C48 C49 1.531(5) . ? C49 C50 1.528(6) . ? C50 C51 1.513(6) . ? C51 C52 1.540(5) . ? C53 C54 1.416(11) . ? C55 C56 1.452(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 P1 Pt1 P2 88.17(4) . . ? P1 Pt1 Cl1 177.36(3) . . ? P2 Pt1 Cl1 93.92(4) . . ? P1 Pt1 Ga1 95.62(3) . . ? P2 Pt1 Ga1 176.13(2) . . ? Cl1 Pt1 Ga1 82.27(3) . . ? N1 Ga1 N2 88.09(12) . . ? N1 Ga1 Pt1 133.37(9) . . ? N2 Ga1 Pt1 134.78(9) . . ? C27 P1 C35 102.83(18) . . ? C27 P1 C29 107.22(17) . . ? C35 P1 C29 104.42(17) . . ? C27 P1 Pt1 107.58(12) . . ? C35 P1 Pt1 116.53(13) . . ? C29 P1 Pt1 117.04(12) . . ? C47 P2 C28 107.79(16) . . ? C47 P2 C41 105.45(16) . . ? C28 P2 C41 104.38(16) . . ? C47 P2 Pt1 113.57(11) . . ? C28 P2 Pt1 106.88(12) . . ? C41 P2 Pt1 118.03(12) . . ? C55 O1 C53 111.5(5) . . ? C1 N1 C3 116.5(3) . . ? C1 N1 Ga1 108.0(2) . . ? C3 N1 Ga1 132.1(2) . . ? C2 N2 C15 118.8(3) . . ? C2 N2 Ga1 107.9(2) . . ? C15 N2 Ga1 132.0(2) . . ? C2 C1 N1 117.1(3) . . ? C1 C2 N2 118.2(3) . . ? C8 C3 C4 119.8(3) . . ? C8 C3 N1 120.2(3) . . ? C4 C3 N1 120.0(3) . . ? C5 C4 C3 118.4(3) . . ? C5 C4 C9 121.2(3) . . ? C3 C4 C9 120.4(3) . . ? C6 C5 C4 121.8(3) . . ? C5 C6 C7 119.5(3) . . ? C6 C7 C8 121.2(4) . . ? C7 C8 C3 119.1(3) . . ? C7 C8 C12 118.9(3) . . ? C3 C8 C12 121.9(3) . . ? C10 C9 C4 111.0(3) . . ? C10 C9 C11 110.8(4) . . ? C4 C9 C11 113.4(3) . . ? C13 C12 C8 113.8(3) . . ? C13 C12 C14 110.0(3) . . ? C8 C12 C14 111.0(3) . . ? C20 C15 C16 120.1(3) . . ? C20 C15 N2 121.1(3) . . ? C16 C15 N2 118.8(3) . . ? C17 C16 C15 118.5(3) . . ? C17 C16 C21 121.5(3) . . ? C15 C16 C21 120.0(3) . . ? C16 C17 C18 121.5(4) . . ? C19 C18 C17 119.5(3) . . ? C18 C19 C20 121.3(3) . . ? C19 C20 C15 119.1(3) . . ? C19 C20 C24 118.6(3) . . ? C15 C20 C24 122.3(3) . . ? C16 C21 C22 110.3(3) . . ? C16 C21 C23 113.0(3) . . ? C22 C21 C23 110.8(3) . . ? C20 C24 C26 112.0(3) . . ? C20 C24 C25 111.5(3) . . ? C26 C24 C25 110.5(3) . . ? C28 C27 P1 112.8(2) . . ? C27 C28 P2 111.3(2) . . ? C30 C29 C34 109.6(3) . . ? C30 C29 P1 111.4(2) . . ? C34 C29 P1 113.7(2) . . ? C31 C30 C29 112.2(3) . . ? C32 C31 C30 110.9(3) . . ? C31 C32 C33 110.4(3) . . ? C32 C33 C34 111.1(3) . . ? C33 C34 C29 110.3(3) . . ? C36 C35 C40 111.1(4) . . ? C36 C35 P1 115.6(3) . . ? C40 C35 P1 110.9(3) . . ? C35 C36 C37 111.5(4) . . ? C38 C37 C36 109.0(5) . . ? C39 C38 C37 111.0(5) . . ? C38 C39 C40 111.9(4) . . ? C39 C40 C35 111.3(4) . . ? C46 C41 C42 109.6(3) . . ? C46 C41 P2 113.1(2) . . ? C42 C41 P2 110.0(2) . . ? C43 C42 C41 111.7(3) . . ? C44 C43 C42 111.9(3) . . ? C43 C44 C45 110.8(3) . . ? C44 C45 C46 110.9(3) . . ? C45 C46 C41 110.0(3) . . ? C52 C47 C48 109.4(3) . . ? C52 C47 P2 115.8(2) . . ? C48 C47 P2 112.1(2) . . ? C49 C48 C47 111.0(3) . . ? C50 C49 C48 111.9(3) . . ? C51 C50 C49 111.9(3) . . ? C50 C51 C52 111.6(3) . . ? C47 C52 C51 109.5(3) . . ? O1 C53 C54 112.3(7) . . ? O1 C55 C56 111.4(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.450 _refine_diff_density_min -0.868 _refine_diff_density_rms 0.105 # Attachment 'compound12.CIF' data_compound12 _database_code_depnum_ccdc_archive 'CCDC 664052' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H70 Cl Ga N2 O P2 Pt' _chemical_formula_weight 1149.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.141(2) _cell_length_b 16.274(3) _cell_length_c 26.622(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5260.0(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 3.320 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.521 _exptl_absorpt_correction_T_max 0.732 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31076 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 26.71 _reflns_number_total 11024 _reflns_number_gt 9745 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One molecule of diethyl ether was located in the asymmetric unit. The non-hydrogen atoms of this molecule were refined anisotropically. ; _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^)+(0.0104P)^2^+8.7056P] 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 -0.017(5) _refine_ls_number_reflns 11024 _refine_ls_number_parameters 588 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0665 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 0.890535(15) 0.607394(12) 0.092118(7) 0.01640(5) Uani 1 1 d . . . Ga1 Ga 0.85760(4) 0.50609(4) 0.15551(2) 0.01760(13) Uani 1 1 d . . . Cl1 Cl 0.69928(11) 0.63138(9) 0.09953(6) 0.0334(4) Uani 1 1 d . . . P1 P 0.91565(11) 0.67710(9) 0.01680(5) 0.0194(3) Uani 1 1 d . . . O1 O 0.6192(4) 0.9851(3) 0.12956(15) 0.0398(11) Uani 1 1 d . . . N1 N 0.8831(4) 0.4706(2) 0.22159(15) 0.0197(9) Uani 1 1 d . . . C1 C 0.8418(4) 0.3901(4) 0.2268(2) 0.0245(12) Uani 1 1 d . . . H1 H 0.8483 0.3606 0.2574 0.029 Uiso 1 1 calc R . . P2 P 1.07057(10) 0.58899(7) 0.09378(6) 0.0173(3) Uani 1 1 d . . . N2 N 0.7890(3) 0.4043(3) 0.14281(15) 0.0196(10) Uani 1 1 d . . . C2 C 0.7927(4) 0.3568(3) 0.1861(2) 0.0215(13) Uani 1 1 d . . . H2 H 0.7620 0.3031 0.1871 0.026 Uiso 1 1 calc R . . C3 C 0.9221(4) 0.5126(3) 0.26512(19) 0.0215(12) Uani 1 1 d . . . C4 C 0.8630(5) 0.5810(3) 0.2835(2) 0.0277(14) Uani 1 1 d . . . C5 C 0.9006(6) 0.6213(3) 0.3262(2) 0.0339(15) Uani 1 1 d . . . H5 H 0.8613 0.6675 0.3386 0.041 Uiso 1 1 calc R . . C6 C 0.9950(5) 0.5947(4) 0.3510(2) 0.0347(15) Uani 1 1 d . . . H6 H 1.0192 0.6219 0.3806 0.042 Uiso 1 1 calc R . . C7 C 1.0534(5) 0.5287(4) 0.3323(2) 0.0335(15) Uani 1 1 d . . . H7 H 1.1185 0.5115 0.3491 0.040 Uiso 1 1 calc R . . C8 C 1.0194(4) 0.4859(3) 0.2891(2) 0.0232(12) Uani 1 1 d . . . C9 C 0.7541(5) 0.6061(4) 0.2590(2) 0.0337(15) Uani 1 1 d . . . H9 H 0.7646 0.6028 0.2218 0.040 Uiso 1 1 calc R . . C10 C 0.6639(6) 0.5475(5) 0.2724(3) 0.058(2) Uani 1 1 d . . . H10A H 0.6862 0.4915 0.2636 0.086 Uiso 1 1 calc R . . H10B H 0.5970 0.5621 0.2539 0.086 Uiso 1 1 calc R . . H10C H 0.6495 0.5506 0.3086 0.086 Uiso 1 1 calc R . . C11 C 0.7180(7) 0.6946(4) 0.2712(3) 0.059(2) Uani 1 1 d . . . H11A H 0.6916 0.6973 0.3060 0.088 Uiso 1 1 calc R . . H11B H 0.6586 0.7110 0.2484 0.088 Uiso 1 1 calc R . . H11C H 0.7808 0.7319 0.2671 0.088 Uiso 1 1 calc R . . C12 C 1.0880(5) 0.4140(3) 0.2709(2) 0.0270(14) Uani 1 1 d . . . H12 H 1.0550 0.3934 0.2389 0.032 Uiso 1 1 calc R . . C13 C 1.0848(5) 0.3439(4) 0.3094(2) 0.0369(16) Uani 1 1 d . . . H13A H 1.1187 0.3622 0.3409 0.055 Uiso 1 1 calc R . . H13B H 1.1256 0.2966 0.2962 0.055 Uiso 1 1 calc R . . H13C H 1.0082 0.3280 0.3156 0.055 Uiso 1 1 calc R . . C14 C 1.2076(5) 0.4406(4) 0.2600(2) 0.0352(16) Uani 1 1 d . . . H14A H 1.2076 0.4848 0.2349 0.053 Uiso 1 1 calc R . . H14B H 1.2494 0.3936 0.2471 0.053 Uiso 1 1 calc R . . H14C H 1.2420 0.4605 0.2910 0.053 Uiso 1 1 calc R . . C15 C 0.7124(4) 0.3846(3) 0.10352(19) 0.0183(12) Uani 1 1 d . . . C16 C 0.5980(5) 0.3864(3) 0.1122(2) 0.0257(12) Uani 1 1 d . . . C17 C 0.5271(5) 0.3687(4) 0.0730(2) 0.0353(16) Uani 1 1 d . . . H17 H 0.4500 0.3680 0.0790 0.042 Uiso 1 1 calc R . . C18 C 0.5654(5) 0.3520(4) 0.0254(3) 0.0410(19) Uani 1 1 d . . . H18 H 0.5154 0.3413 -0.0013 0.049 Uiso 1 1 calc R . . C19 C 0.6785(5) 0.3511(4) 0.0168(2) 0.0330(16) Uani 1 1 d . . . H19 H 0.7048 0.3403 -0.0161 0.040 Uiso 1 1 calc R . . C20 C 0.7538(5) 0.3655(3) 0.0551(2) 0.0224(13) Uani 1 1 d . . . C21 C 0.5502(5) 0.4090(4) 0.1635(3) 0.0355(16) Uani 1 1 d . . . H21 H 0.6124 0.4264 0.1857 0.043 Uiso 1 1 calc R . . C22 C 0.4702(5) 0.4802(4) 0.1594(3) 0.0437(18) Uani 1 1 d . . . H22A H 0.5070 0.5270 0.1434 0.066 Uiso 1 1 calc R . . H22B H 0.4453 0.4961 0.1930 0.066 Uiso 1 1 calc R . . H22C H 0.4067 0.4637 0.1391 0.066 Uiso 1 1 calc R . . C23 C 0.4946(6) 0.3341(4) 0.1877(3) 0.0486(19) Uani 1 1 d . . . H23A H 0.4721 0.3478 0.2220 0.073 Uiso 1 1 calc R . . H23B H 0.5466 0.2881 0.1885 0.073 Uiso 1 1 calc R . . H23C H 0.4296 0.3186 0.1680 0.073 Uiso 1 1 calc R . . C24 C 0.8776(5) 0.3563(3) 0.0471(2) 0.0289(14) Uani 1 1 d . . . H24 H 0.9152 0.4026 0.0648 0.035 Uiso 1 1 calc R . . C25 C 0.9119(6) 0.3588(4) -0.0086(2) 0.0449(18) Uani 1 1 d . . . H25A H 0.8844 0.3096 -0.0257 0.067 Uiso 1 1 calc R . . H25B H 0.9924 0.3606 -0.0110 0.067 Uiso 1 1 calc R . . H25C H 0.8806 0.4079 -0.0245 0.067 Uiso 1 1 calc R . . C26 C 0.9156(5) 0.2765(4) 0.0709(2) 0.0386(16) Uani 1 1 d . . . H26A H 0.9021 0.2784 0.1072 0.058 Uiso 1 1 calc R . . H26B H 0.9945 0.2690 0.0648 0.058 Uiso 1 1 calc R . . H26C H 0.8747 0.2304 0.0562 0.058 Uiso 1 1 calc R . . C27 C 1.0556(4) 0.6492(4) -0.0031(2) 0.0221(13) Uani 1 1 d . . . H27A H 1.0550 0.5939 -0.0187 0.026 Uiso 1 1 calc R . . H27B H 1.0824 0.6890 -0.0284 0.026 Uiso 1 1 calc R . . C28 C 1.1318(4) 0.6493(3) 0.0420(2) 0.0220(13) Uani 1 1 d . . . H28A H 1.1445 0.7065 0.0532 0.026 Uiso 1 1 calc R . . H28B H 1.2038 0.6253 0.0325 0.026 Uiso 1 1 calc R . . C29 C 0.9113(4) 0.7891(3) 0.0181(2) 0.0217(13) Uani 1 1 d . . . C30 C 0.8400(5) 0.8259(3) 0.0519(2) 0.0227(13) Uani 1 1 d . . . H30 H 0.7963 0.7928 0.0736 0.027 Uiso 1 1 calc R . . C31 C 0.8321(5) 0.9106(3) 0.0544(2) 0.0281(14) Uani 1 1 d . . . H31 H 0.7824 0.9353 0.0775 0.034 Uiso 1 1 calc R . . C32 C 0.8958(6) 0.9596(3) 0.0237(2) 0.0324(14) Uani 1 1 d . . . H32 H 0.8909 1.0177 0.0259 0.039 Uiso 1 1 calc R . . C33 C 0.9667(5) 0.9235(4) -0.0104(2) 0.0336(16) Uani 1 1 d . . . H33 H 1.0103 0.9570 -0.0318 0.040 Uiso 1 1 calc R . . C34 C 0.9749(5) 0.8383(4) -0.0135(2) 0.0279(14) Uani 1 1 d . . . H34 H 1.0236 0.8138 -0.0371 0.034 Uiso 1 1 calc R . . C35 C 0.8267(4) 0.6440(3) -0.0345(2) 0.0196(12) Uani 1 1 d . . . C36 C 0.8196(5) 0.6871(4) -0.0795(2) 0.0261(14) Uani 1 1 d . . . H36 H 0.8588 0.7372 -0.0835 0.031 Uiso 1 1 calc R . . C37 C 0.7556(5) 0.6572(4) -0.1184(2) 0.0331(16) Uani 1 1 d . . . H37 H 0.7512 0.6866 -0.1492 0.040 Uiso 1 1 calc R . . C38 C 0.6986(5) 0.5855(4) -0.1127(2) 0.0347(16) Uani 1 1 d . . . H38 H 0.6558 0.5649 -0.1398 0.042 Uiso 1 1 calc R . . C39 C 0.7024(6) 0.5423(4) -0.0679(2) 0.0396(17) Uani 1 1 d . . . H39 H 0.6610 0.4933 -0.0638 0.048 Uiso 1 1 calc R . . C40 C 0.7679(5) 0.5718(4) -0.0290(2) 0.0343(16) Uani 1 1 d . . . H40 H 0.7722 0.5421 0.0017 0.041 Uiso 1 1 calc R . . C41 C 1.1254(4) 0.4844(3) 0.0879(2) 0.0166(10) Uani 1 1 d . . . C42 C 1.1224(5) 0.4351(3) 0.1304(2) 0.0244(13) Uani 1 1 d . . . H42 H 1.0906 0.4555 0.1605 0.029 Uiso 1 1 calc R . . C43 C 1.1653(5) 0.3571(4) 0.1291(2) 0.0283(15) Uani 1 1 d . . . H43 H 1.1627 0.3238 0.1584 0.034 Uiso 1 1 calc R . . C44 C 1.2124(4) 0.3262(4) 0.0856(3) 0.0335(16) Uani 1 1 d . . . H44 H 1.2428 0.2724 0.0850 0.040 Uiso 1 1 calc R . . C45 C 1.2144(5) 0.3743(4) 0.0434(2) 0.0297(15) Uani 1 1 d . . . H45 H 1.2454 0.3532 0.0132 0.036 Uiso 1 1 calc R . . C46 C 1.1719(5) 0.4536(4) 0.0439(2) 0.0261(14) Uani 1 1 d . . . H46 H 1.1746 0.4866 0.0145 0.031 Uiso 1 1 calc R . . C47 C 1.1429(4) 0.6258(3) 0.1493(2) 0.0194(12) Uani 1 1 d . . . C48 C 1.0866(5) 0.6530(3) 0.1917(2) 0.0225(13) Uani 1 1 d . . . H48 H 1.0084 0.6541 0.1918 0.027 Uiso 1 1 calc R . . C49 C 1.1442(5) 0.6784(3) 0.2338(2) 0.0303(15) Uani 1 1 d . . . H49 H 1.1055 0.6961 0.2629 0.036 Uiso 1 1 calc R . . C50 C 1.2583(5) 0.6781(4) 0.2336(2) 0.0326(16) Uani 1 1 d . . . H50 H 1.2979 0.6956 0.2624 0.039 Uiso 1 1 calc R . . C51 C 1.3150(5) 0.6520(4) 0.1908(2) 0.0317(16) Uani 1 1 d . . . H51 H 1.3932 0.6530 0.1904 0.038 Uiso 1 1 calc R . . C52 C 1.2579(4) 0.6250(3) 0.1494(2) 0.0232(13) Uani 1 1 d . . . H52 H 1.2969 0.6057 0.1207 0.028 Uiso 1 1 calc R . . C53 C 0.5813(6) 0.8449(4) 0.1512(3) 0.050(2) Uani 1 1 d . . . H53A H 0.5986 0.8303 0.1163 0.075 Uiso 1 1 calc R . . H53B H 0.5232 0.8086 0.1638 0.075 Uiso 1 1 calc R . . H53C H 0.6474 0.8386 0.1719 0.075 Uiso 1 1 calc R . . C54 C 0.5428(6) 0.9321(4) 0.1533(3) 0.0478(19) Uani 1 1 d . . . H54A H 0.4704 0.9368 0.1365 0.057 Uiso 1 1 calc R . . H54B H 0.5336 0.9489 0.1888 0.057 Uiso 1 1 calc R . . C55 C 0.5869(6) 1.0688(4) 0.1322(3) 0.053(2) Uani 1 1 d . . . H55A H 0.5784 1.0852 0.1678 0.064 Uiso 1 1 calc R . . H55B H 0.5148 1.0759 0.1153 0.064 Uiso 1 1 calc R . . C56 C 0.6704(6) 1.1225(5) 0.1076(3) 0.056(2) Uani 1 1 d . . . H56A H 0.7399 1.1194 0.1262 0.084 Uiso 1 1 calc R . . H56B H 0.6439 1.1794 0.1074 0.084 Uiso 1 1 calc R . . H56C H 0.6823 1.1041 0.0730 0.084 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 0.01628(8) 0.01805(9) 0.01485(9) 0.00260(9) -0.00002(9) -0.00040(9) Ga1 0.0183(3) 0.0174(3) 0.0170(3) 0.0020(2) -0.0004(2) -0.0024(2) Cl1 0.0171(6) 0.0456(9) 0.0375(10) 0.0096(8) 0.0007(7) 0.0035(6) P1 0.0206(8) 0.0228(8) 0.0147(7) 0.0022(6) -0.0004(6) 0.0004(6) O1 0.040(3) 0.043(3) 0.037(3) 0.003(2) 0.004(2) 0.005(3) N1 0.022(2) 0.019(2) 0.018(2) 0.0004(18) 0.001(2) 0.000(2) C1 0.032(3) 0.019(3) 0.023(3) 0.007(3) 0.005(2) -0.006(3) P2 0.0156(6) 0.0197(7) 0.0165(7) 0.0010(7) -0.0001(6) 0.0005(5) N2 0.022(2) 0.023(3) 0.014(2) 0.002(2) 0.0015(18) -0.001(2) C2 0.024(3) 0.018(3) 0.022(3) 0.000(2) 0.003(2) 0.000(2) C3 0.028(3) 0.025(3) 0.011(3) 0.003(2) 0.001(2) -0.007(2) C4 0.028(3) 0.025(3) 0.029(3) 0.005(2) 0.006(3) -0.002(2) C5 0.057(4) 0.016(3) 0.028(3) -0.008(2) 0.003(3) -0.009(3) C6 0.053(4) 0.031(4) 0.020(3) -0.004(3) -0.003(3) -0.017(3) C7 0.042(4) 0.032(4) 0.026(4) -0.003(3) -0.007(3) -0.005(3) C8 0.026(3) 0.020(3) 0.023(3) 0.000(2) -0.005(3) -0.006(3) C9 0.038(3) 0.030(3) 0.032(4) -0.001(4) 0.006(3) 0.005(4) C10 0.041(4) 0.066(5) 0.066(6) 0.003(4) -0.003(4) 0.009(4) C11 0.070(6) 0.042(5) 0.065(6) 0.000(4) -0.005(4) 0.023(4) C12 0.034(3) 0.027(3) 0.020(3) -0.004(2) -0.009(3) 0.003(3) C13 0.043(4) 0.036(4) 0.031(4) 0.001(3) -0.006(3) 0.002(3) C14 0.029(3) 0.038(4) 0.038(4) 0.002(3) -0.005(3) 0.003(3) C15 0.021(2) 0.012(3) 0.022(3) 0.003(2) -0.004(2) -0.002(2) C16 0.022(3) 0.020(3) 0.035(3) 0.008(3) -0.004(3) 0.001(3) C17 0.024(3) 0.040(4) 0.042(4) 0.002(3) -0.010(3) -0.003(3) C18 0.035(4) 0.044(4) 0.044(5) -0.009(4) -0.022(3) 0.000(3) C19 0.041(4) 0.028(4) 0.029(4) -0.006(3) -0.011(3) 0.002(3) C20 0.029(3) 0.012(3) 0.026(3) 0.002(2) -0.005(3) -0.003(2) C21 0.024(3) 0.037(4) 0.046(4) 0.001(3) 0.000(3) -0.001(3) C22 0.041(4) 0.035(4) 0.055(5) -0.002(4) 0.011(4) 0.007(3) C23 0.049(4) 0.043(4) 0.054(5) 0.020(4) 0.009(4) 0.002(4) C24 0.027(3) 0.033(3) 0.027(3) -0.008(3) 0.000(3) -0.002(3) C25 0.047(4) 0.058(5) 0.030(4) -0.009(3) 0.004(3) -0.008(4) C26 0.029(4) 0.040(4) 0.046(4) -0.007(3) -0.002(3) 0.006(3) C27 0.025(3) 0.024(3) 0.018(3) 0.001(2) 0.002(2) -0.001(2) C28 0.015(3) 0.026(3) 0.024(3) 0.005(2) 0.002(2) 0.002(2) C29 0.022(3) 0.029(3) 0.015(3) 0.000(2) -0.006(2) -0.001(3) C30 0.027(3) 0.025(3) 0.016(3) -0.001(2) 0.000(2) -0.003(3) C31 0.034(3) 0.027(4) 0.023(3) -0.005(3) -0.003(3) 0.005(3) C32 0.038(3) 0.024(3) 0.036(4) 0.000(3) -0.012(3) -0.010(3) C33 0.036(4) 0.028(3) 0.037(4) 0.004(3) 0.003(3) -0.012(3) C34 0.031(3) 0.025(3) 0.028(4) 0.002(3) 0.007(3) 0.002(3) C35 0.015(3) 0.024(3) 0.020(3) 0.001(2) 0.002(2) 0.002(2) C36 0.032(3) 0.027(3) 0.019(3) 0.005(2) -0.008(2) 0.001(3) C37 0.039(4) 0.032(4) 0.028(4) 0.004(3) -0.011(3) 0.003(3) C38 0.037(4) 0.039(4) 0.027(4) -0.007(3) -0.014(3) 0.001(3) C39 0.048(4) 0.047(4) 0.025(4) -0.001(3) -0.003(3) -0.017(4) C40 0.050(4) 0.035(4) 0.018(3) -0.001(3) -0.004(3) -0.013(3) C41 0.014(2) 0.015(2) 0.020(3) -0.001(2) -0.005(2) -0.002(2) C42 0.032(3) 0.019(3) 0.023(3) -0.004(2) 0.003(3) 0.005(3) C43 0.036(4) 0.022(3) 0.027(4) 0.003(3) -0.005(3) 0.005(3) C44 0.021(3) 0.023(3) 0.057(5) -0.005(3) -0.007(3) 0.011(3) C45 0.033(3) 0.029(4) 0.027(4) -0.009(3) 0.006(3) 0.006(3) C46 0.026(3) 0.030(3) 0.022(3) 0.000(3) -0.001(3) 0.003(3) C47 0.024(3) 0.014(3) 0.020(3) 0.005(2) -0.002(2) -0.004(2) C48 0.024(3) 0.018(3) 0.025(3) -0.006(2) 0.002(2) 0.003(2) C49 0.044(4) 0.027(3) 0.020(3) -0.010(3) 0.000(3) -0.002(3) C50 0.042(4) 0.023(3) 0.034(4) -0.006(3) -0.020(3) 0.001(3) C51 0.028(3) 0.023(3) 0.044(4) 0.000(3) -0.012(3) -0.001(3) C52 0.018(3) 0.024(3) 0.028(3) -0.001(3) -0.003(2) -0.002(2) C53 0.050(5) 0.055(5) 0.046(5) 0.000(4) -0.004(4) 0.004(4) C54 0.036(4) 0.055(5) 0.052(5) -0.006(4) -0.004(4) -0.002(4) C55 0.043(5) 0.055(5) 0.061(5) 0.010(4) -0.001(4) 0.009(4) C56 0.049(4) 0.059(5) 0.059(5) 0.015(4) 0.002(4) 0.009(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 Pt1 P2 2.2067(13) . ? Pt1 P1 2.3239(14) . ? Pt1 Cl1 2.3629(14) . ? Pt1 Ga1 2.3929(7) . ? Ga1 N1 1.877(4) . ? Ga1 N2 1.885(4) . ? P1 C35 1.823(6) . ? P1 C29 1.823(6) . ? P1 C27 1.837(5) . ? O1 C54 1.415(8) . ? O1 C55 1.419(7) . ? N1 C1 1.410(7) . ? N1 C3 1.426(6) . ? C1 C2 1.349(7) . ? P2 C47 1.820(5) . ? P2 C41 1.834(5) . ? P2 C28 1.849(5) . ? N2 C2 1.389(7) . ? N2 C15 1.436(6) . ? C3 C8 1.410(7) . ? C3 C4 1.411(7) . ? C4 C5 1.390(8) . ? C4 C9 1.529(8) . ? C5 C6 1.392(9) . ? C6 C7 1.380(8) . ? C7 C8 1.406(8) . ? C8 C12 1.516(8) . ? C9 C10 1.494(9) . ? C9 C11 1.541(9) . ? C12 C13 1.534(8) . ? C12 C14 1.544(8) . ? C15 C16 1.408(7) . ? C15 C20 1.420(7) . ? C16 C17 1.384(8) . ? C16 C21 1.529(8) . ? C17 C18 1.377(9) . ? C18 C19 1.391(9) . ? C19 C20 1.389(8) . ? C20 C24 1.525(8) . ? C21 C22 1.516(8) . ? C21 C23 1.535(8) . ? C24 C26 1.518(8) . ? C24 C25 1.539(8) . ? C27 C28 1.515(7) . ? C29 C30 1.385(7) . ? C29 C34 1.396(8) . ? C30 C31 1.384(8) . ? C31 C32 1.379(8) . ? C32 C33 1.382(9) . ? C33 C34 1.392(8) . ? C35 C40 1.383(8) . ? C35 C36 1.391(7) . ? C36 C37 1.383(8) . ? C37 C38 1.365(8) . ? C38 C39 1.386(8) . ? C39 C40 1.391(8) . ? C41 C42 1.387(7) . ? C41 C46 1.393(7) . ? C42 C43 1.373(7) . ? C43 C44 1.387(9) . ? C44 C45 1.370(9) . ? C45 C46 1.389(8) . ? C47 C48 1.393(7) . ? C47 C52 1.396(7) . ? C48 C49 1.385(7) . ? C49 C50 1.385(8) . ? C50 C51 1.395(9) . ? C51 C52 1.376(8) . ? C53 C54 1.496(9) . ? C55 C56 1.490(9) . ? 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 87.34(5) . . ? P2 Pt1 Cl1 173.81(6) . . ? P1 Pt1 Cl1 96.91(5) . . ? P2 Pt1 Ga1 93.32(4) . . ? P1 Pt1 Ga1 165.19(4) . . ? Cl1 Pt1 Ga1 83.72(4) . . ? N1 Ga1 N2 88.31(18) . . ? N1 Ga1 Pt1 147.71(13) . . ? N2 Ga1 Pt1 123.57(13) . . ? C35 P1 C29 107.0(2) . . ? C35 P1 C27 105.0(2) . . ? C29 P1 C27 106.3(3) . . ? C35 P1 Pt1 115.14(18) . . ? C29 P1 Pt1 117.86(18) . . ? C27 P1 Pt1 104.44(19) . . ? C54 O1 C55 112.5(5) . . ? C1 N1 C3 119.0(4) . . ? C1 N1 Ga1 108.6(3) . . ? C3 N1 Ga1 131.9(3) . . ? C2 C1 N1 116.9(5) . . ? C47 P2 C41 101.5(2) . . ? C47 P2 C28 103.7(2) . . ? C41 P2 C28 106.5(2) . . ? C47 P2 Pt1 116.72(18) . . ? C41 P2 Pt1 118.91(15) . . ? C28 P2 Pt1 108.14(17) . . ? C2 N2 C15 120.1(4) . . ? C2 N2 Ga1 109.0(3) . . ? C15 N2 Ga1 127.8(4) . . ? C1 C2 N2 117.2(5) . . ? C8 C3 C4 120.8(5) . . ? C8 C3 N1 119.8(5) . . ? C4 C3 N1 119.4(5) . . ? C5 C4 C3 119.2(5) . . ? C5 C4 C9 120.4(6) . . ? C3 C4 C9 120.2(5) . . ? C4 C5 C6 120.8(6) . . ? C7 C6 C5 119.6(6) . . ? C6 C7 C8 121.9(6) . . ? C7 C8 C3 117.6(5) . . ? C7 C8 C12 118.7(5) . . ? C3 C8 C12 123.7(5) . . ? C10 C9 C4 111.2(6) . . ? C10 C9 C11 109.7(6) . . ? C4 C9 C11 114.0(6) . . ? C8 C12 C13 110.4(5) . . ? C8 C12 C14 111.1(5) . . ? C13 C12 C14 111.0(5) . . ? C16 C15 C20 120.2(5) . . ? C16 C15 N2 121.0(5) . . ? C20 C15 N2 118.7(4) . . ? C17 C16 C15 119.1(5) . . ? C17 C16 C21 119.2(5) . . ? C15 C16 C21 121.7(5) . . ? C18 C17 C16 121.7(6) . . ? C17 C18 C19 119.1(6) . . ? C20 C19 C18 121.9(6) . . ? C19 C20 C15 118.0(5) . . ? C19 C20 C24 122.0(5) . . ? C15 C20 C24 119.9(5) . . ? C22 C21 C16 111.3(5) . . ? C22 C21 C23 110.9(5) . . ? C16 C21 C23 110.5(5) . . ? C26 C24 C20 109.0(5) . . ? C26 C24 C25 110.1(5) . . ? C20 C24 C25 113.5(5) . . ? C28 C27 P1 109.6(4) . . ? C27 C28 P2 110.1(4) . . ? C30 C29 C34 119.3(5) . . ? C30 C29 P1 117.6(4) . . ? C34 C29 P1 123.1(4) . . ? C31 C30 C29 120.4(5) . . ? C32 C31 C30 120.6(6) . . ? C31 C32 C33 119.5(5) . . ? C32 C33 C34 120.5(6) . . ? C33 C34 C29 119.7(6) . . ? C40 C35 C36 119.3(5) . . ? C40 C35 P1 118.5(4) . . ? C36 C35 P1 122.2(4) . . ? C37 C36 C35 120.1(6) . . ? C38 C37 C36 120.2(6) . . ? C37 C38 C39 120.8(6) . . ? C38 C39 C40 119.1(6) . . ? C35 C40 C39 120.6(6) . . ? C42 C41 C46 119.2(5) . . ? C42 C41 P2 117.2(4) . . ? C46 C41 P2 123.5(4) . . ? C43 C42 C41 120.2(5) . . ? C42 C43 C44 120.9(6) . . ? C45 C44 C43 119.0(5) . . ? C44 C45 C46 121.0(6) . . ? C45 C46 C41 119.6(5) . . ? C48 C47 C52 119.5(5) . . ? C48 C47 P2 121.7(4) . . ? C52 C47 P2 118.7(4) . . ? C49 C48 C47 120.2(5) . . ? C48 C49 C50 120.0(6) . . ? C49 C50 C51 119.8(6) . . ? C52 C51 C50 120.3(6) . . ? C51 C52 C47 120.1(5) . . ? O1 C54 C53 110.9(6) . . ? O1 C55 C56 110.7(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.71 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.706 _refine_diff_density_min -1.016 _refine_diff_density_rms 0.123 # Attachment 'compound13.CIF' data_compound13 _database_code_depnum_ccdc_archive 'CCDC 664053' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H106 Ga2 N4 O P2 Pt' _chemical_formula_weight 1560.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.516(3) _cell_length_b 19.145(4) _cell_length_c 25.876(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.43(3) _cell_angle_gamma 90.00 _cell_volume 7604(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3216 _exptl_absorpt_coefficient_mu 2.627 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.409 _exptl_absorpt_correction_T_max 0.532 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28846 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 26.50 _reflns_number_total 15604 _reflns_number_gt 12139 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One molecule of diethyl ether was located in the asymmetric unit. The non-hydrogen atoms of this molecule were refined anisotropically. ; _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^)+(0.0198P)^2^+7.2294P] 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 15604 _refine_ls_number_parameters 847 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0785 _refine_ls_wR_factor_gt 0.0724 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.190251(10) 0.242346(7) 0.405607(5) 0.01265(5) Uani 1 1 d . . . Ga1 Ga 0.16294(3) 0.32775(2) 0.336420(15) 0.01503(10) Uani 1 1 d . . . Ga2 Ga 0.33358(3) 0.21296(2) 0.386231(15) 0.01479(10) Uani 1 1 d . . . P1 P 0.08139(7) 0.28543(5) 0.44905(4) 0.0157(2) Uani 1 1 d . . . P2 P 0.18233(7) 0.14381(5) 0.45565(4) 0.0153(2) Uani 1 1 d . . . O1 O 0.1615(2) -0.18513(18) 0.47262(12) 0.0475(9) Uani 1 1 d . . . N1 N 0.0669(2) 0.31430(16) 0.28259(11) 0.0191(8) Uani 1 1 d . . . N2 N 0.1577(2) 0.42501(16) 0.31973(11) 0.0185(7) Uani 1 1 d . . . N3 N 0.4323(2) 0.22606(16) 0.43882(12) 0.0176(7) Uani 1 1 d . . . N4 N 0.4021(2) 0.14918(16) 0.35240(11) 0.0180(7) Uani 1 1 d . . . C1 C 0.0403(3) 0.3791(2) 0.26115(14) 0.0213(9) Uani 1 1 d . . . H1 H -0.0083 0.3834 0.2344 0.026 Uiso 1 1 calc R . . C2 C 0.0863(3) 0.4351(2) 0.28002(14) 0.0186(9) Uani 1 1 d . . . H2 H 0.0713 0.4805 0.2669 0.022 Uiso 1 1 calc R . . C3 C 0.0384(3) 0.25244(19) 0.25316(14) 0.0212(9) Uani 1 1 d . . . C4 C -0.0412(3) 0.2205(2) 0.25857(15) 0.0249(10) Uani 1 1 d . . . C5 C -0.0636(3) 0.1588(2) 0.23118(15) 0.0335(12) Uani 1 1 d . . . H5 H -0.1174 0.1367 0.2343 0.040 Uiso 1 1 calc R . . C6 C -0.0089(4) 0.1291(2) 0.19955(16) 0.0407(13) Uani 1 1 d . . . H6 H -0.0231 0.0855 0.1830 0.049 Uiso 1 1 calc R . . C7 C 0.0662(3) 0.1634(2) 0.19233(16) 0.0360(12) Uani 1 1 d . . . H7 H 0.1021 0.1440 0.1692 0.043 Uiso 1 1 calc R . . C8 C 0.0912(3) 0.2257(2) 0.21791(14) 0.0254(10) Uani 1 1 d . . . C9 C -0.1047(3) 0.2546(2) 0.29024(16) 0.0280(10) Uani 1 1 d . . . H9 H -0.0725 0.2915 0.3126 0.034 Uiso 1 1 calc R . . C10 C -0.1421(3) 0.2033(3) 0.32605(16) 0.0373(12) Uani 1 1 d . . . H10A H -0.1741 0.1664 0.3050 0.056 Uiso 1 1 calc R . . H10B H -0.1818 0.2280 0.3459 0.056 Uiso 1 1 calc R . . H10C H -0.0946 0.1824 0.3502 0.056 Uiso 1 1 calc R . . C11 C -0.1791(3) 0.2902(3) 0.2538(2) 0.0457(13) Uani 1 1 d . . . H11A H -0.1547 0.3244 0.2318 0.069 Uiso 1 1 calc R . . H11B H -0.2179 0.3139 0.2748 0.069 Uiso 1 1 calc R . . H11C H -0.2121 0.2549 0.2317 0.069 Uiso 1 1 calc R . . C12 C 0.1696(3) 0.2646(2) 0.20454(16) 0.0270(10) Uani 1 1 d . . . H12 H 0.1775 0.3074 0.2269 0.032 Uiso 1 1 calc R . . C13 C 0.2524(4) 0.2219(3) 0.2156(2) 0.0588(16) Uani 1 1 d . . . H13A H 0.2621 0.2083 0.2525 0.088 Uiso 1 1 calc R . . H13B H 0.3018 0.2498 0.2077 0.088 Uiso 1 1 calc R . . H13C H 0.2467 0.1799 0.1937 0.088 Uiso 1 1 calc R . . C14 C 0.1544(3) 0.2884(3) 0.14727(17) 0.0443(13) Uani 1 1 d . . . H14A H 0.1482 0.2474 0.1244 0.066 Uiso 1 1 calc R . . H14B H 0.2041 0.3164 0.1400 0.066 Uiso 1 1 calc R . . H14C H 0.1012 0.3166 0.1409 0.066 Uiso 1 1 calc R . . C15 C 0.2175(3) 0.48223(19) 0.32646(14) 0.0170(9) Uani 1 1 d . . . C16 C 0.2318(3) 0.51884(19) 0.37407(14) 0.0165(9) Uani 1 1 d . . . C17 C 0.2805(3) 0.5799(2) 0.37660(15) 0.0236(10) Uani 1 1 d . . . H17 H 0.2880 0.6063 0.4080 0.028 Uiso 1 1 calc R . . C18 C 0.3186(3) 0.6035(2) 0.33457(16) 0.0309(11) Uani 1 1 d . . . H18 H 0.3512 0.6457 0.3371 0.037 Uiso 1 1 calc R . . C19 C 0.3086(3) 0.5651(2) 0.28921(16) 0.0267(10) Uani 1 1 d . . . H19 H 0.3363 0.5803 0.2608 0.032 Uiso 1 1 calc R . . C20 C 0.2587(3) 0.5047(2) 0.28413(15) 0.0222(10) Uani 1 1 d . . . C21 C 0.1939(3) 0.4956(2) 0.42191(14) 0.0206(9) Uani 1 1 d . . . H21 H 0.1818 0.4444 0.4179 0.025 Uiso 1 1 calc R . . C22 C 0.2572(3) 0.5051(3) 0.47259(15) 0.0414(13) Uani 1 1 d . . . H22A H 0.3113 0.4798 0.4701 0.062 Uiso 1 1 calc R . . H22B H 0.2308 0.4868 0.5020 0.062 Uiso 1 1 calc R . . H22C H 0.2701 0.5549 0.4781 0.062 Uiso 1 1 calc R . . C23 C 0.1076(3) 0.5312(3) 0.42594(18) 0.0429(13) Uani 1 1 d . . . H23A H 0.1172 0.5815 0.4312 0.064 Uiso 1 1 calc R . . H23B H 0.0828 0.5117 0.4555 0.064 Uiso 1 1 calc R . . H23C H 0.0672 0.5235 0.3936 0.064 Uiso 1 1 calc R . . C24 C 0.2541(3) 0.4630(2) 0.23331(15) 0.0278(11) Uani 1 1 d . . . H24 H 0.2106 0.4247 0.2343 0.033 Uiso 1 1 calc R . . C25 C 0.3413(4) 0.4296(4) 0.2290(2) 0.082(2) Uani 1 1 d . . . H25A H 0.3370 0.4033 0.1962 0.123 Uiso 1 1 calc R . . H25B H 0.3575 0.3979 0.2585 0.123 Uiso 1 1 calc R . . H25C H 0.3857 0.4661 0.2294 0.123 Uiso 1 1 calc R . . C26 C 0.2250(3) 0.5067(2) 0.18537(15) 0.0364(12) Uani 1 1 d . . . H26A H 0.1696 0.5295 0.1888 0.055 Uiso 1 1 calc R . . H26B H 0.2174 0.4766 0.1544 0.055 Uiso 1 1 calc R . . H26C H 0.2692 0.5422 0.1818 0.055 Uiso 1 1 calc R . . C27 C 0.4983(3) 0.1826(2) 0.42752(14) 0.0195(9) Uani 1 1 d . . . H27 H 0.5527 0.1804 0.4498 0.023 Uiso 1 1 calc R . . C28 C 0.4830(3) 0.1437(2) 0.38432(14) 0.0219(9) Uani 1 1 d . . . H28 H 0.5264 0.1128 0.3753 0.026 Uiso 1 1 calc R . . C29 C 0.4577(3) 0.2821(2) 0.47501(15) 0.0194(9) Uani 1 1 d . . . C30 C 0.4819(3) 0.3474(2) 0.45623(15) 0.0215(9) Uani 1 1 d . . . C31 C 0.5066(3) 0.4009(2) 0.49126(16) 0.0286(11) Uani 1 1 d . . . H31 H 0.5206 0.4454 0.4785 0.034 Uiso 1 1 calc R . . C32 C 0.5112(3) 0.3906(2) 0.54457(17) 0.0335(12) Uani 1 1 d . . . H32 H 0.5287 0.4276 0.5683 0.040 Uiso 1 1 calc R . . C33 C 0.4904(3) 0.3267(2) 0.56270(16) 0.0292(11) Uani 1 1 d . . . H33 H 0.4948 0.3198 0.5993 0.035 Uiso 1 1 calc R . . C34 C 0.4632(3) 0.2715(2) 0.52938(15) 0.0207(9) Uani 1 1 d . . . C35 C 0.4855(3) 0.3605(2) 0.39880(16) 0.0250(10) Uani 1 1 d . . . H35 H 0.4687 0.3160 0.3798 0.030 Uiso 1 1 calc R . . C36 C 0.5756(4) 0.3784(4) 0.3893(2) 0.087(3) Uani 1 1 d . . . H36A H 0.5931 0.4231 0.4061 0.130 Uiso 1 1 calc R . . H36B H 0.5767 0.3820 0.3517 0.130 Uiso 1 1 calc R . . H36C H 0.6160 0.3417 0.4041 0.130 Uiso 1 1 calc R . . C37 C 0.4205(5) 0.4150(3) 0.3772(2) 0.082(2) Uani 1 1 d . . . H37A H 0.3623 0.4013 0.3839 0.122 Uiso 1 1 calc R . . H37B H 0.4204 0.4194 0.3395 0.122 Uiso 1 1 calc R . . H37C H 0.4363 0.4600 0.3941 0.122 Uiso 1 1 calc R . . C38 C 0.4466(3) 0.2009(2) 0.55271(15) 0.0254(10) Uani 1 1 d . . . H38 H 0.4170 0.1706 0.5240 0.030 Uiso 1 1 calc R . . C39 C 0.5321(3) 0.1654(2) 0.57562(18) 0.0421(13) Uani 1 1 d . . . H39A H 0.5688 0.1595 0.5482 0.063 Uiso 1 1 calc R . . H39B H 0.5195 0.1195 0.5896 0.063 Uiso 1 1 calc R . . H39C H 0.5626 0.1943 0.6037 0.063 Uiso 1 1 calc R . . C40 C 0.3864(3) 0.2064(2) 0.59503(16) 0.0313(11) Uani 1 1 d . . . H40A H 0.3783 0.1600 0.6095 0.047 Uiso 1 1 calc R . . H40B H 0.3297 0.2252 0.5794 0.047 Uiso 1 1 calc R . . H40C H 0.4128 0.2377 0.6229 0.047 Uiso 1 1 calc R . . C41 C 0.4034(3) 0.1273(2) 0.29897(14) 0.0196(9) Uani 1 1 d . . . C42 C 0.3522(3) 0.0712(2) 0.27819(15) 0.0242(10) Uani 1 1 d . . . C43 C 0.3624(3) 0.0474(2) 0.22822(16) 0.0328(11) Uani 1 1 d . . . H43 H 0.3285 0.0088 0.2139 0.039 Uiso 1 1 calc R . . C44 C 0.4198(3) 0.0780(3) 0.19926(16) 0.0374(13) Uani 1 1 d . . . H44 H 0.4261 0.0603 0.1657 0.045 Uiso 1 1 calc R . . C45 C 0.4682(3) 0.1346(2) 0.21965(15) 0.0304(11) Uani 1 1 d . . . H45 H 0.5069 0.1565 0.1994 0.037 Uiso 1 1 calc R . . C46 C 0.4614(3) 0.1605(2) 0.26917(15) 0.0228(10) Uani 1 1 d . . . C47 C 0.2910(3) 0.0328(2) 0.30973(16) 0.0303(11) Uani 1 1 d . . . H47 H 0.2740 0.0662 0.3361 0.036 Uiso 1 1 calc R . . C48 C 0.3397(4) -0.0276(3) 0.33936(19) 0.0535(16) Uani 1 1 d . . . H48A H 0.3524 -0.0634 0.3145 0.080 Uiso 1 1 calc R . . H48B H 0.3036 -0.0477 0.3636 0.080 Uiso 1 1 calc R . . H48C H 0.3944 -0.0104 0.3590 0.080 Uiso 1 1 calc R . . C49 C 0.2072(4) 0.0069(3) 0.27633(19) 0.0555(16) Uani 1 1 d . . . H49A H 0.2217 -0.0285 0.2517 0.083 Uiso 1 1 calc R . . H49B H 0.1778 0.0463 0.2570 0.083 Uiso 1 1 calc R . . H49C H 0.1686 -0.0135 0.2990 0.083 Uiso 1 1 calc R . . C50 C 0.5134(3) 0.2252(2) 0.28789(16) 0.0257(10) Uani 1 1 d . . . H50 H 0.4949 0.2403 0.3216 0.031 Uiso 1 1 calc R . . C51 C 0.6121(3) 0.2097(3) 0.29841(19) 0.0425(13) Uani 1 1 d . . . H51A H 0.6331 0.1993 0.2653 0.064 Uiso 1 1 calc R . . H51B H 0.6228 0.1695 0.3219 0.064 Uiso 1 1 calc R . . H51C H 0.6431 0.2506 0.3147 0.064 Uiso 1 1 calc R . . C52 C 0.4972(4) 0.2858(3) 0.24952(19) 0.0467(14) Uani 1 1 d . . . H52A H 0.5169 0.2729 0.2165 0.070 Uiso 1 1 calc R . . H52B H 0.5295 0.3270 0.2642 0.070 Uiso 1 1 calc R . . H52C H 0.4348 0.2965 0.2432 0.070 Uiso 1 1 calc R . . C53 C 0.0425(3) 0.2119(2) 0.48540(15) 0.0214(9) Uani 1 1 d . . . H53A H 0.0130 0.2300 0.5141 0.026 Uiso 1 1 calc R . . H53B H -0.0001 0.1839 0.4618 0.026 Uiso 1 1 calc R . . C54 C 0.1193(3) 0.1663(2) 0.50773(14) 0.0218(9) Uani 1 1 d . . . H54A H 0.0979 0.1232 0.5228 0.026 Uiso 1 1 calc R . . H54B H 0.1566 0.1917 0.5359 0.026 Uiso 1 1 calc R . . C55 C -0.0198(3) 0.3308(2) 0.42398(15) 0.0197(9) Uani 1 1 d . . . C56 C -0.0980(3) 0.3151(2) 0.44213(17) 0.0270(10) Uani 1 1 d . . . H56 H -0.0990 0.2804 0.4683 0.032 Uiso 1 1 calc R . . C57 C -0.1738(3) 0.3495(2) 0.42244(19) 0.0392(12) Uani 1 1 d . . . H57 H -0.2265 0.3383 0.4352 0.047 Uiso 1 1 calc R . . C58 C -0.1738(3) 0.4001(2) 0.38452(19) 0.0374(12) Uani 1 1 d . . . H58 H -0.2264 0.4232 0.3708 0.045 Uiso 1 1 calc R . . C59 C -0.0967(3) 0.4169(2) 0.36647(16) 0.0281(10) Uani 1 1 d . . . H59 H -0.0962 0.4519 0.3405 0.034 Uiso 1 1 calc R . . C60 C -0.0203(3) 0.3827(2) 0.38641(14) 0.0206(9) Uani 1 1 d . . . H60 H 0.0326 0.3949 0.3742 0.025 Uiso 1 1 calc R . . C61 C 0.1323(3) 0.3404(2) 0.50273(14) 0.0193(9) Uani 1 1 d . . . C62 C 0.2209(3) 0.3345(2) 0.52011(15) 0.0216(9) Uani 1 1 d . . . H62 H 0.2558 0.3059 0.5014 0.026 Uiso 1 1 calc R . . C63 C 0.2597(3) 0.3700(2) 0.56486(16) 0.0282(10) Uani 1 1 d . . . H63 H 0.3204 0.3655 0.5766 0.034 Uiso 1 1 calc R . . C64 C 0.2088(3) 0.4117(2) 0.59162(15) 0.0259(10) Uani 1 1 d . . . H64 H 0.2341 0.4356 0.6223 0.031 Uiso 1 1 calc R . . C65 C 0.1210(3) 0.4188(2) 0.57377(16) 0.0282(10) Uani 1 1 d . . . H65 H 0.0868 0.4486 0.5919 0.034 Uiso 1 1 calc R . . C66 C 0.0818(3) 0.3833(2) 0.52991(15) 0.0236(10) Uani 1 1 d . . . H66 H 0.0211 0.3881 0.5184 0.028 Uiso 1 1 calc R . . C67 C 0.2692(3) 0.08862(19) 0.48820(15) 0.0185(9) Uani 1 1 d . . . C68 C 0.3262(3) 0.0579(2) 0.45857(15) 0.0221(9) Uani 1 1 d . . . H68 H 0.3233 0.0703 0.4228 0.027 Uiso 1 1 calc R . . C69 C 0.3872(3) 0.0095(2) 0.48001(16) 0.0261(10) Uani 1 1 d . . . H69 H 0.4248 -0.0118 0.4588 0.031 Uiso 1 1 calc R . . C70 C 0.3936(3) -0.0080(2) 0.53235(17) 0.0314(11) Uani 1 1 d . . . H70 H 0.4355 -0.0412 0.5472 0.038 Uiso 1 1 calc R . . C71 C 0.3382(3) 0.0234(2) 0.56277(16) 0.0281(10) Uani 1 1 d . . . H71 H 0.3432 0.0122 0.5989 0.034 Uiso 1 1 calc R . . C72 C 0.2758(3) 0.0707(2) 0.54124(15) 0.0232(10) Uani 1 1 d . . . H72 H 0.2374 0.0911 0.5624 0.028 Uiso 1 1 calc R . . C73 C 0.1131(3) 0.0785(2) 0.41830(15) 0.0199(9) Uani 1 1 d . . . C74 C 0.0730(3) 0.0925(2) 0.36793(15) 0.0281(11) Uani 1 1 d . . . H74 H 0.0824 0.1359 0.3518 0.034 Uiso 1 1 calc R . . C75 C 0.0186(3) 0.0422(3) 0.34100(18) 0.0390(13) Uani 1 1 d . . . H75 H -0.0088 0.0514 0.3064 0.047 Uiso 1 1 calc R . . C76 C 0.0044(3) -0.0197(2) 0.36385(18) 0.0347(12) Uani 1 1 d . . . H76 H -0.0329 -0.0534 0.3451 0.042 Uiso 1 1 calc R . . C77 C 0.0435(3) -0.0343(2) 0.41375(19) 0.0403(13) Uani 1 1 d . . . H77 H 0.0336 -0.0778 0.4295 0.048 Uiso 1 1 calc R . . C78 C 0.0976(3) 0.0151(2) 0.44091(17) 0.0334(12) Uani 1 1 d . . . H78 H 0.1245 0.0053 0.4755 0.040 Uiso 1 1 calc R . . C79 C 0.2290(5) -0.1489(4) 0.5038(2) 0.089(3) Uani 1 1 d . . . H79A H 0.2463 -0.1076 0.4847 0.107 Uiso 1 1 calc R . . H79B H 0.2805 -0.1797 0.5121 0.107 Uiso 1 1 calc R . . C80 C 0.1970(5) -0.1264(4) 0.5532(2) 0.099(2) Uani 1 1 d U . . H80A H 0.1431 -0.0995 0.5445 0.149 Uiso 1 1 calc R . . H80B H 0.2413 -0.0973 0.5738 0.149 Uiso 1 1 calc R . . H80C H 0.1856 -0.1677 0.5735 0.149 Uiso 1 1 calc R . . C81 C 0.1851(5) -0.2084(4) 0.4250(3) 0.083(2) Uani 1 1 d . . . H81A H 0.2348 -0.2411 0.4319 0.100 Uiso 1 1 calc R . . H81B H 0.2032 -0.1681 0.4051 0.100 Uiso 1 1 calc R . . C82 C 0.1107(6) -0.2436(4) 0.3944(2) 0.097(3) Uani 1 1 d . . . H82A H 0.0950 -0.2849 0.4134 0.145 Uiso 1 1 calc R . . H82B H 0.1262 -0.2579 0.3606 0.145 Uiso 1 1 calc R . . H82C H 0.0610 -0.2115 0.3887 0.145 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 0.01261(8) 0.01241(8) 0.01305(8) 0.00041(6) 0.00231(5) 0.00169(6) Ga1 0.0178(2) 0.0131(2) 0.0141(2) 0.00082(17) 0.00185(18) 0.00005(18) Ga2 0.0133(2) 0.0153(2) 0.0161(2) -0.00141(17) 0.00332(18) 0.00184(18) P1 0.0132(6) 0.0166(5) 0.0178(5) -0.0008(4) 0.0039(4) 0.0030(4) P2 0.0160(6) 0.0145(5) 0.0156(5) 0.0023(4) 0.0031(4) 0.0020(4) O1 0.053(3) 0.052(2) 0.0372(19) -0.0015(17) 0.0064(18) -0.0196(19) N1 0.025(2) 0.0162(17) 0.0144(16) 0.0007(14) -0.0036(14) -0.0031(15) N2 0.023(2) 0.0160(17) 0.0156(16) 0.0012(14) -0.0003(15) -0.0026(15) N3 0.0166(19) 0.0147(17) 0.0207(17) -0.0048(14) 0.0007(14) 0.0005(14) N4 0.019(2) 0.0198(18) 0.0149(16) -0.0005(14) 0.0017(14) 0.0079(15) C1 0.023(3) 0.024(2) 0.015(2) 0.0019(17) -0.0046(18) -0.0013(19) C2 0.020(2) 0.014(2) 0.019(2) 0.0066(17) -0.0043(18) 0.0000(17) C3 0.033(3) 0.014(2) 0.0147(19) 0.0032(17) -0.0026(18) 0.0008(19) C4 0.033(3) 0.025(2) 0.016(2) -0.0030(18) 0.0026(19) -0.009(2) C5 0.044(3) 0.036(3) 0.021(2) -0.004(2) 0.004(2) -0.019(2) C6 0.072(4) 0.027(3) 0.025(2) -0.009(2) 0.011(3) -0.016(3) C7 0.057(4) 0.027(3) 0.026(2) -0.009(2) 0.015(2) -0.006(2) C8 0.038(3) 0.025(2) 0.013(2) -0.0013(18) 0.0030(19) -0.003(2) C9 0.025(3) 0.027(2) 0.031(2) -0.008(2) 0.004(2) -0.006(2) C10 0.041(3) 0.046(3) 0.027(2) 0.005(2) 0.014(2) -0.004(2) C11 0.036(3) 0.041(3) 0.061(3) 0.015(3) 0.011(3) -0.002(3) C12 0.034(3) 0.023(2) 0.025(2) -0.0056(19) 0.007(2) 0.001(2) C13 0.034(4) 0.057(4) 0.082(4) 0.012(3) -0.003(3) 0.005(3) C14 0.045(3) 0.052(3) 0.037(3) 0.013(3) 0.011(2) 0.001(3) C15 0.018(2) 0.014(2) 0.019(2) 0.0018(16) 0.0023(17) 0.0020(17) C16 0.015(2) 0.014(2) 0.019(2) 0.0014(16) 0.0015(17) 0.0034(16) C17 0.024(3) 0.024(2) 0.023(2) -0.0044(18) 0.0025(19) -0.0044(19) C18 0.035(3) 0.026(2) 0.032(3) 0.001(2) 0.008(2) -0.013(2) C19 0.028(3) 0.026(2) 0.028(2) 0.003(2) 0.013(2) -0.006(2) C20 0.027(3) 0.021(2) 0.019(2) 0.0005(18) 0.0043(19) -0.0014(19) C21 0.025(3) 0.019(2) 0.018(2) 0.0001(17) 0.0034(18) -0.0033(18) C22 0.039(3) 0.062(4) 0.021(2) 0.007(2) -0.003(2) -0.017(3) C23 0.044(3) 0.048(3) 0.043(3) 0.014(3) 0.028(3) 0.010(3) C24 0.043(3) 0.022(2) 0.021(2) -0.0007(19) 0.012(2) 0.002(2) C25 0.096(6) 0.110(6) 0.035(3) -0.028(3) -0.010(3) 0.072(5) C26 0.045(3) 0.039(3) 0.023(2) -0.005(2) -0.001(2) -0.001(2) C27 0.017(2) 0.022(2) 0.019(2) 0.0006(18) 0.0024(17) 0.0057(18) C28 0.022(2) 0.024(2) 0.020(2) 0.0013(18) 0.0040(18) 0.0116(19) C29 0.013(2) 0.021(2) 0.024(2) -0.0049(18) 0.0023(17) 0.0026(17) C30 0.016(2) 0.021(2) 0.026(2) 0.0008(18) -0.0013(18) 0.0026(18) C31 0.034(3) 0.017(2) 0.035(3) -0.0046(19) 0.005(2) -0.006(2) C32 0.041(3) 0.026(3) 0.032(3) -0.014(2) 0.001(2) -0.010(2) C33 0.024(3) 0.039(3) 0.022(2) -0.007(2) -0.0019(19) -0.006(2) C34 0.015(2) 0.025(2) 0.022(2) -0.0071(18) 0.0036(17) -0.0002(18) C35 0.025(3) 0.019(2) 0.030(2) 0.0030(19) 0.000(2) 0.0029(19) C36 0.047(4) 0.175(8) 0.042(3) -0.005(4) 0.019(3) -0.037(5) C37 0.126(7) 0.072(4) 0.038(3) -0.010(3) -0.020(4) 0.063(4) C38 0.030(3) 0.024(2) 0.021(2) -0.0037(19) 0.0031(19) 0.002(2) C39 0.046(4) 0.034(3) 0.046(3) 0.004(2) 0.008(3) 0.011(2) C40 0.038(3) 0.031(3) 0.025(2) 0.002(2) 0.004(2) 0.001(2) C41 0.022(2) 0.020(2) 0.016(2) -0.0007(17) 0.0016(18) 0.0099(18) C42 0.028(3) 0.021(2) 0.023(2) -0.0025(18) -0.0001(19) 0.0108(19) C43 0.041(3) 0.032(3) 0.023(2) -0.011(2) -0.001(2) 0.007(2) C44 0.047(3) 0.051(3) 0.014(2) -0.009(2) 0.006(2) 0.011(3) C45 0.029(3) 0.042(3) 0.022(2) -0.002(2) 0.012(2) 0.011(2) C46 0.019(2) 0.027(2) 0.022(2) -0.0052(19) 0.0002(18) 0.0106(19) C47 0.038(3) 0.025(2) 0.028(2) -0.006(2) 0.003(2) -0.003(2) C48 0.082(5) 0.036(3) 0.042(3) 0.002(3) 0.009(3) 0.008(3) C49 0.054(4) 0.068(4) 0.044(3) -0.015(3) 0.006(3) -0.027(3) C50 0.023(3) 0.029(2) 0.026(2) -0.0002(19) 0.0081(19) 0.004(2) C51 0.031(3) 0.045(3) 0.051(3) -0.005(3) 0.006(2) 0.004(2) C52 0.053(4) 0.035(3) 0.048(3) 0.006(3) -0.004(3) 0.005(3) C53 0.020(2) 0.022(2) 0.024(2) 0.0005(18) 0.0083(18) 0.0007(18) C54 0.023(3) 0.025(2) 0.018(2) 0.0043(18) 0.0068(18) 0.0019(19) C55 0.023(2) 0.014(2) 0.021(2) -0.0045(17) 0.0028(18) 0.0003(17) C56 0.019(2) 0.026(2) 0.037(3) 0.003(2) 0.008(2) 0.0021(19) C57 0.017(3) 0.035(3) 0.066(3) -0.005(3) 0.008(2) 0.003(2) C58 0.020(3) 0.029(3) 0.059(3) -0.006(2) -0.007(2) 0.011(2) C59 0.029(3) 0.024(2) 0.029(2) 0.0014(19) -0.003(2) 0.013(2) C60 0.018(2) 0.024(2) 0.020(2) -0.0056(18) 0.0023(18) 0.0011(18) C61 0.021(2) 0.018(2) 0.018(2) 0.0002(17) 0.0012(18) 0.0002(18) C62 0.018(2) 0.021(2) 0.027(2) -0.0048(18) 0.0054(18) 0.0044(18) C63 0.023(3) 0.029(2) 0.029(2) -0.006(2) -0.009(2) 0.000(2) C64 0.032(3) 0.025(2) 0.020(2) -0.0026(19) 0.002(2) -0.003(2) C65 0.029(3) 0.026(2) 0.030(2) -0.006(2) 0.008(2) 0.005(2) C66 0.021(3) 0.022(2) 0.028(2) -0.0050(19) 0.0050(19) 0.0034(19) C67 0.020(2) 0.0111(19) 0.023(2) 0.0033(17) -0.0005(18) -0.0039(17) C68 0.023(3) 0.022(2) 0.022(2) 0.0035(18) 0.0034(18) 0.0036(19) C69 0.022(3) 0.023(2) 0.034(3) 0.003(2) 0.006(2) 0.0034(19) C70 0.024(3) 0.025(2) 0.042(3) 0.010(2) -0.003(2) 0.005(2) C71 0.026(3) 0.030(3) 0.028(2) 0.012(2) 0.001(2) 0.002(2) C72 0.026(3) 0.021(2) 0.023(2) 0.0026(18) 0.0053(19) 0.0002(19) C73 0.020(2) 0.017(2) 0.022(2) -0.0035(17) 0.0018(18) 0.0013(18) C74 0.034(3) 0.024(2) 0.024(2) 0.0003(19) -0.002(2) -0.005(2) C75 0.041(3) 0.042(3) 0.030(3) -0.006(2) -0.009(2) -0.011(3) C76 0.030(3) 0.031(3) 0.041(3) -0.014(2) -0.002(2) -0.007(2) C77 0.044(3) 0.022(3) 0.052(3) 0.007(2) 0.000(3) -0.015(2) C78 0.041(3) 0.023(2) 0.033(3) 0.005(2) -0.006(2) -0.009(2) C79 0.086(6) 0.113(6) 0.065(4) 0.006(4) -0.002(4) -0.062(5) C80 0.123(5) 0.099(4) 0.073(4) 0.001(3) 0.005(3) -0.062(4) C81 0.074(6) 0.107(6) 0.077(5) -0.017(4) 0.039(4) -0.015(5) C82 0.143(8) 0.092(6) 0.057(4) -0.031(4) 0.022(5) -0.038(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.3016(10) . ? Pt1 P1 2.3138(11) . ? Pt1 Ga1 2.4157(6) . ? Pt1 Ga2 2.4167(7) . ? Ga1 N1 1.902(3) . ? Ga1 N2 1.911(3) . ? Ga2 N3 1.911(3) . ? Ga2 N4 1.913(3) . ? P1 C61 1.827(4) . ? P1 C55 1.829(4) . ? P1 C53 1.843(4) . ? P2 C67 1.819(4) . ? P2 C73 1.829(4) . ? P2 C54 1.829(4) . ? O1 C79 1.407(6) . ? O1 C81 1.408(6) . ? N1 C1 1.397(5) . ? N1 C3 1.442(5) . ? N2 C2 1.409(5) . ? N2 C15 1.430(5) . ? N3 C27 1.384(5) . ? N3 C29 1.440(5) . ? N4 C28 1.402(5) . ? N4 C41 1.447(4) . ? C1 C2 1.339(5) . ? C3 C4 1.403(6) . ? C3 C8 1.408(6) . ? C4 C5 1.395(6) . ? C4 C9 1.518(6) . ? C5 C6 1.385(6) . ? C6 C7 1.372(6) . ? C7 C8 1.392(6) . ? C8 C12 1.510(6) . ? C9 C10 1.522(6) . ? C9 C11 1.538(6) . ? C12 C13 1.514(6) . ? C12 C14 1.535(6) . ? C15 C16 1.406(5) . ? C15 C20 1.414(5) . ? C16 C17 1.389(5) . ? C16 C21 1.513(5) . ? C17 C18 1.388(5) . ? C18 C19 1.375(6) . ? C19 C20 1.388(5) . ? C20 C24 1.531(5) . ? C21 C23 1.520(6) . ? C21 C22 1.530(5) . ? C24 C26 1.509(6) . ? C24 C25 1.515(7) . ? C27 C28 1.335(5) . ? C29 C34 1.411(5) . ? C29 C30 1.412(5) . ? C30 C31 1.384(5) . ? C30 C35 1.516(5) . ? C31 C32 1.385(6) . ? C32 C33 1.365(6) . ? C33 C34 1.390(5) . ? C34 C38 1.519(6) . ? C35 C36 1.493(6) . ? C35 C37 1.502(6) . ? C38 C39 1.530(6) . ? C38 C40 1.544(6) . ? C41 C42 1.397(6) . ? C41 C46 1.418(6) . ? C42 C43 1.402(5) . ? C42 C47 1.528(6) . ? C43 C44 1.377(6) . ? C44 C45 1.379(6) . ? C45 C46 1.392(5) . ? C46 C50 1.518(6) . ? C47 C48 1.524(6) . ? C47 C49 1.534(6) . ? C50 C52 1.523(6) . ? C50 C51 1.544(6) . ? C53 C54 1.521(5) . ? C55 C60 1.389(5) . ? C55 C56 1.396(6) . ? C56 C57 1.379(6) . ? C57 C58 1.378(6) . ? C58 C59 1.385(6) . ? C59 C60 1.387(5) . ? C61 C62 1.387(5) . ? C61 C66 1.394(5) . ? C62 C63 1.401(5) . ? C63 C64 1.379(6) . ? C64 C65 1.379(6) . ? C65 C66 1.385(6) . ? C67 C68 1.384(5) . ? C67 C72 1.404(5) . ? C68 C69 1.382(5) . ? C69 C70 1.384(6) . ? C70 C71 1.384(6) . ? C71 C72 1.382(6) . ? C73 C78 1.384(5) . ? C73 C74 1.386(5) . ? C74 C75 1.398(6) . ? C75 C76 1.357(6) . ? C76 C77 1.372(6) . ? C77 C78 1.385(6) . ? C79 C80 1.502(8) . ? C81 C82 1.465(9) . ? 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 85.18(4) . . ? P2 Pt1 Ga1 162.49(3) . . ? P1 Pt1 Ga1 93.30(3) . . ? P2 Pt1 Ga2 93.01(3) . . ? P1 Pt1 Ga2 160.61(3) . . ? Ga1 Pt1 Ga2 94.05(3) . . ? N1 Ga1 N2 87.91(13) . . ? N1 Ga1 Pt1 118.98(10) . . ? N2 Ga1 Pt1 145.51(9) . . ? N3 Ga2 N4 88.17(13) . . ? N3 Ga2 Pt1 119.21(10) . . ? N4 Ga2 Pt1 146.46(10) . . ? C61 P1 C55 104.44(18) . . ? C61 P1 C53 100.89(18) . . ? C55 P1 C53 102.44(19) . . ? C61 P1 Pt1 108.04(14) . . ? C55 P1 Pt1 130.33(13) . . ? C53 P1 Pt1 107.02(13) . . ? C67 P2 C73 100.67(18) . . ? C67 P2 C54 103.61(18) . . ? C73 P2 C54 102.36(19) . . ? C67 P2 Pt1 129.77(13) . . ? C73 P2 Pt1 109.79(13) . . ? C54 P2 Pt1 107.47(13) . . ? C79 O1 C81 112.9(5) . . ? C1 N1 C3 118.1(3) . . ? C1 N1 Ga1 108.9(2) . . ? C3 N1 Ga1 130.1(3) . . ? C2 N2 C15 114.3(3) . . ? C2 N2 Ga1 107.5(2) . . ? C15 N2 Ga1 135.5(3) . . ? C27 N3 C29 116.5(3) . . ? C27 N3 Ga2 108.1(2) . . ? C29 N3 Ga2 132.4(3) . . ? C28 N4 C41 113.8(3) . . ? C28 N4 Ga2 106.7(2) . . ? C41 N4 Ga2 135.1(2) . . ? C2 C1 N1 117.0(4) . . ? C1 C2 N2 118.5(3) . . ? C4 C3 C8 120.7(4) . . ? C4 C3 N1 120.7(4) . . ? C8 C3 N1 118.6(4) . . ? C5 C4 C3 118.4(4) . . ? C5 C4 C9 120.3(4) . . ? C3 C4 C9 121.2(4) . . ? C6 C5 C4 121.3(4) . . ? C7 C6 C5 119.4(4) . . ? C6 C7 C8 121.8(4) . . ? C7 C8 C3 118.1(4) . . ? C7 C8 C12 119.5(4) . . ? C3 C8 C12 122.3(4) . . ? C4 C9 C10 112.8(4) . . ? C4 C9 C11 110.4(4) . . ? C10 C9 C11 109.9(4) . . ? C8 C12 C13 112.3(4) . . ? C8 C12 C14 110.6(4) . . ? C13 C12 C14 110.4(4) . . ? C16 C15 C20 119.8(4) . . ? C16 C15 N2 120.3(3) . . ? C20 C15 N2 119.8(3) . . ? C17 C16 C15 118.4(4) . . ? C17 C16 C21 118.9(3) . . ? C15 C16 C21 122.7(3) . . ? C18 C17 C16 122.0(4) . . ? C19 C18 C17 119.1(4) . . ? C18 C19 C20 121.3(4) . . ? C19 C20 C15 119.3(4) . . ? C19 C20 C24 118.1(4) . . ? C15 C20 C24 122.5(4) . . ? C16 C21 C23 112.1(3) . . ? C16 C21 C22 112.9(3) . . ? C23 C21 C22 110.4(4) . . ? C26 C24 C25 109.6(4) . . ? C26 C24 C20 112.9(3) . . ? C25 C24 C20 110.7(4) . . ? C28 C27 N3 117.8(4) . . ? C27 C28 N4 119.1(4) . . ? C34 C29 C30 119.3(4) . . ? C34 C29 N3 120.8(4) . . ? C30 C29 N3 119.8(3) . . ? C31 C30 C29 119.5(4) . . ? C31 C30 C35 118.2(4) . . ? C29 C30 C35 122.3(4) . . ? C30 C31 C32 121.1(4) . . ? C33 C32 C31 119.3(4) . . ? C32 C33 C34 122.2(4) . . ? C33 C34 C29 118.6(4) . . ? C33 C34 C38 119.0(4) . . ? C29 C34 C38 122.3(3) . . ? C36 C35 C37 112.0(5) . . ? C36 C35 C30 111.6(4) . . ? C37 C35 C30 111.1(4) . . ? C34 C38 C39 111.2(4) . . ? C34 C38 C40 112.1(3) . . ? C39 C38 C40 109.7(4) . . ? C42 C41 C46 120.4(3) . . ? C42 C41 N4 120.2(4) . . ? C46 C41 N4 119.3(4) . . ? C41 C42 C43 118.1(4) . . ? C41 C42 C47 121.8(4) . . ? C43 C42 C47 119.9(4) . . ? C44 C43 C42 122.2(4) . . ? C43 C44 C45 119.1(4) . . ? C44 C45 C46 121.5(4) . . ? C45 C46 C41 118.7(4) . . ? C45 C46 C50 118.4(4) . . ? C41 C46 C50 122.8(3) . . ? C48 C47 C42 109.4(4) . . ? C48 C47 C49 110.8(4) . . ? C42 C47 C49 113.3(4) . . ? C46 C50 C52 112.6(4) . . ? C46 C50 C51 111.5(4) . . ? C52 C50 C51 109.0(4) . . ? C54 C53 P1 109.6(3) . . ? C53 C54 P2 109.2(3) . . ? C60 C55 C56 118.3(4) . . ? C60 C55 P1 120.2(3) . . ? C56 C55 P1 121.5(3) . . ? C57 C56 C55 120.6(4) . . ? C58 C57 C56 120.7(5) . . ? C57 C58 C59 119.6(4) . . ? C58 C59 C60 119.9(4) . . ? C59 C60 C55 120.9(4) . . ? C62 C61 C66 119.2(4) . . ? C62 C61 P1 119.8(3) . . ? C66 C61 P1 120.7(3) . . ? C61 C62 C63 120.9(4) . . ? C64 C63 C62 119.2(4) . . ? C65 C64 C63 119.9(4) . . ? C64 C65 C66 121.3(4) . . ? C65 C66 C61 119.4(4) . . ? C68 C67 C72 118.4(4) . . ? C68 C67 P2 118.7(3) . . ? C72 C67 P2 122.6(3) . . ? C69 C68 C67 121.2(4) . . ? C68 C69 C70 120.1(4) . . ? C71 C70 C69 119.4(4) . . ? C72 C71 C70 120.8(4) . . ? C71 C72 C67 120.1(4) . . ? C78 C73 C74 119.0(4) . . ? C78 C73 P2 120.1(3) . . ? C74 C73 P2 120.9(3) . . ? C73 C74 C75 119.4(4) . . ? C76 C75 C74 120.6(4) . . ? C75 C76 C77 120.7(4) . . ? C76 C77 C78 119.3(4) . . ? C73 C78 C77 120.9(4) . . ? O1 C79 C80 108.5(5) . . ? O1 C81 C82 109.5(5) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.799 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.121 # Attachment 'compound14.CIF' data_compound14 _database_code_depnum_ccdc_archive 'CCDC 664054' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H88 Ga2 N6 Ni' _chemical_formula_weight 1067.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.104(4) _cell_length_b 12.811(3) _cell_length_c 20.515(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.04(3) _cell_angle_gamma 90.00 _cell_volume 5583.2(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 1.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_T_max 0.936 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8566 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.1059 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4825 _reflns_number_gt 3225 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0134P)^2^+8.8652P] 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 4825 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1009 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.059251(18) 0.21621(3) 0.232075(19) 0.02152(13) Uani 1 1 d . . . Ni1 Ni 0.0000 0.35578(6) 0.2500 0.02245(19) Uani 1 2 d S . . N1 N 0.07691(13) 0.1774(2) 0.14928(14) 0.0216(8) Uani 1 1 d . . . C1 C 0.11488(16) 0.0879(3) 0.16020(19) 0.0259(9) Uani 1 1 d . . . H1 H 0.1276 0.0557 0.1244 0.031 Uiso 1 1 calc R . . N2 N 0.11072(13) 0.1023(2) 0.27293(14) 0.0218(8) Uani 1 1 d . . . C2 C 0.13222(16) 0.0503(3) 0.22330(18) 0.0256(10) Uani 1 1 d . . . H2 H 0.1583 -0.0098 0.2343 0.031 Uiso 1 1 calc R . . N3 N 0.05983(14) 0.4723(2) 0.23903(15) 0.0291(8) Uani 1 1 d . . . C3 C 0.07662(17) 0.2418(3) 0.09209(17) 0.0232(9) Uani 1 1 d . . . C4 C 0.13365(16) 0.2812(3) 0.08344(17) 0.0266(9) Uani 1 1 d . . . C5 C 0.13144(19) 0.3456(3) 0.0281(2) 0.0367(11) Uani 1 1 d . . . H5 H 0.1696 0.3701 0.0209 0.044 Uiso 1 1 calc R . . C6 C 0.07458(19) 0.3745(4) -0.0167(2) 0.0421(12) Uani 1 1 d . . . H6 H 0.0737 0.4200 -0.0535 0.051 Uiso 1 1 calc R . . C7 C 0.01911(18) 0.3364(3) -0.0070(2) 0.0348(11) Uani 1 1 d . . . H7 H -0.0198 0.3570 -0.0374 0.042 Uiso 1 1 calc R . . C8 C 0.01859(17) 0.2688(3) 0.04590(18) 0.0264(10) Uani 1 1 d . . . C9 C 0.19724(16) 0.2636(3) 0.13514(18) 0.0302(10) Uani 1 1 d . . . H9 H 0.1894 0.2257 0.1746 0.036 Uiso 1 1 calc R . . C10 C 0.24052(18) 0.1948(4) 0.1059(2) 0.0443(12) Uani 1 1 d . . . H10A H 0.2199 0.1277 0.0915 0.066 Uiso 1 1 calc R . . H10B H 0.2803 0.1829 0.1408 0.066 Uiso 1 1 calc R . . H10C H 0.2489 0.2300 0.0669 0.066 Uiso 1 1 calc R . . C11 C 0.23059(18) 0.3658(3) 0.1617(2) 0.0370(11) Uani 1 1 d . . . H11A H 0.2431 0.4012 0.1251 0.055 Uiso 1 1 calc R . . H11B H 0.2681 0.3510 0.1991 0.055 Uiso 1 1 calc R . . H11C H 0.2020 0.4109 0.1780 0.055 Uiso 1 1 calc R . . C12 C -0.04367(16) 0.2279(3) 0.05239(18) 0.0299(10) Uani 1 1 d . . . H12 H -0.0342 0.1768 0.0907 0.036 Uiso 1 1 calc R . . C13 C -0.07962(19) 0.1689(4) -0.0119(2) 0.0494(13) Uani 1 1 d . . . H13A H -0.1187 0.1404 -0.0054 0.074 Uiso 1 1 calc R . . H13B H -0.0534 0.1117 -0.0206 0.074 Uiso 1 1 calc R . . H13C H -0.0896 0.2169 -0.0506 0.074 Uiso 1 1 calc R . . C14 C -0.08434(19) 0.3131(4) 0.0696(2) 0.0528(14) Uani 1 1 d . . . H14A H -0.0929 0.3665 0.0340 0.079 Uiso 1 1 calc R . . H14B H -0.0622 0.3449 0.1131 0.079 Uiso 1 1 calc R . . H14C H -0.1241 0.2829 0.0729 0.079 Uiso 1 1 calc R . . C15 C 0.14499(16) 0.0786(3) 0.34170(17) 0.0241(9) Uani 1 1 d . . . C16 C 0.20193(16) 0.1309(3) 0.37159(18) 0.0234(9) Uani 1 1 d . . . C17 C 0.23546(17) 0.1032(3) 0.43762(19) 0.0308(10) Uani 1 1 d . . . H17 H 0.2734 0.1390 0.4591 0.037 Uiso 1 1 calc R . . C18 C 0.21455(18) 0.0251(3) 0.47202(19) 0.0327(11) Uani 1 1 d . . . H18 H 0.2383 0.0070 0.5167 0.039 Uiso 1 1 calc R . . C19 C 0.15944(18) -0.0267(3) 0.44198(18) 0.0306(10) Uani 1 1 d . . . H19 H 0.1458 -0.0813 0.4659 0.037 Uiso 1 1 calc R . . C20 C 0.12326(17) -0.0002(3) 0.37687(18) 0.0257(10) Uani 1 1 d . . . C21 C 0.22995(17) 0.2122(3) 0.33428(19) 0.0301(10) Uani 1 1 d . . . H21 H 0.1967 0.2318 0.2921 0.036 Uiso 1 1 calc R . . C22 C 0.28534(18) 0.1648(4) 0.3127(2) 0.0417(12) Uani 1 1 d . . . H22A H 0.3180 0.1421 0.3531 0.062 Uiso 1 1 calc R . . H22B H 0.3028 0.2175 0.2884 0.062 Uiso 1 1 calc R . . H22C H 0.2705 0.1048 0.2830 0.062 Uiso 1 1 calc R . . C23 C 0.25039(18) 0.3121(3) 0.3756(2) 0.0407(12) Uani 1 1 d . . . H23A H 0.2148 0.3401 0.3899 0.061 Uiso 1 1 calc R . . H23B H 0.2642 0.3639 0.3477 0.061 Uiso 1 1 calc R . . H23C H 0.2852 0.2961 0.4157 0.061 Uiso 1 1 calc R . . C24 C 0.06387(18) -0.0621(3) 0.3448(2) 0.0348(11) Uani 1 1 d . . . H24 H 0.0394 -0.0221 0.3042 0.042 Uiso 1 1 calc R . . C25 C 0.0799(2) -0.1673(4) 0.3199(3) 0.0673(16) Uani 1 1 d . . . H25A H 0.1037 -0.1568 0.2866 0.101 Uiso 1 1 calc R . . H25B H 0.0410 -0.2054 0.2987 0.101 Uiso 1 1 calc R . . H25C H 0.1054 -0.2076 0.3583 0.101 Uiso 1 1 calc R . . C26 C 0.02131(19) -0.0766(4) 0.3908(2) 0.0472(12) Uani 1 1 d . . . H26A H 0.0424 -0.1209 0.4293 0.071 Uiso 1 1 calc R . . H26B H -0.0180 -0.1099 0.3653 0.071 Uiso 1 1 calc R . . H26C H 0.0120 -0.0085 0.4074 0.071 Uiso 1 1 calc R . . C27 C 0.03439(19) 0.5688(4) 0.2611(3) 0.0533(14) Uani 1 1 d . . . H27A H 0.0488 0.5741 0.3112 0.064 Uiso 1 1 calc R . . H27B H 0.0505 0.6303 0.2420 0.064 Uiso 1 1 calc R . . C28 C 0.12578(18) 0.4616(4) 0.2817(2) 0.0461(13) Uani 1 1 d . . . H28A H 0.1497 0.5239 0.2766 0.069 Uiso 1 1 calc R . . H28B H 0.1450 0.3999 0.2673 0.069 Uiso 1 1 calc R . . H28C H 0.1261 0.4538 0.3293 0.069 Uiso 1 1 calc R . . C29 C 0.06130(19) 0.4822(3) 0.1677(2) 0.0394(11) Uani 1 1 d . . . H29A H 0.0182 0.4897 0.1384 0.059 Uiso 1 1 calc R . . H29B H 0.0806 0.4197 0.1545 0.059 Uiso 1 1 calc R . . H29C H 0.0860 0.5438 0.1630 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.0201(2) 0.0214(3) 0.0231(2) 0.0002(2) 0.00602(17) 0.0009(2) Ni1 0.0202(4) 0.0201(4) 0.0279(4) 0.000 0.0080(3) 0.000 N1 0.0202(16) 0.022(2) 0.0224(17) -0.0001(15) 0.0053(14) 0.0005(14) C1 0.028(2) 0.025(3) 0.027(2) -0.007(2) 0.0125(18) 0.0023(19) N2 0.0248(17) 0.021(2) 0.0193(16) -0.0019(15) 0.0049(14) 0.0051(15) C2 0.022(2) 0.025(3) 0.028(2) -0.005(2) 0.0056(18) 0.0043(18) N3 0.0289(18) 0.023(2) 0.036(2) -0.0001(17) 0.0108(16) -0.0031(16) C3 0.027(2) 0.023(2) 0.022(2) -0.0005(18) 0.0095(18) -0.0028(18) C4 0.028(2) 0.030(3) 0.024(2) 0.003(2) 0.0089(18) 0.001(2) C5 0.032(2) 0.044(3) 0.036(2) 0.000(2) 0.012(2) -0.009(2) C6 0.043(3) 0.051(3) 0.032(2) 0.015(2) 0.010(2) -0.007(2) C7 0.026(2) 0.041(3) 0.033(2) 0.013(2) 0.0027(19) -0.001(2) C8 0.024(2) 0.027(3) 0.028(2) 0.000(2) 0.0069(18) -0.0038(19) C9 0.025(2) 0.039(3) 0.026(2) -0.002(2) 0.0063(18) -0.005(2) C10 0.031(2) 0.052(3) 0.048(3) -0.005(2) 0.008(2) 0.004(2) C11 0.031(2) 0.042(3) 0.037(2) -0.001(2) 0.008(2) -0.008(2) C12 0.021(2) 0.039(3) 0.029(2) 0.011(2) 0.0064(18) 0.005(2) C13 0.035(3) 0.072(4) 0.037(3) 0.005(2) 0.004(2) -0.017(2) C14 0.036(3) 0.062(4) 0.067(3) 0.016(3) 0.025(2) 0.006(2) C15 0.024(2) 0.025(3) 0.021(2) -0.0020(19) 0.0032(18) 0.0077(19) C16 0.023(2) 0.023(3) 0.024(2) -0.0033(19) 0.0064(18) 0.0062(18) C17 0.021(2) 0.034(3) 0.034(2) -0.007(2) 0.0017(19) 0.0033(19) C18 0.030(2) 0.039(3) 0.026(2) 0.003(2) 0.0017(19) 0.010(2) C19 0.034(2) 0.030(3) 0.030(2) 0.005(2) 0.012(2) 0.008(2) C20 0.024(2) 0.027(3) 0.026(2) 0.001(2) 0.0057(18) 0.0053(19) C21 0.025(2) 0.032(3) 0.032(2) 0.002(2) 0.0057(18) 0.000(2) C22 0.037(3) 0.046(3) 0.047(3) 0.003(2) 0.021(2) 0.001(2) C23 0.033(2) 0.042(3) 0.045(3) -0.009(2) 0.006(2) -0.006(2) C24 0.032(2) 0.031(3) 0.038(2) 0.008(2) 0.003(2) -0.005(2) C25 0.056(3) 0.070(4) 0.079(4) -0.037(3) 0.023(3) -0.026(3) C26 0.034(3) 0.042(3) 0.069(3) 0.001(3) 0.020(2) -0.001(2) C27 0.060(3) 0.030(3) 0.082(4) -0.011(3) 0.040(3) -0.009(2) C28 0.031(2) 0.055(4) 0.048(3) 0.008(2) 0.004(2) -0.021(2) C29 0.039(3) 0.035(3) 0.044(3) 0.005(2) 0.011(2) -0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N2 1.897(3) . ? Ga1 N1 1.911(3) . ? Ga1 Ni1 2.3051(8) . ? Ni1 N3 2.047(3) . ? Ni1 N3 2.047(3) 2 ? Ni1 Ga1 2.3051(8) 2 ? N1 C1 1.401(4) . ? N1 C3 1.433(4) . ? C1 C2 1.335(5) . ? N2 C2 1.405(4) . ? N2 C15 1.437(4) . ? N3 C29 1.478(5) . ? N3 C27 1.481(5) . ? N3 C28 1.485(5) . ? C3 C8 1.411(5) . ? C3 C4 1.414(5) . ? C4 C5 1.393(5) . ? C4 C9 1.525(5) . ? C5 C6 1.387(5) . ? C6 C7 1.384(5) . ? C7 C8 1.391(5) . ? C8 C12 1.512(5) . ? C9 C11 1.527(5) . ? C9 C10 1.539(5) . ? C12 C14 1.516(5) . ? C12 C13 1.537(5) . ? C15 C20 1.401(5) . ? C15 C16 1.408(5) . ? C16 C17 1.398(5) . ? C16 C21 1.522(5) . ? C17 C18 1.376(5) . ? C18 C19 1.375(5) . ? C19 C20 1.396(5) . ? C20 C24 1.519(5) . ? C21 C23 1.533(5) . ? C21 C22 1.537(5) . ? C24 C26 1.516(5) . ? C24 C25 1.518(6) . ? C27 C27 1.461(8) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ga1 N1 87.00(12) . . ? N2 Ga1 Ni1 145.48(9) . . ? N1 Ga1 Ni1 127.47(9) . . ? N3 Ni1 N3 86.41(18) . 2 ? N3 Ni1 Ga1 174.69(9) . 2 ? N3 Ni1 Ga1 97.76(9) 2 2 ? N3 Ni1 Ga1 97.76(9) . . ? N3 Ni1 Ga1 174.69(9) 2 . ? Ga1 Ni1 Ga1 78.27(3) 2 . ? C1 N1 C3 117.9(3) . . ? C1 N1 Ga1 109.3(2) . . ? C3 N1 Ga1 128.5(2) . . ? C2 C1 N1 116.7(3) . . ? C2 N2 C15 114.8(3) . . ? C2 N2 Ga1 109.0(2) . . ? C15 N2 Ga1 133.3(2) . . ? C1 C2 N2 117.9(3) . . ? C29 N3 C27 110.2(3) . . ? C29 N3 C28 107.8(3) . . ? C27 N3 C28 106.9(3) . . ? C29 N3 Ni1 111.3(2) . . ? C27 N3 Ni1 105.3(2) . . ? C28 N3 Ni1 115.3(2) . . ? C8 C3 C4 120.3(3) . . ? C8 C3 N1 119.3(3) . . ? C4 C3 N1 120.4(3) . . ? C5 C4 C3 118.8(3) . . ? C5 C4 C9 118.2(3) . . ? C3 C4 C9 122.9(3) . . ? C6 C5 C4 121.3(4) . . ? C7 C6 C5 119.2(4) . . ? C6 C7 C8 122.0(4) . . ? C7 C8 C3 118.4(3) . . ? C7 C8 C12 119.2(3) . . ? C3 C8 C12 122.4(3) . . ? C4 C9 C11 112.5(3) . . ? C4 C9 C10 111.5(3) . . ? C11 C9 C10 109.8(3) . . ? C8 C12 C14 112.6(4) . . ? C8 C12 C13 111.2(3) . . ? C14 C12 C13 110.8(3) . . ? C20 C15 C16 120.7(3) . . ? C20 C15 N2 119.7(3) . . ? C16 C15 N2 119.5(3) . . ? C17 C16 C15 118.2(4) . . ? C17 C16 C21 118.7(3) . . ? C15 C16 C21 123.1(3) . . ? C18 C17 C16 121.2(4) . . ? C19 C18 C17 120.2(4) . . ? C18 C19 C20 120.9(4) . . ? C19 C20 C15 118.7(3) . . ? C19 C20 C24 119.0(4) . . ? C15 C20 C24 122.1(3) . . ? C16 C21 C23 113.1(3) . . ? C16 C21 C22 110.0(3) . . ? C23 C21 C22 110.6(3) . . ? C26 C24 C25 110.1(4) . . ? C26 C24 C20 114.0(3) . . ? C25 C24 C20 110.8(3) . . ? C27 C27 N3 110.8(3) 2 . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.383 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.085 # Attachment 'compound15.CIF' data_compound15 _database_code_depnum_ccdc_archive 'CCDC 664055' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H88 Ga2 N6 Pd' _chemical_formula_weight 1115.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.248(4) _cell_length_b 13.012(3) _cell_length_c 20.412(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.17(3) _cell_angle_gamma 90.00 _cell_volume 5646(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 1.304 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.680 _exptl_absorpt_correction_T_max 0.961 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7384 _diffrn_reflns_av_R_equivalents 0.0596 _diffrn_reflns_av_sigmaI/netI 0.1290 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4958 _reflns_number_gt 3166 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0140P)^2^+20.0963P] 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 4958 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1210 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_ref 0.1015 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.5000 0.15689(5) 0.2500 0.01989(18) Uani 1 2 d S . . Ga1 Ga 0.55964(3) 0.29624(5) 0.23035(3) 0.01892(18) Uani 1 1 d . . . N1 N 0.5614(2) 0.0276(3) 0.2371(3) 0.0286(12) Uani 1 1 d . . . N3 N 0.61338(18) 0.4057(3) 0.2721(2) 0.0182(11) Uani 1 1 d . . . N2 N 0.57835(18) 0.3281(3) 0.1473(2) 0.0203(11) Uani 1 1 d . . . C1 C 0.6352(2) 0.4541(4) 0.2210(3) 0.0241(14) Uani 1 1 d . . . H1 H 0.6612 0.5134 0.2311 0.029 Uiso 1 1 calc R . . C2 C 0.6175(2) 0.4127(4) 0.1580(3) 0.0214(13) Uani 1 1 d . . . H2 H 0.6314 0.4407 0.1220 0.026 Uiso 1 1 calc R . . C3 C 0.6462(2) 0.4289(4) 0.3409(3) 0.0183(13) Uani 1 1 d . . . C4 C 0.6255(2) 0.5085(4) 0.3757(3) 0.0225(14) Uani 1 1 d . . . C5 C 0.6607(3) 0.5333(4) 0.4423(3) 0.0299(15) Uani 1 1 d . . . H5 H 0.6471 0.5873 0.4658 0.036 Uiso 1 1 calc R . . C6 C 0.7156(2) 0.4799(4) 0.4748(3) 0.0283(15) Uani 1 1 d . . . H6 H 0.7390 0.4966 0.5206 0.034 Uiso 1 1 calc R . . C7 C 0.7357(3) 0.4026(5) 0.4402(3) 0.0313(15) Uani 1 1 d . . . H7 H 0.7733 0.3665 0.4626 0.038 Uiso 1 1 calc R . . C8 C 0.7029(2) 0.3761(4) 0.3741(3) 0.0232(14) Uani 1 1 d . . . C9 C 0.5666(3) 0.5695(5) 0.3401(3) 0.0318(15) Uani 1 1 d . . . H9 H 0.5440 0.5322 0.2971 0.038 Uiso 1 1 calc R . . C10 C 0.5834(3) 0.6755(5) 0.3202(4) 0.063(2) Uani 1 1 d . . . H10A H 0.6069 0.7130 0.3614 0.094 Uiso 1 1 calc R . . H10B H 0.5448 0.7131 0.2971 0.094 Uiso 1 1 calc R . . H10C H 0.6094 0.6688 0.2891 0.094 Uiso 1 1 calc R . . C11 C 0.5217(3) 0.5785(5) 0.3837(3) 0.0475(19) Uani 1 1 d . . . H11A H 0.5101 0.5097 0.3952 0.071 Uiso 1 1 calc R . . H11B H 0.4838 0.6156 0.3579 0.071 Uiso 1 1 calc R . . H11C H 0.5424 0.6161 0.4259 0.071 Uiso 1 1 calc R . . C12 C 0.7300(2) 0.2944(4) 0.3372(3) 0.0227(13) Uani 1 1 d . . . H12 H 0.6966 0.2755 0.2941 0.027 Uiso 1 1 calc R . . C13 C 0.7862(3) 0.3386(5) 0.3169(3) 0.0398(17) Uani 1 1 d . . . H13A H 0.7720 0.3963 0.2853 0.060 Uiso 1 1 calc R . . H13B H 0.8040 0.2850 0.2944 0.060 Uiso 1 1 calc R . . H13C H 0.8184 0.3625 0.3580 0.060 Uiso 1 1 calc R . . C14 C 0.7492(3) 0.1969(4) 0.3796(3) 0.0345(16) Uani 1 1 d . . . H14A H 0.7844 0.2122 0.4204 0.052 Uiso 1 1 calc R . . H14B H 0.7622 0.1445 0.3521 0.052 Uiso 1 1 calc R . . H14C H 0.7135 0.1713 0.3937 0.052 Uiso 1 1 calc R . . C15 C 0.5761(2) 0.2613(4) 0.0910(3) 0.0187(13) Uani 1 1 d . . . C16 C 0.6326(2) 0.2186(4) 0.0838(3) 0.0223(14) Uani 1 1 d . . . C17 C 0.6287(3) 0.1527(5) 0.0288(3) 0.0360(16) Uani 1 1 d . . . H17 H 0.6663 0.1261 0.0222 0.043 Uiso 1 1 calc R . . C18 C 0.5718(3) 0.1256(5) -0.0159(3) 0.0421(18) Uani 1 1 d . . . H18 H 0.5700 0.0787 -0.0521 0.050 Uiso 1 1 calc R . . C19 C 0.5171(3) 0.1666(5) -0.0083(3) 0.0339(16) Uani 1 1 d . . . H19 H 0.4779 0.1482 -0.0399 0.041 Uiso 1 1 calc R . . C20 C 0.5182(2) 0.2339(4) 0.0446(3) 0.0248(14) Uani 1 1 d . . . C21 C 0.6970(2) 0.2368(4) 0.1358(3) 0.0259(15) Uani 1 1 d . . . H21 H 0.6901 0.2750 0.1755 0.031 Uiso 1 1 calc R . . C22 C 0.7304(2) 0.1366(4) 0.1631(3) 0.0323(16) Uani 1 1 d . . . H22A H 0.7034 0.0949 0.1829 0.049 Uiso 1 1 calc R . . H22B H 0.7700 0.1517 0.1984 0.049 Uiso 1 1 calc R . . H22C H 0.7392 0.0988 0.1255 0.049 Uiso 1 1 calc R . . C23 C 0.7396(3) 0.3027(5) 0.1061(3) 0.0417(17) Uani 1 1 d . . . H23A H 0.7463 0.2679 0.0662 0.063 Uiso 1 1 calc R . . H23B H 0.7802 0.3128 0.1410 0.063 Uiso 1 1 calc R . . H23C H 0.7197 0.3696 0.0921 0.063 Uiso 1 1 calc R . . C24 C 0.4560(2) 0.2793(4) 0.0496(3) 0.0263(15) Uani 1 1 d . . . H24 H 0.4660 0.3262 0.0902 0.032 Uiso 1 1 calc R . . C25 C 0.4124(3) 0.1952(5) 0.0611(3) 0.0436(18) Uani 1 1 d . . . H25A H 0.4040 0.1455 0.0234 0.065 Uiso 1 1 calc R . . H25B H 0.3726 0.2259 0.0628 0.065 Uiso 1 1 calc R . . H25C H 0.4324 0.1600 0.1045 0.065 Uiso 1 1 calc R . . C26 C 0.4238(3) 0.3431(5) -0.0138(3) 0.0440(17) Uani 1 1 d . . . H26A H 0.4509 0.4010 -0.0172 0.066 Uiso 1 1 calc R . . H26B H 0.3836 0.3691 -0.0101 0.066 Uiso 1 1 calc R . . H26C H 0.4163 0.3001 -0.0548 0.066 Uiso 1 1 calc R . . C27 C 0.6262(3) 0.0365(5) 0.2816(3) 0.0500(19) Uani 1 1 d . . . H27A H 0.6260 0.0459 0.3292 0.075 Uiso 1 1 calc R . . H27B H 0.6464 0.0957 0.2673 0.075 Uiso 1 1 calc R . . H27C H 0.6494 -0.0262 0.2781 0.075 Uiso 1 1 calc R . . C28 C 0.5620(3) 0.0172(5) 0.1657(3) 0.0397(17) Uani 1 1 d . . . H28A H 0.5844 -0.0458 0.1607 0.059 Uiso 1 1 calc R . . H28B H 0.5833 0.0766 0.1531 0.059 Uiso 1 1 calc R . . H28C H 0.5187 0.0137 0.1355 0.059 Uiso 1 1 calc R . . C29 C 0.5332(3) -0.0638(5) 0.2592(4) 0.061(2) Uani 1 1 d . . . H29A H 0.5469 -0.1255 0.2392 0.073 Uiso 1 1 calc R . . H29B H 0.5498 -0.0696 0.3097 0.073 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 0.0178(3) 0.0187(4) 0.0244(4) 0.000 0.0082(3) 0.000 Ga1 0.0169(3) 0.0199(4) 0.0200(4) -0.0003(3) 0.0055(3) -0.0009(3) N1 0.024(3) 0.022(3) 0.042(4) 0.003(2) 0.015(3) 0.007(2) N3 0.017(2) 0.022(3) 0.014(3) 0.003(2) 0.002(2) -0.004(2) N2 0.018(2) 0.026(3) 0.014(3) -0.001(2) 0.000(2) 0.000(2) C1 0.017(3) 0.023(4) 0.029(4) 0.005(3) 0.002(3) -0.002(3) C2 0.024(3) 0.024(4) 0.018(3) 0.003(3) 0.008(3) -0.003(3) C3 0.020(3) 0.021(3) 0.012(3) -0.001(3) 0.002(3) -0.005(3) C4 0.028(3) 0.017(3) 0.024(4) 0.002(3) 0.010(3) -0.002(3) C5 0.035(4) 0.031(4) 0.027(4) -0.004(3) 0.014(3) -0.002(3) C6 0.025(3) 0.039(4) 0.016(3) 0.001(3) -0.001(3) -0.006(3) C7 0.024(3) 0.038(4) 0.027(4) 0.004(3) 0.001(3) 0.007(3) C8 0.024(3) 0.025(4) 0.017(4) 0.007(3) 0.001(3) -0.001(3) C9 0.028(3) 0.033(4) 0.034(4) -0.008(3) 0.007(3) 0.002(3) C10 0.033(4) 0.061(6) 0.095(7) 0.035(5) 0.019(4) 0.016(4) C11 0.027(4) 0.050(5) 0.067(5) 0.001(4) 0.017(4) 0.004(3) C12 0.018(3) 0.022(3) 0.026(3) 0.004(3) 0.003(3) 0.003(3) C13 0.034(4) 0.045(4) 0.046(4) -0.004(4) 0.021(3) 0.002(3) C14 0.033(4) 0.030(4) 0.039(4) -0.001(3) 0.008(3) 0.005(3) C15 0.027(3) 0.013(3) 0.017(3) -0.004(3) 0.009(3) -0.005(2) C16 0.024(3) 0.023(4) 0.020(3) -0.003(3) 0.006(3) -0.001(3) C17 0.029(4) 0.048(4) 0.034(4) -0.005(4) 0.014(3) 0.004(3) C18 0.039(4) 0.051(5) 0.038(4) -0.021(3) 0.015(4) 0.002(3) C19 0.026(3) 0.043(4) 0.030(4) -0.018(3) 0.004(3) -0.006(3) C20 0.019(3) 0.030(4) 0.025(4) -0.002(3) 0.006(3) -0.001(3) C21 0.016(3) 0.036(4) 0.026(4) 0.001(3) 0.008(3) 0.003(3) C22 0.020(3) 0.038(4) 0.037(4) 0.000(3) 0.005(3) 0.010(3) C23 0.029(4) 0.050(5) 0.044(4) 0.012(3) 0.008(3) 0.001(3) C24 0.016(3) 0.036(4) 0.028(4) -0.009(3) 0.008(3) -0.004(3) C25 0.040(4) 0.054(5) 0.039(4) -0.005(3) 0.015(4) -0.007(3) C26 0.036(4) 0.055(5) 0.041(4) -0.005(4) 0.011(3) 0.014(4) C27 0.035(4) 0.067(5) 0.042(5) -0.005(4) 0.002(4) 0.024(4) C28 0.038(4) 0.037(4) 0.045(5) -0.011(3) 0.014(4) 0.009(3) C29 0.068(5) 0.020(4) 0.114(7) 0.012(4) 0.055(6) 0.012(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 Pd1 N1 2.231(4) . ? Pd1 N1 2.231(4) 2_655 ? Pd1 Ga1 2.3503(8) . ? Pd1 Ga1 2.3503(8) 2_655 ? Ga1 N3 1.893(4) . ? Ga1 N2 1.907(4) . ? N1 C27 1.463(7) . ? N1 C28 1.469(7) . ? N1 C29 1.475(7) . ? N3 C3 1.412(6) . ? N3 C1 1.420(6) . ? N2 C2 1.381(6) . ? N2 C15 1.430(6) . ? C1 C2 1.343(7) . ? C3 C4 1.408(7) . ? C3 C8 1.421(7) . ? C4 C5 1.392(7) . ? C4 C9 1.521(7) . ? C5 C6 1.391(7) . ? C6 C7 1.379(7) . ? C7 C8 1.374(7) . ? C8 C12 1.526(7) . ? C9 C10 1.516(8) . ? C9 C11 1.524(7) . ? C12 C14 1.524(7) . ? C12 C13 1.540(6) . ? C15 C20 1.401(7) . ? C15 C16 1.422(7) . ? C16 C17 1.394(7) . ? C16 C21 1.528(7) . ? C17 C18 1.371(8) . ? C18 C19 1.378(7) . ? C19 C20 1.385(7) . ? C20 C24 1.535(7) . ? C21 C22 1.522(7) . ? C21 C23 1.531(7) . ? C24 C26 1.526(8) . ? C24 C25 1.528(7) . ? C29 C29 1.412(12) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N1 82.1(2) . 2_655 ? N1 Pd1 Ga1 99.53(11) . . ? N1 Pd1 Ga1 176.42(13) 2_655 . ? N1 Pd1 Ga1 176.42(13) . 2_655 ? N1 Pd1 Ga1 99.53(11) 2_655 2_655 ? Ga1 Pd1 Ga1 79.02(4) . 2_655 ? N3 Ga1 N2 87.81(17) . . ? N3 Ga1 Pd1 144.80(12) . . ? N2 Ga1 Pd1 127.02(13) . . ? C27 N1 C28 109.1(4) . . ? C27 N1 C29 107.8(5) . . ? C28 N1 C29 111.0(5) . . ? C27 N1 Pd1 113.1(4) . . ? C28 N1 Pd1 111.8(3) . . ? C29 N1 Pd1 103.9(3) . . ? C3 N3 C1 116.5(4) . . ? C3 N3 Ga1 133.0(3) . . ? C1 N3 Ga1 108.1(3) . . ? C2 N2 C15 118.9(4) . . ? C2 N2 Ga1 109.0(3) . . ? C15 N2 Ga1 128.0(3) . . ? C2 C1 N3 117.3(5) . . ? C1 C2 N2 117.6(5) . . ? C4 C3 N3 120.6(5) . . ? C4 C3 C8 119.5(5) . . ? N3 C3 C8 119.8(5) . . ? C5 C4 C3 119.3(5) . . ? C5 C4 C9 120.1(5) . . ? C3 C4 C9 120.5(5) . . ? C6 C5 C4 120.8(5) . . ? C7 C6 C5 119.5(6) . . ? C8 C7 C6 121.8(5) . . ? C7 C8 C3 119.1(5) . . ? C7 C8 C12 119.1(5) . . ? C3 C8 C12 121.8(5) . . ? C10 C9 C4 110.9(5) . . ? C10 C9 C11 110.1(5) . . ? C4 C9 C11 112.5(5) . . ? C14 C12 C8 112.6(4) . . ? C14 C12 C13 110.5(4) . . ? C8 C12 C13 110.0(4) . . ? C20 C15 C16 119.7(5) . . ? C20 C15 N2 120.4(4) . . ? C16 C15 N2 119.9(5) . . ? C17 C16 C15 118.4(5) . . ? C17 C16 C21 118.6(5) . . ? C15 C16 C21 122.9(5) . . ? C18 C17 C16 121.4(5) . . ? C17 C18 C19 119.8(5) . . ? C18 C19 C20 121.3(5) . . ? C19 C20 C15 119.2(5) . . ? C19 C20 C24 119.1(5) . . ? C15 C20 C24 121.6(5) . . ? C22 C21 C16 112.1(5) . . ? C22 C21 C23 109.4(4) . . ? C16 C21 C23 112.0(5) . . ? C26 C24 C25 111.0(5) . . ? C26 C24 C20 111.1(4) . . ? C25 C24 C20 111.1(5) . . ? C29 C29 N1 115.2(5) 2_655 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.590 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.114 # Attachment 'compound16.CIF' data_compound16 _database_code_depnum_ccdc_archive 'CCDC 664056' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C77 H94 Ga2 N4 P2 Pd' _chemical_formula_weight 1383.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.434(4) _cell_length_b 20.121(4) _cell_length_c 19.066(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.89(3) _cell_angle_gamma 90.00 _cell_volume 7071(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2888 _exptl_absorpt_coefficient_mu 1.098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.876 _exptl_absorpt_correction_T_max 0.947 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17638 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.1099 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12362 _reflns_number_gt 8494 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0134P)^2^+14.0102P] 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 12362 _refine_ls_number_parameters 791 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1158 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Pd1 Pd 0.49439(2) 0.19149(2) 0.676268(19) 0.01784(11) Uani 1 1 d . . . Ga1 Ga 0.57333(3) 0.23282(3) 0.76726(3) 0.01772(15) Uani 1 1 d . . . P1 P 0.55771(8) 0.09637(7) 0.63418(7) 0.0234(3) Uani 1 1 d . . . N1 N 0.6627(2) 0.2798(2) 0.7608(2) 0.0221(10) Uani 1 1 d . . . C1 C 0.6905(3) 0.2898(3) 0.8283(2) 0.0234(13) Uani 1 1 d . . . H1 H 0.7351 0.3125 0.8363 0.028 Uiso 1 1 calc R . . Ga2 Ga 0.42166(3) 0.28058(3) 0.72102(3) 0.01919(15) Uani 1 1 d . . . P2 P 0.43201(8) 0.15196(7) 0.57344(7) 0.0219(3) Uani 1 1 d . . . N2 N 0.5880(2) 0.2316(2) 0.8655(2) 0.0175(10) Uani 1 1 d . . . C2 C 0.6518(3) 0.2660(3) 0.8813(3) 0.0220(12) Uani 1 1 d . . . H2 H 0.6674 0.2723 0.9286 0.026 Uiso 1 1 calc R . . N3 N 0.4095(2) 0.3733(2) 0.7356(2) 0.0202(10) Uani 1 1 d . . . C3 C 0.7143(3) 0.2868(3) 0.7056(2) 0.0189(12) Uani 1 1 d . . . N4 N 0.3296(2) 0.2679(2) 0.7639(2) 0.0222(10) Uani 1 1 d . . . C4 C 0.7062(3) 0.3388(3) 0.6561(3) 0.0215(12) Uani 1 1 d . . . C5 C 0.7579(3) 0.3463(3) 0.6045(3) 0.0245(13) Uani 1 1 d . . . H5 H 0.7525 0.3808 0.5709 0.029 Uiso 1 1 calc R . . C6 C 0.8172(3) 0.3042(3) 0.6014(3) 0.0304(14) Uani 1 1 d . . . H6 H 0.8524 0.3099 0.5660 0.037 Uiso 1 1 calc R . . C7 C 0.8249(3) 0.2541(3) 0.6498(3) 0.0272(14) Uani 1 1 d . . . H7 H 0.8659 0.2257 0.6475 0.033 Uiso 1 1 calc R . . C8 C 0.7744(3) 0.2436(3) 0.7022(3) 0.0219(13) Uani 1 1 d . . . C9 C 0.6439(3) 0.3874(3) 0.6564(3) 0.0260(13) Uani 1 1 d . . . H9 H 0.6176 0.3815 0.7015 0.031 Uiso 1 1 calc R . . C10 C 0.6690(3) 0.4590(3) 0.6526(3) 0.0426(17) Uani 1 1 d . . . H10A H 0.7037 0.4679 0.6910 0.064 Uiso 1 1 calc R . . H10B H 0.6271 0.4886 0.6569 0.064 Uiso 1 1 calc R . . H10C H 0.6924 0.4668 0.6076 0.064 Uiso 1 1 calc R . . C11 C 0.5907(3) 0.3720(4) 0.5961(3) 0.0499(19) Uani 1 1 d . . . H11A H 0.5747 0.3257 0.5995 0.075 Uiso 1 1 calc R . . H11B H 0.6147 0.3789 0.5512 0.075 Uiso 1 1 calc R . . H11C H 0.5485 0.4015 0.5990 0.075 Uiso 1 1 calc R . . C12 C 0.7849(3) 0.1862(3) 0.7523(3) 0.0313(14) Uani 1 1 d . . . H12 H 0.7407 0.1831 0.7820 0.038 Uiso 1 1 calc R . . C13 C 0.8503(3) 0.1951(3) 0.8007(3) 0.0429(17) Uani 1 1 d . . . H13A H 0.8946 0.1949 0.7730 0.064 Uiso 1 1 calc R . . H13B H 0.8521 0.1585 0.8347 0.064 Uiso 1 1 calc R . . H13C H 0.8463 0.2374 0.8257 0.064 Uiso 1 1 calc R . . C14 C 0.7922(4) 0.1204(3) 0.7116(4) 0.056(2) Uani 1 1 d . . . H14A H 0.8364 0.1215 0.6838 0.084 Uiso 1 1 calc R . . H14B H 0.7499 0.1146 0.6803 0.084 Uiso 1 1 calc R . . H14C H 0.7948 0.0832 0.7448 0.084 Uiso 1 1 calc R . . C15 C 0.5570(3) 0.1981(3) 0.9242(2) 0.0189(12) Uani 1 1 d . . . C16 C 0.5716(3) 0.1300(3) 0.9368(3) 0.0234(13) Uani 1 1 d . . . C17 C 0.5460(3) 0.1005(3) 0.9971(3) 0.0291(14) Uani 1 1 d . . . H17 H 0.5550 0.0547 1.0057 0.035 Uiso 1 1 calc R . . C18 C 0.5073(3) 0.1375(3) 1.0451(3) 0.0298(14) Uani 1 1 d . . . H18 H 0.4907 0.1170 1.0868 0.036 Uiso 1 1 calc R . . C19 C 0.4926(3) 0.2032(3) 1.0333(3) 0.0306(15) Uani 1 1 d . . . H19 H 0.4664 0.2277 1.0671 0.037 Uiso 1 1 calc R . . C20 C 0.5152(3) 0.2346(3) 0.9726(3) 0.0227(13) Uani 1 1 d . . . C21 C 0.6209(3) 0.0908(3) 0.8879(3) 0.0288(14) Uani 1 1 d . . . H21 H 0.6127 0.1073 0.8390 0.035 Uiso 1 1 calc R . . C22 C 0.7007(3) 0.1026(3) 0.9080(3) 0.0399(16) Uani 1 1 d . . . H22A H 0.7103 0.0851 0.9552 0.060 Uiso 1 1 calc R . . H22B H 0.7110 0.1503 0.9071 0.060 Uiso 1 1 calc R . . H22C H 0.7318 0.0798 0.8744 0.060 Uiso 1 1 calc R . . C23 C 0.6059(4) 0.0161(3) 0.8887(3) 0.0444(17) Uani 1 1 d . . . H23A H 0.6358 -0.0059 0.8536 0.067 Uiso 1 1 calc R . . H23B H 0.5545 0.0081 0.8778 0.067 Uiso 1 1 calc R . . H23C H 0.6178 -0.0019 0.9353 0.067 Uiso 1 1 calc R . . C24 C 0.4952(3) 0.3064(3) 0.9603(3) 0.0253(13) Uani 1 1 d . . . H24 H 0.5212 0.3219 0.9176 0.030 Uiso 1 1 calc R . . C25 C 0.4144(3) 0.3149(3) 0.9468(3) 0.0389(16) Uani 1 1 d . . . H25A H 0.3998 0.2896 0.9050 0.058 Uiso 1 1 calc R . . H25B H 0.4034 0.3621 0.9394 0.058 Uiso 1 1 calc R . . H25C H 0.3876 0.2986 0.9874 0.058 Uiso 1 1 calc R . . C26 C 0.5184(3) 0.3506(3) 1.0215(3) 0.0462(18) Uani 1 1 d . . . H26A H 0.5077 0.3971 1.0100 0.069 Uiso 1 1 calc R . . H26B H 0.5706 0.3455 1.0305 0.069 Uiso 1 1 calc R . . H26C H 0.4917 0.3378 1.0635 0.069 Uiso 1 1 calc R . . C27 C 0.3433(3) 0.3832(3) 0.7699(3) 0.0242(13) Uani 1 1 d . . . H27 H 0.3279 0.4265 0.7829 0.029 Uiso 1 1 calc R . . C28 C 0.3027(3) 0.3299(3) 0.7837(3) 0.0282(14) Uani 1 1 d . . . H28 H 0.2573 0.3341 0.8062 0.034 Uiso 1 1 calc R . . C29 C 0.4413(3) 0.4327(3) 0.7092(3) 0.0230(13) Uani 1 1 d . . . C30 C 0.4237(3) 0.4553(3) 0.6409(3) 0.0259(13) Uani 1 1 d . . . C31 C 0.4513(3) 0.5162(3) 0.6197(3) 0.0332(15) Uani 1 1 d . . . H31 H 0.4391 0.5324 0.5742 0.040 Uiso 1 1 calc R . . C32 C 0.4960(3) 0.5537(3) 0.6628(3) 0.0353(15) Uani 1 1 d . . . H32 H 0.5150 0.5947 0.6466 0.042 Uiso 1 1 calc R . . C33 C 0.5130(3) 0.5313(3) 0.7297(3) 0.0292(14) Uani 1 1 d . . . H33 H 0.5430 0.5576 0.7596 0.035 Uiso 1 1 calc R . . C34 C 0.4867(3) 0.4709(3) 0.7536(3) 0.0259(13) Uani 1 1 d . . . C35 C 0.3736(3) 0.4170(3) 0.5924(3) 0.0346(15) Uani 1 1 d . . . H35 H 0.3760 0.3692 0.6065 0.042 Uiso 1 1 calc R . . C36 C 0.3930(4) 0.4212(4) 0.5150(3) 0.0479(19) Uani 1 1 d . . . H36A H 0.3650 0.3880 0.4884 0.072 Uiso 1 1 calc R . . H36B H 0.4449 0.4125 0.5097 0.072 Uiso 1 1 calc R . . H36C H 0.3814 0.4657 0.4972 0.072 Uiso 1 1 calc R . . C37 C 0.2944(3) 0.4404(3) 0.6012(3) 0.0455(18) Uani 1 1 d . . . H37A H 0.2807 0.4360 0.6504 0.068 Uiso 1 1 calc R . . H37B H 0.2621 0.4130 0.5718 0.068 Uiso 1 1 calc R . . H37C H 0.2901 0.4870 0.5868 0.068 Uiso 1 1 calc R . . C38 C 0.5037(3) 0.4498(3) 0.8287(3) 0.0258(13) Uani 1 1 d . . . H38 H 0.4866 0.4030 0.8342 0.031 Uiso 1 1 calc R . . C39 C 0.5844(3) 0.4510(3) 0.8474(3) 0.0427(17) Uani 1 1 d . . . H39A H 0.6110 0.4237 0.8138 0.064 Uiso 1 1 calc R . . H39B H 0.5919 0.4333 0.8948 0.064 Uiso 1 1 calc R . . H39C H 0.6023 0.4969 0.8455 0.064 Uiso 1 1 calc R . . C40 C 0.4611(4) 0.4928(4) 0.8797(3) 0.0499(19) Uani 1 1 d . . . H40A H 0.4744 0.5396 0.8733 0.075 Uiso 1 1 calc R . . H40B H 0.4726 0.4792 0.9279 0.075 Uiso 1 1 calc R . . H40C H 0.4090 0.4873 0.8704 0.075 Uiso 1 1 calc R . . C41 C 0.2788(3) 0.2147(3) 0.7597(3) 0.0259(14) Uani 1 1 d . . . C42 C 0.2141(3) 0.2217(3) 0.7193(3) 0.0291(14) Uani 1 1 d . . . C43 C 0.1628(3) 0.1724(3) 0.7211(3) 0.0355(16) Uani 1 1 d . . . H43 H 0.1187 0.1779 0.6954 0.043 Uiso 1 1 calc R . . C44 C 0.1738(3) 0.1150(4) 0.7593(3) 0.0427(18) Uani 1 1 d . . . H44 H 0.1375 0.0815 0.7602 0.051 Uiso 1 1 calc R . . C45 C 0.2380(3) 0.1067(3) 0.7961(3) 0.0370(16) Uani 1 1 d . . . H45 H 0.2460 0.0665 0.8212 0.044 Uiso 1 1 calc R . . C46 C 0.2916(3) 0.1553(3) 0.7978(3) 0.0258(13) Uani 1 1 d . . . C47 C 0.2004(3) 0.2816(3) 0.6707(3) 0.0342(15) Uani 1 1 d . . . H47 H 0.2440 0.3111 0.6744 0.041 Uiso 1 1 calc R . . C48 C 0.1346(3) 0.3226(4) 0.6940(3) 0.053(2) Uani 1 1 d . . . H48A H 0.0908 0.2951 0.6909 0.080 Uiso 1 1 calc R . . H48B H 0.1289 0.3614 0.6635 0.080 Uiso 1 1 calc R . . H48C H 0.1422 0.3372 0.7426 0.080 Uiso 1 1 calc R . . C49 C 0.1923(4) 0.2607(3) 0.5937(3) 0.0431(17) Uani 1 1 d . . . H49A H 0.2356 0.2361 0.5795 0.065 Uiso 1 1 calc R . . H49B H 0.1865 0.3003 0.5642 0.065 Uiso 1 1 calc R . . H49C H 0.1495 0.2322 0.5880 0.065 Uiso 1 1 calc R . . C50 C 0.3597(3) 0.1433(3) 0.8412(3) 0.0294(14) Uani 1 1 d . . . H50 H 0.3879 0.1858 0.8413 0.035 Uiso 1 1 calc R . . C51 C 0.3433(4) 0.1272(4) 0.9172(3) 0.0497(19) Uani 1 1 d . . . H51A H 0.3126 0.1622 0.9368 0.075 Uiso 1 1 calc R . . H51B H 0.3889 0.1246 0.9444 0.075 Uiso 1 1 calc R . . H51C H 0.3180 0.0845 0.9196 0.075 Uiso 1 1 calc R . . C52 C 0.4071(3) 0.0911(3) 0.8089(3) 0.0429(17) Uani 1 1 d . . . H52A H 0.3811 0.0486 0.8075 0.064 Uiso 1 1 calc R . . H52B H 0.4517 0.0862 0.8370 0.064 Uiso 1 1 calc R . . H52C H 0.4193 0.1044 0.7611 0.064 Uiso 1 1 calc R . . C53 C 0.4779(3) 0.0713(3) 0.5812(3) 0.0257(13) Uani 1 1 d . . . H53A H 0.4918 0.0536 0.5348 0.031 Uiso 1 1 calc R . . H53B H 0.4478 0.0382 0.6058 0.031 Uiso 1 1 calc R . . C54 C 0.5858(3) 0.0182(3) 0.6763(3) 0.0288(14) Uani 1 1 d . . . C55 C 0.5346(3) -0.0183(3) 0.7122(3) 0.0360(15) Uani 1 1 d . . . H55 H 0.4862 -0.0023 0.7154 0.043 Uiso 1 1 calc R . . C56 C 0.5539(4) -0.0779(3) 0.7436(3) 0.0459(18) Uani 1 1 d . . . H56 H 0.5186 -0.1030 0.7679 0.055 Uiso 1 1 calc R . . C57 C 0.6235(4) -0.1010(3) 0.7399(3) 0.0480(19) Uani 1 1 d . . . H57 H 0.6363 -0.1423 0.7607 0.058 Uiso 1 1 calc R . . C58 C 0.6750(4) -0.0641(3) 0.7058(3) 0.0458(18) Uani 1 1 d . . . H58 H 0.7236 -0.0796 0.7043 0.055 Uiso 1 1 calc R . . C59 C 0.6566(3) -0.0048(3) 0.6739(3) 0.0349(15) Uani 1 1 d . . . H59 H 0.6925 0.0202 0.6504 0.042 Uiso 1 1 calc R . . C60 C 0.6252(3) 0.1149(3) 0.5686(3) 0.0250(13) Uani 1 1 d . . . C61 C 0.6499(3) 0.1795(3) 0.5638(3) 0.0311(15) Uani 1 1 d . . . H61 H 0.6347 0.2118 0.5968 0.037 Uiso 1 1 calc R . . C62 C 0.6969(3) 0.1974(4) 0.5108(3) 0.050(2) Uani 1 1 d . . . H62 H 0.7136 0.2420 0.5077 0.060 Uiso 1 1 calc R . . C63 C 0.7194(4) 0.1508(5) 0.4627(3) 0.064(3) Uani 1 1 d . . . H63 H 0.7517 0.1630 0.4266 0.077 Uiso 1 1 calc R . . C64 C 0.6949(4) 0.0872(4) 0.4676(3) 0.054(2) Uani 1 1 d . . . H64 H 0.7105 0.0552 0.4344 0.065 Uiso 1 1 calc R . . C65 C 0.6479(3) 0.0679(3) 0.5198(3) 0.0376(16) Uani 1 1 d . . . H65 H 0.6313 0.0233 0.5222 0.045 Uiso 1 1 calc R . . C66 C 0.3393(3) 0.1268(3) 0.5526(3) 0.0238(13) Uani 1 1 d . . . C67 C 0.2987(3) 0.1006(3) 0.6062(3) 0.0344(16) Uani 1 1 d . . . H67 H 0.3173 0.1019 0.6530 0.041 Uiso 1 1 calc R . . C68 C 0.2315(3) 0.0727(3) 0.5930(3) 0.0385(16) Uani 1 1 d . . . H68 H 0.2043 0.0547 0.6304 0.046 Uiso 1 1 calc R . . C69 C 0.2038(3) 0.0711(3) 0.5253(3) 0.0348(15) Uani 1 1 d . . . H69 H 0.1578 0.0515 0.5160 0.042 Uiso 1 1 calc R . . C70 C 0.2427(3) 0.0975(3) 0.4719(3) 0.0342(15) Uani 1 1 d . . . H70 H 0.2234 0.0966 0.4254 0.041 Uiso 1 1 calc R . . C71 C 0.3106(3) 0.1259(3) 0.4849(3) 0.0243(13) Uani 1 1 d . . . H71 H 0.3372 0.1446 0.4474 0.029 Uiso 1 1 calc R . . C72 C 0.4690(3) 0.1897(3) 0.4955(2) 0.0223(12) Uani 1 1 d . . . C73 C 0.4818(3) 0.2577(3) 0.4956(3) 0.0333(15) Uani 1 1 d . . . H73 H 0.4663 0.2835 0.5343 0.040 Uiso 1 1 calc R . . C74 C 0.5162(3) 0.2886(3) 0.4413(3) 0.0427(17) Uani 1 1 d . . . H74 H 0.5236 0.3353 0.4425 0.051 Uiso 1 1 calc R . . C75 C 0.5399(3) 0.2524(4) 0.3853(3) 0.0447(18) Uani 1 1 d . . . H75 H 0.5650 0.2736 0.3484 0.054 Uiso 1 1 calc R . . C76 C 0.5269(3) 0.1849(4) 0.3831(3) 0.0399(16) Uani 1 1 d . . . H76 H 0.5422 0.1597 0.3438 0.048 Uiso 1 1 calc R . . C77 C 0.4917(3) 0.1534(3) 0.4373(3) 0.0376(16) Uani 1 1 d . . . H77 H 0.4830 0.1069 0.4351 0.045 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 0.0185(2) 0.0168(2) 0.0182(2) -0.00232(18) -0.00181(16) 0.00027(19) Ga1 0.0169(3) 0.0193(4) 0.0169(3) -0.0007(3) -0.0003(2) -0.0024(3) P1 0.0240(8) 0.0198(9) 0.0264(7) -0.0055(7) -0.0043(6) 0.0022(7) N1 0.021(2) 0.025(3) 0.020(2) -0.003(2) -0.0008(19) -0.002(2) C1 0.020(3) 0.026(4) 0.023(3) -0.008(3) -0.003(2) -0.004(2) Ga2 0.0186(3) 0.0188(4) 0.0202(3) -0.0020(3) 0.0002(2) 0.0004(3) P2 0.0233(8) 0.0220(9) 0.0203(7) -0.0031(6) -0.0038(6) 0.0002(7) N2 0.016(2) 0.015(3) 0.022(2) 0.0002(19) 0.0015(18) -0.0061(19) C2 0.026(3) 0.019(3) 0.020(3) -0.003(2) -0.002(2) -0.001(3) N3 0.021(3) 0.018(3) 0.022(2) -0.003(2) -0.0014(19) 0.004(2) C3 0.020(3) 0.020(3) 0.017(3) -0.002(2) -0.001(2) -0.010(2) N4 0.017(2) 0.030(3) 0.020(2) 0.003(2) 0.0010(18) -0.006(2) C4 0.018(3) 0.023(3) 0.023(3) -0.004(3) 0.003(2) 0.001(2) C5 0.024(3) 0.028(4) 0.022(3) 0.007(3) 0.000(2) 0.000(3) C6 0.028(3) 0.043(4) 0.021(3) -0.003(3) 0.010(2) 0.003(3) C7 0.021(3) 0.029(4) 0.032(3) -0.001(3) 0.001(3) 0.005(3) C8 0.019(3) 0.023(3) 0.024(3) -0.004(2) 0.000(2) -0.005(2) C9 0.030(3) 0.021(3) 0.027(3) 0.004(3) 0.007(3) 0.006(3) C10 0.035(4) 0.026(4) 0.067(4) 0.003(3) 0.009(3) 0.015(3) C11 0.037(4) 0.056(5) 0.056(4) -0.011(4) -0.011(3) 0.018(4) C12 0.030(3) 0.025(4) 0.039(3) 0.007(3) -0.002(3) 0.008(3) C13 0.039(4) 0.041(4) 0.048(4) 0.009(3) -0.013(3) 0.004(3) C14 0.069(5) 0.022(4) 0.076(5) -0.003(4) -0.026(4) 0.006(4) C15 0.022(3) 0.019(3) 0.015(2) 0.002(2) -0.006(2) -0.007(2) C16 0.025(3) 0.022(3) 0.023(3) 0.001(3) -0.003(2) -0.004(3) C17 0.035(4) 0.027(4) 0.025(3) 0.002(3) -0.004(3) -0.004(3) C18 0.029(3) 0.038(4) 0.023(3) 0.008(3) 0.002(2) -0.008(3) C19 0.022(3) 0.045(5) 0.025(3) -0.003(3) 0.007(2) 0.000(3) C20 0.017(3) 0.029(4) 0.022(3) -0.001(3) 0.002(2) -0.002(3) C21 0.044(4) 0.020(3) 0.023(3) 0.007(3) -0.005(3) 0.000(3) C22 0.040(4) 0.031(4) 0.049(4) -0.006(3) 0.009(3) 0.007(3) C23 0.053(4) 0.032(4) 0.049(4) -0.011(3) 0.000(3) 0.006(3) C24 0.027(3) 0.024(3) 0.024(3) -0.006(3) 0.006(2) -0.001(3) C25 0.033(4) 0.032(4) 0.051(4) -0.002(3) -0.011(3) 0.003(3) C26 0.048(4) 0.034(4) 0.056(4) -0.003(3) -0.021(3) 0.002(3) C27 0.021(3) 0.028(4) 0.024(3) -0.004(3) -0.003(2) 0.002(3) C28 0.022(3) 0.037(4) 0.026(3) -0.014(3) 0.002(2) 0.005(3) C29 0.027(3) 0.014(3) 0.027(3) -0.001(3) 0.001(2) 0.011(3) C30 0.026(3) 0.021(3) 0.030(3) 0.001(3) 0.002(2) 0.009(3) C31 0.033(4) 0.034(4) 0.032(3) 0.004(3) -0.006(3) 0.014(3) C32 0.032(4) 0.024(4) 0.050(4) 0.014(3) -0.002(3) 0.008(3) C33 0.024(3) 0.026(4) 0.037(3) 0.001(3) -0.008(3) 0.001(3) C34 0.023(3) 0.022(3) 0.033(3) -0.001(3) -0.001(3) 0.006(3) C35 0.041(4) 0.027(4) 0.036(3) -0.006(3) -0.014(3) 0.009(3) C36 0.058(5) 0.055(5) 0.030(3) -0.007(3) -0.007(3) 0.017(4) C37 0.051(4) 0.051(5) 0.034(3) -0.004(3) -0.013(3) -0.005(4) C38 0.031(3) 0.017(3) 0.029(3) 0.000(3) -0.008(2) -0.003(3) C39 0.033(4) 0.054(5) 0.041(4) 0.007(3) -0.011(3) -0.001(3) C40 0.058(5) 0.058(5) 0.033(3) -0.012(3) -0.007(3) 0.020(4) C41 0.021(3) 0.036(4) 0.021(3) -0.009(3) 0.003(2) -0.008(3) C42 0.018(3) 0.046(4) 0.023(3) -0.008(3) 0.003(2) 0.001(3) C43 0.023(3) 0.049(5) 0.034(3) -0.001(3) -0.001(3) -0.008(3) C44 0.028(4) 0.059(5) 0.041(4) -0.010(4) 0.006(3) -0.028(3) C45 0.041(4) 0.043(4) 0.027(3) 0.004(3) -0.001(3) -0.019(3) C46 0.028(3) 0.027(4) 0.023(3) 0.001(3) 0.008(2) -0.010(3) C47 0.025(3) 0.048(4) 0.030(3) -0.006(3) -0.004(3) -0.002(3) C48 0.038(4) 0.071(6) 0.050(4) -0.010(4) -0.008(3) 0.022(4) C49 0.051(4) 0.051(5) 0.027(3) -0.009(3) -0.010(3) 0.001(4) C50 0.040(4) 0.022(3) 0.026(3) 0.000(3) -0.007(3) -0.012(3) C51 0.055(4) 0.070(6) 0.024(3) 0.003(3) -0.006(3) -0.018(4) C52 0.042(4) 0.046(5) 0.041(4) 0.003(3) -0.004(3) 0.001(3) C53 0.033(3) 0.016(3) 0.029(3) -0.002(3) -0.006(2) 0.003(3) C54 0.038(4) 0.022(4) 0.026(3) -0.008(3) -0.013(3) 0.007(3) C55 0.043(4) 0.030(4) 0.035(3) -0.003(3) -0.004(3) 0.000(3) C56 0.062(5) 0.042(5) 0.033(4) 0.006(3) -0.011(3) -0.002(4) C57 0.083(6) 0.023(4) 0.037(4) -0.011(3) -0.022(4) 0.015(4) C58 0.061(5) 0.029(4) 0.046(4) -0.008(3) -0.021(4) 0.021(4) C59 0.045(4) 0.021(4) 0.037(3) -0.007(3) -0.011(3) 0.006(3) C60 0.024(3) 0.031(4) 0.020(3) -0.003(3) -0.007(2) 0.003(3) C61 0.029(3) 0.038(4) 0.026(3) -0.007(3) -0.004(3) -0.003(3) C62 0.046(4) 0.074(6) 0.031(3) 0.006(4) 0.000(3) -0.026(4) C63 0.040(5) 0.125(9) 0.027(4) 0.006(5) 0.006(3) -0.011(5) C64 0.046(5) 0.078(6) 0.038(4) -0.007(4) 0.010(3) 0.032(4) C65 0.040(4) 0.031(4) 0.041(4) -0.006(3) -0.001(3) 0.014(3) C66 0.024(3) 0.022(3) 0.025(3) -0.005(3) -0.001(2) 0.000(3) C67 0.037(4) 0.044(4) 0.022(3) 0.000(3) -0.007(3) -0.005(3) C68 0.032(4) 0.055(5) 0.028(3) -0.003(3) 0.002(3) -0.009(3) C69 0.028(3) 0.031(4) 0.045(4) -0.003(3) -0.001(3) 0.001(3) C70 0.034(4) 0.034(4) 0.033(3) -0.002(3) -0.021(3) 0.003(3) C71 0.027(3) 0.020(3) 0.025(3) 0.002(3) -0.004(2) 0.001(3) C72 0.028(3) 0.020(3) 0.019(3) 0.000(3) -0.002(2) 0.002(3) C73 0.041(4) 0.037(4) 0.022(3) 0.000(3) -0.007(3) 0.010(3) C74 0.056(5) 0.035(4) 0.037(4) 0.010(3) 0.003(3) -0.006(3) C75 0.046(4) 0.052(5) 0.037(4) 0.015(3) -0.001(3) -0.011(4) C76 0.045(4) 0.049(5) 0.027(3) -0.012(3) 0.012(3) -0.007(4) C77 0.046(4) 0.036(4) 0.032(3) -0.003(3) 0.009(3) -0.008(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 Pd1 P1 2.3871(16) . ? Pd1 P2 2.3934(15) . ? Pd1 Ga1 2.3959(9) . ? Pd1 Ga2 2.4032(8) . ? Ga1 N2 1.888(4) . ? Ga1 N1 1.905(4) . ? P1 C60 1.816(6) . ? P1 C54 1.837(6) . ? P1 C53 1.843(5) . ? N1 C1 1.394(6) . ? N1 C3 1.436(6) . ? C1 C2 1.335(7) . ? Ga2 N3 1.901(4) . ? Ga2 N4 1.911(4) . ? P2 C72 1.812(5) . ? P2 C66 1.820(5) . ? P2 C53 1.835(5) . ? N2 C2 1.394(6) . ? N2 C15 1.433(6) . ? N3 C27 1.408(6) . ? N3 C29 1.425(7) . ? C3 C8 1.411(7) . ? C3 C4 1.415(7) . ? N4 C28 1.398(7) . ? N4 C41 1.424(7) . ? C4 C5 1.388(7) . ? C4 C9 1.508(7) . ? C5 C6 1.385(7) . ? C6 C7 1.372(8) . ? C7 C8 1.392(7) . ? C8 C12 1.510(7) . ? C9 C10 1.514(8) . ? C9 C11 1.532(7) . ? C12 C13 1.517(7) . ? C12 C14 1.542(8) . ? C15 C16 1.417(7) . ? C15 C20 1.417(7) . ? C16 C17 1.383(7) . ? C16 C21 1.532(8) . ? C17 C18 1.386(8) . ? C18 C19 1.367(8) . ? C19 C20 1.389(7) . ? C20 C24 1.507(8) . ? C21 C23 1.528(8) . ? C21 C22 1.532(8) . ? C24 C25 1.519(7) . ? C24 C26 1.525(7) . ? C27 C28 1.335(8) . ? C29 C34 1.409(7) . ? C29 C30 1.413(7) . ? C30 C31 1.389(8) . ? C30 C35 1.509(7) . ? C31 C32 1.379(8) . ? C32 C33 1.384(7) . ? C33 C34 1.388(8) . ? C34 C38 1.521(7) . ? C35 C36 1.525(8) . ? C35 C37 1.546(8) . ? C38 C39 1.524(7) . ? C38 C40 1.528(8) . ? C41 C46 1.416(8) . ? C41 C42 1.417(7) . ? C42 C43 1.371(8) . ? C42 C47 1.539(8) . ? C43 C44 1.379(9) . ? C44 C45 1.377(8) . ? C45 C46 1.391(7) . ? C46 C50 1.513(7) . ? C47 C49 1.533(7) . ? C47 C48 1.538(8) . ? C50 C52 1.505(8) . ? C50 C51 1.520(7) . ? C54 C55 1.385(8) . ? C54 C59 1.387(8) . ? C55 C56 1.385(9) . ? C56 C57 1.367(9) . ? C57 C58 1.375(9) . ? C58 C59 1.377(8) . ? C60 C61 1.381(8) . ? C60 C65 1.395(8) . ? C61 C62 1.388(8) . ? C62 C63 1.380(10) . ? C63 C64 1.360(10) . ? C64 C65 1.385(9) . ? C66 C67 1.381(7) . ? C66 C71 1.387(7) . ? C67 C68 1.379(8) . ? C68 C69 1.381(7) . ? C69 C70 1.363(8) . ? C70 C71 1.394(7) . ? C72 C73 1.388(8) . ? C72 C77 1.397(7) . ? C73 C74 1.371(8) . ? C74 C75 1.367(9) . ? C75 C76 1.381(9) . ? C76 C77 1.383(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 P1 Pd1 P2 71.91(5) . . ? P1 Pd1 Ga1 103.12(4) . . ? P2 Pd1 Ga1 170.80(4) . . ? P1 Pd1 Ga2 174.79(4) . . ? P2 Pd1 Ga2 105.96(4) . . ? Ga1 Pd1 Ga2 79.63(3) . . ? N2 Ga1 N1 87.72(17) . . ? N2 Ga1 Pd1 142.15(12) . . ? N1 Ga1 Pd1 129.90(12) . . ? C60 P1 C54 106.6(3) . . ? C60 P1 C53 103.2(2) . . ? C54 P1 C53 102.9(3) . . ? C60 P1 Pd1 114.2(2) . . ? C54 P1 Pd1 132.51(19) . . ? C53 P1 Pd1 90.75(18) . . ? C1 N1 C3 115.1(4) . . ? C1 N1 Ga1 108.6(3) . . ? C3 N1 Ga1 132.8(3) . . ? C2 C1 N1 117.0(5) . . ? N3 Ga2 N4 87.79(19) . . ? N3 Ga2 Pd1 148.43(13) . . ? N4 Ga2 Pd1 123.78(14) . . ? C72 P2 C66 107.6(2) . . ? C72 P2 C53 104.9(3) . . ? C66 P2 C53 101.6(3) . . ? C72 P2 Pd1 110.52(17) . . ? C66 P2 Pd1 135.15(17) . . ? C53 P2 Pd1 90.75(16) . . ? C2 N2 C15 114.2(4) . . ? C2 N2 Ga1 108.4(3) . . ? C15 N2 Ga1 136.7(3) . . ? C1 C2 N2 118.2(4) . . ? C27 N3 C29 114.2(4) . . ? C27 N3 Ga2 108.1(4) . . ? C29 N3 Ga2 136.2(3) . . ? C8 C3 C4 120.0(5) . . ? C8 C3 N1 120.1(5) . . ? C4 C3 N1 119.9(5) . . ? C28 N4 C41 116.7(4) . . ? C28 N4 Ga2 108.5(4) . . ? C41 N4 Ga2 131.6(4) . . ? C5 C4 C3 119.1(5) . . ? C5 C4 C9 117.7(5) . . ? C3 C4 C9 123.3(5) . . ? C6 C5 C4 121.0(5) . . ? C7 C6 C5 119.5(5) . . ? C6 C7 C8 122.1(5) . . ? C7 C8 C3 118.3(5) . . ? C7 C8 C12 119.4(5) . . ? C3 C8 C12 122.4(5) . . ? C4 C9 C10 112.5(5) . . ? C4 C9 C11 110.2(5) . . ? C10 C9 C11 110.4(5) . . ? C8 C12 C13 112.8(5) . . ? C8 C12 C14 110.4(5) . . ? C13 C12 C14 109.4(5) . . ? C16 C15 C20 119.7(5) . . ? C16 C15 N2 120.8(5) . . ? C20 C15 N2 119.5(5) . . ? C17 C16 C15 119.4(5) . . ? C17 C16 C21 119.9(5) . . ? C15 C16 C21 120.5(5) . . ? C16 C17 C18 120.2(6) . . ? C19 C18 C17 120.9(5) . . ? C18 C19 C20 121.1(5) . . ? C19 C20 C15 118.6(5) . . ? C19 C20 C24 119.4(5) . . ? C15 C20 C24 122.0(5) . . ? C23 C21 C22 108.9(5) . . ? C23 C21 C16 113.0(5) . . ? C22 C21 C16 110.2(4) . . ? C20 C24 C25 111.8(5) . . ? C20 C24 C26 112.1(4) . . ? C25 C24 C26 109.0(5) . . ? C28 C27 N3 118.2(5) . . ? C27 C28 N4 117.4(5) . . ? C34 C29 C30 120.2(5) . . ? C34 C29 N3 119.3(4) . . ? C30 C29 N3 120.3(5) . . ? C31 C30 C29 118.2(5) . . ? C31 C30 C35 119.7(5) . . ? C29 C30 C35 122.0(5) . . ? C32 C31 C30 121.8(5) . . ? C31 C32 C33 119.7(6) . . ? C32 C33 C34 120.9(5) . . ? C33 C34 C29 119.1(5) . . ? C33 C34 C38 119.1(5) . . ? C29 C34 C38 121.7(5) . . ? C30 C35 C36 114.5(5) . . ? C30 C35 C37 110.4(5) . . ? C36 C35 C37 108.9(5) . . ? C34 C38 C39 113.7(5) . . ? C34 C38 C40 109.8(5) . . ? C39 C38 C40 110.6(5) . . ? C46 C41 C42 119.6(5) . . ? C46 C41 N4 120.1(5) . . ? C42 C41 N4 120.3(5) . . ? C43 C42 C41 119.3(6) . . ? C43 C42 C47 118.4(5) . . ? C41 C42 C47 122.2(5) . . ? C42 C43 C44 121.6(5) . . ? C45 C44 C43 119.3(6) . . ? C44 C45 C46 122.0(6) . . ? C45 C46 C41 118.1(5) . . ? C45 C46 C50 118.9(5) . . ? C41 C46 C50 123.0(5) . . ? C49 C47 C48 111.0(5) . . ? C49 C47 C42 111.9(5) . . ? C48 C47 C42 111.6(5) . . ? C52 C50 C46 111.6(4) . . ? C52 C50 C51 111.5(5) . . ? C46 C50 C51 112.4(5) . . ? P2 C53 P1 99.5(3) . . ? C55 C54 C59 119.2(6) . . ? C55 C54 P1 118.7(4) . . ? C59 C54 P1 122.1(5) . . ? C56 C55 C54 120.0(6) . . ? C57 C56 C55 120.4(7) . . ? C56 C57 C58 119.8(7) . . ? C57 C58 C59 120.6(7) . . ? C58 C59 C54 120.0(7) . . ? C61 C60 C65 119.4(5) . . ? C61 C60 P1 118.0(4) . . ? C65 C60 P1 122.4(5) . . ? C60 C61 C62 120.2(6) . . ? C63 C62 C61 120.3(7) . . ? C64 C63 C62 119.4(7) . . ? C63 C64 C65 121.6(7) . . ? C64 C65 C60 119.1(7) . . ? C67 C66 C71 118.7(5) . . ? C67 C66 P2 117.5(4) . . ? C71 C66 P2 123.4(4) . . ? C68 C67 C66 121.0(5) . . ? C67 C68 C69 119.9(6) . . ? C70 C69 C68 119.9(6) . . ? C69 C70 C71 120.5(5) . . ? C66 C71 C70 120.0(5) . . ? C73 C72 C77 117.6(5) . . ? C73 C72 P2 118.5(4) . . ? C77 C72 P2 123.6(5) . . ? C74 C73 C72 121.7(6) . . ? C75 C74 C73 120.3(6) . . ? C74 C75 C76 119.4(6) . . ? C75 C76 C77 120.7(6) . . ? C76 C77 C72 120.3(6) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.593 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.105 # Attachment 'compound17.CIF' data_compound17 _database_code_depnum_ccdc_archive 'CCDC 664057' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C77 H94 Ga2 N4 P2 Pt' _chemical_formula_weight 1472.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.622(4) _cell_length_b 19.979(4) _cell_length_c 18.985(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.15(3) _cell_angle_gamma 90.00 _cell_volume 7062(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3016 _exptl_absorpt_coefficient_mu 2.823 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.757 _exptl_absorpt_correction_T_max 0.868 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23749 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12402 _reflns_number_gt 9696 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0135P)^2^+13.8005P] 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 12402 _refine_ls_number_parameters 791 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.003 _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 0.503619(10) 0.191116(9) 0.827936(10) 0.01645(6) Uani 1 1 d . . . Ga1 Ga 0.58300(3) 0.27675(2) 0.78378(3) 0.01805(13) Uani 1 1 d . . . P1 P 0.56367(7) 0.15427(6) 0.92994(7) 0.0206(3) Uani 1 1 d . . . N1 N 0.6725(2) 0.26512(18) 0.73856(19) 0.0197(9) Uani 1 1 d . . . C1 C 0.6983(3) 0.3272(2) 0.7164(2) 0.0219(12) Uani 1 1 d . . . H1 H 0.7422 0.3314 0.6921 0.026 Uiso 1 1 calc R . . Ga2 Ga 0.42096(3) 0.22765(2) 0.73598(3) 0.01695(12) Uani 1 1 d . . . P2 P 0.44023(7) 0.10080(6) 0.87307(7) 0.0218(3) Uani 1 1 d . . . N2 N 0.5940(2) 0.37001(17) 0.76797(19) 0.0167(9) Uani 1 1 d . . . C2 C 0.6572(3) 0.3807(2) 0.7314(2) 0.0237(12) Uani 1 1 d . . . H2 H 0.6709 0.4245 0.7175 0.028 Uiso 1 1 calc R . . N3 N 0.4093(2) 0.22873(17) 0.63655(19) 0.0165(9) Uani 1 1 d . . . C3 C 0.7232(3) 0.2112(2) 0.7402(2) 0.0236(12) Uani 1 1 d . . . N4 N 0.3330(2) 0.27592(18) 0.74123(19) 0.0176(9) Uani 1 1 d . . . C4 C 0.7878(3) 0.2182(3) 0.7795(3) 0.0302(13) Uani 1 1 d . . . C5 C 0.8391(3) 0.1671(3) 0.7758(3) 0.0361(14) Uani 1 1 d . . . H5 H 0.8838 0.1721 0.8002 0.043 Uiso 1 1 calc R . . C6 C 0.8258(3) 0.1099(3) 0.7373(3) 0.0397(15) Uani 1 1 d . . . H6 H 0.8611 0.0756 0.7358 0.048 Uiso 1 1 calc R . . C7 C 0.7618(3) 0.1022(3) 0.7011(3) 0.0354(14) Uani 1 1 d . . . H7 H 0.7528 0.0620 0.6757 0.042 Uiso 1 1 calc R . . C8 C 0.7099(3) 0.1521(3) 0.7010(3) 0.0271(12) Uani 1 1 d . . . C9 C 0.8030(3) 0.2778(3) 0.8272(3) 0.0336(14) Uani 1 1 d . . . H9 H 0.7599 0.3075 0.8246 0.040 Uiso 1 1 calc R . . C10 C 0.8672(3) 0.3193(3) 0.8034(3) 0.0498(17) Uani 1 1 d . . . H10A H 0.9110 0.2922 0.8071 0.075 Uiso 1 1 calc R . . H10B H 0.8723 0.3589 0.8335 0.075 Uiso 1 1 calc R . . H10C H 0.8593 0.3333 0.7544 0.075 Uiso 1 1 calc R . . C11 C 0.8136(3) 0.2567(3) 0.9051(3) 0.0414(15) Uani 1 1 d . . . H11A H 0.8557 0.2276 0.9097 0.062 Uiso 1 1 calc R . . H11B H 0.7709 0.2326 0.9206 0.062 Uiso 1 1 calc R . . H11C H 0.8208 0.2967 0.9343 0.062 Uiso 1 1 calc R . . C12 C 0.6413(3) 0.1420(3) 0.6576(3) 0.0290(13) Uani 1 1 d . . . H12 H 0.6145 0.1854 0.6575 0.035 Uiso 1 1 calc R . . C13 C 0.6571(4) 0.1247(3) 0.5809(3) 0.0485(17) Uani 1 1 d . . . H13A H 0.6891 0.1586 0.5614 0.073 Uiso 1 1 calc R . . H13B H 0.6120 0.1236 0.5533 0.073 Uiso 1 1 calc R . . H13C H 0.6803 0.0807 0.5788 0.073 Uiso 1 1 calc R . . C14 C 0.5929(3) 0.0894(3) 0.6902(3) 0.0432(16) Uani 1 1 d . . . H14A H 0.6188 0.0468 0.6939 0.065 Uiso 1 1 calc R . . H14B H 0.5498 0.0834 0.6604 0.065 Uiso 1 1 calc R . . H14C H 0.5789 0.1041 0.7372 0.065 Uiso 1 1 calc R . . C15 C 0.5613(3) 0.4298(2) 0.7941(2) 0.0192(11) Uani 1 1 d . . . C16 C 0.5766(3) 0.4514(2) 0.8643(3) 0.0256(12) Uani 1 1 d . . . C17 C 0.5478(3) 0.5113(2) 0.8869(3) 0.0294(13) Uani 1 1 d . . . H17 H 0.5582 0.5266 0.9334 0.035 Uiso 1 1 calc R . . C18 C 0.5044(3) 0.5489(3) 0.8435(3) 0.0343(14) Uani 1 1 d . . . H18 H 0.4845 0.5895 0.8604 0.041 Uiso 1 1 calc R . . C19 C 0.4893(3) 0.5286(2) 0.7754(3) 0.0273(13) Uani 1 1 d . . . H19 H 0.4599 0.5558 0.7456 0.033 Uiso 1 1 calc R . . C20 C 0.5168(3) 0.4685(2) 0.7497(3) 0.0222(12) Uani 1 1 d . . . C21 C 0.6273(3) 0.4117(3) 0.9127(3) 0.0301(13) Uani 1 1 d . . . H21 H 0.6234 0.3635 0.8988 0.036 Uiso 1 1 calc R . . C22 C 0.6098(3) 0.4166(3) 0.9904(3) 0.0437(16) Uani 1 1 d . . . H22A H 0.6196 0.4621 1.0072 0.066 Uiso 1 1 calc R . . H22B H 0.6396 0.3848 1.0173 0.066 Uiso 1 1 calc R . . H22C H 0.5590 0.4060 0.9969 0.066 Uiso 1 1 calc R . . C23 C 0.7056(3) 0.4334(3) 0.9019(3) 0.0438(16) Uani 1 1 d . . . H23A H 0.7116 0.4801 0.9168 0.066 Uiso 1 1 calc R . . H23B H 0.7172 0.4293 0.8519 0.066 Uiso 1 1 calc R . . H23C H 0.7378 0.4047 0.9299 0.066 Uiso 1 1 calc R . . C24 C 0.5021(3) 0.4496(2) 0.6736(3) 0.0244(12) Uani 1 1 d . . . H24 H 0.5213 0.4035 0.6663 0.029 Uiso 1 1 calc R . . C25 C 0.5418(3) 0.4965(3) 0.6245(3) 0.0441(16) Uani 1 1 d . . . H25A H 0.5251 0.5425 0.6315 0.066 Uiso 1 1 calc R . . H25B H 0.5323 0.4832 0.5755 0.066 Uiso 1 1 calc R . . H25C H 0.5935 0.4940 0.6348 0.066 Uiso 1 1 calc R . . C26 C 0.4218(3) 0.4484(3) 0.6544(3) 0.0356(14) Uani 1 1 d . . . H26A H 0.3974 0.4160 0.6844 0.053 Uiso 1 1 calc R . . H26B H 0.4153 0.4354 0.6049 0.053 Uiso 1 1 calc R . . H26C H 0.4013 0.4930 0.6615 0.053 Uiso 1 1 calc R . . C27 C 0.3474(3) 0.2648(2) 0.6190(3) 0.0209(11) Uani 1 1 d . . . H27 H 0.3335 0.2726 0.5713 0.025 Uiso 1 1 calc R . . C28 C 0.3084(3) 0.2876(2) 0.6717(3) 0.0210(11) Uani 1 1 d . . . H28 H 0.2650 0.3114 0.6627 0.025 Uiso 1 1 calc R . . C29 C 0.4425(3) 0.1961(2) 0.5780(2) 0.0198(11) Uani 1 1 d . . . C30 C 0.4275(3) 0.1281(2) 0.5640(2) 0.0210(11) Uani 1 1 d . . . C31 C 0.4540(3) 0.0996(2) 0.5024(3) 0.0261(12) Uani 1 1 d . . . H31 H 0.4454 0.0536 0.4930 0.031 Uiso 1 1 calc R . . C32 C 0.4919(3) 0.1366(3) 0.4557(3) 0.0288(13) Uani 1 1 d . . . H32 H 0.5086 0.1167 0.4136 0.035 Uiso 1 1 calc R . . C33 C 0.5061(3) 0.2032(2) 0.4697(3) 0.0257(12) Uani 1 1 d . . . H33 H 0.5322 0.2286 0.4365 0.031 Uiso 1 1 calc R . . C34 C 0.4831(3) 0.2341(2) 0.5310(2) 0.0207(11) Uani 1 1 d . . . C35 C 0.3802(3) 0.0864(2) 0.6117(3) 0.0278(13) Uani 1 1 d . . . H35 H 0.3908 0.1005 0.6614 0.033 Uiso 1 1 calc R . . C36 C 0.3005(3) 0.1006(3) 0.5961(3) 0.0412(15) Uani 1 1 d . . . H36A H 0.2874 0.0834 0.5492 0.062 Uiso 1 1 calc R . . H36B H 0.2920 0.1490 0.5976 0.062 Uiso 1 1 calc R . . H36C H 0.2712 0.0784 0.6315 0.062 Uiso 1 1 calc R . . C37 C 0.3938(3) 0.0118(2) 0.6072(3) 0.0391(15) Uani 1 1 d . . . H37A H 0.3788 -0.0045 0.5605 0.059 Uiso 1 1 calc R . . H37B H 0.3662 -0.0113 0.6433 0.059 Uiso 1 1 calc R . . H37C H 0.4451 0.0029 0.6149 0.059 Uiso 1 1 calc R . . C38 C 0.5022(3) 0.3065(2) 0.5450(3) 0.0260(12) Uani 1 1 d . . . H38 H 0.4787 0.3207 0.5895 0.031 Uiso 1 1 calc R . . C39 C 0.5837(3) 0.3144(3) 0.5553(3) 0.0355(14) Uani 1 1 d . . . H39A H 0.5998 0.2884 0.5964 0.053 Uiso 1 1 calc R . . H39B H 0.5954 0.3617 0.5627 0.053 Uiso 1 1 calc R . . H39C H 0.6080 0.2981 0.5133 0.053 Uiso 1 1 calc R . . C40 C 0.4757(3) 0.3523(2) 0.4858(3) 0.0383(15) Uani 1 1 d . . . H40A H 0.4980 0.3391 0.4416 0.058 Uiso 1 1 calc R . . H40B H 0.4886 0.3987 0.4970 0.058 Uiso 1 1 calc R . . H40C H 0.4234 0.3486 0.4808 0.058 Uiso 1 1 calc R . . C41 C 0.2817(2) 0.2862(2) 0.7946(2) 0.0170(11) Uani 1 1 d . . . C42 C 0.2212(3) 0.2436(2) 0.7991(3) 0.0217(11) Uani 1 1 d . . . C43 C 0.1700(3) 0.2563(2) 0.8493(3) 0.0272(12) Uani 1 1 d . . . H43 H 0.1292 0.2279 0.8521 0.033 Uiso 1 1 calc R . . C44 C 0.1772(3) 0.3098(3) 0.8958(3) 0.0295(12) Uani 1 1 d . . . H44 H 0.1416 0.3182 0.9298 0.035 Uiso 1 1 calc R . . C45 C 0.2368(3) 0.3503(2) 0.8915(3) 0.0242(12) Uani 1 1 d . . . H45 H 0.2422 0.3864 0.9238 0.029 Uiso 1 1 calc R . . C46 C 0.2885(3) 0.3403(2) 0.8420(3) 0.0213(11) Uani 1 1 d . . . C47 C 0.2114(3) 0.1832(2) 0.7513(3) 0.0308(13) Uani 1 1 d . . . H47 H 0.2562 0.1772 0.7238 0.037 Uiso 1 1 calc R . . C48 C 0.1997(4) 0.1201(3) 0.7948(3) 0.0527(19) Uani 1 1 d . . . H48A H 0.2360 0.1179 0.8329 0.079 Uiso 1 1 calc R . . H48B H 0.2040 0.0807 0.7645 0.079 Uiso 1 1 calc R . . H48C H 0.1517 0.1213 0.8150 0.079 Uiso 1 1 calc R . . C49 C 0.1479(3) 0.1922(3) 0.6989(3) 0.0437(16) Uani 1 1 d . . . H49A H 0.1034 0.1973 0.7249 0.066 Uiso 1 1 calc R . . H49B H 0.1443 0.1528 0.6683 0.066 Uiso 1 1 calc R . . H49C H 0.1558 0.2322 0.6702 0.066 Uiso 1 1 calc R . . C50 C 0.3511(3) 0.3887(2) 0.8397(3) 0.0266(12) Uani 1 1 d . . . H50 H 0.3765 0.3813 0.7945 0.032 Uiso 1 1 calc R . . C51 C 0.3264(3) 0.4613(3) 0.8414(3) 0.0439(16) Uani 1 1 d . . . H51A H 0.2926 0.4695 0.8020 0.066 Uiso 1 1 calc R . . H51B H 0.3680 0.4909 0.8372 0.066 Uiso 1 1 calc R . . H51C H 0.3025 0.4702 0.8860 0.066 Uiso 1 1 calc R . . C52 C 0.4035(3) 0.3744(3) 0.8997(3) 0.0530(19) Uani 1 1 d . . . H52A H 0.3786 0.3775 0.9446 0.080 Uiso 1 1 calc R . . H52B H 0.4426 0.4072 0.8991 0.080 Uiso 1 1 calc R . . H52C H 0.4233 0.3293 0.8943 0.080 Uiso 1 1 calc R . . C53 C 0.5170(3) 0.0728(2) 0.9285(3) 0.0265(12) Uani 1 1 d . . . H53A H 0.5454 0.0372 0.9057 0.032 Uiso 1 1 calc R . . H53B H 0.5024 0.0581 0.9759 0.032 Uiso 1 1 calc R . . C54 C 0.6565(3) 0.1295(2) 0.9464(3) 0.0238(12) Uani 1 1 d . . . C55 C 0.6893(3) 0.1311(2) 1.0133(3) 0.0265(12) Uani 1 1 d . . . H55 H 0.6660 0.1521 1.0515 0.032 Uiso 1 1 calc R . . C56 C 0.7561(3) 0.1015(3) 1.0236(3) 0.0327(14) Uani 1 1 d . . . H56 H 0.7783 0.1020 1.0691 0.039 Uiso 1 1 calc R . . C57 C 0.7903(3) 0.0716(3) 0.9687(3) 0.0344(14) Uani 1 1 d . . . H57 H 0.8360 0.0513 0.9763 0.041 Uiso 1 1 calc R . . C58 C 0.7585(3) 0.0708(3) 0.9021(3) 0.0372(14) Uani 1 1 d . . . H58 H 0.7822 0.0500 0.8641 0.045 Uiso 1 1 calc R . . C59 C 0.6923(3) 0.1002(3) 0.8913(3) 0.0319(13) Uani 1 1 d . . . H59 H 0.6709 0.1002 0.8454 0.038 Uiso 1 1 calc R . . C60 C 0.5301(3) 0.1952(2) 1.0079(3) 0.0237(11) Uani 1 1 d . . . C61 C 0.5159(3) 0.1614(3) 1.0705(3) 0.0388(15) Uani 1 1 d . . . H61 H 0.5301 0.1160 1.0758 0.047 Uiso 1 1 calc R . . C62 C 0.4814(3) 0.1932(3) 1.1247(3) 0.0455(16) Uani 1 1 d . . . H62 H 0.4725 0.1694 1.1670 0.055 Uiso 1 1 calc R . . C63 C 0.4599(3) 0.2580(3) 1.1184(3) 0.0406(15) Uani 1 1 d . . . H63 H 0.4345 0.2790 1.1553 0.049 Uiso 1 1 calc R . . C64 C 0.4754(3) 0.2930(3) 1.0579(3) 0.0380(15) Uani 1 1 d . . . H64 H 0.4618 0.3387 1.0538 0.046 Uiso 1 1 calc R . . C65 C 0.5107(3) 0.2622(2) 1.0029(3) 0.0299(13) Uani 1 1 d . . . H65 H 0.5216 0.2870 0.9618 0.036 Uiso 1 1 calc R . . C66 C 0.3717(3) 0.1213(2) 0.9351(3) 0.0256(12) Uani 1 1 d . . . C67 C 0.3469(3) 0.1864(3) 0.9380(3) 0.0319(13) Uani 1 1 d . . . H67 H 0.3626 0.2181 0.9043 0.038 Uiso 1 1 calc R . . C68 C 0.2999(3) 0.2060(3) 0.9888(3) 0.0441(16) Uani 1 1 d . . . H68 H 0.2843 0.2512 0.9908 0.053 Uiso 1 1 calc R . . C69 C 0.2754(3) 0.1600(4) 1.0370(3) 0.0551(19) Uani 1 1 d . . . H69 H 0.2415 0.1733 1.0709 0.066 Uiso 1 1 calc R . . C70 C 0.2998(4) 0.0954(4) 1.0360(3) 0.0537(18) Uani 1 1 d . . . H70 H 0.2838 0.0642 1.0701 0.064 Uiso 1 1 calc R . . C71 C 0.3475(3) 0.0754(3) 0.9855(3) 0.0438(16) Uani 1 1 d . . . H71 H 0.3641 0.0304 0.9847 0.053 Uiso 1 1 calc R . . C72 C 0.4116(3) 0.0239(2) 0.8281(3) 0.0304(13) Uani 1 1 d . . . C73 C 0.4627(3) -0.0111(3) 0.7900(3) 0.0355(14) Uani 1 1 d . . . H73 H 0.5098 0.0064 0.7855 0.043 Uiso 1 1 calc R . . C74 C 0.4442(4) -0.0715(3) 0.7587(3) 0.0455(17) Uani 1 1 d . . . H74 H 0.4792 -0.0960 0.7336 0.055 Uiso 1 1 calc R . . C75 C 0.3755(4) -0.0964(3) 0.7638(3) 0.0480(19) Uani 1 1 d . . . H75 H 0.3631 -0.1379 0.7422 0.058 Uiso 1 1 calc R . . C76 C 0.3254(4) -0.0613(3) 0.7998(3) 0.0461(18) Uani 1 1 d . . . H76 H 0.2779 -0.0782 0.8029 0.055 Uiso 1 1 calc R . . C77 C 0.3428(3) -0.0017(3) 0.8317(3) 0.0381(15) Uani 1 1 d . . . H77 H 0.3073 0.0223 0.8566 0.046 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 0.01769(10) 0.01569(10) 0.01591(10) 0.00184(8) -0.00123(7) 0.00003(9) Ga1 0.0180(3) 0.0173(3) 0.0189(3) 0.0024(2) 0.0000(2) 0.0000(2) P1 0.0237(7) 0.0193(7) 0.0187(7) 0.0038(6) -0.0041(6) 0.0002(6) N1 0.020(2) 0.024(2) 0.016(2) 0.0025(18) 0.0016(18) 0.0029(18) C1 0.016(3) 0.035(3) 0.015(3) 0.012(2) 0.004(2) -0.005(2) Ga2 0.0177(3) 0.0179(3) 0.0152(3) 0.0006(2) -0.0002(2) 0.0014(2) P2 0.0226(7) 0.0183(7) 0.0244(7) 0.0036(6) -0.0033(6) -0.0033(6) N2 0.020(2) 0.014(2) 0.016(2) 0.0048(17) -0.0001(18) -0.0033(17) C2 0.027(3) 0.024(3) 0.020(3) 0.008(2) -0.005(2) -0.008(2) N3 0.018(2) 0.017(2) 0.015(2) -0.0001(17) -0.0018(17) 0.0020(17) C3 0.020(3) 0.033(3) 0.018(3) 0.005(2) 0.000(2) 0.001(2) N4 0.014(2) 0.021(2) 0.018(2) 0.0015(18) 0.0005(17) 0.0025(17) C4 0.021(3) 0.040(3) 0.030(3) 0.006(3) 0.004(2) 0.000(3) C5 0.022(3) 0.056(4) 0.030(3) 0.014(3) -0.001(3) 0.003(3) C6 0.035(4) 0.046(4) 0.039(4) 0.002(3) 0.006(3) 0.022(3) C7 0.042(4) 0.037(3) 0.028(3) -0.003(3) 0.003(3) 0.014(3) C8 0.031(3) 0.032(3) 0.019(3) 0.002(2) -0.002(2) 0.009(3) C9 0.021(3) 0.043(3) 0.036(3) 0.008(3) -0.010(3) -0.004(3) C10 0.039(4) 0.066(4) 0.043(4) 0.018(3) -0.012(3) -0.018(3) C11 0.039(4) 0.054(4) 0.032(3) 0.003(3) -0.008(3) 0.001(3) C12 0.030(3) 0.031(3) 0.026(3) 0.000(2) 0.001(2) 0.008(3) C13 0.059(5) 0.061(4) 0.025(3) -0.001(3) -0.005(3) 0.007(3) C14 0.042(4) 0.045(4) 0.042(4) -0.001(3) -0.009(3) -0.005(3) C15 0.018(3) 0.019(3) 0.021(3) 0.002(2) 0.003(2) -0.005(2) C16 0.026(3) 0.022(3) 0.028(3) 0.001(2) 0.002(2) -0.011(2) C17 0.033(3) 0.025(3) 0.030(3) -0.007(2) 0.002(3) -0.006(3) C18 0.036(3) 0.021(3) 0.045(4) -0.011(3) 0.000(3) -0.005(3) C19 0.027(3) 0.018(3) 0.036(3) -0.001(2) -0.003(3) 0.002(2) C20 0.017(3) 0.022(3) 0.028(3) -0.004(2) -0.001(2) -0.009(2) C21 0.040(4) 0.026(3) 0.024(3) 0.003(2) -0.005(3) -0.009(3) C22 0.056(4) 0.043(4) 0.032(3) 0.002(3) -0.007(3) -0.015(3) C23 0.043(4) 0.057(4) 0.031(3) 0.004(3) -0.012(3) 0.007(3) C24 0.027(3) 0.014(2) 0.032(3) 0.004(2) -0.005(2) -0.002(2) C25 0.055(4) 0.047(4) 0.030(3) 0.013(3) -0.009(3) -0.014(3) C26 0.039(4) 0.043(3) 0.025(3) -0.001(3) -0.007(3) 0.003(3) C27 0.025(3) 0.020(3) 0.018(3) 0.001(2) -0.007(2) 0.006(2) C28 0.016(3) 0.018(3) 0.029(3) 0.001(2) -0.001(2) 0.003(2) C29 0.021(3) 0.023(3) 0.015(2) -0.001(2) -0.001(2) 0.003(2) C30 0.024(3) 0.021(3) 0.017(3) -0.001(2) -0.003(2) -0.001(2) C31 0.032(3) 0.019(3) 0.027(3) -0.004(2) 0.002(3) 0.004(2) C32 0.030(3) 0.036(3) 0.021(3) -0.009(2) 0.000(2) 0.011(3) C33 0.023(3) 0.032(3) 0.022(3) 0.003(2) 0.000(2) 0.002(2) C34 0.018(3) 0.023(3) 0.021(3) 0.000(2) 0.000(2) 0.007(2) C35 0.043(4) 0.022(3) 0.018(3) -0.004(2) -0.002(3) 0.001(2) C36 0.037(4) 0.034(3) 0.052(4) -0.003(3) 0.010(3) -0.010(3) C37 0.049(4) 0.028(3) 0.040(4) 0.004(3) 0.003(3) -0.001(3) C38 0.027(3) 0.024(3) 0.027(3) 0.001(2) 0.006(2) 0.003(2) C39 0.032(3) 0.031(3) 0.043(3) 0.000(3) -0.002(3) 0.003(3) C40 0.039(4) 0.026(3) 0.050(4) 0.008(3) -0.013(3) -0.003(3) C41 0.014(3) 0.021(3) 0.017(3) 0.002(2) 0.005(2) 0.006(2) C42 0.020(3) 0.020(3) 0.025(3) -0.001(2) -0.005(2) 0.004(2) C43 0.023(3) 0.028(3) 0.030(3) -0.001(2) -0.002(2) -0.008(2) C44 0.026(3) 0.041(3) 0.022(3) 0.003(3) 0.010(2) 0.001(3) C45 0.027(3) 0.023(3) 0.022(3) -0.005(2) 0.002(2) -0.001(2) C46 0.021(3) 0.021(3) 0.022(3) 0.002(2) 0.000(2) 0.004(2) C47 0.024(3) 0.029(3) 0.039(3) -0.011(3) 0.002(3) -0.002(2) C48 0.060(5) 0.027(3) 0.070(5) -0.008(3) -0.018(4) -0.004(3) C49 0.039(4) 0.049(4) 0.042(4) -0.016(3) -0.015(3) -0.003(3) C50 0.027(3) 0.022(3) 0.032(3) -0.007(2) 0.004(2) -0.003(2) C51 0.027(3) 0.031(3) 0.073(5) 0.000(3) 0.003(3) -0.007(3) C52 0.031(4) 0.056(4) 0.071(5) 0.013(4) -0.014(3) -0.023(3) C53 0.029(3) 0.020(3) 0.031(3) 0.004(2) -0.003(2) -0.002(2) C54 0.021(3) 0.022(3) 0.028(3) 0.007(2) -0.003(2) 0.001(2) C55 0.026(3) 0.026(3) 0.027(3) 0.003(2) -0.008(2) -0.003(2) C56 0.035(3) 0.033(3) 0.029(3) 0.001(3) -0.014(3) -0.003(3) C57 0.025(3) 0.032(3) 0.045(4) 0.006(3) -0.007(3) -0.002(3) C58 0.032(3) 0.048(4) 0.033(3) 0.001(3) 0.010(3) 0.007(3) C59 0.030(3) 0.040(3) 0.025(3) 0.011(3) 0.000(3) 0.002(3) C60 0.022(3) 0.027(3) 0.023(3) 0.002(2) -0.004(2) -0.001(2) C61 0.054(4) 0.035(3) 0.027(3) 0.012(3) 0.004(3) 0.006(3) C62 0.065(4) 0.047(4) 0.026(3) 0.006(3) 0.017(3) 0.007(3) C63 0.044(4) 0.050(4) 0.028(3) -0.010(3) -0.002(3) 0.013(3) C64 0.052(4) 0.024(3) 0.037(4) -0.005(3) -0.008(3) 0.000(3) C65 0.035(3) 0.029(3) 0.025(3) -0.001(2) -0.004(3) -0.004(3) C66 0.025(3) 0.028(3) 0.024(3) 0.008(2) -0.002(2) -0.009(2) C67 0.035(3) 0.037(3) 0.023(3) 0.008(3) -0.002(3) 0.001(3) C68 0.044(4) 0.058(4) 0.030(3) 0.000(3) 0.001(3) 0.012(3) C69 0.033(4) 0.096(6) 0.038(4) 0.006(4) 0.010(3) 0.005(4) C70 0.050(4) 0.074(5) 0.038(4) 0.018(4) 0.014(3) -0.019(4) C71 0.047(4) 0.040(4) 0.044(4) 0.014(3) -0.001(3) -0.014(3) C72 0.042(4) 0.017(3) 0.031(3) 0.004(2) -0.012(3) -0.002(3) C73 0.047(4) 0.029(3) 0.030(3) -0.003(3) -0.003(3) -0.011(3) C74 0.078(5) 0.034(3) 0.024(3) -0.003(3) -0.001(3) 0.005(3) C75 0.090(6) 0.025(3) 0.028(3) 0.004(3) -0.018(4) -0.015(4) C76 0.060(5) 0.034(4) 0.043(4) 0.008(3) -0.018(4) -0.024(3) C77 0.039(4) 0.030(3) 0.045(4) 0.004(3) -0.007(3) -0.005(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 2.3291(13) . ? Pt1 P1 2.3356(13) . ? Pt1 Ga2 2.4170(8) . ? Pt1 Ga1 2.4218(7) . ? Ga1 N2 1.899(4) . ? Ga1 N1 1.905(4) . ? P1 C60 1.812(5) . ? P1 C54 1.819(5) . ? P1 C53 1.846(5) . ? N1 C1 1.397(6) . ? N1 C3 1.432(6) . ? C1 C2 1.349(7) . ? Ga2 N3 1.896(4) . ? Ga2 N4 1.906(4) . ? P2 C66 1.800(6) . ? P2 C72 1.832(5) . ? P2 C53 1.845(5) . ? N2 C2 1.395(6) . ? N2 C15 1.434(6) . ? N3 C27 1.395(6) . ? N3 C29 1.439(6) . ? C3 C4 1.409(7) . ? C3 C8 1.415(7) . ? N4 C28 1.407(6) . ? N4 C41 1.421(6) . ? C4 C5 1.401(7) . ? C4 C9 1.519(7) . ? C5 C6 1.377(8) . ? C6 C7 1.373(7) . ? C7 C8 1.388(7) . ? C8 C12 1.521(7) . ? C9 C10 1.530(7) . ? C9 C11 1.546(7) . ? C12 C14 1.523(7) . ? C12 C13 1.531(7) . ? C15 C20 1.402(6) . ? C15 C16 1.424(7) . ? C16 C17 1.384(7) . ? C16 C21 1.525(7) . ? C17 C18 1.367(7) . ? C18 C19 1.378(7) . ? C19 C20 1.398(7) . ? C20 C24 1.513(7) . ? C21 C22 1.521(7) . ? C21 C23 1.539(8) . ? C24 C25 1.524(7) . ? C24 C26 1.533(7) . ? C27 C28 1.329(7) . ? C29 C34 1.403(7) . ? C29 C30 1.412(6) . ? C30 C31 1.399(7) . ? C30 C35 1.524(7) . ? C31 C32 1.364(7) . ? C32 C33 1.380(7) . ? C33 C34 1.394(7) . ? C34 C38 1.513(6) . ? C35 C37 1.515(7) . ? C35 C36 1.534(7) . ? C38 C40 1.523(7) . ? C38 C39 1.534(7) . ? C41 C46 1.412(6) . ? C41 C42 1.416(6) . ? C42 C43 1.386(7) . ? C42 C47 1.519(7) . ? C43 C44 1.390(7) . ? C44 C45 1.378(7) . ? C45 C46 1.374(7) . ? C46 C50 1.514(7) . ? C47 C48 1.524(8) . ? C47 C49 1.540(7) . ? C50 C52 1.513(7) . ? C50 C51 1.521(7) . ? C54 C59 1.382(7) . ? C54 C55 1.400(6) . ? C55 C56 1.388(7) . ? C56 C57 1.370(8) . ? C57 C58 1.386(7) . ? C58 C59 1.377(7) . ? C60 C65 1.389(7) . ? C60 C61 1.397(7) . ? C61 C62 1.379(8) . ? C62 C63 1.360(8) . ? C63 C64 1.380(8) . ? C64 C65 1.389(8) . ? C66 C67 1.383(7) . ? C66 C71 1.405(7) . ? C67 C68 1.372(8) . ? C68 C69 1.380(8) . ? C69 C70 1.369(9) . ? C70 C71 1.380(9) . ? C72 C77 1.382(7) . ? C72 C73 1.394(8) . ? C73 C74 1.386(7) . ? C74 C75 1.378(9) . ? C75 C76 1.363(9) . ? C76 C77 1.372(7) . ? 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 71.85(5) . . ? P2 Pt1 Ga2 100.34(4) . . ? P1 Pt1 Ga2 168.93(4) . . ? P2 Pt1 Ga1 172.80(3) . . ? P1 Pt1 Ga1 102.96(4) . . ? Ga2 Pt1 Ga1 85.46(2) . . ? N2 Ga1 N1 87.15(17) . . ? N2 Ga1 Pt1 144.73(12) . . ? N1 Ga1 Pt1 128.00(11) . . ? C60 P1 C54 108.9(2) . . ? C60 P1 C53 103.9(2) . . ? C54 P1 C53 102.0(2) . . ? C60 P1 Pt1 111.58(16) . . ? C54 P1 Pt1 131.71(18) . . ? C53 P1 Pt1 92.76(15) . . ? C1 N1 C3 116.3(4) . . ? C1 N1 Ga1 109.7(3) . . ? C3 N1 Ga1 131.6(3) . . ? C2 C1 N1 116.1(4) . . ? N3 Ga2 N4 88.01(16) . . ? N3 Ga2 Pt1 141.35(12) . . ? N4 Ga2 Pt1 130.60(11) . . ? C66 P2 C72 107.0(3) . . ? C66 P2 C53 104.3(2) . . ? C72 P2 C53 103.1(2) . . ? C66 P2 Pt1 115.83(17) . . ? C72 P2 Pt1 128.54(19) . . ? C53 P2 Pt1 93.00(16) . . ? C2 N2 C15 114.4(4) . . ? C2 N2 Ga1 108.9(3) . . ? C15 N2 Ga1 135.7(3) . . ? C1 C2 N2 118.2(4) . . ? C27 N3 C29 114.5(4) . . ? C27 N3 Ga2 108.7(3) . . ? C29 N3 Ga2 136.2(3) . . ? C4 C3 C8 120.0(5) . . ? C4 C3 N1 119.4(4) . . ? C8 C3 N1 120.5(4) . . ? C28 N4 C41 115.7(4) . . ? C28 N4 Ga2 107.4(3) . . ? C41 N4 Ga2 134.5(3) . . ? C5 C4 C3 118.4(5) . . ? C5 C4 C9 118.8(5) . . ? C3 C4 C9 122.8(5) . . ? C6 C5 C4 121.1(5) . . ? C7 C6 C5 120.2(5) . . ? C6 C7 C8 121.2(5) . . ? C7 C8 C3 119.0(5) . . ? C7 C8 C12 118.9(5) . . ? C3 C8 C12 122.1(4) . . ? C4 C9 C10 112.7(5) . . ? C4 C9 C11 112.1(4) . . ? C10 C9 C11 110.2(4) . . ? C8 C12 C14 111.6(4) . . ? C8 C12 C13 111.7(5) . . ? C14 C12 C13 111.0(5) . . ? C20 C15 C16 120.0(4) . . ? C20 C15 N2 120.1(4) . . ? C16 C15 N2 119.8(4) . . ? C17 C16 C15 118.7(5) . . ? C17 C16 C21 120.2(5) . . ? C15 C16 C21 121.1(4) . . ? C18 C17 C16 121.1(5) . . ? C17 C18 C19 120.7(5) . . ? C18 C19 C20 120.7(5) . . ? C19 C20 C15 118.7(4) . . ? C19 C20 C24 119.1(4) . . ? C15 C20 C24 122.0(4) . . ? C22 C21 C16 114.1(5) . . ? C22 C21 C23 109.4(4) . . ? C16 C21 C23 110.4(4) . . ? C20 C24 C25 110.5(4) . . ? C20 C24 C26 112.9(4) . . ? C25 C24 C26 110.3(4) . . ? C28 C27 N3 117.3(4) . . ? C27 C28 N4 118.5(4) . . ? C34 C29 C30 120.5(4) . . ? C34 C29 N3 119.4(4) . . ? C30 C29 N3 119.6(4) . . ? C31 C30 C29 118.5(5) . . ? C31 C30 C35 119.5(4) . . ? C29 C30 C35 121.9(4) . . ? C32 C31 C30 121.3(5) . . ? C31 C32 C33 119.8(5) . . ? C32 C33 C34 121.8(5) . . ? C33 C34 C29 118.1(4) . . ? C33 C34 C38 119.7(4) . . ? C29 C34 C38 122.3(4) . . ? C37 C35 C30 113.9(4) . . ? C37 C35 C36 109.4(4) . . ? C30 C35 C36 110.7(4) . . ? C34 C38 C40 112.0(4) . . ? C34 C38 C39 110.4(4) . . ? C40 C38 C39 109.8(4) . . ? C46 C41 C42 118.9(4) . . ? C46 C41 N4 120.8(4) . . ? C42 C41 N4 120.2(4) . . ? C43 C42 C41 119.4(4) . . ? C43 C42 C47 118.7(5) . . ? C41 C42 C47 121.9(5) . . ? C42 C43 C44 121.2(5) . . ? C45 C44 C43 118.9(5) . . ? C46 C45 C44 122.2(5) . . ? C45 C46 C41 119.4(5) . . ? C45 C46 C50 118.5(4) . . ? C41 C46 C50 122.0(5) . . ? C42 C47 C48 110.5(4) . . ? C42 C47 C49 112.0(4) . . ? C48 C47 C49 109.3(5) . . ? C52 C50 C46 110.0(4) . . ? C52 C50 C51 110.8(5) . . ? C46 C50 C51 112.0(4) . . ? P2 C53 P1 95.7(2) . . ? C59 C54 C55 119.3(5) . . ? C59 C54 P1 117.1(4) . . ? C55 C54 P1 123.0(4) . . ? C56 C55 C54 119.4(5) . . ? C57 C56 C55 120.6(5) . . ? C56 C57 C58 120.1(5) . . ? C59 C58 C57 119.8(5) . . ? C58 C59 C54 120.7(5) . . ? C65 C60 C61 118.0(5) . . ? C65 C60 P1 118.2(4) . . ? C61 C60 P1 123.5(4) . . ? C62 C61 C60 120.8(5) . . ? C63 C62 C61 121.0(5) . . ? C62 C63 C64 119.2(6) . . ? C63 C64 C65 120.8(5) . . ? C64 C65 C60 120.2(5) . . ? C67 C66 C71 118.3(5) . . ? C67 C66 P2 118.8(4) . . ? C71 C66 P2 122.6(4) . . ? C68 C67 C66 121.0(5) . . ? C67 C68 C69 120.0(6) . . ? C70 C69 C68 120.3(6) . . ? C69 C70 C71 120.0(6) . . ? C70 C71 C66 120.3(6) . . ? C77 C72 C73 119.0(5) . . ? C77 C72 P2 123.2(5) . . ? C73 C72 P2 117.8(4) . . ? C74 C73 C72 119.5(6) . . ? C75 C74 C73 120.5(6) . . ? C76 C75 C74 119.7(6) . . ? C75 C76 C77 120.7(6) . . ? C76 C77 C72 120.6(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.630 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.109 # Attachment 'compound18.CIF' data_compound18 _database_code_depnum_ccdc_archive 'CCDC 664058' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H84 Ga2 N4 Pt' _chemical_formula_weight 1195.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.484(3) _cell_length_b 20.568(4) _cell_length_c 20.344(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5642(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour turquoise _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 3.461 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.436 _exptl_absorpt_correction_T_max 0.598 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11677 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6144 _reflns_number_gt 4181 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The largest residual electron density peak (2.515 e-/ang.3) in the final difference map is located close to Pt(1). ; _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^)+(0.0386P)^2^+21.5428P] 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 6144 _refine_ls_number_parameters 311 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.020 _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 0.574182(18) 0.2500 0.7500 0.03286(10) Uani 1 2 d S . . Ga1 Ga 0.44265(4) 0.17300(3) 0.74172(3) 0.03995(16) Uani 1 1 d . . . N1 N 0.4200(3) 0.1113(2) 0.6758(2) 0.0452(12) Uani 1 1 d . . . N2 N 0.3358(3) 0.1359(2) 0.7882(2) 0.0439(12) Uani 1 1 d . . . C1 C 0.3393(4) 0.0733(3) 0.6927(3) 0.0409(13) Uani 1 1 d . . . H1 H 0.3157 0.0399 0.6644 0.049 Uiso 1 1 calc R . . C2 C 0.2959(4) 0.0855(3) 0.7504(3) 0.0470(13) Uani 1 1 d . . . H2 H 0.2404 0.0610 0.7652 0.056 Uiso 1 1 calc R . . C3 C 0.4864(4) 0.0894(3) 0.6245(3) 0.0458(14) Uani 1 1 d . . . C4 C 0.4985(5) 0.1281(3) 0.5682(3) 0.0544(16) Uani 1 1 d . . . C5 C 0.5675(5) 0.1079(4) 0.5213(4) 0.070(2) Uani 1 1 d . . . H5 H 0.5777 0.1340 0.4834 0.084 Uiso 1 1 calc R . . C6 C 0.6210(6) 0.0517(4) 0.5283(4) 0.078(2) Uani 1 1 d . . . H6 H 0.6656 0.0382 0.4948 0.093 Uiso 1 1 calc R . . C7 C 0.6091(5) 0.0144(3) 0.5850(4) 0.066(2) Uani 1 1 d . . . H7 H 0.6490 -0.0232 0.5911 0.080 Uiso 1 1 calc R . . C8 C 0.5399(5) 0.0313(3) 0.6329(3) 0.0540(16) Uani 1 1 d . . . C9 C 0.4362(5) 0.1876(3) 0.5560(3) 0.0588(18) Uani 1 1 d . . . H9 H 0.3879 0.1912 0.5931 0.071 Uiso 1 1 calc R . . C10 C 0.5006(7) 0.2485(4) 0.5569(5) 0.097(3) Uani 1 1 d U . . H10A H 0.5563 0.2430 0.5264 0.145 Uiso 1 1 calc R . . H10B H 0.5262 0.2555 0.6015 0.145 Uiso 1 1 calc R . . H10C H 0.4608 0.2861 0.5436 0.145 Uiso 1 1 calc R . . C11 C 0.3786(8) 0.1844(5) 0.4946(5) 0.120(3) Uani 1 1 d U . . H11A H 0.4228 0.1733 0.4580 0.181 Uiso 1 1 calc R . . H11B H 0.3477 0.2267 0.4862 0.181 Uiso 1 1 calc R . . H11C H 0.3271 0.1511 0.4986 0.181 Uiso 1 1 calc R . . C12 C 0.5296(5) -0.0111(3) 0.6936(3) 0.0583(18) Uani 1 1 d . . . H12 H 0.4820 0.0105 0.7242 0.070 Uiso 1 1 calc R . . C13 C 0.6257(6) -0.0226(4) 0.7306(4) 0.079(2) Uani 1 1 d . . . H13A H 0.6707 -0.0486 0.7034 0.119 Uiso 1 1 calc R . . H13B H 0.6117 -0.0458 0.7716 0.119 Uiso 1 1 calc R . . H13C H 0.6569 0.0193 0.7406 0.119 Uiso 1 1 calc R . . C14 C 0.4855(7) -0.0777(4) 0.6737(4) 0.084(2) Uani 1 1 d . . . H14A H 0.4251 -0.0708 0.6478 0.125 Uiso 1 1 calc R . . H14B H 0.4694 -0.1026 0.7134 0.125 Uiso 1 1 calc R . . H14C H 0.5340 -0.1018 0.6474 0.125 Uiso 1 1 calc R . . C15 C 0.3125(5) 0.1352(3) 0.8575(3) 0.0523(16) Uani 1 1 d . . . C16 C 0.2336(5) 0.1725(4) 0.8817(3) 0.0641(19) Uani 1 1 d . . . C17 C 0.2126(6) 0.1696(4) 0.9485(4) 0.076(2) Uani 1 1 d . . . H17 H 0.1612 0.1960 0.9661 0.091 Uiso 1 1 calc R . . C18 C 0.2649(7) 0.1291(4) 0.9897(4) 0.086(3) Uani 1 1 d . . . H18 H 0.2480 0.1267 1.0349 0.104 Uiso 1 1 calc R . . C19 C 0.3421(6) 0.0918(4) 0.9655(3) 0.073(2) Uani 1 1 d . . . H19 H 0.3783 0.0643 0.9944 0.088 Uiso 1 1 calc R . . C20 C 0.3673(5) 0.0942(3) 0.8991(3) 0.0585(18) Uani 1 1 d . . . C21 C 0.1706(5) 0.2156(4) 0.8373(3) 0.0612(18) Uani 1 1 d . . . H21 H 0.1947 0.2086 0.7913 0.073 Uiso 1 1 calc R . . C22 C 0.1819(6) 0.2869(4) 0.8516(5) 0.095(3) Uani 1 1 d . . . H22A H 0.1621 0.2956 0.8971 0.142 Uiso 1 1 calc R . . H22B H 0.1398 0.3120 0.8217 0.142 Uiso 1 1 calc R . . H22C H 0.2513 0.2997 0.8454 0.142 Uiso 1 1 calc R . . C23 C 0.0596(6) 0.1978(5) 0.8379(5) 0.102(3) Uani 1 1 d . . . H23A H 0.0519 0.1513 0.8284 0.153 Uiso 1 1 calc R . . H23B H 0.0247 0.2232 0.8043 0.153 Uiso 1 1 calc R . . H23C H 0.0316 0.2074 0.8812 0.153 Uiso 1 1 calc R . . C24 C 0.4517(6) 0.0528(4) 0.8744(3) 0.0646(19) Uani 1 1 d . . . H24 H 0.4560 0.0587 0.8257 0.078 Uiso 1 1 calc R . . C25 C 0.5517(6) 0.0727(4) 0.9041(4) 0.085(3) Uani 1 1 d . . . H25A H 0.5625 0.1193 0.8971 0.127 Uiso 1 1 calc R . . H25B H 0.6050 0.0481 0.8828 0.127 Uiso 1 1 calc R . . H25C H 0.5516 0.0634 0.9514 0.127 Uiso 1 1 calc R . . C26 C 0.4318(6) -0.0191(4) 0.8882(5) 0.090(3) Uani 1 1 d . . . H26A H 0.4249 -0.0258 0.9356 0.135 Uiso 1 1 calc R . . H26B H 0.4871 -0.0452 0.8716 0.135 Uiso 1 1 calc R . . H26C H 0.3704 -0.0323 0.8661 0.135 Uiso 1 1 calc R . . C27 C 0.6916(5) 0.3155(4) 0.7945(4) 0.0618(19) Uani 1 1 d . . . H27 H 0.6403 0.3381 0.8169 0.074 Uiso 1 1 calc R . . C28 C 0.7568(7) 0.2759(5) 0.8346(5) 0.100(3) Uani 1 1 d . . . H28A H 0.7296 0.2754 0.8798 0.120 Uiso 1 1 calc R . . H28B H 0.8220 0.2979 0.8366 0.120 Uiso 1 1 calc R . . C29 C 0.7739(6) 0.2081(5) 0.8148(5) 0.097(3) Uani 1 1 d . . . H29A H 0.7800 0.1816 0.8551 0.116 Uiso 1 1 calc R . . H29B H 0.8385 0.2061 0.7917 0.116 Uiso 1 1 calc R . . C30 C 0.6959(5) 0.1763(3) 0.7706(4) 0.065(2) Uani 1 1 d . . . H30 H 0.6477 0.1491 0.7906 0.078 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 0.02418(14) 0.03551(16) 0.03889(16) 0.00251(14) 0.000 0.000 Ga1 0.0291(3) 0.0396(3) 0.0511(4) -0.0044(3) 0.0016(3) -0.0030(2) N1 0.032(3) 0.049(3) 0.055(3) -0.005(2) 0.006(2) -0.003(2) N2 0.041(3) 0.050(3) 0.040(3) 0.000(2) 0.004(2) -0.009(2) C1 0.031(3) 0.046(3) 0.046(3) -0.006(3) 0.003(2) -0.006(3) C2 0.039(3) 0.051(3) 0.051(3) -0.001(3) 0.003(3) -0.007(3) C3 0.036(3) 0.053(4) 0.049(3) -0.002(3) 0.010(3) -0.002(3) C4 0.053(4) 0.052(4) 0.058(4) -0.002(3) 0.012(3) 0.002(3) C5 0.072(5) 0.067(5) 0.072(5) 0.010(4) 0.032(4) 0.013(4) C6 0.073(5) 0.075(5) 0.086(6) -0.001(4) 0.038(4) 0.019(4) C7 0.056(4) 0.052(4) 0.092(5) 0.012(4) 0.030(4) 0.012(3) C8 0.038(3) 0.057(4) 0.066(4) -0.003(3) 0.005(3) 0.002(3) C9 0.068(5) 0.061(4) 0.048(4) 0.005(3) 0.009(3) 0.008(4) C10 0.105(5) 0.077(5) 0.109(5) 0.009(4) 0.012(5) 0.008(5) C11 0.124(6) 0.123(6) 0.115(6) -0.014(5) -0.027(5) 0.028(5) C12 0.043(4) 0.057(4) 0.074(4) 0.015(4) 0.010(3) 0.007(3) C13 0.062(5) 0.075(5) 0.100(6) 0.003(5) -0.013(4) 0.017(4) C14 0.094(6) 0.061(5) 0.095(6) 0.016(4) 0.002(5) -0.013(5) C15 0.048(4) 0.062(4) 0.047(4) 0.000(3) 0.008(3) -0.015(3) C16 0.054(4) 0.078(5) 0.061(4) -0.007(4) 0.015(3) -0.015(4) C17 0.078(5) 0.094(6) 0.057(4) -0.008(4) 0.028(4) -0.017(5) C18 0.105(7) 0.097(7) 0.056(5) -0.006(5) 0.023(5) -0.045(6) C19 0.090(6) 0.078(6) 0.052(4) 0.010(4) 0.002(4) -0.034(5) C20 0.071(5) 0.059(4) 0.045(4) 0.001(3) -0.001(3) -0.017(4) C21 0.046(4) 0.078(5) 0.061(4) -0.007(4) 0.017(3) 0.002(4) C22 0.073(6) 0.081(7) 0.131(8) -0.017(6) 0.003(5) -0.008(5) C23 0.064(5) 0.122(9) 0.121(8) -0.011(6) 0.002(5) -0.018(5) C24 0.073(5) 0.071(5) 0.049(4) 0.006(3) -0.016(3) -0.016(4) C25 0.071(5) 0.101(7) 0.082(6) 0.004(5) -0.008(4) -0.018(5) C26 0.088(6) 0.067(6) 0.115(7) 0.006(5) -0.016(5) -0.013(5) C27 0.034(4) 0.065(5) 0.087(5) -0.018(4) -0.008(3) -0.017(3) C28 0.065(5) 0.126(8) 0.108(7) -0.023(6) -0.050(5) 0.005(5) C29 0.056(5) 0.111(8) 0.123(8) 0.028(6) -0.034(5) 0.021(5) C30 0.033(3) 0.037(4) 0.126(7) 0.015(4) -0.005(4) 0.017(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 C27 2.268(6) . ? Pt1 C27 2.268(6) 3_556 ? Pt1 C30 2.273(6) 3_556 ? Pt1 C30 2.273(6) . ? Pt1 Ga1 2.3838(7) 3_556 ? Pt1 Ga1 2.3838(7) . ? Ga1 N1 1.871(5) . ? Ga1 N2 1.885(5) . ? N1 C1 1.383(7) . ? N1 C3 1.448(7) . ? N2 C2 1.398(7) . ? N2 C15 1.443(7) . ? C1 C2 1.336(8) . ? C3 C4 1.405(9) . ? C3 C8 1.407(8) . ? C4 C5 1.395(9) . ? C4 C9 1.504(9) . ? C5 C6 1.371(10) . ? C6 C7 1.394(10) . ? C7 C8 1.394(9) . ? C8 C12 1.518(9) . ? C9 C11 1.473(11) . ? C9 C10 1.525(11) . ? C12 C13 1.516(9) . ? C12 C14 1.547(10) . ? C15 C16 1.402(9) . ? C15 C20 1.405(9) . ? C16 C17 1.391(9) . ? C16 C21 1.525(10) . ? C17 C18 1.376(11) . ? C18 C19 1.384(11) . ? C19 C20 1.393(9) . ? C20 C24 1.507(10) . ? C21 C22 1.503(10) . ? C21 C23 1.541(10) . ? C24 C26 1.529(10) . ? C24 C25 1.533(10) . ? C27 C30 1.336(10) 3_556 ? C27 C28 1.450(11) . ? C28 C29 1.470(12) . ? C29 C30 1.530(11) . ? C30 C27 1.336(10) 3_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C27 Pt1 C27 91.4(4) . 3_556 ? C27 Pt1 C30 34.2(3) . 3_556 ? C27 Pt1 C30 79.6(2) 3_556 3_556 ? C27 Pt1 C30 79.6(2) . . ? C27 Pt1 C30 34.2(3) 3_556 . ? C30 Pt1 C30 87.6(4) 3_556 . ? C27 Pt1 Ga1 95.54(19) . 3_556 ? C27 Pt1 Ga1 160.5(2) 3_556 3_556 ? C30 Pt1 Ga1 96.14(18) 3_556 3_556 ? C30 Pt1 Ga1 165.3(2) . 3_556 ? C27 Pt1 Ga1 160.5(2) . . ? C27 Pt1 Ga1 95.54(19) 3_556 . ? C30 Pt1 Ga1 165.3(2) 3_556 . ? C30 Pt1 Ga1 96.14(18) . . ? Ga1 Pt1 Ga1 83.84(3) 3_556 . ? N1 Ga1 N2 87.7(2) . . ? N1 Ga1 Pt1 128.51(14) . . ? N2 Ga1 Pt1 143.35(15) . . ? C1 N1 C3 119.3(5) . . ? C1 N1 Ga1 109.5(4) . . ? C3 N1 Ga1 128.9(4) . . ? C2 N2 C15 116.5(5) . . ? C2 N2 Ga1 108.6(4) . . ? C15 N2 Ga1 131.3(4) . . ? C2 C1 N1 117.2(5) . . ? C1 C2 N2 117.0(5) . . ? C4 C3 C8 121.4(6) . . ? C4 C3 N1 118.9(5) . . ? C8 C3 N1 119.6(5) . . ? C5 C4 C3 117.8(6) . . ? C5 C4 C9 120.1(6) . . ? C3 C4 C9 122.0(6) . . ? C6 C5 C4 122.1(7) . . ? C5 C6 C7 119.3(6) . . ? C6 C7 C8 121.3(7) . . ? C7 C8 C3 118.0(6) . . ? C7 C8 C12 119.1(6) . . ? C3 C8 C12 122.7(6) . . ? C11 C9 C4 113.5(7) . . ? C11 C9 C10 110.3(7) . . ? C4 C9 C10 110.4(6) . . ? C13 C12 C8 114.5(6) . . ? C13 C12 C14 108.7(6) . . ? C8 C12 C14 109.3(6) . . ? C16 C15 C20 121.1(6) . . ? C16 C15 N2 120.1(6) . . ? C20 C15 N2 118.7(6) . . ? C17 C16 C15 118.3(7) . . ? C17 C16 C21 119.4(7) . . ? C15 C16 C21 122.3(6) . . ? C18 C17 C16 121.1(8) . . ? C17 C18 C19 120.4(7) . . ? C18 C19 C20 120.5(8) . . ? C19 C20 C15 118.5(7) . . ? C19 C20 C24 119.2(7) . . ? C15 C20 C24 122.3(6) . . ? C22 C21 C16 113.3(7) . . ? C22 C21 C23 109.3(7) . . ? C16 C21 C23 113.4(7) . . ? C20 C24 C26 110.6(6) . . ? C20 C24 C25 112.5(6) . . ? C26 C24 C25 109.9(7) . . ? C30 C27 C28 127.1(8) 3_556 . ? C30 C27 Pt1 73.1(4) 3_556 . ? C28 C27 Pt1 108.3(5) . . ? C27 C28 C29 118.3(7) . . ? C28 C29 C30 117.4(6) . . ? C27 C30 C29 123.9(7) 3_556 . ? C27 C30 Pt1 72.7(4) 3_556 . ? C29 C30 Pt1 108.6(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.515 _refine_diff_density_min -1.338 _refine_diff_density_rms 0.104 # Attachment 'compound20.CIF' data_compound20 _database_code_depnum_ccdc_archive 'CCDC 664059' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H119 Ga2 N4 P3 Pt' _chemical_formula_weight 1672.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.355(3) _cell_length_b 23.357(5) _cell_length_c 24.185(5) _cell_angle_alpha 84.43(3) _cell_angle_beta 89.45(3) _cell_angle_gamma 78.52(3) _cell_volume 9010(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3464 _exptl_absorpt_coefficient_mu 2.238 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.641 _exptl_absorpt_correction_T_max 0.841 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63867 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 26.00 _reflns_number_total 35058 _reflns_number_gt 24553 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains 2 crystallographically independent molecules of 20 with no significant geometric differences. Four molecules of hexane were also located in the asymmetric unit and their carbon atoms refined isotropically. ; _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^)+(0.0543P)^2^+16.5368P] 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 35058 _refine_ls_number_parameters 1817 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1350 _refine_ls_wR_factor_gt 0.1192 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.025 _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 0.341318(17) 0.511471(10) 0.254195(9) 0.04346(8) Uani 1 1 d . . . Pt2 Pt 0.847477(13) 0.018909(9) 0.256509(8) 0.02742(6) Uani 1 1 d . . . Ga1 Ga 0.36862(4) 0.59976(3) 0.20410(2) 0.04102(17) Uani 1 1 d . . . Ga2 Ga 0.31643(5) 0.58033(3) 0.32432(3) 0.0522(2) Uani 1 1 d . . . Ga3 Ga 0.69815(4) 0.02762(3) 0.26008(2) 0.02970(14) Uani 1 1 d . . . Ga4 Ga 0.81509(4) 0.08448(2) 0.32883(2) 0.02931(13) Uani 1 1 d . . . P1 P 0.47800(12) 0.64825(8) 0.21207(6) 0.0504(4) Uani 1 1 d . . . P2 P 0.39278(12) 0.45037(7) 0.18855(6) 0.0452(4) Uani 1 1 d . . . P3 P 0.33120(12) 0.42771(7) 0.31141(6) 0.0496(4) Uani 1 1 d . . . P4 P 0.61649(10) -0.01314(7) 0.32577(6) 0.0406(4) Uani 1 1 d . . . P5 P 0.86353(10) -0.05590(6) 0.20093(6) 0.0334(3) Uani 1 1 d . . . P6 P 0.99184(9) -0.00039(6) 0.26479(5) 0.0295(3) Uani 1 1 d . . . N1 N 0.3279(3) 0.64461(19) 0.13806(17) 0.0365(11) Uani 1 1 d . . . N2 N 0.2680(3) 0.78145(19) 0.08531(17) 0.0347(11) Uani 1 1 d . . . N3 N 0.2343(4) 0.6101(2) 0.3758(2) 0.0588(16) Uani 1 1 d . . . N4 N 0.3986(4) 0.5972(2) 0.37193(19) 0.0545(16) Uani 1 1 d . . . N5 N 0.6109(3) 0.05115(19) 0.20840(16) 0.0307(10) Uani 1 1 d . . . N6 N 0.4117(3) 0.1232(2) 0.20267(19) 0.0422(12) Uani 1 1 d . . . N7 N 0.8363(3) 0.15648(18) 0.35068(17) 0.0313(10) Uani 1 1 d . . . N8 N 0.8076(3) 0.05884(19) 0.40564(17) 0.0340(11) Uani 1 1 d . . . C1 C 0.4475(4) 0.6942(3) 0.1538(2) 0.0426(14) Uani 1 1 d . . . C2 C 0.5091(4) 0.7304(3) 0.1265(2) 0.0456(15) Uani 1 1 d . . . C3 C 0.5679(5) 0.6893(3) 0.0897(3) 0.072(2) Uani 1 1 d . . . H3A H 0.5975 0.6548 0.1130 0.109 Uiso 1 1 calc R . . H3B H 0.6084 0.7105 0.0715 0.109 Uiso 1 1 calc R . . H3C H 0.5348 0.6765 0.0614 0.109 Uiso 1 1 calc R . . C4 C 0.4689(5) 0.7835(3) 0.0879(3) 0.072(2) Uani 1 1 d . . . H4A H 0.5124 0.8003 0.0680 0.108 Uiso 1 1 calc R . . H4B H 0.4358 0.8129 0.1098 0.108 Uiso 1 1 calc R . . H4C H 0.4325 0.7715 0.0611 0.108 Uiso 1 1 calc R . . C5 C 0.5602(6) 0.7514(4) 0.1699(3) 0.098(3) Uani 1 1 d . . . H5A H 0.5904 0.7174 0.1936 0.147 Uiso 1 1 calc R . . H5B H 0.5228 0.7773 0.1929 0.147 Uiso 1 1 calc R . . H5C H 0.6001 0.7728 0.1513 0.147 Uiso 1 1 calc R . . C6 C 0.3671(4) 0.6956(2) 0.1218(2) 0.0357(13) Uani 1 1 d . . . H6 H 0.3812 0.6951 0.0815 0.043 Uiso 1 1 calc R . . C7 C 0.2996(3) 0.7494(2) 0.1278(2) 0.0346(13) Uani 1 1 d . . . H7 H 0.2810 0.7591 0.1637 0.042 Uiso 1 1 calc R . . C8 C 0.2625(4) 0.6370(2) 0.1025(2) 0.0402(14) Uani 1 1 d . . . C9 C 0.1807(4) 0.6410(2) 0.1223(3) 0.0455(15) Uani 1 1 d . . . C10 C 0.1200(4) 0.6312(3) 0.0860(3) 0.0542(17) Uani 1 1 d . . . H10 H 0.0651 0.6319 0.0994 0.065 Uiso 1 1 calc R . . C11 C 0.1365(5) 0.6206(3) 0.0315(3) 0.0551(18) Uani 1 1 d . . . H11 H 0.0934 0.6152 0.0077 0.066 Uiso 1 1 calc R . . C12 C 0.2161(4) 0.6179(3) 0.0124(3) 0.0488(16) Uani 1 1 d . . . H12 H 0.2274 0.6114 -0.0253 0.059 Uiso 1 1 calc R . . C13 C 0.2816(4) 0.6244(2) 0.0468(2) 0.0389(14) Uani 1 1 d . . . C14 C 0.1541(4) 0.6559(3) 0.1806(3) 0.0525(17) Uani 1 1 d . . . H14 H 0.2040 0.6632 0.2003 0.063 Uiso 1 1 calc R . . C15 C 0.1243(5) 0.6056(3) 0.2137(3) 0.069(2) Uani 1 1 d . . . H15A H 0.0755 0.5973 0.1953 0.104 Uiso 1 1 calc R . . H15B H 0.1092 0.6163 0.2512 0.104 Uiso 1 1 calc R . . H15C H 0.1690 0.5706 0.2162 0.104 Uiso 1 1 calc R . . C16 C 0.0865(5) 0.7123(3) 0.1786(3) 0.068(2) Uani 1 1 d . . . H16A H 0.1090 0.7453 0.1607 0.102 Uiso 1 1 calc R . . H16B H 0.0695 0.7203 0.2165 0.102 Uiso 1 1 calc R . . H16C H 0.0382 0.7073 0.1574 0.102 Uiso 1 1 calc R . . C17 C 0.3696(4) 0.6164(2) 0.0236(2) 0.0422(14) Uani 1 1 d . . . H17 H 0.4083 0.6185 0.0548 0.051 Uiso 1 1 calc R . . C18 C 0.3975(5) 0.5568(3) 0.0012(3) 0.0575(18) Uani 1 1 d . . . H18A H 0.3967 0.5255 0.0312 0.086 Uiso 1 1 calc R . . H18B H 0.4542 0.5536 -0.0133 0.086 Uiso 1 1 calc R . . H18C H 0.3594 0.5530 -0.0286 0.086 Uiso 1 1 calc R . . C19 C 0.3773(4) 0.6662(3) -0.0219(2) 0.0505(16) Uani 1 1 d . . . H19A H 0.3433 0.6633 -0.0543 0.076 Uiso 1 1 calc R . . H19B H 0.4358 0.6627 -0.0329 0.076 Uiso 1 1 calc R . . H19C H 0.3576 0.7043 -0.0074 0.076 Uiso 1 1 calc R . . C20 C 0.2016(3) 0.8312(2) 0.0871(2) 0.0343(13) Uani 1 1 d . . . C21 C 0.1314(4) 0.8331(2) 0.0530(2) 0.0360(13) Uani 1 1 d . . . C22 C 0.0707(4) 0.8835(3) 0.0471(2) 0.0428(14) Uani 1 1 d . . . H22 H 0.0235 0.8849 0.0240 0.051 Uiso 1 1 calc R . . C23 C 0.0767(4) 0.9323(3) 0.0740(2) 0.0472(16) Uani 1 1 d . . . H23 H 0.0347 0.9670 0.0691 0.057 Uiso 1 1 calc R . . C24 C 0.1447(4) 0.9296(3) 0.1082(2) 0.0453(15) Uani 1 1 d . . . H24 H 0.1486 0.9628 0.1271 0.054 Uiso 1 1 calc R . . C25 C 0.2079(4) 0.8798(2) 0.1158(2) 0.0370(13) Uani 1 1 d . . . C26 C 0.1234(4) 0.7810(3) 0.0213(2) 0.0424(14) Uani 1 1 d . . . H26 H 0.1565 0.7450 0.0422 0.051 Uiso 1 1 calc R . . C27 C 0.0342(4) 0.7721(3) 0.0172(3) 0.0631(19) Uani 1 1 d . . . H27A H 0.0092 0.7719 0.0542 0.095 Uiso 1 1 calc R . . H27B H 0.0340 0.7346 0.0023 0.095 Uiso 1 1 calc R . . H27C H 0.0017 0.8042 -0.0076 0.095 Uiso 1 1 calc R . . C28 C 0.1622(5) 0.7872(3) -0.0363(2) 0.0589(19) Uani 1 1 d . . . H28A H 0.1315 0.8225 -0.0578 0.088 Uiso 1 1 calc R . . H28B H 0.1592 0.7526 -0.0556 0.088 Uiso 1 1 calc R . . H28C H 0.2207 0.7903 -0.0323 0.088 Uiso 1 1 calc R . . C29 C 0.2821(4) 0.8812(3) 0.1523(2) 0.0436(15) Uani 1 1 d . . . H29 H 0.3207 0.8421 0.1528 0.052 Uiso 1 1 calc R . . C30 C 0.2572(4) 0.8905(3) 0.2125(2) 0.0512(16) Uani 1 1 d . . . H30A H 0.3075 0.8865 0.2354 0.077 Uiso 1 1 calc R . . H30B H 0.2250 0.8612 0.2267 0.077 Uiso 1 1 calc R . . H30C H 0.2231 0.9299 0.2139 0.077 Uiso 1 1 calc R . . C31 C 0.3298(5) 0.9273(3) 0.1287(3) 0.070(2) Uani 1 1 d . . . H31A H 0.3473 0.9197 0.0908 0.105 Uiso 1 1 calc R . . H31B H 0.3790 0.9258 0.1520 0.105 Uiso 1 1 calc R . . H31C H 0.2937 0.9663 0.1280 0.105 Uiso 1 1 calc R . . C32 C 0.2753(6) 0.6219(3) 0.4226(3) 0.062(2) Uani 1 1 d . . . H32 H 0.2451 0.6346 0.4544 0.074 Uiso 1 1 calc R . . C33 C 0.3575(5) 0.6148(3) 0.4210(2) 0.059(2) Uani 1 1 d . . . H33 H 0.3882 0.6213 0.4522 0.070 Uiso 1 1 calc R . . C34 C 0.1486(5) 0.6394(4) 0.3694(3) 0.067(2) Uani 1 1 d . . . C35 C 0.1272(6) 0.7011(4) 0.3627(3) 0.086(3) Uani 1 1 d . . . C36 C 0.0421(7) 0.7264(4) 0.3594(4) 0.107(4) Uani 1 1 d . . . H36 H 0.0258 0.7679 0.3560 0.129 Uiso 1 1 calc R . . C37 C -0.0165(7) 0.6946(5) 0.3607(4) 0.096(3) Uani 1 1 d U . . H37 H -0.0733 0.7140 0.3584 0.116 Uiso 1 1 calc R . . C38 C 0.0028(6) 0.6333(4) 0.3656(3) 0.094(3) Uani 1 1 d . . . H38 H -0.0399 0.6110 0.3655 0.113 Uiso 1 1 calc R . . C39 C 0.0875(6) 0.6056(4) 0.3706(3) 0.077(3) Uani 1 1 d . . . C40 C 0.1919(7) 0.7389(4) 0.3587(4) 0.094(3) Uani 1 1 d . . . H40 H 0.2474 0.7126 0.3673 0.113 Uiso 1 1 calc R . . C41 C 0.1949(9) 0.7675(5) 0.2991(5) 0.165(6) Uani 1 1 d . . . H41A H 0.2165 0.7372 0.2744 0.247 Uiso 1 1 calc R . . H41B H 0.2315 0.7961 0.2978 0.247 Uiso 1 1 calc R . . H41C H 0.1386 0.7874 0.2869 0.247 Uiso 1 1 calc R . . C42 C 0.1781(9) 0.7846(5) 0.4008(6) 0.178(6) Uani 1 1 d . . . H42A H 0.1222 0.8091 0.3955 0.267 Uiso 1 1 calc R . . H42B H 0.2200 0.8093 0.3954 0.267 Uiso 1 1 calc R . . H42C H 0.1834 0.7647 0.4386 0.267 Uiso 1 1 calc R . . C43 C 0.1082(6) 0.5384(4) 0.3805(3) 0.081(2) Uani 1 1 d . . . H43 H 0.1621 0.5248 0.3614 0.097 Uiso 1 1 calc R . . C44 C 0.0437(7) 0.5081(5) 0.3572(5) 0.113(3) Uani 1 1 d U . . H44A H -0.0062 0.5136 0.3804 0.170 Uiso 1 1 calc R . . H44B H 0.0671 0.4661 0.3571 0.170 Uiso 1 1 calc R . . H44C H 0.0287 0.5252 0.3192 0.170 Uiso 1 1 calc R . . C45 C 0.1227(6) 0.5203(3) 0.4429(4) 0.092(3) Uani 1 1 d . . . H45A H 0.0704 0.5318 0.4628 0.138 Uiso 1 1 calc R . . H45B H 0.1651 0.5399 0.4567 0.138 Uiso 1 1 calc R . . H45C H 0.1419 0.4777 0.4491 0.138 Uiso 1 1 calc R . . C46 C 0.4810(5) 0.6068(3) 0.3623(2) 0.0519(18) Uani 1 1 d . . . C47 C 0.4967(5) 0.6641(3) 0.3572(2) 0.0562(19) Uani 1 1 d . . . C48 C 0.5780(6) 0.6717(3) 0.3496(3) 0.066(2) Uani 1 1 d . . . H48 H 0.5889 0.7103 0.3476 0.079 Uiso 1 1 calc R . . C49 C 0.6434(6) 0.6256(3) 0.3449(3) 0.072(2) Uani 1 1 d . . . H49 H 0.6987 0.6319 0.3396 0.087 Uiso 1 1 calc R . . C50 C 0.6262(5) 0.5691(3) 0.3481(3) 0.067(2) Uani 1 1 d . . . H50 H 0.6706 0.5367 0.3442 0.081 Uiso 1 1 calc R . . C51 C 0.5467(5) 0.5591(3) 0.3568(3) 0.0579(19) Uani 1 1 d . . . C52 C 0.4268(6) 0.7173(3) 0.3601(2) 0.066(2) Uani 1 1 d . . . H52 H 0.3725 0.7041 0.3578 0.079 Uiso 1 1 calc R . . C53 C 0.4297(6) 0.7651(3) 0.3116(3) 0.089(3) Uani 1 1 d . . . H53A H 0.3806 0.7968 0.3130 0.134 Uiso 1 1 calc R . . H53B H 0.4297 0.7478 0.2762 0.134 Uiso 1 1 calc R . . H53C H 0.4804 0.7809 0.3147 0.134 Uiso 1 1 calc R . . C54 C 0.4287(6) 0.7453(3) 0.4152(3) 0.083(3) Uani 1 1 d . . . H54A H 0.4286 0.7154 0.4465 0.125 Uiso 1 1 calc R . . H54B H 0.3794 0.7767 0.4171 0.125 Uiso 1 1 calc R . . H54C H 0.4792 0.7617 0.4170 0.125 Uiso 1 1 calc R . . C55 C 0.5333(5) 0.4958(3) 0.3631(3) 0.0596(19) Uani 1 1 d . . . H55 H 0.4718 0.4971 0.3635 0.072 Uiso 1 1 calc R . . C56 C 0.5701(6) 0.4635(3) 0.4184(3) 0.088(3) Uani 1 1 d . . . H56A H 0.5567 0.4243 0.4230 0.132 Uiso 1 1 calc R . . H56B H 0.5463 0.4856 0.4491 0.132 Uiso 1 1 calc R . . H56C H 0.6308 0.4600 0.4184 0.132 Uiso 1 1 calc R . . C57 C 0.5697(5) 0.4626(3) 0.3147(3) 0.072(2) Uani 1 1 d . . . H57A H 0.5485 0.4851 0.2797 0.107 Uiso 1 1 calc R . . H57B H 0.5535 0.4242 0.3174 0.107 Uiso 1 1 calc R . . H57C H 0.6307 0.4570 0.3158 0.107 Uiso 1 1 calc R . . C58 C 0.3882(5) 0.3754(3) 0.2175(2) 0.0560(18) Uani 1 1 d . . . H58A H 0.3333 0.3668 0.2083 0.067 Uiso 1 1 calc R . . H58B H 0.4317 0.3472 0.2001 0.067 Uiso 1 1 calc R . . C59 C 0.4009(5) 0.3666(3) 0.2802(2) 0.0543(18) Uani 1 1 d . . . H59A H 0.4598 0.3662 0.2896 0.065 Uiso 1 1 calc R . . H59B H 0.3875 0.3286 0.2951 0.065 Uiso 1 1 calc R . . C60 C 0.5023(4) 0.4493(3) 0.1714(2) 0.0488(17) Uani 1 1 d . . . C61 C 0.5233(4) 0.4995(3) 0.1451(2) 0.0507(17) Uani 1 1 d . . . H61 H 0.4808 0.5330 0.1352 0.061 Uiso 1 1 calc R . . C62 C 0.6055(5) 0.5017(4) 0.1330(3) 0.070(2) Uani 1 1 d . . . H62 H 0.6197 0.5364 0.1151 0.083 Uiso 1 1 calc R . . C63 C 0.6682(5) 0.4516(4) 0.1479(3) 0.076(2) Uani 1 1 d . . . H63 H 0.7250 0.4527 0.1405 0.092 Uiso 1 1 calc R . . C64 C 0.6470(6) 0.4018(4) 0.1726(3) 0.075(2) Uani 1 1 d . . . H64 H 0.6892 0.3679 0.1815 0.090 Uiso 1 1 calc R . . C65 C 0.5654(5) 0.4002(3) 0.1849(3) 0.064(2) Uani 1 1 d . . . H65 H 0.5517 0.3653 0.2027 0.076 Uiso 1 1 calc R . . C66 C 0.3433(4) 0.4500(3) 0.1211(2) 0.0470(16) Uani 1 1 d . . . C67 C 0.2630(5) 0.4806(3) 0.1102(3) 0.0515(17) Uani 1 1 d . . . H67 H 0.2354 0.5065 0.1356 0.062 Uiso 1 1 calc R . . C68 C 0.2226(5) 0.4732(3) 0.0614(3) 0.0623(19) Uani 1 1 d . . . H68 H 0.1672 0.4940 0.0537 0.075 Uiso 1 1 calc R . . C69 C 0.2623(5) 0.4363(3) 0.0248(3) 0.066(2) Uani 1 1 d . . . H69 H 0.2342 0.4314 -0.0081 0.079 Uiso 1 1 calc R . . C70 C 0.3430(5) 0.4061(3) 0.0353(3) 0.065(2) Uani 1 1 d . . . H70 H 0.3705 0.3808 0.0095 0.079 Uiso 1 1 calc R . . C71 C 0.3835(5) 0.4128(3) 0.0831(2) 0.0529(17) Uani 1 1 d . . . H71 H 0.4391 0.3920 0.0902 0.063 Uiso 1 1 calc R . . C72 C 0.3611(4) 0.4149(3) 0.3849(2) 0.0514(17) Uani 1 1 d . . . C73 C 0.4109(5) 0.3620(3) 0.4071(3) 0.059(2) Uani 1 1 d . . . H73 H 0.4306 0.3320 0.3835 0.071 Uiso 1 1 calc R . . C74 C 0.4318(5) 0.3530(3) 0.4629(3) 0.070(2) Uani 1 1 d . . . H74 H 0.4665 0.3172 0.4775 0.085 Uiso 1 1 calc R . . C75 C 0.4019(5) 0.3964(4) 0.4980(3) 0.072(2) Uani 1 1 d . . . H75 H 0.4158 0.3900 0.5364 0.086 Uiso 1 1 calc R . . C76 C 0.3523(5) 0.4485(3) 0.4767(3) 0.066(2) Uani 1 1 d . . . H76 H 0.3318 0.4781 0.5004 0.080 Uiso 1 1 calc R . . C77 C 0.3320(5) 0.4577(3) 0.4203(2) 0.0573(19) Uani 1 1 d . . . H77 H 0.2979 0.4937 0.4058 0.069 Uiso 1 1 calc R . . C78 C 0.2310(5) 0.4057(3) 0.3084(3) 0.0528(17) Uani 1 1 d . . . C79 C 0.1769(5) 0.4274(3) 0.2633(3) 0.063(2) Uani 1 1 d . . . H79 H 0.1907 0.4563 0.2363 0.076 Uiso 1 1 calc R . . C80 C 0.1042(6) 0.4074(4) 0.2575(4) 0.079(2) Uani 1 1 d . . . H80 H 0.0685 0.4219 0.2263 0.095 Uiso 1 1 calc R . . C81 C 0.0832(6) 0.3661(4) 0.2974(4) 0.084(3) Uani 1 1 d . . . H81 H 0.0331 0.3519 0.2938 0.101 Uiso 1 1 calc R . . C82 C 0.1350(6) 0.3460(4) 0.3417(4) 0.079(2) Uani 1 1 d . . . H82 H 0.1206 0.3174 0.3687 0.095 Uiso 1 1 calc R . . C83 C 0.2075(5) 0.3656(3) 0.3485(3) 0.068(2) Uani 1 1 d . . . H83 H 0.2415 0.3519 0.3805 0.082 Uiso 1 1 calc R . . C84 C 0.5310(4) 0.0058(3) 0.2836(2) 0.0381(14) Uani 1 1 d . . . C85 C 0.4526(4) -0.0195(3) 0.3006(3) 0.0540(18) Uani 1 1 d . . . C86 C 0.4724(6) -0.0833(4) 0.2942(5) 0.107(3) Uani 1 1 d U . . H86A H 0.4240 -0.1005 0.3049 0.161 Uiso 1 1 calc R . . H86B H 0.5201 -0.1022 0.3181 0.161 Uiso 1 1 calc R . . H86C H 0.4862 -0.0892 0.2554 0.161 Uiso 1 1 calc R . . C87 C 0.4299(6) -0.0071(5) 0.3622(3) 0.096(3) Uani 1 1 d U . . H87A H 0.4283 0.0344 0.3664 0.145 Uiso 1 1 calc R . . H87B H 0.4721 -0.0316 0.3875 0.145 Uiso 1 1 calc R . . H87C H 0.3751 -0.0164 0.3710 0.145 Uiso 1 1 calc R . . C88 C 0.3728(4) 0.0061(3) 0.2677(3) 0.0497(16) Uani 1 1 d . . . H88A H 0.3833 0.0030 0.2280 0.074 Uiso 1 1 calc R . . H88B H 0.3544 0.0475 0.2740 0.074 Uiso 1 1 calc R . . H88C H 0.3293 -0.0157 0.2798 0.074 Uiso 1 1 calc R . . C89 C 0.5280(3) 0.0435(2) 0.2283(2) 0.0350(13) Uani 1 1 d . . . H89 H 0.5015 0.0246 0.1998 0.042 Uiso 1 1 calc R . . C90 C 0.4759(4) 0.1045(3) 0.2331(2) 0.0381(14) Uani 1 1 d . . . H90 H 0.4915 0.1287 0.2590 0.046 Uiso 1 1 calc R . . C91 C 0.6133(3) 0.0805(2) 0.1530(2) 0.0333(12) Uani 1 1 d . . . C92 C 0.5963(4) 0.0533(3) 0.1060(2) 0.0395(14) Uani 1 1 d . . . C93 C 0.6021(4) 0.0820(3) 0.0532(2) 0.0471(16) Uani 1 1 d . . . H93 H 0.5894 0.0641 0.0216 0.056 Uiso 1 1 calc R . . C94 C 0.6255(4) 0.1350(3) 0.0460(2) 0.0535(18) Uani 1 1 d . . . H94 H 0.6305 0.1533 0.0096 0.064 Uiso 1 1 calc R . . C95 C 0.6420(4) 0.1618(3) 0.0917(2) 0.0476(16) Uani 1 1 d . . . H95 H 0.6585 0.1988 0.0865 0.057 Uiso 1 1 calc R . . C96 C 0.6350(4) 0.1360(3) 0.1458(2) 0.0394(14) Uani 1 1 d . . . C97 C 0.5704(4) -0.0064(3) 0.1093(2) 0.0494(17) Uani 1 1 d . . . H97 H 0.5745 -0.0234 0.1490 0.059 Uiso 1 1 calc R . . C98 C 0.4802(4) 0.0011(4) 0.0901(3) 0.076(3) Uani 1 1 d . . . H98A H 0.4441 0.0281 0.1128 0.114 Uiso 1 1 calc R . . H98B H 0.4634 -0.0371 0.0941 0.114 Uiso 1 1 calc R . . H98C H 0.4750 0.0171 0.0510 0.114 Uiso 1 1 calc R . . C99 C 0.6252(5) -0.0500(3) 0.0750(3) 0.0586(19) Uani 1 1 d . . . H99A H 0.6175 -0.0363 0.0355 0.088 Uiso 1 1 calc R . . H99B H 0.6095 -0.0885 0.0819 0.088 Uiso 1 1 calc R . . H99C H 0.6838 -0.0535 0.0855 0.088 Uiso 1 1 calc R . . C100 C 0.6509(4) 0.1708(3) 0.1932(2) 0.0466(16) Uani 1 1 d . . . H100 H 0.6428 0.1474 0.2289 0.056 Uiso 1 1 calc R . . C101 C 0.7405(5) 0.1813(3) 0.1925(3) 0.068(2) Uani 1 1 d . . . H10A H 0.7797 0.1435 0.1955 0.101 Uiso 1 1 calc R . . H10B H 0.7491 0.2031 0.2239 0.101 Uiso 1 1 calc R . . H10C H 0.7499 0.2041 0.1576 0.101 Uiso 1 1 calc R . . C102 C 0.5885(5) 0.2298(3) 0.1912(3) 0.070(2) Uani 1 1 d . . . H10D H 0.5946 0.2533 0.1562 0.104 Uiso 1 1 calc R . . H10E H 0.5997 0.2511 0.2224 0.104 Uiso 1 1 calc R . . H10F H 0.5316 0.2226 0.1939 0.104 Uiso 1 1 calc R . . C103 C 0.3620(4) 0.1806(3) 0.2033(2) 0.0436(15) Uani 1 1 d . . . C104 C 0.3501(4) 0.2136(3) 0.1509(3) 0.0529(17) Uani 1 1 d . . . C105 C 0.2933(5) 0.2667(3) 0.1470(3) 0.067(2) Uani 1 1 d . . . H105 H 0.2856 0.2905 0.1126 0.081 Uiso 1 1 calc R . . C106 C 0.2476(5) 0.2855(3) 0.1931(3) 0.076(2) Uani 1 1 d . . . H106 H 0.2069 0.3209 0.1894 0.091 Uiso 1 1 calc R . . C107 C 0.2609(4) 0.2534(4) 0.2434(3) 0.070(2) Uani 1 1 d . . . H107 H 0.2301 0.2673 0.2746 0.084 Uiso 1 1 calc R . . C108 C 0.3189(4) 0.2004(3) 0.2502(3) 0.0518(17) Uani 1 1 d . . . C109 C 0.3955(5) 0.1912(3) 0.1004(3) 0.0610(19) Uani 1 1 d . . . H109 H 0.4482 0.1638 0.1137 0.073 Uiso 1 1 calc R . . C110 C 0.4200(6) 0.2393(4) 0.0607(3) 0.095(3) Uani 1 1 d . . . H11A H 0.3697 0.2674 0.0473 0.142 Uiso 1 1 calc R . . H11B H 0.4498 0.2220 0.0291 0.142 Uiso 1 1 calc R . . H11C H 0.4563 0.2597 0.0801 0.142 Uiso 1 1 calc R . . C111 C 0.3423(5) 0.1552(4) 0.0714(3) 0.089(3) Uani 1 1 d . . . H11D H 0.3299 0.1236 0.0979 0.133 Uiso 1 1 calc R . . H11E H 0.3731 0.1383 0.0400 0.133 Uiso 1 1 calc R . . H11F H 0.2900 0.1809 0.0580 0.133 Uiso 1 1 calc R . . C112 C 0.3316(4) 0.1666(3) 0.3078(3) 0.0511(16) Uani 1 1 d . . . H112 H 0.3732 0.1295 0.3045 0.061 Uiso 1 1 calc R . . C113 C 0.2497(5) 0.1500(4) 0.3308(3) 0.081(3) Uani 1 1 d . . . H11G H 0.2106 0.1856 0.3392 0.122 Uiso 1 1 calc R . . H11H H 0.2621 0.1232 0.3648 0.122 Uiso 1 1 calc R . . H11I H 0.2248 0.1307 0.3030 0.122 Uiso 1 1 calc R . . C114 C 0.3670(5) 0.2021(3) 0.3489(3) 0.064(2) Uani 1 1 d . . . H11J H 0.4207 0.2101 0.3354 0.096 Uiso 1 1 calc R . . H11K H 0.3751 0.1794 0.3854 0.096 Uiso 1 1 calc R . . H11L H 0.3279 0.2392 0.3521 0.096 Uiso 1 1 calc R . . C115 C 0.8442(3) 0.1500(2) 0.4093(2) 0.0352(13) Uani 1 1 d . . . H115 H 0.8592 0.1800 0.4286 0.042 Uiso 1 1 calc R . . C116 C 0.8300(4) 0.1005(2) 0.4366(2) 0.0352(13) Uani 1 1 d . . . H116 H 0.8350 0.0940 0.4759 0.042 Uiso 1 1 calc R . . C117 C 0.8207(4) 0.2159(2) 0.3252(2) 0.0344(13) Uani 1 1 d . . . C118 C 0.8763(4) 0.2336(2) 0.2854(2) 0.0359(13) Uani 1 1 d . . . C119 C 0.8615(4) 0.2922(3) 0.2633(2) 0.0439(15) Uani 1 1 d . . . H119 H 0.8986 0.3046 0.2364 0.053 Uiso 1 1 calc R . . C120 C 0.7946(5) 0.3325(3) 0.2796(3) 0.0588(19) Uani 1 1 d . . . H120 H 0.7870 0.3725 0.2653 0.071 Uiso 1 1 calc R . . C121 C 0.7390(5) 0.3143(3) 0.3165(3) 0.0579(18) Uani 1 1 d . . . H121 H 0.6917 0.3420 0.3264 0.070 Uiso 1 1 calc R . . C122 C 0.7496(4) 0.2563(2) 0.3400(2) 0.0434(15) Uani 1 1 d . . . C123 C 0.9525(4) 0.1913(3) 0.2679(3) 0.0472(15) Uani 1 1 d . . . H123 H 0.9393 0.1511 0.2720 0.057 Uiso 1 1 calc R . . C124 C 0.9769(6) 0.2043(4) 0.2071(3) 0.088(3) Uani 1 1 d U . . H12A H 0.9280 0.2076 0.1830 0.131 Uiso 1 1 calc R . . H12B H 1.0210 0.1723 0.1968 0.131 Uiso 1 1 calc R . . H12C H 0.9970 0.2413 0.2029 0.131 Uiso 1 1 calc R . . C125 C 1.0247(5) 0.1910(4) 0.3073(4) 0.090(3) Uani 1 1 d U . . H12D H 1.0404 0.2295 0.3032 0.134 Uiso 1 1 calc R . . H12E H 1.0725 0.1608 0.2984 0.134 Uiso 1 1 calc R . . H12F H 1.0076 0.1823 0.3456 0.134 Uiso 1 1 calc R . . C126 C 0.6839(4) 0.2391(3) 0.3791(3) 0.0550(18) Uani 1 1 d . . . H126 H 0.7033 0.1968 0.3929 0.066 Uiso 1 1 calc R . . C127 C 0.6736(6) 0.2747(4) 0.4300(3) 0.085(3) Uani 1 1 d . . . H12G H 0.7277 0.2704 0.4487 0.128 Uiso 1 1 calc R . . H12H H 0.6341 0.2602 0.4559 0.128 Uiso 1 1 calc R . . H12I H 0.6523 0.3163 0.4179 0.128 Uiso 1 1 calc R . . C128 C 0.5999(5) 0.2448(4) 0.3502(4) 0.087(3) Uani 1 1 d . . . H12J H 0.5819 0.2849 0.3327 0.131 Uiso 1 1 calc R . . H12K H 0.5585 0.2358 0.3775 0.131 Uiso 1 1 calc R . . H12L H 0.6052 0.2172 0.3216 0.131 Uiso 1 1 calc R . . C129 C 0.7683(4) 0.0147(2) 0.4341(2) 0.0339(13) Uani 1 1 d . . . C130 C 0.6905(4) 0.0314(3) 0.4599(2) 0.0380(14) Uani 1 1 d . . . C131 C 0.6576(4) -0.0117(3) 0.4907(2) 0.0462(15) Uani 1 1 d . . . H131 H 0.6061 -0.0010 0.5092 0.055 Uiso 1 1 calc R . . C132 C 0.6983(4) -0.0701(3) 0.4951(2) 0.0491(16) Uani 1 1 d . . . H132 H 0.6751 -0.0989 0.5170 0.059 Uiso 1 1 calc R . . C133 C 0.7715(4) -0.0861(3) 0.4680(2) 0.0468(16) Uani 1 1 d . . . H133 H 0.7980 -0.1264 0.4701 0.056 Uiso 1 1 calc R . . C134 C 0.8082(4) -0.0445(2) 0.4373(2) 0.0393(14) Uani 1 1 d . . . C135 C 0.6407(4) 0.0939(3) 0.4543(2) 0.0420(14) Uani 1 1 d . . . H135 H 0.6684 0.1170 0.4255 0.050 Uiso 1 1 calc R . . C136 C 0.5507(4) 0.0978(3) 0.4347(3) 0.068(2) Uani 1 1 d . . . H13A H 0.5511 0.0792 0.4001 0.102 Uiso 1 1 calc R . . H13B H 0.5228 0.1391 0.4282 0.102 Uiso 1 1 calc R . . H13C H 0.5207 0.0777 0.4632 0.102 Uiso 1 1 calc R . . C137 C 0.6407(4) 0.1228(3) 0.5086(3) 0.0568(18) Uani 1 1 d . . . H13D H 0.6158 0.1003 0.5381 0.085 Uiso 1 1 calc R . . H13E H 0.6081 0.1630 0.5033 0.085 Uiso 1 1 calc R . . H13F H 0.6982 0.1237 0.5190 0.085 Uiso 1 1 calc R . . C138 C 0.8917(4) -0.0633(2) 0.4094(2) 0.0444(15) Uani 1 1 d . . . H138 H 0.8973 -0.0316 0.3796 0.053 Uiso 1 1 calc R . . C139 C 0.9633(5) -0.0689(4) 0.4495(3) 0.075(2) Uani 1 1 d . . . H13G H 0.9626 -0.0308 0.4636 0.113 Uiso 1 1 calc R . . H13H H 1.0161 -0.0814 0.4305 0.113 Uiso 1 1 calc R . . H13I H 0.9579 -0.0980 0.4806 0.113 Uiso 1 1 calc R . . C140 C 0.8973(6) -0.1204(3) 0.3811(3) 0.076(2) Uani 1 1 d . . . H14A H 0.8910 -0.1524 0.4091 0.114 Uiso 1 1 calc R . . H14B H 0.9517 -0.1301 0.3633 0.114 Uiso 1 1 calc R . . H14C H 0.8529 -0.1149 0.3531 0.114 Uiso 1 1 calc R . . C141 C 0.9758(4) -0.0868(3) 0.1978(2) 0.0421(15) Uani 1 1 d . . . H14D H 0.9838 -0.1295 0.1946 0.051 Uiso 1 1 calc R . . H14E H 0.9991 -0.0686 0.1642 0.051 Uiso 1 1 calc R . . C142 C 1.0232(4) -0.0770(2) 0.2485(2) 0.0366(13) Uani 1 1 d . . . H14F H 1.0839 -0.0860 0.2413 0.044 Uiso 1 1 calc R . . H14G H 1.0116 -0.1038 0.2806 0.044 Uiso 1 1 calc R . . C143 C 0.8391(4) -0.0432(2) 0.1270(2) 0.0376(13) Uani 1 1 d . . . C144 C 0.8176(3) 0.0134(3) 0.1008(2) 0.0368(13) Uani 1 1 d . . . H144 H 0.8081 0.0461 0.1222 0.044 Uiso 1 1 calc R . . C145 C 0.8098(4) 0.0224(3) 0.0429(2) 0.0419(14) Uani 1 1 d . . . H145 H 0.7957 0.0611 0.0250 0.050 Uiso 1 1 calc R . . C146 C 0.8227(4) -0.0251(3) 0.0119(2) 0.0459(15) Uani 1 1 d . . . H146 H 0.8175 -0.0191 -0.0274 0.055 Uiso 1 1 calc R . . C147 C 0.8431(4) -0.0809(3) 0.0379(2) 0.0472(16) Uani 1 1 d . . . H147 H 0.8506 -0.1134 0.0163 0.057 Uiso 1 1 calc R . . C148 C 0.8529(4) -0.0908(3) 0.0945(2) 0.0412(14) Uani 1 1 d . . . H148 H 0.8690 -0.1298 0.1116 0.049 Uiso 1 1 calc R . . C149 C 0.8140(5) -0.1171(3) 0.2234(2) 0.0477(16) Uani 1 1 d . . . C150 C 0.7300(5) -0.1114(3) 0.2139(3) 0.0578(19) Uani 1 1 d . . . H150 H 0.7001 -0.0757 0.1955 0.069 Uiso 1 1 calc R . . C151 C 0.6871(6) -0.1559(4) 0.2301(3) 0.080(3) Uani 1 1 d . . . H151 H 0.6288 -0.1509 0.2236 0.096 Uiso 1 1 calc R . . C152 C 0.7316(7) -0.2072(5) 0.2558(4) 0.099(3) Uani 1 1 d U . . H152 H 0.7027 -0.2371 0.2692 0.119 Uiso 1 1 calc R . . C153 C 0.8170(7) -0.2170(4) 0.2629(4) 0.100(3) Uani 1 1 d U . . H153 H 0.8473 -0.2543 0.2776 0.120 Uiso 1 1 calc R . . C154 C 0.8583(6) -0.1703(3) 0.2478(3) 0.087(3) Uani 1 1 d . . . H154 H 0.9166 -0.1753 0.2543 0.104 Uiso 1 1 calc R . . C155 C 1.0527(3) 0.0007(2) 0.3272(2) 0.0322(12) Uani 1 1 d . . . C156 C 1.0331(4) 0.0478(3) 0.3589(2) 0.0395(14) Uani 1 1 d . . . H156 H 0.9848 0.0774 0.3501 0.047 Uiso 1 1 calc R . . C157 C 1.0842(4) 0.0519(3) 0.4035(2) 0.0490(16) Uani 1 1 d . . . H157 H 1.0698 0.0839 0.4256 0.059 Uiso 1 1 calc R . . C158 C 1.1553(4) 0.0100(3) 0.4161(2) 0.0501(17) Uani 1 1 d . . . H158 H 1.1908 0.0137 0.4459 0.060 Uiso 1 1 calc R . . C159 C 1.1744(4) -0.0367(3) 0.3854(2) 0.0502(16) Uani 1 1 d . . . H159 H 1.2227 -0.0661 0.3945 0.060 Uiso 1 1 calc R . . C160 C 1.1242(4) -0.0419(3) 0.3410(2) 0.0414(14) Uani 1 1 d . . . H160 H 1.1386 -0.0746 0.3198 0.050 Uiso 1 1 calc R . . C161 C 1.0455(3) 0.0399(2) 0.2116(2) 0.0307(12) Uani 1 1 d . . . C162 C 1.0059(4) 0.0591(2) 0.1605(2) 0.0397(14) Uani 1 1 d . . . H162 H 0.9508 0.0535 0.1547 0.048 Uiso 1 1 calc R . . C163 C 1.0461(4) 0.0862(3) 0.1181(2) 0.0454(15) Uani 1 1 d . . . H163 H 1.0189 0.0979 0.0831 0.054 Uiso 1 1 calc R . . C164 C 1.1251(4) 0.0963(3) 0.1260(2) 0.0464(15) Uani 1 1 d . . . H164 H 1.1522 0.1151 0.0967 0.056 Uiso 1 1 calc R . . C165 C 1.1650(4) 0.0788(2) 0.1774(2) 0.0431(14) Uani 1 1 d . . . H165 H 1.2191 0.0861 0.1836 0.052 Uiso 1 1 calc R . . C166 C 1.1248(4) 0.0504(2) 0.2197(2) 0.0380(13) Uani 1 1 d . . . H166 H 1.1521 0.0382 0.2545 0.046 Uiso 1 1 calc R . . C167 C 0.0974(11) 0.2560(6) 0.0940(7) 0.078(5) Uiso 0.50 1 d PD . . H16D H 0.1127 0.2502 0.1335 0.117 Uiso 0.50 1 calc PR . . H16E H 0.1423 0.2343 0.0726 0.117 Uiso 0.50 1 calc PR . . H16F H 0.0458 0.2417 0.0887 0.117 Uiso 0.50 1 calc PR . . C168 C 0.0846(8) 0.3171(5) 0.0752(5) 0.049(3) Uiso 0.50 1 d PD . . H16G H 0.0708 0.3223 0.0350 0.058 Uiso 0.50 1 calc PR . . H16H H 0.1374 0.3309 0.0799 0.058 Uiso 0.50 1 calc PR . . C169 C 0.0192(8) 0.3535(5) 0.1039(5) 0.058(4) Uiso 0.50 1 d PD . . H16I H -0.0343 0.3418 0.0962 0.070 Uiso 0.50 1 calc PR . . H16J H 0.0303 0.3450 0.1443 0.070 Uiso 0.50 1 calc PR . . C170 C 0.0092(11) 0.4157(6) 0.0899(7) 0.090(5) Uiso 0.50 1 d PD . . H17A H 0.0113 0.4220 0.0488 0.108 Uiso 0.50 1 calc PR . . H17B H 0.0594 0.4272 0.1042 0.108 Uiso 0.50 1 calc PR . . C171 C -0.0666(13) 0.4602(8) 0.1080(9) 0.118(7) Uiso 0.50 1 d PD . . H17C H -0.1188 0.4488 0.0968 0.141 Uiso 0.50 1 calc PR . . H17D H -0.0662 0.4601 0.1489 0.141 Uiso 0.50 1 calc PR . . C172 C -0.0635(12) 0.5200(7) 0.0816(8) 0.098(6) Uiso 0.50 1 d PD . . H17E H -0.0137 0.5322 0.0946 0.147 Uiso 0.50 1 calc PR . . H17F H -0.1134 0.5477 0.0916 0.147 Uiso 0.50 1 calc PR . . H17G H -0.0614 0.5195 0.0411 0.147 Uiso 0.50 1 calc PR . . C173 C -0.1684(9) 0.6027(6) 0.4469(5) 0.062(4) Uiso 0.50 1 d PD . . H17H H -0.2137 0.5849 0.4632 0.092 Uiso 0.50 1 calc PR . . H17I H -0.1192 0.5718 0.4423 0.092 Uiso 0.50 1 calc PR . . H17J H -0.1863 0.6236 0.4106 0.092 Uiso 0.50 1 calc PR . . C174 C -0.1465(9) 0.6455(6) 0.4851(6) 0.064(4) Uiso 0.50 1 d PD . . H17K H -0.1263 0.6239 0.5212 0.077 Uiso 0.50 1 calc PR . . H17L H -0.1006 0.6633 0.4685 0.077 Uiso 0.50 1 calc PR . . C175 C -0.2184(8) 0.6926(5) 0.4946(5) 0.057(3) Uiso 0.50 1 d PD . . H17M H -0.2007 0.7153 0.5232 0.069 Uiso 0.50 1 calc PR . . H17N H -0.2623 0.6731 0.5116 0.069 Uiso 0.50 1 calc PR . . C176 C -0.2595(8) 0.7360(5) 0.4495(5) 0.050(3) Uiso 0.50 1 d PD . . H17O H -0.2173 0.7580 0.4337 0.060 Uiso 0.50 1 calc PR . . H17P H -0.2757 0.7141 0.4198 0.060 Uiso 0.50 1 calc PR . . C177 C -0.3334(8) 0.7792(6) 0.4633(5) 0.061(4) Uiso 0.50 1 d PD . . H17Q H -0.3194 0.8015 0.4935 0.073 Uiso 0.50 1 calc PR . . H17R H -0.3784 0.7586 0.4765 0.073 Uiso 0.50 1 calc PR . . C178 C -0.3636(9) 0.8214(6) 0.4121(5) 0.064(4) Uiso 0.50 1 d PD . . H17S H -0.3199 0.8430 0.4001 0.096 Uiso 0.50 1 calc PR . . H17T H -0.4140 0.8492 0.4213 0.096 Uiso 0.50 1 calc PR . . H17U H -0.3763 0.7991 0.3821 0.096 Uiso 0.50 1 calc PR . . C179 C 0.7980(10) -0.2452(7) 0.0652(6) 0.073(4) Uiso 0.50 1 d PD . . H17V H 0.7862 -0.2704 0.0374 0.109 Uiso 0.50 1 calc PR . . H17W H 0.8318 -0.2180 0.0486 0.109 Uiso 0.50 1 calc PR . . H17$ H 0.7454 -0.2229 0.0784 0.109 Uiso 0.50 1 calc PR . . C180 C 0.8421(12) -0.2805(8) 0.1106(7) 0.107(6) Uiso 0.50 1 d PD . . H18D H 0.8544 -0.2534 0.1370 0.128 Uiso 0.50 1 calc PR . . H18E H 0.8964 -0.2998 0.0961 0.128 Uiso 0.50 1 calc PR . . C181 C 0.8089(10) -0.3252(7) 0.1426(6) 0.078(5) Uiso 0.50 1 d PD . . H18F H 0.7537 -0.3057 0.1555 0.093 Uiso 0.50 1 calc PR . . H18G H 0.7978 -0.3524 0.1159 0.093 Uiso 0.50 1 calc PR . . C182 C 0.8481(12) -0.3611(8) 0.1890(7) 0.105(6) Uiso 0.50 1 d PD . . H18H H 0.8764 -0.3334 0.2062 0.125 Uiso 0.50 1 calc PR . . H18I H 0.8935 -0.3873 0.1711 0.125 Uiso 0.50 1 calc PR . . C183 C 0.8317(17) -0.3992(11) 0.2376(10) 0.164(10) Uiso 0.50 1 d PD . . H18J H 0.8831 -0.4264 0.2521 0.197 Uiso 0.50 1 calc PR . . H18K H 0.8047 -0.3766 0.2677 0.197 Uiso 0.50 1 calc PR . . C184 C 0.7777(14) -0.4282(10) 0.2130(9) 0.121(7) Uiso 0.50 1 d PD . . H18L H 0.7200 -0.4099 0.2208 0.181 Uiso 0.50 1 calc PR . . H18M H 0.7885 -0.4695 0.2280 0.181 Uiso 0.50 1 calc PR . . H18N H 0.7863 -0.4256 0.1727 0.181 Uiso 0.50 1 calc PR . . C185 C 1.0168(10) 0.2337(7) 0.4772(7) 0.080(5) Uiso 0.50 1 d PD . . H18O H 1.0408 0.2442 0.5108 0.120 Uiso 0.50 1 calc PR . . H18P H 1.0616 0.2134 0.4547 0.120 Uiso 0.50 1 calc PR . . H18Q H 0.9777 0.2078 0.4875 0.120 Uiso 0.50 1 calc PR . . C186 C 0.9738(11) 0.2856(7) 0.4459(7) 0.089(5) Uiso 0.50 1 d PD . . H18R H 1.0164 0.3091 0.4346 0.107 Uiso 0.50 1 calc PR . . H18S H 0.9541 0.2729 0.4113 0.107 Uiso 0.50 1 calc PR . . C187 C 0.9089(12) 0.3231(8) 0.4649(8) 0.116(7) Uiso 0.50 1 d PD . . H18T H 0.9322 0.3415 0.4947 0.139 Uiso 0.50 1 calc PR . . H18U H 0.8725 0.2981 0.4836 0.139 Uiso 0.50 1 calc PR . . C188 C 0.8512(9) 0.3720(6) 0.4322(6) 0.067(4) Uiso 0.50 1 d PD . . H18V H 0.8182 0.3550 0.4064 0.081 Uiso 0.50 1 calc PR . . H18W H 0.8117 0.3932 0.4581 0.081 Uiso 0.50 1 calc PR . . C189 C 0.8907(10) 0.4125(7) 0.4015(7) 0.086(5) Uiso 0.50 1 d PD . . H18$ H 0.9295 0.3915 0.3751 0.104 Uiso 0.50 1 calc PR . . H18 H 0.9242 0.4294 0.4271 0.104 Uiso 0.50 1 calc PR . . C190 C 0.8328(12) 0.4604(8) 0.3704(8) 0.103(6) Uiso 0.50 1 d PD . . H19D H 0.7912 0.4443 0.3512 0.154 Uiso 0.50 1 calc PR . . H19E H 0.8638 0.4813 0.3430 0.154 Uiso 0.50 1 calc PR . . H19F H 0.8046 0.4877 0.3961 0.154 Uiso 0.50 1 calc PR . . 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 0.06003(18) 0.03425(13) 0.02772(12) -0.00100(9) 0.00613(11) 0.00944(11) Pt2 0.02808(12) 0.03171(12) 0.02228(10) -0.00450(8) -0.00359(8) -0.00440(9) Ga1 0.0535(4) 0.0381(4) 0.0253(3) -0.0015(3) -0.0004(3) 0.0049(3) Ga2 0.0774(6) 0.0372(4) 0.0299(3) -0.0025(3) 0.0069(3) 0.0174(4) Ga3 0.0301(3) 0.0362(3) 0.0233(3) -0.0019(2) -0.0039(2) -0.0082(3) Ga4 0.0290(3) 0.0316(3) 0.0267(3) -0.0063(2) -0.0020(2) -0.0028(3) P1 0.0548(11) 0.0591(11) 0.0329(8) -0.0028(7) -0.0121(8) -0.0010(9) P2 0.0634(12) 0.0369(8) 0.0291(8) -0.0043(6) 0.0081(7) 0.0051(8) P3 0.0686(13) 0.0377(9) 0.0334(8) 0.0016(7) 0.0126(8) 0.0083(8) P4 0.0416(10) 0.0561(10) 0.0262(7) 0.0045(7) -0.0049(6) -0.0182(8) P5 0.0403(9) 0.0336(8) 0.0284(7) -0.0081(6) -0.0060(6) -0.0097(7) P6 0.0294(8) 0.0331(7) 0.0250(7) -0.0051(6) -0.0046(6) -0.0024(6) N1 0.044(3) 0.036(3) 0.028(2) -0.0019(19) -0.003(2) -0.003(2) N2 0.036(3) 0.037(3) 0.031(2) -0.006(2) -0.001(2) -0.006(2) N3 0.079(4) 0.045(3) 0.037(3) -0.006(2) 0.009(3) 0.024(3) N4 0.089(5) 0.036(3) 0.026(3) -0.003(2) 0.004(3) 0.015(3) N5 0.026(3) 0.042(3) 0.025(2) 0.0026(19) -0.0014(18) -0.011(2) N6 0.029(3) 0.060(3) 0.037(3) -0.005(2) -0.002(2) -0.008(2) N7 0.034(3) 0.029(2) 0.029(2) -0.0075(18) -0.0051(19) -0.001(2) N8 0.040(3) 0.034(2) 0.028(2) -0.0093(19) -0.005(2) -0.004(2) C1 0.043(4) 0.048(4) 0.036(3) -0.014(3) 0.000(3) -0.002(3) C2 0.042(4) 0.060(4) 0.035(3) -0.004(3) -0.006(3) -0.011(3) C3 0.064(5) 0.074(5) 0.078(5) -0.015(4) 0.030(4) -0.007(4) C4 0.051(5) 0.067(5) 0.092(6) 0.020(4) 0.015(4) -0.010(4) C5 0.109(8) 0.150(9) 0.063(5) -0.019(5) -0.011(5) -0.084(7) C6 0.037(3) 0.039(3) 0.029(3) -0.007(2) -0.003(2) -0.002(3) C7 0.037(3) 0.040(3) 0.028(3) -0.010(2) 0.001(2) -0.009(3) C8 0.048(4) 0.037(3) 0.034(3) 0.000(2) -0.005(3) -0.007(3) C9 0.050(4) 0.032(3) 0.052(4) 0.001(3) 0.001(3) -0.006(3) C10 0.047(4) 0.046(4) 0.073(5) -0.006(3) -0.002(4) -0.015(3) C11 0.055(5) 0.048(4) 0.065(5) -0.008(3) -0.019(4) -0.015(3) C12 0.065(5) 0.038(3) 0.042(3) -0.005(3) -0.007(3) -0.005(3) C13 0.047(4) 0.035(3) 0.032(3) -0.002(2) -0.007(3) -0.002(3) C14 0.049(4) 0.059(4) 0.047(4) -0.001(3) 0.006(3) -0.007(3) C15 0.072(6) 0.081(5) 0.052(4) 0.011(4) 0.016(4) -0.014(4) C16 0.059(5) 0.068(5) 0.071(5) -0.006(4) 0.013(4) 0.003(4) C17 0.050(4) 0.045(3) 0.030(3) -0.003(3) -0.001(3) -0.005(3) C18 0.077(5) 0.049(4) 0.042(4) -0.010(3) 0.005(3) 0.000(4) C19 0.063(5) 0.052(4) 0.033(3) -0.004(3) 0.005(3) -0.006(3) C20 0.034(3) 0.036(3) 0.031(3) 0.003(2) 0.002(2) -0.003(3) C21 0.039(4) 0.038(3) 0.031(3) 0.000(2) 0.004(2) -0.008(3) C22 0.039(4) 0.049(4) 0.034(3) 0.001(3) -0.002(3) 0.001(3) C23 0.058(4) 0.039(3) 0.035(3) -0.001(3) 0.010(3) 0.010(3) C24 0.056(4) 0.037(3) 0.040(3) -0.007(3) 0.008(3) -0.002(3) C25 0.044(4) 0.036(3) 0.033(3) -0.005(2) 0.006(3) -0.012(3) C26 0.042(4) 0.039(3) 0.045(3) -0.001(3) -0.012(3) -0.005(3) C27 0.051(5) 0.056(4) 0.082(5) -0.004(4) -0.018(4) -0.012(4) C28 0.074(5) 0.059(4) 0.042(4) -0.016(3) -0.002(3) -0.005(4) C29 0.045(4) 0.046(4) 0.044(3) -0.011(3) 0.009(3) -0.017(3) C30 0.054(4) 0.055(4) 0.043(4) -0.004(3) 0.003(3) -0.009(3) C31 0.078(6) 0.093(6) 0.054(4) -0.017(4) 0.005(4) -0.046(5) C32 0.094(6) 0.040(4) 0.035(4) -0.004(3) 0.003(4) 0.024(4) C33 0.095(6) 0.042(4) 0.029(3) -0.005(3) 0.002(4) 0.012(4) C34 0.071(6) 0.069(5) 0.046(4) -0.007(4) 0.006(4) 0.025(4) C35 0.101(7) 0.071(6) 0.055(5) 0.003(4) 0.011(5) 0.050(5) C36 0.117(9) 0.077(7) 0.095(7) 0.009(5) 0.007(7) 0.052(6) C37 0.089(6) 0.096(6) 0.084(5) -0.001(4) 0.002(5) 0.024(5) C38 0.087(7) 0.106(7) 0.069(5) -0.016(5) 0.005(5) 0.033(6) C39 0.086(7) 0.081(6) 0.045(4) -0.016(4) -0.001(4) 0.037(5) C40 0.112(8) 0.055(5) 0.093(7) 0.009(5) 0.012(6) 0.029(5) C41 0.188(14) 0.146(11) 0.144(11) 0.086(9) -0.035(10) -0.042(10) C42 0.163(13) 0.127(10) 0.229(16) -0.103(11) -0.012(11) 0.048(9) C43 0.073(6) 0.082(6) 0.078(6) -0.025(5) 0.004(5) 0.014(5) C44 0.101(6) 0.109(6) 0.130(6) -0.039(5) 0.002(5) -0.007(5) C45 0.105(8) 0.058(5) 0.102(7) -0.003(5) 0.022(6) 0.009(5) C46 0.081(6) 0.042(4) 0.026(3) -0.004(3) 0.006(3) 0.004(4) C47 0.095(6) 0.040(4) 0.025(3) -0.004(3) 0.005(3) 0.008(4) C48 0.102(7) 0.051(4) 0.040(4) -0.007(3) 0.012(4) -0.005(5) C49 0.106(7) 0.063(5) 0.052(4) -0.010(4) 0.023(4) -0.025(5) C50 0.084(6) 0.056(5) 0.058(4) -0.013(4) 0.016(4) -0.001(4) C51 0.081(6) 0.042(4) 0.046(4) -0.010(3) 0.012(4) 0.003(4) C52 0.120(7) 0.037(4) 0.034(3) -0.003(3) 0.003(4) 0.001(4) C53 0.159(9) 0.045(4) 0.049(4) 0.001(3) 0.005(5) 0.011(5) C54 0.132(8) 0.057(5) 0.047(4) -0.015(4) 0.008(5) 0.019(5) C55 0.072(5) 0.037(4) 0.062(4) -0.011(3) 0.010(4) 0.010(3) C56 0.147(9) 0.063(5) 0.060(5) -0.004(4) 0.012(5) -0.035(6) C57 0.100(7) 0.049(4) 0.059(4) -0.019(3) 0.000(4) 0.009(4) C58 0.083(5) 0.036(3) 0.044(4) -0.008(3) 0.016(3) 0.003(3) C59 0.076(5) 0.035(3) 0.043(4) 0.000(3) 0.016(3) 0.008(3) C60 0.068(5) 0.048(4) 0.024(3) -0.014(3) 0.005(3) 0.008(3) C61 0.056(5) 0.052(4) 0.040(3) -0.015(3) 0.007(3) 0.003(3) C62 0.074(6) 0.077(5) 0.062(5) -0.033(4) 0.015(4) -0.015(5) C63 0.061(6) 0.107(7) 0.063(5) -0.043(5) 0.002(4) -0.004(5) C64 0.073(6) 0.089(6) 0.047(4) -0.015(4) -0.014(4) 0.025(5) C65 0.076(6) 0.069(5) 0.036(4) -0.013(3) 0.003(4) 0.013(4) C66 0.066(5) 0.040(3) 0.032(3) -0.002(3) 0.008(3) -0.003(3) C67 0.066(5) 0.043(4) 0.046(4) -0.010(3) 0.010(3) -0.009(3) C68 0.065(5) 0.051(4) 0.070(5) 0.000(4) -0.009(4) -0.011(4) C69 0.090(6) 0.055(4) 0.053(4) -0.011(3) -0.009(4) -0.014(4) C70 0.097(7) 0.050(4) 0.048(4) -0.014(3) 0.002(4) -0.006(4) C71 0.072(5) 0.041(4) 0.039(3) -0.004(3) 0.008(3) 0.004(3) C72 0.069(5) 0.040(4) 0.035(3) 0.004(3) 0.012(3) 0.008(3) C73 0.079(5) 0.049(4) 0.039(4) 0.009(3) 0.018(3) 0.009(4) C74 0.074(6) 0.068(5) 0.050(4) 0.013(4) 0.005(4) 0.022(4) C75 0.076(6) 0.086(6) 0.040(4) 0.011(4) 0.011(4) 0.007(5) C76 0.084(6) 0.070(5) 0.034(4) -0.005(3) 0.012(4) 0.009(4) C77 0.074(5) 0.049(4) 0.036(3) 0.005(3) 0.016(3) 0.013(4) C78 0.068(5) 0.044(4) 0.043(4) -0.007(3) 0.020(3) -0.002(3) C79 0.077(6) 0.059(5) 0.055(4) -0.010(3) 0.015(4) -0.012(4) C80 0.072(6) 0.088(6) 0.080(6) -0.021(5) 0.006(5) -0.017(5) C81 0.077(7) 0.081(6) 0.103(7) -0.031(5) 0.036(6) -0.025(5) C82 0.085(7) 0.064(5) 0.081(6) -0.005(4) 0.027(5) 0.000(5) C83 0.072(6) 0.063(5) 0.064(5) -0.004(4) 0.022(4) -0.003(4) C84 0.040(4) 0.054(4) 0.024(3) -0.006(2) -0.004(2) -0.017(3) C85 0.044(4) 0.078(5) 0.043(4) 0.016(3) -0.012(3) -0.028(4) C86 0.083(5) 0.083(5) 0.158(6) 0.022(5) -0.025(5) -0.036(4) C87 0.078(5) 0.146(6) 0.071(4) 0.002(4) -0.002(4) -0.042(5) C88 0.043(4) 0.057(4) 0.054(4) -0.010(3) 0.004(3) -0.021(3) C89 0.036(3) 0.049(3) 0.021(3) 0.001(2) -0.003(2) -0.014(3) C90 0.040(4) 0.049(4) 0.031(3) -0.008(3) 0.005(3) -0.019(3) C91 0.030(3) 0.045(3) 0.023(3) 0.001(2) -0.002(2) -0.006(3) C92 0.030(3) 0.064(4) 0.025(3) -0.001(3) -0.001(2) -0.013(3) C93 0.040(4) 0.073(5) 0.026(3) -0.003(3) -0.002(3) -0.007(3) C94 0.046(4) 0.078(5) 0.028(3) 0.015(3) 0.001(3) -0.003(4) C95 0.039(4) 0.058(4) 0.041(4) 0.014(3) -0.002(3) -0.008(3) C96 0.031(3) 0.051(4) 0.033(3) 0.006(3) -0.003(2) -0.005(3) C97 0.051(4) 0.076(5) 0.030(3) -0.008(3) 0.000(3) -0.032(4) C98 0.056(5) 0.142(8) 0.048(4) -0.023(4) 0.007(4) -0.055(5) C99 0.071(5) 0.073(5) 0.043(4) -0.026(3) 0.008(3) -0.031(4) C100 0.062(4) 0.042(4) 0.037(3) 0.008(3) -0.010(3) -0.018(3) C101 0.076(6) 0.077(5) 0.059(4) 0.017(4) -0.018(4) -0.049(5) C102 0.104(7) 0.043(4) 0.059(4) -0.002(3) -0.011(4) -0.009(4) C103 0.028(3) 0.053(4) 0.050(4) -0.013(3) -0.006(3) -0.006(3) C104 0.042(4) 0.058(4) 0.054(4) -0.002(3) -0.015(3) -0.001(3) C105 0.053(5) 0.077(5) 0.066(5) -0.012(4) -0.025(4) 0.005(4) C106 0.065(5) 0.072(5) 0.081(6) -0.026(4) -0.037(4) 0.020(4) C107 0.042(4) 0.090(6) 0.075(5) -0.042(5) -0.010(4) 0.011(4) C108 0.034(4) 0.066(4) 0.057(4) -0.021(3) -0.006(3) -0.007(3) C109 0.050(5) 0.073(5) 0.053(4) 0.003(4) -0.007(3) 0.001(4) C110 0.084(7) 0.101(7) 0.076(6) 0.038(5) 0.008(5) 0.017(5) C111 0.084(7) 0.117(7) 0.059(5) -0.031(5) -0.006(4) 0.006(6) C112 0.030(4) 0.075(5) 0.050(4) -0.018(3) 0.003(3) -0.009(3) C113 0.053(5) 0.135(8) 0.066(5) -0.025(5) 0.010(4) -0.037(5) C114 0.057(5) 0.080(5) 0.055(4) -0.019(4) -0.020(3) -0.007(4) C115 0.034(3) 0.037(3) 0.034(3) -0.013(2) -0.005(2) -0.001(3) C116 0.041(4) 0.039(3) 0.026(3) -0.009(2) -0.005(2) -0.006(3) C117 0.040(4) 0.031(3) 0.031(3) -0.005(2) -0.005(2) -0.004(3) C118 0.037(3) 0.032(3) 0.040(3) -0.006(2) -0.005(3) -0.007(3) C119 0.052(4) 0.040(3) 0.041(3) -0.003(3) -0.001(3) -0.013(3) C120 0.075(5) 0.037(4) 0.056(4) 0.002(3) -0.004(4) 0.007(4) C121 0.060(5) 0.048(4) 0.056(4) -0.001(3) 0.007(4) 0.012(3) C122 0.043(4) 0.036(3) 0.045(3) -0.004(3) 0.002(3) 0.009(3) C123 0.044(4) 0.038(3) 0.061(4) -0.004(3) 0.008(3) -0.010(3) C124 0.099(5) 0.067(4) 0.092(5) -0.006(4) 0.047(4) -0.007(4) C125 0.073(5) 0.067(4) 0.131(6) -0.017(4) -0.018(4) -0.015(4) C126 0.048(4) 0.049(4) 0.057(4) -0.001(3) 0.010(3) 0.014(3) C127 0.097(7) 0.077(6) 0.074(5) -0.013(4) 0.032(5) 0.006(5) C128 0.047(5) 0.111(7) 0.094(6) 0.009(5) 0.005(4) 0.000(5) C129 0.040(4) 0.042(3) 0.022(3) -0.002(2) -0.005(2) -0.013(3) C130 0.034(3) 0.056(4) 0.025(3) -0.005(3) -0.005(2) -0.009(3) C131 0.040(4) 0.067(4) 0.034(3) -0.010(3) -0.001(3) -0.013(3) C132 0.053(4) 0.056(4) 0.041(3) -0.001(3) 0.005(3) -0.020(3) C133 0.061(5) 0.043(4) 0.039(3) -0.003(3) 0.006(3) -0.017(3) C134 0.044(4) 0.040(3) 0.034(3) -0.007(3) -0.002(3) -0.008(3) C135 0.033(3) 0.052(4) 0.039(3) -0.004(3) -0.003(3) -0.001(3) C136 0.048(5) 0.088(6) 0.065(5) -0.023(4) -0.014(4) 0.004(4) C137 0.062(5) 0.061(4) 0.045(4) -0.021(3) 0.004(3) 0.002(4) C138 0.056(4) 0.033(3) 0.039(3) 0.004(3) 0.008(3) 0.000(3) C139 0.049(5) 0.119(7) 0.055(4) -0.001(4) 0.007(4) -0.012(5) C140 0.099(7) 0.054(5) 0.073(5) -0.014(4) 0.033(5) -0.008(4) C141 0.046(4) 0.037(3) 0.041(3) -0.015(3) -0.013(3) 0.004(3) C142 0.039(4) 0.036(3) 0.034(3) -0.007(2) -0.004(2) -0.003(3) C143 0.042(4) 0.042(3) 0.030(3) -0.005(2) -0.004(3) -0.009(3) C144 0.032(3) 0.044(3) 0.036(3) -0.012(3) 0.003(2) -0.008(3) C145 0.034(4) 0.051(4) 0.038(3) 0.005(3) 0.001(3) -0.008(3) C146 0.046(4) 0.063(4) 0.026(3) -0.005(3) 0.000(3) -0.006(3) C147 0.047(4) 0.061(4) 0.033(3) -0.017(3) -0.001(3) -0.005(3) C148 0.046(4) 0.042(3) 0.036(3) -0.009(3) -0.003(3) -0.008(3) C149 0.074(5) 0.047(4) 0.029(3) -0.003(3) -0.004(3) -0.027(4) C150 0.082(6) 0.055(4) 0.049(4) -0.020(3) 0.016(4) -0.037(4) C151 0.100(7) 0.087(6) 0.072(5) -0.027(5) 0.012(5) -0.057(6) C152 0.118(6) 0.095(5) 0.096(5) 0.012(4) -0.002(5) -0.059(5) C153 0.123(6) 0.082(5) 0.094(5) 0.019(4) -0.036(5) -0.031(5) C154 0.134(8) 0.062(5) 0.072(5) 0.018(4) -0.054(5) -0.048(5) C155 0.030(3) 0.044(3) 0.023(3) -0.004(2) -0.001(2) -0.008(3) C156 0.040(4) 0.044(3) 0.035(3) -0.009(3) -0.008(3) -0.005(3) C157 0.052(4) 0.059(4) 0.039(3) -0.017(3) -0.014(3) -0.011(3) C158 0.047(4) 0.071(5) 0.032(3) 0.000(3) -0.017(3) -0.014(4) C159 0.042(4) 0.068(4) 0.035(3) 0.000(3) -0.009(3) 0.000(3) C160 0.035(4) 0.058(4) 0.029(3) -0.005(3) -0.007(3) -0.005(3) C161 0.027(3) 0.032(3) 0.030(3) -0.008(2) 0.001(2) 0.002(2) C162 0.039(4) 0.044(3) 0.034(3) -0.001(3) -0.010(3) -0.003(3) C163 0.050(4) 0.048(4) 0.034(3) 0.005(3) -0.006(3) -0.003(3) C164 0.059(5) 0.042(4) 0.036(3) -0.002(3) 0.009(3) -0.008(3) C165 0.045(4) 0.040(3) 0.046(4) -0.009(3) 0.003(3) -0.010(3) C166 0.040(4) 0.044(3) 0.030(3) -0.004(2) -0.004(3) -0.006(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 2.2806(17) . ? Pt1 P3 2.3169(17) . ? Pt1 Ga1 2.4064(10) . ? Pt1 Ga2 2.4258(10) . ? Pt2 P5 2.2795(15) . ? Pt2 P6 2.3206(15) . ? Pt2 Ga3 2.4114(8) . ? Pt2 Ga4 2.4217(9) . ? Ga1 N1 1.873(4) . ? Ga1 P1 2.319(2) . ? Ga2 N3 1.898(5) . ? Ga2 N4 1.902(6) . ? Ga3 N5 1.868(4) . ? Ga3 P4 2.3207(17) . ? Ga4 N8 1.906(4) . ? Ga4 N7 1.907(4) . ? P1 C1 1.701(6) . ? P2 C66 1.829(6) . ? P2 C60 1.830(7) . ? P2 C58 1.838(6) . ? P3 C78 1.817(8) . ? P3 C72 1.829(6) . ? P3 C59 1.858(6) . ? P4 C84 1.698(6) . ? P5 C149 1.816(6) . ? P5 C143 1.819(5) . ? P5 C141 1.838(6) . ? P6 C155 1.822(5) . ? P6 C161 1.839(5) . ? P6 C142 1.841(5) . ? N1 C8 1.426(7) . ? N1 C6 1.481(7) . ? N2 C7 1.261(6) . ? N2 C20 1.428(7) . ? N3 C32 1.398(9) . ? N3 C34 1.435(9) . ? N4 C33 1.414(8) . ? N4 C46 1.423(9) . ? N5 C91 1.448(6) . ? N5 C89 1.473(7) . ? N6 C90 1.267(7) . ? N6 C103 1.424(7) . ? N7 C115 1.414(6) . ? N7 C117 1.437(6) . ? N8 C116 1.390(6) . ? N8 C129 1.437(7) . ? C1 C6 1.525(8) . ? C1 C2 1.544(8) . ? C2 C4 1.517(9) . ? C2 C5 1.524(9) . ? C2 C3 1.556(9) . ? C6 C7 1.516(7) . ? C8 C9 1.404(8) . ? C8 C13 1.425(8) . ? C9 C10 1.399(9) . ? C9 C14 1.524(9) . ? C10 C11 1.377(9) . ? C11 C12 1.369(9) . ? C12 C13 1.403(8) . ? C13 C17 1.523(8) . ? C14 C15 1.515(9) . ? C14 C16 1.539(9) . ? C17 C18 1.525(8) . ? C17 C19 1.547(8) . ? C20 C25 1.408(7) . ? C20 C21 1.411(8) . ? C21 C22 1.379(8) . ? C21 C26 1.525(8) . ? C22 C23 1.387(8) . ? C23 C24 1.380(9) . ? C24 C25 1.393(8) . ? C25 C29 1.515(8) . ? C26 C27 1.520(8) . ? C26 C28 1.531(8) . ? C29 C31 1.517(8) . ? C29 C30 1.531(8) . ? C32 C33 1.322(10) . ? C34 C39 1.389(12) . ? C34 C35 1.408(11) . ? C35 C36 1.400(13) . ? C35 C40 1.503(13) . ? C36 C37 1.322(14) . ? C37 C38 1.397(13) . ? C38 C39 1.408(11) . ? C39 C43 1.534(11) . ? C40 C42 1.530(13) . ? C40 C41 1.534(12) . ? C43 C44 1.521(12) . ? C43 C45 1.536(11) . ? C46 C51 1.401(9) . ? C46 C47 1.405(9) . ? C47 C48 1.386(10) . ? C47 C52 1.517(9) . ? C48 C49 1.370(10) . ? C49 C50 1.398(10) . ? C50 C51 1.377(10) . ? C51 C55 1.530(9) . ? C52 C54 1.543(9) . ? C52 C53 1.547(9) . ? C55 C57 1.520(9) . ? C55 C56 1.535(10) . ? C58 C59 1.521(8) . ? C60 C61 1.383(9) . ? C60 C65 1.397(9) . ? C61 C62 1.383(10) . ? C62 C63 1.413(11) . ? C63 C64 1.360(11) . ? C64 C65 1.372(11) . ? C66 C67 1.380(9) . ? C66 C71 1.396(8) . ? C67 C68 1.401(9) . ? C68 C69 1.365(10) . ? C69 C70 1.380(10) . ? C70 C71 1.375(9) . ? C72 C77 1.387(8) . ? C72 C73 1.398(8) . ? C73 C74 1.382(9) . ? C74 C75 1.394(10) . ? C75 C76 1.378(10) . ? C76 C77 1.393(9) . ? C78 C83 1.387(9) . ? C78 C79 1.400(10) . ? C79 C80 1.374(10) . ? C80 C81 1.389(11) . ? C81 C82 1.359(12) . ? C82 C83 1.370(11) . ? C84 C89 1.525(7) . ? C84 C85 1.551(8) . ? C85 C86 1.483(11) . ? C85 C88 1.521(8) . ? C85 C87 1.570(10) . ? C89 C90 1.523(8) . ? C91 C96 1.405(8) . ? C91 C92 1.411(7) . ? C92 C93 1.395(8) . ? C92 C97 1.530(8) . ? C93 C94 1.362(9) . ? C94 C95 1.379(9) . ? C95 C96 1.398(8) . ? C96 C100 1.521(8) . ? C97 C99 1.521(9) . ? C97 C98 1.523(9) . ? C100 C101 1.533(9) . ? C100 C102 1.538(9) . ? C103 C108 1.398(8) . ? C103 C104 1.411(8) . ? C104 C105 1.390(9) . ? C104 C109 1.507(9) . ? C105 C106 1.392(10) . ? C106 C107 1.361(10) . ? C107 C108 1.399(9) . ? C108 C112 1.526(9) . ? C109 C110 1.520(10) . ? C109 C111 1.540(10) . ? C112 C114 1.540(8) . ? C112 C113 1.550(9) . ? C115 C116 1.336(7) . ? C117 C118 1.405(8) . ? C117 C122 1.412(8) . ? C118 C119 1.396(8) . ? C118 C123 1.514(8) . ? C119 C120 1.375(9) . ? C120 C121 1.366(9) . ? C121 C122 1.395(8) . ? C122 C126 1.512(9) . ? C123 C125 1.523(10) . ? C123 C124 1.536(9) . ? C126 C128 1.524(10) . ? C126 C127 1.543(10) . ? C129 C134 1.402(8) . ? C129 C130 1.413(8) . ? C130 C131 1.386(8) . ? C130 C135 1.517(8) . ? C131 C132 1.389(9) . ? C132 C133 1.363(9) . ? C133 C134 1.394(8) . ? C134 C138 1.520(8) . ? C135 C136 1.533(8) . ? C135 C137 1.534(8) . ? C138 C139 1.507(9) . ? C138 C140 1.542(9) . ? C141 C142 1.515(7) . ? C143 C144 1.389(8) . ? C143 C148 1.405(8) . ? C144 C145 1.399(7) . ? C145 C146 1.379(8) . ? C146 C147 1.371(8) . ? C147 C148 1.371(8) . ? C149 C150 1.373(9) . ? C149 C154 1.385(10) . ? C150 C151 1.392(9) . ? C151 C152 1.365(12) . ? C152 C153 1.379(13) . ? C153 C154 1.411(11) . ? C155 C156 1.386(7) . ? C155 C160 1.395(8) . ? C156 C157 1.394(7) . ? C157 C158 1.379(9) . ? C158 C159 1.363(9) . ? C159 C160 1.388(8) . ? C161 C166 1.386(7) . ? C161 C162 1.392(7) . ? C162 C163 1.382(8) . ? C163 C164 1.378(8) . ? C164 C165 1.397(8) . ? C165 C166 1.394(8) . ? C167 C168 1.430(14) . ? C168 C169 1.444(13) . ? C169 C170 1.437(14) . ? C170 C171 1.541(16) . ? C171 C172 1.489(16) . ? C173 C174 1.521(14) . ? C174 C175 1.475(14) . ? C175 C176 1.482(13) . ? C176 C177 1.470(13) . ? C177 C178 1.526(14) . ? C179 C180 1.416(15) . ? C180 C181 1.430(15) . ? C181 C182 1.411(15) . ? C182 C183 1.460(17) . ? C183 C184 1.386(17) . ? C185 C186 1.425(15) . ? C186 C187 1.343(15) . ? C187 C188 1.493(15) . ? C188 C189 1.400(14) . ? C189 C190 1.464(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pt1 P3 86.76(6) . . ? P2 Pt1 Ga1 96.19(5) . . ? P3 Pt1 Ga1 171.30(5) . . ? P2 Pt1 Ga2 167.83(5) . . ? P3 Pt1 Ga2 97.58(5) . . ? Ga1 Pt1 Ga2 77.95(3) . . ? P5 Pt2 P6 86.87(6) . . ? P5 Pt2 Ga3 92.74(5) . . ? P6 Pt2 Ga3 171.08(4) . . ? P5 Pt2 Ga4 167.41(4) . . ? P6 Pt2 Ga4 98.51(5) . . ? Ga3 Pt2 Ga4 80.18(3) . . ? N1 Ga1 P1 93.65(15) . . ? N1 Ga1 Pt1 134.76(15) . . ? P1 Ga1 Pt1 130.47(5) . . ? N3 Ga2 N4 88.3(3) . . ? N3 Ga2 Pt1 140.9(2) . . ? N4 Ga2 Pt1 125.82(16) . . ? N5 Ga3 P4 93.76(13) . . ? N5 Ga3 Pt2 134.76(13) . . ? P4 Ga3 Pt2 130.03(5) . . ? N8 Ga4 N7 87.98(18) . . ? N8 Ga4 Pt2 124.06(13) . . ? N7 Ga4 Pt2 141.46(13) . . ? C1 P1 Ga1 92.3(2) . . ? C66 P2 C60 103.7(3) . . ? C66 P2 C58 98.7(3) . . ? C60 P2 C58 105.9(3) . . ? C66 P2 Pt1 124.7(2) . . ? C60 P2 Pt1 114.3(2) . . ? C58 P2 Pt1 107.1(2) . . ? C78 P3 C72 104.8(3) . . ? C78 P3 C59 101.5(3) . . ? C72 P3 C59 103.1(3) . . ? C78 P3 Pt1 114.6(2) . . ? C72 P3 Pt1 124.7(2) . . ? C59 P3 Pt1 105.2(2) . . ? C84 P4 Ga3 91.9(2) . . ? C149 P5 C143 102.8(3) . . ? C149 P5 C141 106.0(3) . . ? C143 P5 C141 99.6(3) . . ? C149 P5 Pt2 116.8(2) . . ? C143 P5 Pt2 122.03(19) . . ? C141 P5 Pt2 107.36(18) . . ? C155 P6 C161 102.4(2) . . ? C155 P6 C142 102.8(2) . . ? C161 P6 C142 103.0(2) . . ? C155 P6 Pt2 126.85(18) . . ? C161 P6 Pt2 114.96(17) . . ? C142 P6 Pt2 103.89(19) . . ? C8 N1 C6 116.1(4) . . ? C8 N1 Ga1 128.5(4) . . ? C6 N1 Ga1 115.4(3) . . ? C7 N2 C20 123.8(5) . . ? C32 N3 C34 115.3(6) . . ? C32 N3 Ga2 108.1(5) . . ? C34 N3 Ga2 132.7(4) . . ? C33 N4 C46 119.0(6) . . ? C33 N4 Ga2 106.9(5) . . ? C46 N4 Ga2 132.5(4) . . ? C91 N5 C89 116.0(4) . . ? C91 N5 Ga3 128.1(3) . . ? C89 N5 Ga3 115.7(3) . . ? C90 N6 C103 123.1(5) . . ? C115 N7 C117 115.6(4) . . ? C115 N7 Ga4 107.3(3) . . ? C117 N7 Ga4 133.7(3) . . ? C116 N8 C129 117.9(4) . . ? C116 N8 Ga4 108.3(3) . . ? C129 N8 Ga4 132.1(3) . . ? C6 C1 C2 116.9(5) . . ? C6 C1 P1 123.6(5) . . ? C2 C1 P1 119.0(4) . . ? C4 C2 C5 107.9(6) . . ? C4 C2 C1 114.7(5) . . ? C5 C2 C1 111.4(5) . . ? C4 C2 C3 106.1(6) . . ? C5 C2 C3 109.9(6) . . ? C1 C2 C3 106.6(5) . . ? N1 C6 C7 105.6(4) . . ? N1 C6 C1 113.4(4) . . ? C7 C6 C1 114.5(4) . . ? N2 C7 C6 120.2(5) . . ? C9 C8 C13 120.3(6) . . ? C9 C8 N1 120.6(5) . . ? C13 C8 N1 119.1(5) . . ? C10 C9 C8 117.9(6) . . ? C10 C9 C14 118.1(6) . . ? C8 C9 C14 124.0(6) . . ? C11 C10 C9 122.7(7) . . ? C12 C11 C10 118.9(6) . . ? C11 C12 C13 122.0(6) . . ? C12 C13 C8 118.1(6) . . ? C12 C13 C17 118.8(5) . . ? C8 C13 C17 123.1(5) . . ? C15 C14 C9 111.9(6) . . ? C15 C14 C16 110.6(6) . . ? C9 C14 C16 111.1(5) . . ? C13 C17 C18 112.3(5) . . ? C13 C17 C19 111.2(5) . . ? C18 C17 C19 110.2(5) . . ? C25 C20 C21 120.1(5) . . ? C25 C20 N2 122.8(5) . . ? C21 C20 N2 116.6(5) . . ? C22 C21 C20 119.1(5) . . ? C22 C21 C26 119.9(5) . . ? C20 C21 C26 121.0(5) . . ? C21 C22 C23 121.7(6) . . ? C24 C23 C22 118.7(6) . . ? C23 C24 C25 122.1(6) . . ? C24 C25 C20 118.2(5) . . ? C24 C25 C29 118.8(5) . . ? C20 C25 C29 123.0(5) . . ? C27 C26 C21 113.3(5) . . ? C27 C26 C28 111.2(5) . . ? C21 C26 C28 110.1(5) . . ? C25 C29 C31 111.3(5) . . ? C25 C29 C30 112.4(5) . . ? C31 C29 C30 110.6(5) . . ? C33 C32 N3 117.7(6) . . ? C32 C33 N4 118.4(7) . . ? C39 C34 C35 121.0(8) . . ? C39 C34 N3 118.7(7) . . ? C35 C34 N3 120.3(9) . . ? C36 C35 C34 116.9(11) . . ? C36 C35 C40 120.8(9) . . ? C34 C35 C40 122.3(8) . . ? C37 C36 C35 122.5(10) . . ? C36 C37 C38 122.0(10) . . ? C37 C38 C39 117.8(11) . . ? C34 C39 C38 119.8(8) . . ? C34 C39 C43 122.3(8) . . ? C38 C39 C43 117.8(10) . . ? C35 C40 C42 112.5(9) . . ? C35 C40 C41 109.9(9) . . ? C42 C40 C41 111.6(9) . . ? C44 C43 C39 114.4(8) . . ? C44 C43 C45 111.1(8) . . ? C39 C43 C45 109.1(6) . . ? C51 C46 C47 119.7(7) . . ? C51 C46 N4 119.9(6) . . ? C47 C46 N4 120.3(6) . . ? C48 C47 C46 118.8(7) . . ? C48 C47 C52 119.7(7) . . ? C46 C47 C52 121.5(8) . . ? C49 C48 C47 122.4(7) . . ? C48 C49 C50 118.0(8) . . ? C51 C50 C49 121.8(7) . . ? C50 C51 C46 119.2(7) . . ? C50 C51 C55 118.9(6) . . ? C46 C51 C55 121.8(7) . . ? C47 C52 C54 112.1(6) . . ? C47 C52 C53 112.2(6) . . ? C54 C52 C53 108.3(6) . . ? C57 C55 C51 111.6(6) . . ? C57 C55 C56 110.5(6) . . ? C51 C55 C56 110.9(6) . . ? C59 C58 P2 112.4(4) . . ? C58 C59 P3 108.6(4) . . ? C61 C60 C65 118.9(7) . . ? C61 C60 P2 118.6(5) . . ? C65 C60 P2 122.6(6) . . ? C62 C61 C60 120.8(7) . . ? C61 C62 C63 119.0(8) . . ? C64 C63 C62 120.0(8) . . ? C63 C64 C65 120.7(8) . . ? C64 C65 C60 120.6(8) . . ? C67 C66 C71 119.7(6) . . ? C67 C66 P2 120.5(5) . . ? C71 C66 P2 119.3(5) . . ? C66 C67 C68 119.3(6) . . ? C69 C68 C67 120.5(7) . . ? C68 C69 C70 120.3(7) . . ? C71 C70 C69 120.0(7) . . ? C70 C71 C66 120.2(7) . . ? C77 C72 C73 118.7(6) . . ? C77 C72 P3 119.7(5) . . ? C73 C72 P3 121.6(5) . . ? C74 C73 C72 120.6(6) . . ? C73 C74 C75 120.1(7) . . ? C76 C75 C74 119.8(7) . . ? C75 C76 C77 120.0(7) . . ? C72 C77 C76 120.9(6) . . ? C83 C78 C79 118.4(7) . . ? C83 C78 P3 121.8(6) . . ? C79 C78 P3 119.8(5) . . ? C80 C79 C78 120.8(7) . . ? C79 C80 C81 119.6(8) . . ? C82 C81 C80 119.3(9) . . ? C81 C82 C83 122.0(8) . . ? C82 C83 C78 119.8(8) . . ? C89 C84 C85 117.7(5) . . ? C89 C84 P4 124.0(4) . . ? C85 C84 P4 118.3(4) . . ? C86 C85 C88 107.0(6) . . ? C86 C85 C84 107.6(6) . . ? C88 C85 C84 116.9(5) . . ? C86 C85 C87 111.9(7) . . ? C88 C85 C87 104.5(6) . . ? C84 C85 C87 109.0(5) . . ? N5 C89 C90 107.2(4) . . ? N5 C89 C84 113.3(4) . . ? C90 C89 C84 110.5(4) . . ? N6 C90 C89 120.0(5) . . ? C96 C91 C92 119.5(5) . . ? C96 C91 N5 119.8(5) . . ? C92 C91 N5 120.6(5) . . ? C93 C92 C91 119.0(5) . . ? C93 C92 C97 117.2(5) . . ? C91 C92 C97 123.8(5) . . ? C94 C93 C92 121.6(6) . . ? C93 C94 C95 119.5(6) . . ? C94 C95 C96 121.5(6) . . ? C95 C96 C91 118.7(5) . . ? C95 C96 C100 117.0(5) . . ? C91 C96 C100 124.2(5) . . ? C99 C97 C98 108.8(5) . . ? C99 C97 C92 113.4(5) . . ? C98 C97 C92 110.2(6) . . ? C96 C100 C101 111.4(6) . . ? C96 C100 C102 111.2(5) . . ? C101 C100 C102 110.0(6) . . ? C108 C103 C104 121.7(6) . . ? C108 C103 N6 123.0(6) . . ? C104 C103 N6 114.7(5) . . ? C105 C104 C103 117.8(6) . . ? C105 C104 C109 121.0(6) . . ? C103 C104 C109 121.2(6) . . ? C104 C105 C106 120.7(7) . . ? C107 C106 C105 120.4(7) . . ? C106 C107 C108 121.4(7) . . ? C103 C108 C107 117.8(6) . . ? C103 C108 C112 123.2(6) . . ? C107 C108 C112 119.0(6) . . ? C104 C109 C110 113.4(7) . . ? C104 C109 C111 109.0(6) . . ? C110 C109 C111 111.9(6) . . ? C108 C112 C114 111.0(6) . . ? C108 C112 C113 112.0(6) . . ? C114 C112 C113 109.9(6) . . ? C116 C115 N7 118.0(5) . . ? C115 C116 N8 117.8(5) . . ? C118 C117 C122 120.1(5) . . ? C118 C117 N7 119.9(5) . . ? C122 C117 N7 120.0(5) . . ? C119 C118 C117 118.5(5) . . ? C119 C118 C123 119.8(5) . . ? C117 C118 C123 121.6(5) . . ? C120 C119 C118 121.6(6) . . ? C121 C120 C119 119.4(6) . . ? C120 C121 C122 122.0(6) . . ? C121 C122 C117 118.2(6) . . ? C121 C122 C126 119.0(6) . . ? C117 C122 C126 122.8(5) . . ? C118 C123 C125 109.1(6) . . ? C118 C123 C124 113.5(5) . . ? C125 C123 C124 111.1(7) . . ? C122 C126 C128 112.4(6) . . ? C122 C126 C127 111.6(6) . . ? C128 C126 C127 110.0(6) . . ? C134 C129 C130 120.3(5) . . ? C134 C129 N8 119.9(5) . . ? C130 C129 N8 119.8(5) . . ? C131 C130 C129 118.2(6) . . ? C131 C130 C135 118.7(5) . . ? C129 C130 C135 123.1(5) . . ? C130 C131 C132 121.5(6) . . ? C133 C132 C131 119.8(6) . . ? C132 C133 C134 121.2(6) . . ? C133 C134 C129 119.0(6) . . ? C133 C134 C138 120.0(5) . . ? C129 C134 C138 121.0(5) . . ? C130 C135 C136 112.6(5) . . ? C130 C135 C137 111.8(5) . . ? C136 C135 C137 109.8(5) . . ? C139 C138 C134 111.4(5) . . ? C139 C138 C140 110.6(6) . . ? C134 C138 C140 112.8(6) . . ? C142 C141 P5 112.6(4) . . ? C141 C142 P6 110.3(4) . . ? C144 C143 C148 119.0(5) . . ? C144 C143 P5 121.0(4) . . ? C148 C143 P5 119.5(4) . . ? C143 C144 C145 120.0(5) . . ? C146 C145 C144 120.0(5) . . ? C147 C146 C145 119.8(5) . . ? C148 C147 C146 121.4(6) . . ? C147 C148 C143 119.8(6) . . ? C150 C149 C154 118.7(6) . . ? C150 C149 P5 118.7(5) . . ? C154 C149 P5 122.5(6) . . ? C149 C150 C151 122.4(8) . . ? C152 C151 C150 117.7(9) . . ? C151 C152 C153 122.4(9) . . ? C152 C153 C154 118.4(9) . . ? C149 C154 C153 120.1(9) . . ? C156 C155 C160 118.7(5) . . ? C156 C155 P6 119.6(4) . . ? C160 C155 P6 121.4(4) . . ? C155 C156 C157 120.0(6) . . ? C158 C157 C156 120.7(6) . . ? C159 C158 C157 119.4(5) . . ? C158 C159 C160 120.9(6) . . ? C159 C160 C155 120.2(6) . . ? C166 C161 C162 118.6(5) . . ? C166 C161 P6 122.7(4) . . ? C162 C161 P6 118.7(4) . . ? C163 C162 C161 120.6(5) . . ? C164 C163 C162 120.8(5) . . ? C163 C164 C165 119.4(6) . . ? C166 C165 C164 119.5(6) . . ? C161 C166 C165 121.0(5) . . ? C167 C168 C169 114.1(12) . . ? C170 C169 C168 115.9(12) . . ? C169 C170 C171 122.9(14) . . ? C172 C171 C170 109.9(15) . . ? C175 C174 C173 112.2(12) . . ? C174 C175 C176 122.9(12) . . ? C177 C176 C175 118.2(11) . . ? C176 C177 C178 109.9(11) . . ? C179 C180 C181 122.3(16) . . ? C182 C181 C180 125.5(16) . . ? C181 C182 C183 143(2) . . ? C184 C183 C182 98.4(19) . . ? C187 C186 C185 124.2(16) . . ? C186 C187 C188 127.4(18) . . ? C189 C188 C187 114.8(15) . . ? C188 C189 C190 113.7(15) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.294 _refine_diff_density_min -1.057 _refine_diff_density_rms 0.103