data_2 _audit_creation_date 2013-10-08T17:46:51-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H32 N O3 Pt, C16 H36 N, C H2 Cl2' _chemical_formula_sum 'C59 H70 Cl2 N2 O3 Pt' _chemical_formula_weight 1121.16 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 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 14.5840(2) _cell_length_b 15.9450(3) _cell_length_c 22.7830(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5298.00(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 24698 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.795 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.4202 _exptl_absorpt_correction_T_max 0.5198 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.21325E-2 _diffrn_orient_matrix_ub_12 -0.557515E-1 _diffrn_orient_matrix_ub_13 -0.200561E-1 _diffrn_orient_matrix_ub_21 -0.676014E-1 _diffrn_orient_matrix_ub_22 -0.64232E-2 _diffrn_orient_matrix_ub_23 0.57998E-2 _diffrn_orient_matrix_ub_31 -0.112631E-1 _diffrn_orient_matrix_ub_32 0.279966E-1 _diffrn_orient_matrix_ub_33 -0.386084E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_unetI/netI 0.0408 _diffrn_reflns_number 41615 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.87 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.98 _reflns_number_total 11855 _reflns_number_gt 10756 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0458P)^2^+5.0120P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 11855 _refine_ls_number_parameters 479 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0994 _refine_ls_wR_factor_gt 0.096 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.089(8) _refine_diff_density_max 0.909 _refine_diff_density_min -1.057 _refine_diff_density_rms 0.087 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.3079(3) 0.2816(3) 0.5489(2) 0.0422(12) Uani 1 1 d . . . C2 C 0.2321(4) 0.4126(3) 0.5442(3) 0.0471(13) Uani 1 1 d . . . C3 C 0.1474(4) 0.3709(4) 0.5418(3) 0.0570(16) Uani 1 1 d . . . H3 H 0.0936 0.4019 0.5389 0.068 Uiso 1 1 calc R . . C4 C 0.1429(4) 0.2860(4) 0.5437(3) 0.0568(16) Uani 1 1 d . . . H4 H 0.0862 0.2594 0.5435 0.068 Uiso 1 1 calc R . . C5 C 0.2228(4) 0.1495(4) 0.5452(3) 0.0532(15) Uani 1 1 d . . . H5 H 0.1674 0.1208 0.5436 0.064 Uiso 1 1 calc R . . C6 C 0.3036(5) 0.1069(4) 0.5468(3) 0.0614(17) Uani 1 1 d . . . H6 H 0.3031 0.0486 0.5463 0.074 Uiso 1 1 calc R . . C7 C 0.3867(5) 0.1492(4) 0.5492(3) 0.0604(16) Uani 1 1 d . . . H7 H 0.4411 0.1188 0.55 0.072 Uiso 1 1 calc R . . C8 C 0.3899(4) 0.2353(3) 0.5505(3) 0.0490(14) Uani 1 1 d . . . H8 H 0.446 0.2628 0.5524 0.059 Uiso 1 1 calc R . . C9 C 0.1723(4) 0.5533(4) 0.5673(4) 0.0597(16) Uani 1 1 d . . . H9 H 0.1327 0.528 0.5939 0.072 Uiso 1 1 calc R . . C10 C 0.1671(5) 0.6388(4) 0.5577(4) 0.0678(17) Uani 1 1 d . . . H10 H 0.1243 0.6706 0.5782 0.081 Uiso 1 1 calc R . . C11 C 0.2250(6) 0.6773(5) 0.5181(4) 0.072(2) Uani 1 1 d . . . H11 H 0.2224 0.735 0.5123 0.087 Uiso 1 1 calc R . . C12 C 0.2862(5) 0.6293(5) 0.4876(4) 0.0691(19) Uani 1 1 d . . . H12 H 0.3238 0.6548 0.4599 0.083 Uiso 1 1 calc R . . C13 C 0.2939(4) 0.5425(4) 0.4969(3) 0.0548(15) Uani 1 1 d . . . H13 H 0.3368 0.5109 0.4763 0.066 Uiso 1 1 calc R . . C14 C 0.2360(4) 0.5049(4) 0.5374(3) 0.0495(14) Uani 1 1 d . . . C15 C 0.2245(4) 0.2378(4) 0.5460(3) 0.0490(14) Uani 1 1 d . . . C16 C 0.5636(4) 0.4795(3) 0.5714(2) 0.0428(11) Uani 1 1 d . . . C17 C 0.6371(4) 0.5088(4) 0.5774(3) 0.0468(13) Uani 1 1 d . . . C18 C 0.7299(4) 0.5375(4) 0.5849(3) 0.0472(14) Uani 1 1 d . . . C19 C 0.7990(4) 0.4778(4) 0.5943(2) 0.0487(14) Uani 1 1 d . . . H19 H 0.7836 0.4212 0.5939 0.058 Uiso 1 1 calc R . . C20 C 0.8886(4) 0.5002(5) 0.6039(3) 0.0560(15) Uani 1 1 d . . . C21 C 0.9121(4) 0.5847(5) 0.6036(3) 0.0628(18) Uani 1 1 d . . . H21 H 0.9728 0.6005 0.6093 0.075 Uiso 1 1 calc R . . C22 C 0.8456(5) 0.6456(4) 0.5947(3) 0.0589(16) Uani 1 1 d . . . H22 H 0.8612 0.7021 0.5948 0.071 Uiso 1 1 calc R . . C23 C 0.7537(4) 0.6204(4) 0.5854(3) 0.0497(14) Uani 1 1 d . . . H23 H 0.7087 0.6609 0.5796 0.06 Uiso 1 1 calc R . . C24 C 0.9363(6) 0.3596(5) 0.6213(4) 0.080(2) Uani 1 1 d . . . H24A H 0.9911 0.3275 0.6278 0.12 Uiso 1 1 calc R . . H24B H 0.9058 0.3395 0.5867 0.12 Uiso 1 1 calc R . . H24C H 0.8963 0.3537 0.6545 0.12 Uiso 1 1 calc R . . C25 C 0.4663(3) 0.4064(4) 0.4760(2) 0.0437(13) Uani 1 1 d . . . C26 C 0.4706(4) 0.3930(4) 0.4233(3) 0.0509(14) Uani 1 1 d . . . C27 C 0.4633(5) 0.3809(5) 0.3613(3) 0.0733(8) Uani 1 1 d . . . C28 C 0.3857(6) 0.3463(6) 0.3374(3) 0.0733(8) Uani 1 1 d . . . H28 H 0.3394 0.3283 0.3624 0.088 Uiso 1 1 calc R . . C29 C 0.3735(6) 0.3372(6) 0.2776(3) 0.0733(8) Uani 1 1 d . . . C30 C 0.4401(6) 0.3643(5) 0.2402(3) 0.0733(8) Uani 1 1 d . . . H30 H 0.4325 0.3587 0.1998 0.088 Uiso 1 1 calc R . . C31 C 0.5197(6) 0.4006(5) 0.2628(3) 0.0733(8) Uani 1 1 d . . . H31 H 0.5652 0.4195 0.2374 0.088 Uiso 1 1 calc R . . C32 C 0.5313(5) 0.4086(5) 0.3220(3) 0.0733(8) Uani 1 1 d . . . H32 H 0.5848 0.4327 0.3366 0.088 Uiso 1 1 calc R . . C33 C 0.2771(9) 0.2975(9) 0.1993(4) 0.124(4) Uani 1 1 d . . . H33A H 0.2201 0.269 0.1923 0.187 Uiso 1 1 calc R . . H33B H 0.3259 0.2677 0.1802 0.187 Uiso 1 1 calc R . . H33C H 0.2736 0.3535 0.1839 0.187 Uiso 1 1 calc R . . C34 C 0.4152(4) 0.4473(3) 0.6462(2) 0.0430(12) Uani 1 1 d . . . C35 C 0.4006(4) 0.4570(4) 0.6975(3) 0.0543(15) Uani 1 1 d . . . C36 C 0.3895(5) 0.4635(4) 0.7603(3) 0.0545(15) Uani 1 1 d . . . C37 C 0.4620(5) 0.4473(4) 0.7979(3) 0.0563(16) Uani 1 1 d . . . H37 H 0.5185 0.4324 0.7822 0.068 Uiso 1 1 calc R . . C38 C 0.4522(6) 0.4529(4) 0.8591(3) 0.0652(18) Uani 1 1 d . . . C39 C 0.3703(7) 0.4692(5) 0.8827(4) 0.077(2) Uani 1 1 d . . . H39 H 0.3631 0.4695 0.9232 0.092 Uiso 1 1 calc R . . C40 C 0.2955(7) 0.4857(5) 0.8463(4) 0.081(2) Uani 1 1 d . . . H40 H 0.2393 0.4985 0.8634 0.097 Uiso 1 1 calc R . . C41 C 0.3017(6) 0.4837(5) 0.7852(4) 0.072(2) Uani 1 1 d . . . H41 H 0.2512 0.4951 0.7616 0.086 Uiso 1 1 calc R . . C42 C 0.5234(8) 0.4334(6) 0.9523(3) 0.093(3) Uani 1 1 d . . . H42A H 0.5829 0.424 0.9691 0.139 Uiso 1 1 calc R . . H42B H 0.4836 0.3875 0.9621 0.139 Uiso 1 1 calc R . . H42C H 0.4983 0.4846 0.9676 0.139 Uiso 1 1 calc R . . C43 C 0.4731(7) 0.1599(5) 0.7004(4) 0.0846(6) Uani 1 1 d . . . H43A H 0.5115 0.1157 0.7162 0.102 Uiso 1 1 calc R . . H43B H 0.443 0.1376 0.6658 0.102 Uiso 1 1 calc R . . C44 C 0.5349(7) 0.2319(5) 0.6813(4) 0.0846(6) Uani 1 1 d . . . H44A H 0.5653 0.2555 0.7154 0.102 Uiso 1 1 calc R . . H44B H 0.4981 0.2757 0.6634 0.102 Uiso 1 1 calc R . . C45 C 0.6061(7) 0.2015(5) 0.6378(4) 0.0846(6) Uani 1 1 d . . . H45A H 0.6442 0.1598 0.6568 0.102 Uiso 1 1 calc R . . H45B H 0.5749 0.1743 0.6053 0.102 Uiso 1 1 calc R . . C46 C 0.6660(7) 0.2686(5) 0.6139(4) 0.0846(6) Uani 1 1 d . . . H46A H 0.7093 0.2446 0.587 0.127 Uiso 1 1 calc R . . H46B H 0.6984 0.2952 0.6456 0.127 Uiso 1 1 calc R . . H46C H 0.6292 0.3095 0.5938 0.127 Uiso 1 1 calc R . . C47 C 0.3550(7) 0.0968(5) 0.7639(4) 0.0846(6) Uani 1 1 d . . . H47A H 0.4026 0.0583 0.7763 0.102 Uiso 1 1 calc R . . H47B H 0.3163 0.1079 0.7977 0.102 Uiso 1 1 calc R . . C48 C 0.2968(7) 0.0536(5) 0.7168(4) 0.0846(6) Uani 1 1 d . . . H48A H 0.3367 0.0342 0.6855 0.102 Uiso 1 1 calc R . . H48B H 0.2546 0.0941 0.7002 0.102 Uiso 1 1 calc R . . C49 C 0.2417(7) -0.0216(5) 0.7408(4) 0.0846(6) Uani 1 1 d . . . H49A H 0.2065 -0.0033 0.7746 0.102 Uiso 1 1 calc R . . H49B H 0.1987 -0.04 0.711 0.102 Uiso 1 1 calc R . . C50 C 0.2969(7) -0.0900(5) 0.7574(4) 0.0846(6) Uani 1 1 d . . . H50A H 0.2589 -0.1339 0.7729 0.127 Uiso 1 1 calc R . . H50B H 0.3398 -0.0723 0.7869 0.127 Uiso 1 1 calc R . . H50C H 0.3297 -0.1104 0.7238 0.127 Uiso 1 1 calc R . . C51 C 0.4428(7) 0.2208(5) 0.7993(4) 0.0846(6) Uani 1 1 d . . . H51A H 0.4678 0.2749 0.7882 0.102 Uiso 1 1 calc R . . H51B H 0.3942 0.2309 0.8274 0.102 Uiso 1 1 calc R . . C52 C 0.5178(7) 0.1705(5) 0.8293(4) 0.0846(6) Uani 1 1 d . . . H52A H 0.5641 0.1564 0.8004 0.102 Uiso 1 1 calc R . . H52B H 0.4915 0.1183 0.8433 0.102 Uiso 1 1 calc R . . C53 C 0.5659(7) 0.2155(5) 0.8822(4) 0.0846(6) Uani 1 1 d . . . H53A H 0.6221 0.1864 0.8924 0.102 Uiso 1 1 calc R . . H53B H 0.5812 0.2727 0.8716 0.102 Uiso 1 1 calc R . . C54 C 0.5036(7) 0.2151(5) 0.9317(4) 0.0846(6) Uani 1 1 d . . . H54A H 0.5319 0.2426 0.9645 0.127 Uiso 1 1 calc R . . H54B H 0.4893 0.1582 0.9421 0.127 Uiso 1 1 calc R . . H54C H 0.4482 0.2441 0.9213 0.127 Uiso 1 1 calc R . . C55 C 0.3330(7) 0.2400(5) 0.7164(4) 0.0846(6) Uani 1 1 d . . . H55A H 0.3117 0.2147 0.6802 0.102 Uiso 1 1 calc R . . H55B H 0.3653 0.2911 0.7061 0.102 Uiso 1 1 calc R . . C56 C 0.2489(7) 0.2638(5) 0.7531(4) 0.0846(6) Uani 1 1 d . . . H56A H 0.2677 0.2972 0.7867 0.102 Uiso 1 1 calc R . . H56B H 0.219 0.2135 0.7676 0.102 Uiso 1 1 calc R . . C57 C 0.1832(7) 0.3134(5) 0.7154(4) 0.0846(6) Uani 1 1 d . . . H57A H 0.1598 0.2777 0.6844 0.102 Uiso 1 1 calc R . . H57B H 0.2157 0.3598 0.6973 0.102 Uiso 1 1 calc R . . C58 C 0.1013(7) 0.3481(5) 0.7523(4) 0.0846(6) Uani 1 1 d . . . H58A H 0.0616 0.3803 0.7273 0.127 Uiso 1 1 calc R . . H58B H 0.1243 0.3831 0.7832 0.127 Uiso 1 1 calc R . . H58C H 0.0676 0.3021 0.7689 0.127 Uiso 1 1 calc R . . C59 C 0.9148(7) 0.4064(6) 0.9392(5) 0.101(3) Uani 1 1 d . . . H59A H 0.9223 0.3893 0.9798 0.121 Uiso 1 1 calc R . . H59B H 0.9339 0.4645 0.936 0.121 Uiso 1 1 calc R . . N1 N 0.3121(3) 0.3690(3) 0.5495(2) 0.0443(11) Uani 1 1 d . . . N2 N 0.4010(6) 0.1804(4) 0.7449(3) 0.0846(6) Uani 1 1 d . . . O1 O 0.9596(3) 0.4458(4) 0.6138(3) 0.0781(15) Uani 1 1 d . . . O2 O 0.2941(5) 0.3008(4) 0.2599(2) 0.094(2) Uani 1 1 d . . . O3 O 0.5312(4) 0.4396(4) 0.8903(2) 0.0796(15) Uani 1 1 d . . . Pt1 Pt 0.442200(13) 0.428034(12) 0.560833(9) 0.03973(6) Uani 1 1 d . . . Cl1 Cl 0.8012(2) 0.39823(16) 0.92008(13) 0.1076(8) Uani 1 1 d . . . Cl2 Cl 0.98496(18) 0.3438(2) 0.89415(14) 0.1138(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.040(2) 0.041(3) 0.046(3) 0.002(2) 0.004(2) 0.001(2) C2 0.042(3) 0.043(3) 0.057(3) 0.009(2) -0.003(2) -0.008(2) C3 0.035(3) 0.054(4) 0.082(5) 0.004(3) 0.001(3) 0.000(2) C4 0.038(3) 0.051(3) 0.082(5) 0.003(3) 0.006(3) -0.009(3) C5 0.054(3) 0.044(3) 0.061(4) 0.000(3) 0.007(3) -0.011(3) C6 0.070(4) 0.039(3) 0.075(5) -0.002(3) 0.000(3) -0.004(3) C7 0.058(3) 0.047(3) 0.076(5) -0.001(3) -0.002(3) 0.000(3) C8 0.041(3) 0.038(3) 0.068(4) 0.004(3) 0.001(3) 0.000(2) C9 0.049(3) 0.048(3) 0.082(4) -0.005(3) 0.002(3) 0.001(2) C10 0.064(4) 0.050(3) 0.089(5) 0.002(4) 0.001(4) 0.007(3) C11 0.074(5) 0.046(4) 0.097(6) 0.010(4) -0.004(4) 0.002(3) C12 0.062(4) 0.049(4) 0.096(5) 0.017(4) -0.002(4) 0.001(3) C13 0.048(3) 0.052(3) 0.065(4) 0.007(3) -0.007(3) -0.003(3) C14 0.044(3) 0.042(3) 0.063(4) 0.003(3) 0.002(3) 0.002(2) C15 0.047(3) 0.041(3) 0.059(4) 0.002(2) 0.004(3) -0.008(2) C16 0.040(2) 0.039(2) 0.050(3) 0.012(2) -0.005(3) 0.003(2) C17 0.033(3) 0.047(3) 0.060(4) 0.002(3) -0.001(2) 0.002(2) C18 0.038(3) 0.062(4) 0.042(3) -0.003(3) 0.002(2) -0.010(3) C19 0.041(3) 0.061(4) 0.044(3) 0.002(3) 0.000(2) 0.001(3) C20 0.042(3) 0.070(4) 0.056(4) 0.009(3) 0.000(3) -0.002(3) C21 0.039(3) 0.087(5) 0.062(4) 0.002(4) 0.000(3) -0.016(3) C22 0.058(4) 0.051(4) 0.067(4) 0.000(3) -0.001(3) -0.017(3) C23 0.048(3) 0.046(3) 0.055(3) 0.002(3) 0.001(3) -0.002(3) C24 0.063(4) 0.076(5) 0.102(6) 0.011(4) 0.008(5) 0.023(4) C25 0.035(3) 0.050(3) 0.046(3) 0.002(2) -0.002(2) -0.003(2) C26 0.044(3) 0.049(3) 0.060(4) 0.006(3) 0.007(2) -0.001(2) C27 0.0710(18) 0.086(2) 0.0625(16) 0.0004(15) 0.0111(15) -0.0107(16) C28 0.0710(18) 0.086(2) 0.0625(16) 0.0004(15) 0.0111(15) -0.0107(16) C29 0.0710(18) 0.086(2) 0.0625(16) 0.0004(15) 0.0111(15) -0.0107(16) C30 0.0710(18) 0.086(2) 0.0625(16) 0.0004(15) 0.0111(15) -0.0107(16) C31 0.0710(18) 0.086(2) 0.0625(16) 0.0004(15) 0.0111(15) -0.0107(16) C32 0.0710(18) 0.086(2) 0.0625(16) 0.0004(15) 0.0111(15) -0.0107(16) C33 0.127(9) 0.181(12) 0.065(6) -0.017(7) 0.003(6) -0.049(9) C34 0.045(3) 0.040(3) 0.044(3) 0.003(2) 0.003(2) -0.006(2) C35 0.056(3) 0.035(3) 0.072(4) 0.006(3) 0.004(3) -0.002(2) C36 0.071(4) 0.037(3) 0.055(4) -0.004(3) 0.010(3) -0.004(3) C37 0.073(4) 0.042(3) 0.054(3) -0.010(2) 0.008(3) -0.006(3) C38 0.090(5) 0.052(4) 0.054(3) 0.001(3) 0.015(4) -0.013(4) C39 0.108(7) 0.059(4) 0.062(4) -0.008(3) 0.016(5) -0.006(4) C40 0.102(7) 0.060(5) 0.081(6) -0.008(4) 0.027(5) 0.006(4) C41 0.072(5) 0.063(4) 0.081(5) 0.001(4) 0.019(4) 0.002(4) C42 0.155(8) 0.072(5) 0.051(4) 0.007(4) 0.000(4) -0.030(6) C43 0.1103(17) 0.0591(11) 0.0843(13) 0.0032(9) 0.0138(12) 0.0005(11) C44 0.1103(17) 0.0591(11) 0.0843(13) 0.0032(9) 0.0138(12) 0.0005(11) C45 0.1103(17) 0.0591(11) 0.0843(13) 0.0032(9) 0.0138(12) 0.0005(11) C46 0.1103(17) 0.0591(11) 0.0843(13) 0.0032(9) 0.0138(12) 0.0005(11) C47 0.1103(17) 0.0591(11) 0.0843(13) 0.0032(9) 0.0138(12) 0.0005(11) C48 0.1103(17) 0.0591(11) 0.0843(13) 0.0032(9) 0.0138(12) 0.0005(11) C49 0.1103(17) 0.0591(11) 0.0843(13) 0.0032(9) 0.0138(12) 0.0005(11) C50 0.1103(17) 0.0591(11) 0.0843(13) 0.0032(9) 0.0138(12) 0.0005(11) C51 0.1103(17) 0.0591(11) 0.0843(13) 0.0032(9) 0.0138(12) 0.0005(11) C52 0.1103(17) 0.0591(11) 0.0843(13) 0.0032(9) 0.0138(12) 0.0005(11) C53 0.1103(17) 0.0591(11) 0.0843(13) 0.0032(9) 0.0138(12) 0.0005(11) C54 0.1103(17) 0.0591(11) 0.0843(13) 0.0032(9) 0.0138(12) 0.0005(11) C55 0.1103(17) 0.0591(11) 0.0843(13) 0.0032(9) 0.0138(12) 0.0005(11) C56 0.1103(17) 0.0591(11) 0.0843(13) 0.0032(9) 0.0138(12) 0.0005(11) C57 0.1103(17) 0.0591(11) 0.0843(13) 0.0032(9) 0.0138(12) 0.0005(11) C58 0.1103(17) 0.0591(11) 0.0843(13) 0.0032(9) 0.0138(12) 0.0005(11) C59 0.113(7) 0.084(6) 0.107(7) -0.046(5) -0.002(6) -0.008(5) N1 0.033(2) 0.044(2) 0.057(3) 0.005(2) 0.0006(19) 0.0004(17) N2 0.1103(17) 0.0591(11) 0.0843(13) 0.0032(9) 0.0138(12) 0.0005(11) O1 0.039(2) 0.083(4) 0.112(4) 0.009(3) -0.004(2) 0.007(2) O2 0.107(5) 0.111(5) 0.064(3) -0.018(3) 0.003(3) -0.047(4) O3 0.096(4) 0.082(4) 0.060(3) 0.002(3) -0.006(3) -0.025(3) Pt1 0.03379(8) 0.03679(9) 0.04860(10) 0.00621(9) 0.00006(9) -0.00167(8) Cl1 0.1126(19) 0.0841(15) 0.126(2) -0.0199(13) 0.0242(15) 0.0175(13) Cl2 0.0842(15) 0.132(2) 0.125(2) -0.0460(18) 0.0032(15) 0.0084(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.396(7) . ? C1 C8 1.406(7) . ? C1 C15 1.404(7) . ? C2 N1 1.363(7) . ? C2 C3 1.404(8) . ? C2 C14 1.481(8) . ? C3 C4 1.355(9) . ? C3 H3 0.93 . ? C4 C15 1.417(9) . ? C4 H4 0.93 . ? C5 C6 1.359(9) . ? C5 C15 1.409(8) . ? C5 H5 0.93 . ? C6 C7 1.388(9) . ? C6 H6 0.93 . ? C7 C8 1.374(8) . ? C7 H7 0.93 . ? C8 H8 0.93 . ? C9 C10 1.383(9) . ? C9 C14 1.386(9) . ? C9 H9 0.93 . ? C10 C11 1.380(11) . ? C10 H10 0.93 . ? C11 C12 1.367(11) . ? C11 H11 0.93 . ? C12 C13 1.405(9) . ? C12 H12 0.93 . ? C13 C14 1.387(9) . ? C13 H13 0.93 . ? C16 C17 1.176(8) . ? C16 Pt1 1.966(6) . ? C17 C18 1.440(8) . ? C18 C23 1.366(8) . ? C18 C19 1.403(9) . ? C19 C20 1.372(8) . ? C19 H19 0.93 . ? C20 O1 1.369(8) . ? C20 C21 1.391(11) . ? C21 C22 1.387(10) . ? C21 H21 0.93 . ? C22 C23 1.415(9) . ? C22 H22 0.93 . ? C23 H23 0.93 . ? C24 O1 1.426(10) . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C25 C26 1.221(9) . ? C25 Pt1 1.995(6) . ? C26 C27 1.430(10) . ? C27 C28 1.372(11) . ? C27 C32 1.407(10) . ? C28 C29 1.381(11) . ? C28 H28 0.93 . ? C29 C30 1.363(10) . ? C29 O2 1.356(10) . ? C30 C31 1.396(11) . ? C30 H30 0.93 . ? C31 C32 1.366(11) . ? C31 H31 0.93 . ? C32 H32 0.93 . ? C33 O2 1.405(11) . ? C33 H33A 0.96 . ? C33 H33B 0.96 . ? C33 H33C 0.96 . ? C34 C35 1.198(9) . ? C34 Pt1 2.008(6) . ? C35 C36 1.443(10) . ? C36 C37 1.384(10) . ? C36 C41 1.437(10) . ? C37 C38 1.405(9) . ? C37 H37 0.93 . ? C38 C39 1.335(12) . ? C38 O3 1.371(10) . ? C39 C40 1.395(13) . ? C39 H39 0.93 . ? C40 C41 1.395(11) . ? C40 H40 0.93 . ? C41 H41 0.93 . ? C42 O3 1.421(9) . ? C42 H42A 0.96 . ? C42 H42B 0.96 . ? C42 H42C 0.96 . ? C43 C44 1.523(12) . ? C43 N2 1.497(11) . ? C43 H43A 0.97 . ? C43 H43B 0.97 . ? C44 C45 1.515(12) . ? C44 H44A 0.97 . ? C44 H44B 0.97 . ? C45 C46 1.485(12) . ? C45 H45A 0.97 . ? C45 H45B 0.97 . ? C46 H46A 0.96 . ? C46 H46B 0.96 . ? C46 H46C 0.96 . ? C47 C48 1.532(13) . ? C47 N2 1.553(10) . ? C47 H47A 0.97 . ? C47 H47B 0.97 . ? C48 C49 1.543(12) . ? C48 H48A 0.97 . ? C48 H48B 0.97 . ? C49 C50 1.407(12) . ? C49 H49A 0.97 . ? C49 H49B 0.97 . ? C50 H50A 0.96 . ? C50 H50B 0.96 . ? C50 H50C 0.96 . ? C51 C52 1.519(13) . ? C51 N2 1.524(11) . ? C51 H51A 0.97 . ? C51 H51B 0.97 . ? C52 C53 1.569(13) . ? C52 H52A 0.97 . ? C52 H52B 0.97 . ? C53 C54 1.448(12) . ? C53 H53A 0.97 . ? C53 H53B 0.97 . ? C54 H54A 0.96 . ? C54 H54B 0.96 . ? C54 H54C 0.96 . ? C55 N2 1.519(12) . ? C55 C56 1.532(13) . ? C55 H55A 0.97 . ? C55 H55B 0.97 . ? C56 C57 1.510(13) . ? C56 H56A 0.97 . ? C56 H56B 0.97 . ? C57 C58 1.561(12) . ? C57 H57A 0.97 . ? C57 H57B 0.97 . ? C58 H58A 0.96 . ? C58 H58B 0.96 . ? C58 H58C 0.96 . ? C59 Cl1 1.718(10) . ? C59 Cl2 1.760(9) . ? C59 H59A 0.97 . ? C59 H59B 0.97 . ? N1 Pt1 2.133(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 C1 C8 119.1(5) . . ? N1 C1 C15 122.4(5) . . ? C8 C1 C15 118.5(5) . . ? N1 C2 C3 121.0(5) . . ? N1 C2 C14 118.9(5) . . ? C3 C2 C14 120.0(5) . . ? C4 C3 C2 121.0(6) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C15 120.1(5) . . ? C3 C4 H4 119.9 . . ? C15 C4 H4 119.9 . . ? C6 C5 C15 119.0(6) . . ? C6 C5 H5 120.5 . . ? C15 C5 H5 120.5 . . ? C5 C6 C7 121.0(6) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C8 C7 C6 121.1(6) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C1 119.7(5) . . ? C7 C8 H8 120.2 . . ? C1 C8 H8 120.2 . . ? C10 C9 C14 120.5(7) . . ? C10 C9 H9 119.7 . . ? C14 C9 H9 119.7 . . ? C9 C10 C11 120.6(7) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 118.9(7) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C11 C12 C13 121.8(7) . . ? C11 C12 H12 119.1 . . ? C13 C12 H12 119.1 . . ? C14 C13 C12 118.6(7) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C13 C14 C9 119.6(6) . . ? C13 C14 C2 121.5(6) . . ? C9 C14 C2 118.5(6) . . ? C4 C15 C5 121.8(5) . . ? C4 C15 C1 117.3(5) . . ? C5 C15 C1 120.8(6) . . ? C17 C16 Pt1 178.6(5) . . ? C16 C17 C18 175.2(6) . . ? C23 C18 C19 118.3(6) . . ? C23 C18 C17 123.2(6) . . ? C19 C18 C17 118.5(6) . . ? C20 C19 C18 122.1(6) . . ? C20 C19 H19 118.9 . . ? C18 C19 H19 118.9 . . ? C19 C20 O1 125.6(7) . . ? C19 C20 C21 119.0(6) . . ? O1 C20 C21 115.4(6) . . ? C22 C21 C20 120.5(6) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 119.1(6) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C18 C23 C22 121.1(6) . . ? C18 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? O1 C24 H24A 109.5 . . ? O1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 Pt1 172.8(5) . . ? C25 C26 C27 172.4(7) . . ? C28 C27 C32 117.1(7) . . ? C28 C27 C26 120.5(7) . . ? C32 C27 C26 122.2(7) . . ? C27 C28 C29 122.7(7) . . ? C27 C28 H28 118.7 . . ? C29 C28 H28 118.7 . . ? C30 C29 O2 124.0(7) . . ? C30 C29 C28 119.5(8) . . ? O2 C29 C28 116.5(7) . . ? C29 C30 C31 119.6(7) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C32 C31 C30 120.4(7) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C27 120.8(7) . . ? C31 C32 H32 119.6 . . ? C27 C32 H32 119.6 . . ? O2 C33 H33A 109.5 . . ? O2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 Pt1 178.3(5) . . ? C34 C35 C36 174.9(7) . . ? C37 C36 C41 118.5(6) . . ? C37 C36 C35 121.0(6) . . ? C41 C36 C35 120.5(7) . . ? C36 C37 C38 121.7(7) . . ? C36 C37 H37 119.2 . . ? C38 C37 H37 119.2 . . ? C39 C38 O3 125.0(7) . . ? C39 C38 C37 120.2(8) . . ? O3 C38 C37 114.8(7) . . ? C38 C39 C40 119.8(8) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? C39 C40 C41 122.5(8) . . ? C39 C40 H40 118.7 . . ? C41 C40 H40 118.7 . . ? C40 C41 C36 117.2(8) . . ? C40 C41 H41 121.4 . . ? C36 C41 H41 121.4 . . ? O3 C42 H42A 109.5 . . ? O3 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O3 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 N2 116.4(7) . . ? C44 C43 H43A 108.2 . . ? N2 C43 H43A 108.2 . . ? C44 C43 H43B 108.2 . . ? N2 C43 H43B 108.2 . . ? H43A C43 H43B 107.3 . . ? C43 C44 C45 110.5(7) . . ? C43 C44 H44A 109.5 . . ? C45 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? C45 C44 H44B 109.5 . . ? H44A C44 H44B 108.1 . . ? C46 C45 C44 114.4(7) . . ? C46 C45 H45A 108.7 . . ? C44 C45 H45A 108.7 . . ? C46 C45 H45B 108.7 . . ? C44 C45 H45B 108.7 . . ? H45A C45 H45B 107.6 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 N2 115.5(7) . . ? C48 C47 H47A 108.4 . . ? N2 C47 H47A 108.4 . . ? C48 C47 H47B 108.4 . . ? N2 C47 H47B 108.4 . . ? H47A C47 H47B 107.5 . . ? C47 C48 C49 112.9(7) . . ? C47 C48 H48A 109 . . ? C49 C48 H48A 109 . . ? C47 C48 H48B 109 . . ? C49 C48 H48B 109 . . ? H48A C48 H48B 107.8 . . ? C50 C49 C48 113.5(9) . . ? C50 C49 H49A 108.9 . . ? C48 C49 H49A 108.9 . . ? C50 C49 H49B 108.9 . . ? C48 C49 H49B 108.9 . . ? H49A C49 H49B 107.7 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 N2 115.5(7) . . ? C52 C51 H51A 108.4 . . ? N2 C51 H51A 108.4 . . ? C52 C51 H51B 108.4 . . ? N2 C51 H51B 108.4 . . ? H51A C51 H51B 107.5 . . ? C51 C52 C53 115.3(7) . . ? C51 C52 H52A 108.5 . . ? C53 C52 H52A 108.5 . . ? C51 C52 H52B 108.5 . . ? C53 C52 H52B 108.5 . . ? H52A C52 H52B 107.5 . . ? C54 C53 C52 108.4(8) . . ? C54 C53 H53A 110 . . ? C52 C53 H53A 110 . . ? C54 C53 H53B 110 . . ? C52 C53 H53B 110 . . ? H53A C53 H53B 108.4 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N2 C55 C56 116.4(7) . . ? N2 C55 H55A 108.2 . . ? C56 C55 H55A 108.2 . . ? N2 C55 H55B 108.2 . . ? C56 C55 H55B 108.2 . . ? H55A C55 H55B 107.3 . . ? C55 C56 C57 109.1(7) . . ? C55 C56 H56A 109.9 . . ? C57 C56 H56A 109.9 . . ? C55 C56 H56B 109.9 . . ? C57 C56 H56B 109.9 . . ? H56A C56 H56B 108.3 . . ? C56 C57 C58 111.4(7) . . ? C56 C57 H57A 109.3 . . ? C58 C57 H57A 109.3 . . ? C56 C57 H57B 109.3 . . ? C58 C57 H57B 109.3 . . ? H57A C57 H57B 108 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? Cl1 C59 Cl2 111.7(5) . . ? Cl1 C59 H59A 109.3 . . ? Cl2 C59 H59A 109.3 . . ? Cl1 C59 H59B 109.3 . . ? Cl2 C59 H59B 109.3 . . ? H59A C59 H59B 107.9 . . ? C2 N1 C1 118.0(4) . . ? C2 N1 Pt1 123.2(4) . . ? C1 N1 Pt1 118.8(3) . . ? C51 N2 C43 111.2(8) . . ? C51 N2 C55 110.1(6) . . ? C43 N2 C55 107.8(7) . . ? C51 N2 C47 108.0(6) . . ? C43 N2 C47 107.8(6) . . ? C55 N2 C47 112.0(7) . . ? C20 O1 C24 116.8(6) . . ? C29 O2 C33 117.3(7) . . ? C38 O3 C42 117.3(7) . . ? C16 Pt1 C25 91.9(2) . . ? C16 Pt1 C34 89.6(2) . . ? C25 Pt1 C34 178.4(2) . . ? C16 Pt1 N1 178.51(19) . . ? C25 Pt1 N1 87.9(2) . . ? C34 Pt1 N1 90.6(2) . . ? #===END data_4 _audit_creation_date 2012-03-15T11:53:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common sr180 _chemical_formula_moiety 'C42 H38 N2 Pt2' _chemical_formula_sum 'C42 H38 N2 Pt2' _chemical_formula_weight 960.92 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7312(6) _cell_length_b 11.0656(6) _cell_length_c 16.4790(9) _cell_angle_alpha 82.168(3) _cell_angle_beta 74.397(2) _cell_angle_gamma 63.497(2) _cell_volume 1686.36(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6896 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.892 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.319 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9800 _exptl_absorpt_correction_T_max 1.0000 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.768974E-1 _diffrn_orient_matrix_ub_12 -0.883289E-1 _diffrn_orient_matrix_ub_13 -0.237364E-1 _diffrn_orient_matrix_ub_21 -0.24667E-1 _diffrn_orient_matrix_ub_22 0.278643E-1 _diffrn_orient_matrix_ub_23 -0.560711E-1 _diffrn_orient_matrix_ub_31 0.703834E-1 _diffrn_orient_matrix_ub_32 0.402814E-1 _diffrn_orient_matrix_ub_33 -0.162382E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_unetI/netI 0.03 _diffrn_reflns_number 6384 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25.68 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 6384 _reflns_number_gt 5516 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0378P)^2^+6.1078P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6384 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.667 _refine_diff_density_min -1.155 _refine_diff_density_rms 0.158 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pt2 Pt 0.70967(2) 0.99095(2) 0.270305(13) 0.02028(8) Uani 1 1 d . . . Pt1 Pt 0.51491(2) 1.28846(2) 0.233515(13) 0.02052(8) Uani 1 1 d . . . N1 N 0.3176(5) 1.3737(5) 0.1969(3) 0.0221(10) Uani 1 1 d . . . N2 N 0.7169(5) 0.8869(5) 0.3869(3) 0.0232(11) Uani 1 1 d . . . C1 C 0.4039(6) 1.4354(6) 0.3151(4) 0.0243(13) Uani 1 1 d . . . C2 C 0.4404(7) 1.4591(7) 0.3846(4) 0.0311(14) Uani 1 1 d . . . H2 H 0.5276 1.3993 0.3967 0.037 Uiso 1 1 calc R . . C3 C 0.3514(8) 1.5684(7) 0.4359(5) 0.0379(16) Uani 1 1 d . . . H3 H 0.3786 1.5799 0.4822 0.046 Uiso 1 1 calc R . . C4 C 0.2221(8) 1.6610(7) 0.4192(4) 0.0400(17) Uani 1 1 d . . . H4 H 0.1635 1.7356 0.4532 0.048 Uiso 1 1 calc R . . C5 C 0.1809(7) 1.6414(6) 0.3514(4) 0.0336(15) Uani 1 1 d . . . H5 H 0.0931 1.7018 0.3403 0.04 Uiso 1 1 calc R . . C6 C 0.2712(6) 1.5308(6) 0.2994(4) 0.0254(13) Uani 1 1 d . . . C7 C 0.2255(6) 1.4961(6) 0.2324(4) 0.0255(13) Uani 1 1 d . . . C8 C 0.0972(6) 1.5761(6) 0.2077(4) 0.0292(14) Uani 1 1 d . . . H8 H 0.039 1.6616 0.2301 0.035 Uiso 1 1 calc R . . C9 C 0.0571(7) 1.5310(7) 0.1518(4) 0.0335(15) Uani 1 1 d . . . H9 H -0.0259 1.5866 0.1337 0.04 Uiso 1 1 calc R . . C10 C 0.1417(7) 1.3990(7) 0.1210(4) 0.0304(14) Uani 1 1 d . . . C11 C 0.0996(7) 1.3406(7) 0.0684(4) 0.0355(16) Uani 1 1 d . . . H11 H 0.0157 1.3921 0.0504 0.043 Uiso 1 1 calc R . . C12 C 0.1794(8) 1.2109(8) 0.0439(4) 0.0413(18) Uani 1 1 d . . . H12 H 0.1503 1.174 0.0092 0.05 Uiso 1 1 calc R . . C13 C 0.3065(8) 1.1320(8) 0.0709(4) 0.0392(17) Uani 1 1 d . . . H13 H 0.3601 1.0425 0.0547 0.047 Uiso 1 1 calc R . . C14 C 0.3521(7) 1.1857(7) 0.1208(4) 0.0324(15) Uani 1 1 d . . . H14 H 0.4364 1.1328 0.1383 0.039 Uiso 1 1 calc R . . C15 C 0.6907(8) 0.5811(7) 0.2242(5) 0.0403(17) Uani 1 1 d . . . H15 H 0.6874 0.5005 0.2179 0.048 Uiso 1 1 calc R . . C16 C 0.6856(6) 1.2118(6) 0.2789(4) 0.0229(12) Uani 1 1 d . . . C17 C 0.8003(6) 1.1438(6) 0.2972(4) 0.0232(12) Uani 1 1 d . . . C18 C 0.9484(6) 1.1007(6) 0.3080(4) 0.0275(13) Uani 1 1 d . . . C19 C 1.0574(8) 1.0110(8) 0.2350(4) 0.0458(19) Uani 1 1 d . . . H19A H 1.1525 0.9832 0.2419 0.069 Uiso 1 1 calc R . . H19B H 1.0473 1.0606 0.1828 0.069 Uiso 1 1 calc R . . H19C H 1.0409 0.9327 0.2344 0.069 Uiso 1 1 calc R . . C20 C 0.9672(8) 1.2314(8) 0.3062(6) 0.051(2) Uani 1 1 d . . . H20A H 1.0611 1.2092 0.3132 0.076 Uiso 1 1 calc R . . H20B H 0.8963 1.2885 0.3511 0.076 Uiso 1 1 calc R . . H20C H 0.956 1.2779 0.2532 0.076 Uiso 1 1 calc R . . C21 C 0.9709(7) 1.0253(7) 0.3916(4) 0.0301(14) Uani 1 1 d . . . H21A H 1.0669 1.0001 0.3958 0.045 Uiso 1 1 calc R . . H21B H 0.9556 0.9457 0.394 0.045 Uiso 1 1 calc R . . H21C H 0.9042 1.0829 0.4374 0.045 Uiso 1 1 calc R . . C22 C 0.6993(6) 0.8268(6) 0.2423(4) 0.0232(12) Uani 1 1 d . . . C23 C 0.6659(6) 0.8036(6) 0.1720(4) 0.0299(14) Uani 1 1 d . . . H23 H 0.6462 0.8703 0.1302 0.036 Uiso 1 1 calc R . . C24 C 0.6612(7) 0.6832(7) 0.1625(4) 0.0367(16) Uani 1 1 d . . . H24 H 0.6383 0.6704 0.1148 0.044 Uiso 1 1 calc R . . C26 C 0.7249(7) 0.6013(6) 0.2943(4) 0.0346(15) Uani 1 1 d . . . H26 H 0.7439 0.534 0.3358 0.042 Uiso 1 1 calc R . . C27 C 0.7313(6) 0.7223(6) 0.3038(4) 0.0285(14) Uani 1 1 d . . . C28 C 0.7488(7) 0.7561(6) 0.3814(4) 0.0290(14) Uani 1 1 d . . . C29 C 0.7869(7) 0.6632(7) 0.4482(4) 0.0386(17) Uani 1 1 d . . . H29 H 0.8184 0.5714 0.4412 0.046 Uiso 1 1 calc R . . C30 C 0.7772(8) 0.7095(9) 0.5225(5) 0.0456(19) Uani 1 1 d . . . H30 H 0.8069 0.6485 0.5658 0.055 Uiso 1 1 calc R . . C31 C 0.7228(7) 0.8482(9) 0.5350(4) 0.0418(19) Uani 1 1 d . . . C32 C 0.6912(8) 0.9033(11) 0.6151(4) 0.051(2) Uani 1 1 d . . . H32 H 0.7109 0.8461 0.6615 0.061 Uiso 1 1 calc R . . C33 C 0.6320(8) 1.0402(11) 0.6242(4) 0.051(2) Uani 1 1 d . . . H33 H 0.6134 1.0755 0.6765 0.062 Uiso 1 1 calc R . . C34 C 0.5993(7) 1.1275(9) 0.5553(4) 0.0426(19) Uani 1 1 d . . . H34 H 0.5571 1.2204 0.5625 0.051 Uiso 1 1 calc R . . C35 C 0.6287(7) 1.0774(7) 0.4772(4) 0.0341(15) Uani 1 1 d . . . H35 H 0.6062 1.1368 0.432 0.041 Uiso 1 1 calc R . . C36 C 0.6925(6) 0.9376(7) 0.4647(4) 0.0297(14) Uani 1 1 d . . . C37 C 0.6876(6) 1.0864(6) 0.1618(4) 0.0219(12) Uani 1 1 d . . . C38 C 0.6735(6) 1.1696(6) 0.1047(4) 0.0262(13) Uani 1 1 d . . . C39 C 0.7040(6) 1.2467(6) 0.0260(4) 0.0248(13) Uani 1 1 d . . . C40 C 0.8430(9) 1.1528(7) -0.0306(5) 0.050(2) Uani 1 1 d . . . H40A H 0.8644 1.2 -0.0819 0.075 Uiso 1 1 calc R . . H40B H 0.8331 1.0759 -0.0435 0.075 Uiso 1 1 calc R . . H40C H 0.9194 1.123 -0.0023 0.075 Uiso 1 1 calc R . . C41 C 0.5847(8) 1.2978(8) -0.0206(5) 0.0466(19) Uani 1 1 d . . . H41A H 0.608 1.3464 -0.0707 0.07 Uiso 1 1 calc R . . H41B H 0.4964 1.3567 0.0151 0.07 Uiso 1 1 calc R . . H41C H 0.5743 1.2225 -0.0357 0.07 Uiso 1 1 calc R . . C42 C 0.7225(8) 1.3656(7) 0.0490(4) 0.0421(17) Uani 1 1 d . . . H42A H 0.7417 1.416 -0.0012 0.063 Uiso 1 1 calc R . . H42B H 0.8012 1.3327 0.0757 0.063 Uiso 1 1 calc R . . H42C H 0.6364 1.4232 0.0868 0.063 Uiso 1 1 calc R . . C150 C 0.2715(6) 1.3206(6) 0.1455(4) 0.0251(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt2 0.01952(13) 0.01826(12) 0.02240(12) 0.00244(9) -0.00618(9) -0.00762(10) Pt1 0.01780(13) 0.01822(12) 0.02454(13) 0.00058(9) -0.00686(9) -0.00608(10) N1 0.016(2) 0.017(2) 0.029(3) 0.002(2) -0.006(2) -0.004(2) N2 0.020(3) 0.030(3) 0.020(2) 0.007(2) -0.004(2) -0.014(2) C1 0.028(3) 0.017(3) 0.026(3) 0.001(2) -0.003(3) -0.011(3) C2 0.032(4) 0.029(3) 0.034(3) 0.001(3) -0.013(3) -0.012(3) C3 0.044(4) 0.028(4) 0.043(4) -0.009(3) -0.014(3) -0.012(3) C4 0.047(4) 0.026(4) 0.042(4) -0.008(3) -0.013(3) -0.007(3) C5 0.026(3) 0.023(3) 0.042(4) 0.001(3) -0.007(3) -0.003(3) C6 0.022(3) 0.024(3) 0.029(3) 0.001(3) -0.005(2) -0.009(3) C7 0.019(3) 0.023(3) 0.031(3) 0.000(3) -0.004(2) -0.007(3) C8 0.018(3) 0.023(3) 0.039(4) 0.003(3) -0.004(3) -0.004(3) C9 0.026(3) 0.037(4) 0.037(4) 0.008(3) -0.013(3) -0.012(3) C10 0.027(3) 0.044(4) 0.024(3) 0.010(3) -0.005(3) -0.022(3) C11 0.035(4) 0.047(4) 0.035(4) 0.012(3) -0.018(3) -0.025(3) C12 0.043(4) 0.067(5) 0.035(4) 0.005(4) -0.014(3) -0.041(4) C13 0.043(4) 0.043(4) 0.041(4) -0.005(3) -0.004(3) -0.028(4) C14 0.025(3) 0.036(4) 0.038(4) -0.004(3) -0.005(3) -0.015(3) C15 0.044(4) 0.032(4) 0.051(4) -0.009(3) -0.001(3) -0.025(4) C16 0.026(3) 0.017(3) 0.025(3) 0.002(2) -0.009(2) -0.007(3) C17 0.025(3) 0.018(3) 0.026(3) 0.000(2) -0.008(2) -0.007(3) C18 0.020(3) 0.028(3) 0.032(3) 0.001(3) -0.008(3) -0.008(3) C19 0.030(4) 0.062(5) 0.033(4) -0.005(4) 0.001(3) -0.014(4) C20 0.044(5) 0.042(4) 0.085(6) 0.017(4) -0.032(4) -0.029(4) C21 0.021(3) 0.032(4) 0.039(4) 0.002(3) -0.011(3) -0.011(3) C22 0.017(3) 0.021(3) 0.032(3) -0.002(2) -0.004(2) -0.009(2) C23 0.024(3) 0.027(3) 0.035(3) -0.001(3) -0.011(3) -0.006(3) C24 0.036(4) 0.035(4) 0.044(4) -0.008(3) -0.011(3) -0.017(3) C26 0.032(4) 0.022(3) 0.048(4) 0.003(3) -0.004(3) -0.014(3) C27 0.022(3) 0.027(3) 0.035(3) 0.003(3) -0.004(3) -0.011(3) C28 0.024(3) 0.032(4) 0.029(3) 0.009(3) -0.005(3) -0.014(3) C29 0.037(4) 0.036(4) 0.044(4) 0.021(3) -0.017(3) -0.019(3) C30 0.041(4) 0.064(5) 0.041(4) 0.030(4) -0.022(3) -0.032(4) C31 0.030(4) 0.077(6) 0.027(3) 0.014(4) -0.011(3) -0.032(4) C32 0.042(4) 0.103(7) 0.025(4) 0.013(4) -0.014(3) -0.045(5) C33 0.034(4) 0.107(8) 0.029(4) -0.013(4) 0.000(3) -0.044(5) C34 0.032(4) 0.073(5) 0.035(4) -0.018(4) 0.007(3) -0.036(4) C35 0.030(4) 0.045(4) 0.034(4) -0.006(3) -0.002(3) -0.025(3) C36 0.022(3) 0.047(4) 0.028(3) 0.003(3) -0.004(3) -0.024(3) C37 0.026(3) 0.019(3) 0.028(3) 0.004(2) -0.009(2) -0.016(3) C38 0.026(3) 0.026(3) 0.025(3) -0.001(3) -0.005(3) -0.010(3) C39 0.024(3) 0.019(3) 0.028(3) 0.006(2) -0.008(2) -0.007(3) C40 0.052(5) 0.036(4) 0.041(4) 0.000(3) 0.008(4) -0.010(4) C41 0.053(5) 0.054(5) 0.040(4) 0.025(4) -0.026(4) -0.028(4) C42 0.056(5) 0.034(4) 0.038(4) 0.007(3) -0.005(3) -0.026(4) C150 0.024(3) 0.029(3) 0.026(3) 0.004(3) -0.007(2) -0.015(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Pt2 C37 1.964(6) . ? Pt2 C22 1.990(6) . ? Pt2 N2 2.103(5) . ? Pt2 C16 2.361(6) . ? Pt2 C17 2.431(6) . ? Pt2 Pt1 3.0936(3) . ? Pt1 C16 1.952(6) . ? Pt1 C1 1.969(6) . ? Pt1 N1 2.119(5) . ? Pt1 C37 2.382(6) . ? Pt1 C38 2.440(6) . ? N1 C7 1.365(7) . ? N1 C150 1.388(7) . ? N2 C28 1.340(8) . ? N2 C36 1.383(8) . ? C1 C2 1.396(8) . ? C1 C6 1.410(8) . ? C2 C3 1.379(9) . ? C2 H2 0.93 . ? C3 C4 1.382(10) . ? C3 H3 0.93 . ? C4 C5 1.382(9) . ? C4 H4 0.93 . ? C5 C6 1.396(8) . ? C5 H5 0.93 . ? C6 C7 1.477(8) . ? C7 C8 1.401(8) . ? C8 C9 1.346(9) . ? C8 H8 0.93 . ? C9 C10 1.410(9) . ? C9 H9 0.93 . ? C10 C150 1.409(9) . ? C10 C11 1.413(9) . ? C11 C12 1.352(10) . ? C11 H11 0.93 . ? C12 C13 1.406(10) . ? C12 H12 0.93 . ? C13 C14 1.371(9) . ? C13 H13 0.93 . ? C14 C150 1.402(9) . ? C14 H14 0.93 . ? C15 C26 1.375(10) . ? C15 C24 1.396(10) . ? C15 H15 0.93 . ? C16 C17 1.218(8) . ? C17 C18 1.496(8) . ? C18 C21 1.528(9) . ? C18 C19 1.528(9) . ? C18 C20 1.543(9) . ? C19 H19A 0.96 . ? C19 H19B 0.96 . ? C19 H19C 0.96 . ? C20 H20A 0.96 . ? C20 H20B 0.96 . ? C20 H20C 0.96 . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C21 H21C 0.96 . ? C22 C23 1.387(8) . ? C22 C27 1.413(9) . ? C23 C24 1.386(9) . ? C23 H23 0.93 . ? C24 H24 0.93 . ? C26 C27 1.403(9) . ? C26 H26 0.93 . ? C27 C28 1.459(9) . ? C28 C29 1.413(9) . ? C29 C30 1.350(10) . ? C29 H29 0.93 . ? C30 C31 1.401(11) . ? C30 H30 0.93 . ? C31 C32 1.423(10) . ? C31 C36 1.424(9) . ? C32 C33 1.368(12) . ? C32 H32 0.93 . ? C33 C34 1.400(12) . ? C33 H33 0.93 . ? C34 C35 1.372(9) . ? C34 H34 0.93 . ? C35 C36 1.403(10) . ? C35 H35 0.93 . ? C37 C38 1.214(8) . ? C38 C39 1.494(8) . ? C39 C40 1.520(9) . ? C39 C41 1.522(9) . ? C39 C42 1.525(9) . ? C40 H40A 0.96 . ? C40 H40B 0.96 . ? C40 H40C 0.96 . ? C41 H41A 0.96 . ? C41 H41B 0.96 . ? C41 H41C 0.96 . ? C42 H42A 0.96 . ? C42 H42B 0.96 . ? C42 H42C 0.96 . ? 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 C37 Pt2 C22 96.9(2) . . ? C37 Pt2 N2 175.0(2) . . ? C22 Pt2 N2 80.1(2) . . ? C37 Pt2 C16 70.5(2) . . ? C22 Pt2 C16 165.5(2) . . ? N2 Pt2 C16 112.01(19) . . ? C37 Pt2 C17 87.6(2) . . ? C22 Pt2 C17 162.2(2) . . ? N2 Pt2 C17 96.50(19) . . ? C16 Pt2 C17 29.41(19) . . ? C37 Pt2 Pt1 50.36(17) . . ? C22 Pt2 Pt1 127.13(17) . . ? N2 Pt2 Pt1 128.69(14) . . ? C16 Pt2 Pt1 39.11(14) . . ? C17 Pt2 Pt1 68.38(14) . . ? C16 Pt1 C1 95.1(2) . . ? C16 Pt1 N1 174.3(2) . . ? C1 Pt1 N1 80.7(2) . . ? C16 Pt1 C37 70.2(2) . . ? C1 Pt1 C37 164.6(2) . . ? N1 Pt1 C37 113.64(19) . . ? C16 Pt1 C38 86.0(2) . . ? C1 Pt1 C38 159.6(2) . . ? N1 Pt1 C38 99.31(19) . . ? C37 Pt1 C38 29.12(19) . . ? C16 Pt1 Pt2 49.72(17) . . ? C1 Pt1 Pt2 127.04(17) . . ? N1 Pt1 Pt2 130.33(13) . . ? C37 Pt1 Pt2 39.42(14) . . ? C38 Pt1 Pt2 68.22(14) . . ? C7 N1 C150 118.3(5) . . ? C7 N1 Pt1 112.6(4) . . ? C150 N1 Pt1 129.1(4) . . ? C28 N2 C36 119.0(5) . . ? C28 N2 Pt2 113.0(4) . . ? C36 N2 Pt2 127.9(4) . . ? C2 C1 C6 116.2(5) . . ? C2 C1 Pt1 128.8(5) . . ? C6 C1 Pt1 115.0(4) . . ? C3 C2 C1 122.1(6) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? C2 C3 C4 120.8(6) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 119.2(6) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 119.9(6) . . ? C4 C5 H5 120 . . ? C6 C5 H5 120 . . ? C5 C6 C1 121.8(6) . . ? C5 C6 C7 122.1(6) . . ? C1 C6 C7 115.7(5) . . ? N1 C7 C8 121.0(6) . . ? N1 C7 C6 114.2(5) . . ? C8 C7 C6 124.7(5) . . ? C9 C8 C7 120.9(6) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 119.6(6) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C150 C10 C9 118.7(6) . . ? C150 C10 C11 118.6(6) . . ? C9 C10 C11 122.7(6) . . ? C12 C11 C10 121.1(6) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 120.0(6) . . ? C11 C12 H12 120 . . ? C13 C12 H12 120 . . ? C14 C13 C12 120.7(7) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C150 119.9(6) . . ? C13 C14 H14 120.1 . . ? C150 C14 H14 120.1 . . ? C26 C15 C24 119.2(6) . . ? C26 C15 H15 120.4 . . ? C24 C15 H15 120.4 . . ? C17 C16 Pt1 167.6(5) . . ? C17 C16 Pt2 78.5(4) . . ? Pt1 C16 Pt2 91.2(2) . . ? C16 C17 C18 161.1(6) . . ? C16 C17 Pt2 72.1(4) . . ? C18 C17 Pt2 124.5(4) . . ? C17 C18 C21 112.5(5) . . ? C17 C18 C19 109.4(5) . . ? C21 C18 C19 109.6(5) . . ? C17 C18 C20 106.1(5) . . ? C21 C18 C20 109.1(6) . . ? C19 C18 C20 110.0(6) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C27 117.8(5) . . ? C23 C22 Pt2 128.7(5) . . ? C27 C22 Pt2 113.5(4) . . ? C24 C23 C22 121.6(6) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C23 C24 C15 120.4(6) . . ? C23 C24 H24 119.8 . . ? C15 C24 H24 119.8 . . ? C15 C26 C27 120.7(6) . . ? C15 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C26 C27 C22 120.3(6) . . ? C26 C27 C28 122.9(6) . . ? C22 C27 C28 116.1(5) . . ? N2 C28 C29 121.6(6) . . ? N2 C28 C27 114.2(5) . . ? C29 C28 C27 124.1(6) . . ? C30 C29 C28 119.2(7) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C29 C30 C31 120.7(6) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C30 C31 C32 122.9(7) . . ? C30 C31 C36 118.1(7) . . ? C32 C31 C36 119.0(8) . . ? C33 C32 C31 120.2(7) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C34 120.4(7) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C35 C34 C33 120.7(8) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 120.7(7) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? N2 C36 C35 120.8(6) . . ? N2 C36 C31 120.1(6) . . ? C35 C36 C31 119.0(6) . . ? C38 C37 Pt2 164.4(5) . . ? C38 C37 Pt1 78.1(4) . . ? Pt2 C37 Pt1 90.2(2) . . ? C37 C38 C39 162.6(6) . . ? C37 C38 Pt1 72.8(4) . . ? C39 C38 Pt1 120.4(4) . . ? C38 C39 C40 108.0(5) . . ? C38 C39 C41 111.8(5) . . ? C40 C39 C41 109.2(6) . . ? C38 C39 C42 109.0(5) . . ? C40 C39 C42 109.1(6) . . ? C41 C39 C42 109.7(5) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N1 C150 C14 119.5(5) . . ? N1 C150 C10 120.7(6) . . ? C14 C150 C10 119.7(6) . . ? #===END data_5 _audit_creation_date 2013-10-07T13:44:33-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Compound X' _chemical_formula_moiety 'C48 H34 N2 Pt2, 3(C1 H2 Cl2)' _chemical_formula_sum 'C51 H40 Cl6 N2 Pt2' _chemical_formula_weight 1283.73 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 16.7730(6) _cell_length_b 13.8680(3) _cell_length_c 20.4720(8) _cell_angle_alpha 90 _cell_angle_beta 103.4290(10) _cell_angle_gamma 90 _cell_volume 4631.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10331 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.841 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2472 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.418 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9800 _exptl_absorpt_correction_T_max 1.0000 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.11753E-2 _diffrn_orient_matrix_ub_12 0.212653E-1 _diffrn_orient_matrix_ub_13 0.464412E-1 _diffrn_orient_matrix_ub_21 0.610594E-1 _diffrn_orient_matrix_ub_22 -0.54719E-2 _diffrn_orient_matrix_ub_23 0.137394E-1 _diffrn_orient_matrix_ub_31 0.52284E-2 _diffrn_orient_matrix_ub_32 0.686828E-1 _diffrn_orient_matrix_ub_33 -0.132843E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_unetI/netI 0.0434 _diffrn_reflns_number 10493 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 10493 _reflns_number_gt 8432 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0617P)^2^+44.7252P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10493 _refine_ls_number_parameters 569 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.1019 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 0.831 _refine_ls_restrained_S_all 0.843 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.849 _refine_diff_density_min -0.754 _refine_diff_density_rms 0.146 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Pt Pt -1.7033 8.3905 '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' 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 0.600014(14) 0.469980(16) 0.362256(11) 0.02092(7) Uani 1 1 d . . . Pt2 Pt 0.737886(14) 0.304743(16) 0.387369(11) 0.02136(7) Uani 1 1 d . . . C1 C 0.4967(4) 0.4697(5) 0.2916(3) 0.0273(13) Uani 1 1 d . . . C2 C 0.4461(4) 0.3905(5) 0.2676(3) 0.0300(14) Uani 1 1 d . . . H14 H 0.463 0.3288 0.2824 0.036 Uiso 1 1 calc R . . C3 C 0.3717(4) 0.4027(6) 0.2222(4) 0.0382(17) Uani 1 1 d . . . H13 H 0.3389 0.3492 0.2077 0.046 Uiso 1 1 calc R . . C4 C 0.3454(5) 0.4926(6) 0.1979(4) 0.0439(19) Uani 1 1 d . . . H12 H 0.2956 0.4999 0.1669 0.053 Uiso 1 1 calc R . . C5 C 0.3937(4) 0.5716(5) 0.2203(4) 0.0351(16) Uani 1 1 d . . . H11 H 0.3763 0.6325 0.2039 0.042 Uiso 1 1 calc R . . C6 C 0.4686(4) 0.5618(5) 0.2674(3) 0.0271(13) Uani 1 1 d . . . C7 C 0.5244(4) 0.6420(5) 0.2919(3) 0.0281(14) Uani 1 1 d . . . C8 C 0.5060(5) 0.7378(5) 0.2731(4) 0.0376(17) Uani 1 1 d . . . H8 H 0.455 0.7534 0.246 0.045 Uiso 1 1 calc R . . C9 C 0.5621(5) 0.8082(5) 0.2941(4) 0.0392(17) Uani 1 1 d . . . H7 H 0.5488 0.8723 0.2835 0.047 Uiso 1 1 calc R . . C10 C 0.6413(5) 0.7836(5) 0.3324(3) 0.0321(15) Uani 1 1 d . . . C11 C 0.7042(5) 0.8531(5) 0.3531(4) 0.0382(17) Uani 1 1 d . . . H5 H 0.6929 0.9182 0.3447 0.046 Uiso 1 1 calc R . . C12 C 0.7805(5) 0.8254(5) 0.3850(4) 0.0415(18) Uani 1 1 d . . . H4 H 0.821 0.8716 0.3991 0.05 Uiso 1 1 calc R . . C13 C 0.7993(5) 0.7267(5) 0.3970(4) 0.0373(17) Uani 1 1 d . . . H3 H 0.8528 0.7079 0.4165 0.045 Uiso 1 1 calc R . . C14 C 0.7385(4) 0.6583(5) 0.3799(3) 0.0287(14) Uani 1 1 d . . . H2 H 0.751 0.5936 0.389 0.034 Uiso 1 1 calc R . . C15 C 0.6577(4) 0.6852(4) 0.3490(3) 0.0262(13) Uani 1 1 d . . . C16 C 0.5961(4) 0.3313(4) 0.3780(3) 0.0242(13) Uani 1 1 d . . . C17 C 0.6072(4) 0.2457(5) 0.3903(3) 0.0247(13) Uani 1 1 d . . . C18 C 0.5991(4) 0.1451(4) 0.4076(3) 0.0252(13) Uani 1 1 d . . . C19 C 0.5272(4) 0.0952(5) 0.3809(4) 0.0326(15) Uani 1 1 d . . . H19 H 0.4856 0.125 0.3494 0.039 Uiso 1 1 calc R . . C20 C 0.5166(5) 0.0013(5) 0.4007(4) 0.0415(18) Uani 1 1 d . . . H20 H 0.4676 -0.0307 0.383 0.05 Uiso 1 1 calc R . . C21 C 0.5786(5) -0.0459(5) 0.4470(4) 0.0354(16) Uani 1 1 d . . . C22 C 0.6508(5) 0.0039(5) 0.4716(4) 0.0403(18) Uani 1 1 d . . . H22 H 0.6933 -0.0265 0.5019 0.048 Uiso 1 1 calc R . . C23 C 0.6611(4) 0.0975(5) 0.4524(4) 0.0330(15) Uani 1 1 d . . . H23 H 0.7104 0.129 0.4697 0.04 Uiso 1 1 calc R . . C24 C 0.5660(6) -0.1476(6) 0.4696(5) 0.055(2) Uani 1 1 d . . . H24A H 0.5127 -0.1701 0.4468 0.083 Uiso 1 1 calc R . . H24B H 0.5702 -0.148 0.5172 0.083 Uiso 1 1 calc R . . H24C H 0.6072 -0.1892 0.4593 0.083 Uiso 1 1 calc R . . C25 C 0.8604(4) 0.3050(5) 0.4105(3) 0.0267(14) Uani 1 1 d . . . C26 C 0.9128(4) 0.3683(5) 0.4516(4) 0.0330(15) Uani 1 1 d . . . H38 H 0.8914 0.423 0.4675 0.04 Uiso 1 1 calc R . . C27 C 0.9971(5) 0.3522(6) 0.4698(4) 0.0405(17) Uani 1 1 d . . . H37 H 1.0314 0.3964 0.4969 0.049 Uiso 1 1 calc R . . C28 C 1.0295(4) 0.2699(6) 0.4474(4) 0.0402(18) Uani 1 1 d . . . H36 H 1.0856 0.2585 0.4598 0.048 Uiso 1 1 calc R . . C29 C 0.9787(4) 0.2049(5) 0.4068(4) 0.0365(16) Uani 1 1 d . . . H35 H 1.0007 0.1498 0.392 0.044 Uiso 1 1 calc R . . C30 C 0.8943(4) 0.2218(5) 0.3878(3) 0.0274(14) Uani 1 1 d . . . C31 C 0.8361(4) 0.1572(5) 0.3430(3) 0.0280(14) Uani 1 1 d . . . C32 C 0.8589(5) 0.0701(5) 0.3166(4) 0.0335(15) Uani 1 1 d . . . H32 H 0.9131 0.0494 0.3278 0.04 Uiso 1 1 calc R . . C33 C 0.8006(5) 0.0169(5) 0.2745(4) 0.0365(17) Uani 1 1 d . . . H31 H 0.8138 -0.0435 0.2603 0.044 Uiso 1 1 calc R . . C34 C 0.7210(5) 0.0527(5) 0.2525(3) 0.0321(15) Uani 1 1 d . . . C35 C 0.6589(6) 0.0042(6) 0.2056(4) 0.0435(19) Uani 1 1 d . . . H29 H 0.6698 -0.0563 0.1901 0.052 Uiso 1 1 calc R . . C36 C 0.5827(5) 0.0448(6) 0.1824(4) 0.045(2) Uani 1 1 d . . . H28 H 0.5423 0.0117 0.1518 0.054 Uiso 1 1 calc R . . C37 C 0.5666(5) 0.1354(6) 0.2049(4) 0.0413(18) Uani 1 1 d . . . H27 H 0.5157 0.1636 0.1878 0.05 Uiso 1 1 calc R . . C38 C 0.6238(4) 0.1844(5) 0.2514(3) 0.0313(15) Uani 1 1 d . . . H26 H 0.6117 0.2453 0.2655 0.038 Uiso 1 1 calc R . . C39 C 0.7016(4) 0.1423(5) 0.2783(3) 0.0270(13) Uani 1 1 d . . . C40 C 0.7242(4) 0.4201(4) 0.4380(3) 0.0239(13) Uani 1 1 d . . . C41 C 0.6992(4) 0.4896(4) 0.4655(3) 0.0268(14) Uani 1 1 d . . . C42 C 0.6952(4) 0.5646(4) 0.5132(3) 0.0224(12) Uani 1 1 d . . . C43 C 0.7677(4) 0.6100(5) 0.5476(3) 0.0286(14) Uani 1 1 d . . . H43 H 0.8176 0.5933 0.5383 0.034 Uiso 1 1 calc R . . C44 C 0.7645(4) 0.6794(5) 0.5952(4) 0.0346(16) Uani 1 1 d . . . H44 H 0.8128 0.7094 0.6174 0.042 Uiso 1 1 calc R . . C45 C 0.6915(4) 0.7053(5) 0.6106(3) 0.0290(14) Uani 1 1 d . . . C46 C 0.6203(4) 0.6611(5) 0.5771(3) 0.0307(14) Uani 1 1 d . . . H46 H 0.5709 0.6774 0.5875 0.037 Uiso 1 1 calc R . . C47 C 0.6213(4) 0.5924(5) 0.5279(3) 0.0287(14) Uani 1 1 d . . . H47 H 0.5724 0.5648 0.5045 0.034 Uiso 1 1 calc R . . C48 C 0.6906(5) 0.7816(6) 0.6639(4) 0.047(2) Uani 1 1 d . . . H48A H 0.7454 0.8045 0.6817 0.071 Uiso 1 1 calc R . . H48B H 0.6695 0.7541 0.6995 0.071 Uiso 1 1 calc R . . H48C H 0.6564 0.8345 0.6442 0.071 Uiso 1 1 calc R . . C49 C 0.2125(6) 0.5475(7) 0.3173(5) 0.061(3) Uani 1 1 d . . . H49A H 0.2522 0.5047 0.3449 0.073 Uiso 1 1 calc R . . H49B H 0.2419 0.591 0.2941 0.073 Uiso 1 1 calc R . . C51 C 0.3619(5) 0.7241(6) 0.4380(4) 0.0455(19) Uani 1 1 d . . . H51A H 0.3162 0.6998 0.4546 0.055 Uiso 1 1 calc R . . H51B H 0.3999 0.7551 0.475 0.055 Uiso 1 1 calc R . . N1 N 0.5970(3) 0.6156(3) 0.3321(2) 0.0217(10) Uani 1 1 d . . . N2 N 0.7585(3) 0.1899(4) 0.3274(3) 0.0238(11) Uani 1 1 d . . . Cl1 Cl 0.1426(2) 0.4792(3) 0.25781(15) 0.0940(10) Uani 1 1 d . . . Cl2 Cl 0.16275(17) 0.6149(2) 0.36907(18) 0.0864(9) Uani 1 1 d . . . Cl5 Cl 0.41088(14) 0.62839(15) 0.40836(11) 0.0520(5) Uani 1 1 d . . . Cl6 Cl 0.32591(16) 0.80958(18) 0.37372(13) 0.0677(7) Uani 1 1 d . . . C50A C 0.4037(6) 0.3675(7) 0.0551(4) 0.054(2) Uani 0.5 1 d P A 1 H50A H 0.3902 0.3143 0.0237 0.065 Uiso 0.5 1 calc PRD A 1 H50B H 0.3638 0.3668 0.0826 0.065 Uiso 0.5 1 calc PR A 1 Cl3A Cl 0.3888(10) 0.4728(9) 0.0086(6) 0.0522(19) Uani 0.5 1 d PD A 1 Cl4A Cl 0.4975(10) 0.3432(7) 0.1068(8) 0.064(3) Uani 0.5 1 d PD A 1 C50B C 0.4037(6) 0.3675(7) 0.0551(4) 0.054(2) Uani 0.5 1 d P B 2 H50C H 0.3667 0.3467 0.0824 0.065 Uiso 0.5 1 calc PR B 2 H50D H 0.3996 0.3228 0.018 0.065 Uiso 0.5 1 calc PR B 2 Cl3B Cl 0.3794(10) 0.4893(10) 0.0244(6) 0.061(2) Uani 0.5 1 d PD B 2 Cl4B Cl 0.5064(9) 0.3738(6) 0.1041(7) 0.0480(18) Uani 0.5 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02026(12) 0.01807(12) 0.02369(12) -0.00078(9) 0.00360(9) 0.00031(9) Pt2 0.02012(12) 0.01780(12) 0.02538(12) 0.00013(9) 0.00370(9) -0.00028(9) C1 0.024(3) 0.031(3) 0.026(3) -0.001(3) 0.003(3) 0.005(3) C2 0.027(4) 0.027(3) 0.033(3) -0.004(3) 0.000(3) -0.004(3) C3 0.029(4) 0.047(4) 0.034(4) -0.002(3) -0.001(3) -0.015(3) C4 0.028(4) 0.054(5) 0.043(4) -0.001(4) -0.007(3) 0.000(3) C5 0.020(3) 0.039(4) 0.042(4) 0.002(3) 0.000(3) 0.009(3) C6 0.020(3) 0.033(3) 0.028(3) 0.002(3) 0.005(3) 0.006(3) C7 0.026(3) 0.030(3) 0.031(3) 0.003(3) 0.011(3) 0.004(3) C8 0.034(4) 0.035(4) 0.045(4) 0.008(3) 0.010(3) 0.009(3) C9 0.047(5) 0.025(4) 0.048(4) 0.007(3) 0.017(4) 0.011(3) C10 0.043(4) 0.020(3) 0.036(4) 0.002(3) 0.014(3) 0.000(3) C11 0.045(5) 0.026(4) 0.050(4) 0.002(3) 0.025(4) -0.010(3) C12 0.043(5) 0.036(4) 0.047(4) -0.007(3) 0.015(4) -0.017(3) C13 0.040(4) 0.039(4) 0.032(4) -0.003(3) 0.008(3) -0.011(3) C14 0.029(4) 0.032(4) 0.027(3) 0.001(3) 0.011(3) -0.002(3) C15 0.029(3) 0.022(3) 0.030(3) -0.001(2) 0.011(3) -0.007(3) C16 0.020(3) 0.022(3) 0.029(3) -0.002(2) 0.002(3) -0.001(2) C17 0.024(3) 0.025(3) 0.027(3) -0.002(3) 0.009(3) -0.003(3) C18 0.029(3) 0.022(3) 0.028(3) -0.001(2) 0.011(3) -0.004(3) C19 0.027(4) 0.030(3) 0.042(4) 0.004(3) 0.010(3) -0.005(3) C20 0.041(5) 0.033(4) 0.050(4) -0.002(3) 0.010(4) -0.014(3) C21 0.051(5) 0.019(3) 0.041(4) 0.004(3) 0.019(3) -0.003(3) C22 0.045(5) 0.027(4) 0.045(4) 0.007(3) 0.004(4) 0.001(3) C23 0.031(4) 0.027(3) 0.038(4) 0.003(3) 0.003(3) 0.002(3) C24 0.082(7) 0.028(4) 0.059(5) 0.009(4) 0.025(5) -0.015(4) C25 0.020(3) 0.029(3) 0.030(3) 0.014(3) 0.005(3) 0.000(3) C26 0.024(3) 0.028(3) 0.044(4) 0.004(3) 0.001(3) -0.003(3) C27 0.033(4) 0.039(4) 0.045(4) -0.001(3) 0.000(3) -0.010(3) C28 0.021(4) 0.055(5) 0.042(4) 0.008(4) 0.003(3) 0.000(3) C29 0.026(4) 0.041(4) 0.044(4) 0.006(3) 0.010(3) 0.006(3) C30 0.025(3) 0.030(3) 0.029(3) 0.006(3) 0.010(3) 0.003(3) C31 0.029(4) 0.027(3) 0.032(3) 0.005(3) 0.014(3) 0.001(3) C32 0.040(4) 0.026(3) 0.039(4) 0.002(3) 0.018(3) 0.007(3) C33 0.057(5) 0.023(3) 0.039(4) 0.001(3) 0.031(4) 0.007(3) C34 0.045(4) 0.028(3) 0.027(3) -0.006(3) 0.017(3) -0.005(3) C35 0.065(6) 0.036(4) 0.032(4) -0.008(3) 0.017(4) -0.013(4) C36 0.049(5) 0.048(5) 0.037(4) -0.017(3) 0.007(4) -0.017(4) C37 0.036(4) 0.053(5) 0.034(4) -0.008(3) 0.007(3) -0.007(4) C38 0.029(4) 0.035(4) 0.030(3) -0.003(3) 0.007(3) 0.000(3) C39 0.031(4) 0.029(3) 0.022(3) -0.002(3) 0.010(3) 0.000(3) C40 0.018(3) 0.021(3) 0.032(3) -0.001(2) 0.003(2) 0.000(2) C41 0.029(3) 0.019(3) 0.031(3) 0.002(2) 0.004(3) -0.002(3) C42 0.021(3) 0.020(3) 0.026(3) 0.003(2) 0.005(2) -0.004(2) C43 0.020(3) 0.033(4) 0.033(3) -0.005(3) 0.007(3) -0.002(3) C44 0.029(4) 0.033(4) 0.041(4) -0.009(3) 0.008(3) -0.014(3) C45 0.030(4) 0.027(3) 0.030(3) -0.007(3) 0.006(3) -0.005(3) C46 0.030(4) 0.027(3) 0.034(4) -0.002(3) 0.006(3) 0.003(3) C47 0.025(3) 0.029(3) 0.030(3) 0.000(3) 0.003(3) -0.001(3) C48 0.053(5) 0.039(4) 0.053(5) -0.023(4) 0.020(4) -0.010(4) C49 0.050(6) 0.075(7) 0.051(5) 0.015(5) -0.003(4) -0.014(5) C51 0.050(5) 0.050(5) 0.036(4) 0.004(3) 0.010(4) 0.005(4) N1 0.023(3) 0.018(2) 0.024(2) 0.005(2) 0.005(2) 0.002(2) N2 0.027(3) 0.020(3) 0.028(3) -0.002(2) 0.013(2) 0.001(2) Cl1 0.083(2) 0.124(3) 0.0592(16) -0.0042(16) -0.0156(15) -0.0339(19) Cl2 0.0535(16) 0.0747(19) 0.119(3) -0.0095(17) -0.0037(16) 0.0064(13) Cl5 0.0552(13) 0.0446(11) 0.0606(13) -0.0010(10) 0.0223(10) 0.0033(10) Cl6 0.0602(15) 0.0589(14) 0.0718(15) 0.0198(12) -0.0095(12) 0.0067(11) C50A 0.056(6) 0.060(6) 0.046(5) -0.007(4) 0.009(4) -0.007(5) Cl3A 0.069(5) 0.044(4) 0.044(4) -0.011(3) 0.014(3) 0.017(3) Cl4A 0.063(6) 0.056(6) 0.075(4) 0.019(6) 0.018(4) 0.012(5) C50B 0.056(6) 0.060(6) 0.046(5) -0.007(4) 0.009(4) -0.007(5) Cl3B 0.065(5) 0.061(6) 0.059(6) -0.009(4) 0.015(4) 0.011(4) Cl4B 0.044(3) 0.042(5) 0.055(4) 0.006(4) 0.005(2) -0.005(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C16 1.953(6) . ? Pt1 C1 1.983(6) . ? Pt1 N1 2.109(5) . ? Pt1 C41 2.382(6) . ? Pt1 C40 2.393(6) . ? Pt1 Pt2 3.2111(3) . ? Pt2 C40 1.948(6) . ? Pt2 C25 1.999(6) . ? Pt2 N2 2.088(5) . ? Pt2 C17 2.353(6) . ? Pt2 C16 2.370(6) . ? C1 C6 1.412(9) . ? C1 C2 1.405(9) . ? C2 C3 1.382(9) . ? C2 H14 0.93 . ? C3 C4 1.377(11) . ? C3 H13 0.93 . ? C4 C5 1.375(11) . ? C4 H12 0.93 . ? C5 C6 1.402(9) . ? C5 H11 0.93 . ? C6 C7 1.464(9) . ? C7 N1 1.352(8) . ? C7 C8 1.399(10) . ? C8 C9 1.356(11) . ? C8 H8 0.93 . ? C9 C10 1.417(11) . ? C9 H7 0.93 . ? C10 C11 1.420(10) . ? C10 C15 1.419(9) . ? C11 C12 1.350(11) . ? C11 H5 0.93 . ? C12 C13 1.413(11) . ? C12 H4 0.93 . ? C13 C14 1.377(10) . ? C13 H3 0.93 . ? C14 C15 1.406(9) . ? C14 H2 0.93 . ? C15 N1 1.387(8) . ? C16 C17 1.219(9) . ? C17 C18 1.454(9) . ? C18 C23 1.383(9) . ? C18 C19 1.389(9) . ? C19 C20 1.387(10) . ? C19 H19 0.93 . ? C20 C21 1.396(11) . ? C20 H20 0.93 . ? C21 C22 1.383(11) . ? C21 C24 1.515(9) . ? C22 C23 1.379(10) . ? C22 H22 0.93 . ? C23 H23 0.93 . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C25 C26 1.382(9) . ? C25 C30 1.412(9) . ? C26 C27 1.393(10) . ? C26 H38 0.93 . ? C27 C28 1.388(11) . ? C27 H37 0.93 . ? C28 C29 1.378(11) . ? C28 H36 0.93 . ? C29 C30 1.398(9) . ? C29 H35 0.93 . ? C30 C31 1.477(9) . ? C31 N2 1.345(8) . ? C31 C32 1.412(9) . ? C32 C33 1.361(11) . ? C32 H32 0.93 . ? C33 C34 1.397(11) . ? C33 H31 0.93 . ? C34 C35 1.412(10) . ? C34 C39 1.418(9) . ? C35 C36 1.377(12) . ? C35 H29 0.93 . ? C36 C37 1.386(11) . ? C36 H28 0.93 . ? C37 C38 1.365(10) . ? C37 H27 0.93 . ? C38 C39 1.419(9) . ? C38 H26 0.93 . ? C39 N2 1.383(8) . ? C40 C41 1.239(9) . ? C41 C42 1.438(9) . ? C42 C43 1.405(9) . ? C42 C47 1.396(9) . ? C43 C44 1.379(9) . ? C43 H43 0.93 . ? C44 C45 1.382(10) . ? C44 H44 0.93 . ? C45 C46 1.375(9) . ? C45 C48 1.523(9) . ? C46 C47 1.390(9) . ? C46 H46 0.93 . ? C47 H47 0.93 . ? C48 H48A 0.96 . ? C48 H48B 0.96 . ? C48 H48C 0.96 . ? C49 Cl2 1.762(11) . ? C49 Cl1 1.758(9) . ? C49 H49A 0.97 . ? C49 H49B 0.97 . ? C51 Cl6 1.769(8) . ? C51 Cl5 1.742(8) . ? C51 H51A 0.97 . ? C51 H51B 0.97 . ? C50A Cl3A 1.729(17) . ? C50A Cl4A 1.714(19) . ? C50A H50A 0.97 . ? C50A H50B 0.97 . ? 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 C16 Pt1 C1 93.5(3) . . ? C16 Pt1 N1 172.5(2) . . ? C1 Pt1 N1 80.3(2) . . ? C16 Pt1 C41 90.5(2) . . ? C1 Pt1 C41 163.6(2) . . ? N1 Pt1 C41 96.6(2) . . ? C16 Pt1 C40 70.5(2) . . ? C1 Pt1 C40 162.6(2) . . ? N1 Pt1 C40 115.1(2) . . ? C41 Pt1 C40 30.1(2) . . ? C16 Pt1 Pt2 47.28(18) . . ? C1 Pt1 Pt2 126.17(18) . . ? N1 Pt1 Pt2 134.24(14) . . ? C41 Pt1 Pt2 67.12(16) . . ? C40 Pt1 Pt2 37.20(15) . . ? C40 Pt2 C25 96.5(3) . . ? C40 Pt2 N2 174.3(2) . . ? C25 Pt2 N2 80.7(2) . . ? C40 Pt2 C17 92.7(2) . . ? C25 Pt2 C17 155.1(2) . . ? N2 Pt2 C17 91.8(2) . . ? C40 Pt2 C16 71.1(2) . . ? C25 Pt2 C16 167.5(2) . . ? N2 Pt2 C16 111.8(2) . . ? C17 Pt2 C16 29.9(2) . . ? C40 Pt2 Pt1 47.95(18) . . ? C25 Pt2 Pt1 134.36(18) . . ? N2 Pt2 Pt1 131.42(15) . . ? C17 Pt2 Pt1 67.17(16) . . ? C16 Pt2 Pt1 37.27(15) . . ? C6 C1 C2 117.4(6) . . ? C6 C1 Pt1 114.7(5) . . ? C2 C1 Pt1 127.7(5) . . ? C1 C2 C3 121.1(6) . . ? C1 C2 H14 119.4 . . ? C3 C2 H14 119.4 . . ? C4 C3 C2 121.1(7) . . ? C4 C3 H13 119.4 . . ? C2 C3 H13 119.4 . . ? C3 C4 C5 119.1(7) . . ? C3 C4 H12 120.4 . . ? C5 C4 H12 120.4 . . ? C4 C5 C6 121.1(7) . . ? C4 C5 H11 119.5 . . ? C6 C5 H11 119.5 . . ? C1 C6 C5 120.1(6) . . ? C1 C6 C7 115.6(6) . . ? C5 C6 C7 124.2(6) . . ? N1 C7 C8 122.4(6) . . ? N1 C7 C6 114.6(6) . . ? C8 C7 C6 123.0(6) . . ? C9 C8 C7 120.3(7) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 119.7(6) . . ? C8 C9 H7 120.2 . . ? C10 C9 H7 120.2 . . ? C9 C10 C11 122.5(6) . . ? C9 C10 C15 118.0(6) . . ? C11 C10 C15 119.5(7) . . ? C12 C11 C10 120.4(7) . . ? C12 C11 H5 119.8 . . ? C10 C11 H5 119.8 . . ? C11 C12 C13 120.6(7) . . ? C11 C12 H4 119.7 . . ? C13 C12 H4 119.7 . . ? C14 C13 C12 120.0(7) . . ? C14 C13 H3 120 . . ? C12 C13 H3 120 . . ? C13 C14 C15 120.7(7) . . ? C13 C14 H2 119.6 . . ? C15 C14 H2 119.6 . . ? N1 C15 C14 120.2(6) . . ? N1 C15 C10 121.3(6) . . ? C14 C15 C10 118.5(6) . . ? C17 C16 Pt1 169.6(5) . . ? C17 C16 Pt2 74.3(4) . . ? Pt1 C16 Pt2 95.5(2) . . ? C16 C17 C18 165.1(7) . . ? C16 C17 Pt2 75.8(4) . . ? C18 C17 Pt2 118.7(4) . . ? C23 C18 C19 118.2(6) . . ? C23 C18 C17 121.4(6) . . ? C19 C18 C17 120.3(6) . . ? C20 C19 C18 120.7(7) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 120.9(7) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 117.7(6) . . ? C22 C21 C24 121.7(7) . . ? C20 C21 C24 120.6(7) . . ? C23 C22 C21 121.5(7) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C22 C23 C18 121.0(7) . . ? C22 C23 H23 119.5 . . ? C18 C23 H23 119.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 118.2(6) . . ? C26 C25 Pt2 128.2(5) . . ? C30 C25 Pt2 113.0(5) . . ? C27 C26 C25 121.6(7) . . ? C27 C26 H38 119.2 . . ? C25 C26 H38 119.2 . . ? C28 C27 C26 119.6(7) . . ? C28 C27 H37 120.2 . . ? C26 C27 H37 120.2 . . ? C27 C28 C29 120.2(7) . . ? C27 C28 H36 119.9 . . ? C29 C28 H36 119.9 . . ? C30 C29 C28 120.1(7) . . ? C30 C29 H35 119.9 . . ? C28 C29 H35 119.9 . . ? C29 C30 C25 120.3(6) . . ? C29 C30 C31 123.5(6) . . ? C25 C30 C31 116.2(6) . . ? N2 C31 C32 122.1(6) . . ? N2 C31 C30 114.0(6) . . ? C32 C31 C30 123.9(6) . . ? C33 C32 C31 119.2(7) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C32 C33 C34 120.3(6) . . ? C32 C33 H31 119.9 . . ? C34 C33 H31 119.9 . . ? C33 C34 C35 123.3(7) . . ? C33 C34 C39 118.4(6) . . ? C35 C34 C39 118.3(7) . . ? C36 C35 C34 121.3(7) . . ? C36 C35 H29 119.4 . . ? C34 C35 H29 119.4 . . ? C35 C36 C37 119.5(7) . . ? C35 C36 H28 120.2 . . ? C37 C36 H28 120.2 . . ? C38 C37 C36 121.6(8) . . ? C38 C37 H27 119.2 . . ? C36 C37 H27 119.2 . . ? C37 C38 C39 120.0(7) . . ? C37 C38 H26 120 . . ? C39 C38 H26 120 . . ? N2 C39 C38 120.2(6) . . ? N2 C39 C34 120.7(6) . . ? C38 C39 C34 119.1(6) . . ? C41 C40 Pt2 167.3(5) . . ? C41 C40 Pt1 74.5(4) . . ? Pt2 C40 Pt1 94.9(2) . . ? C40 C41 C42 161.0(7) . . ? C40 C41 Pt1 75.4(4) . . ? C42 C41 Pt1 123.5(4) . . ? C43 C42 C47 118.5(6) . . ? C43 C42 C41 119.5(6) . . ? C47 C42 C41 121.9(6) . . ? C44 C43 C42 119.7(6) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 121.6(6) . . ? C43 C44 H44 119.2 . . ? C45 C44 H44 119.2 . . ? C46 C45 C44 118.9(6) . . ? C46 C45 C48 121.1(7) . . ? C44 C45 C48 120.1(6) . . ? C45 C46 C47 120.9(7) . . ? C45 C46 H46 119.6 . . ? C47 C46 H46 119.6 . . ? C46 C47 C42 120.4(6) . . ? C46 C47 H47 119.8 . . ? C42 C47 H47 119.8 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? Cl2 C49 Cl1 111.7(6) . . ? Cl2 C49 H49A 109.3 . . ? Cl1 C49 H49A 109.3 . . ? Cl2 C49 H49B 109.3 . . ? Cl1 C49 H49B 109.3 . . ? H49A C49 H49B 107.9 . . ? Cl6 C51 Cl5 111.1(4) . . ? Cl6 C51 H51A 109.4 . . ? Cl5 C51 H51A 109.4 . . ? Cl6 C51 H51B 109.4 . . ? Cl5 C51 H51B 109.4 . . ? H51A C51 H51B 108 . . ? C7 N1 C15 117.9(5) . . ? C7 N1 Pt1 113.2(4) . . ? C15 N1 Pt1 128.8(4) . . ? C31 N2 C39 118.5(5) . . ? C31 N2 Pt2 113.7(4) . . ? C39 N2 Pt2 127.7(4) . . ? Cl3A C50A Cl4A 120.1(8) . . ? Cl3A C50A H50A 107.3 . . ? Cl4A C50A H50A 107.3 . . ? Cl3A C50A H50B 107.3 . . ? Cl4A C50A H50B 107.3 . . ? H50A C50A H50B 106.9 . . ? #===END