# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1b _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H98 Cu2 N8 O P2' _chemical_formula_weight 1568.84 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_H-M_alt 'P c a 21' _space_group_name_Hall 'P 2c -2ac' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 16.3089(15) _cell_length_b 21.3025(18) _cell_length_c 24.111(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8376.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 32291 _cell_measurement_theta_min 1.573 _cell_measurement_theta_max 24.998 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.244 _exptl_crystal_F_000 3304 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.100 _exptl_absorpt_coefficient_mu 0.599 _shelx_estimated_absorpt_T_min 0.754 _shelx_estimated_absorpt_T_max 0.943 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.6074 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'Bruker Apex 2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker Kappa Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32291 _diffrn_reflns_av_unetI/netI 0.0591 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.573 _diffrn_reflns_theta_max 24.998 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.971 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.971 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.972 _reflns_number_total 14563 _reflns_number_gt 12125 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.948 _reflns_Friedel_fraction_max 0.998 _reflns_Friedel_fraction_full 0.972 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker Apex 2 software package' _computing_cell_refinement 'Bruker Apex 2 software package' _computing_data_reduction 'Bruker Apex 2 software package' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'ORTEP and POV-Ray' _computing_publication_material 'SHELXL-2013 (Sheldrick, 2013)' _refine_special_details ; Refined as a 2-component inversion twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+1.8612P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.278(13) _chemical_absolute_configuration ? _refine_ls_number_reflns 14563 _refine_ls_number_parameters 997 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 1.025 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.70921(4) -0.27737(3) -0.30965(3) 0.02316(16) Uani 1 1 d . . . . . Cu2 Cu -1.17769(4) -0.21006(3) -0.07930(3) 0.02585(17) Uani 1 1 d . . . . . P1 P -0.68824(8) -0.26541(6) -0.21796(6) 0.0202(3) Uani 1 1 d . . . . . P2 P -1.20172(9) -0.22189(6) -0.17071(6) 0.0217(3) Uani 1 1 d . . . . . N1 N -0.8225(3) -0.3489(2) -0.2905(2) 0.0282(11) Uani 1 1 d . . . . . N2 N -0.8074(3) -0.2148(2) -0.3251(2) 0.0268(11) Uani 1 1 d . . . . . N3 N -0.6175(3) -0.3487(2) -0.39848(19) 0.0273(11) Uani 1 1 d . . . . . N4 N -0.5975(3) -0.2499(2) -0.40247(19) 0.0271(11) Uani 1 1 d . . . . . N5 N -1.0828(3) -0.2890(2) -0.0737(2) 0.0272(10) Uani 1 1 d . . . . . N6 N -1.0688(3) -0.1506(2) -0.08876(19) 0.0258(10) Uani 1 1 d . . . . . N7 N -1.2818(3) -0.2442(2) 0.0165(2) 0.0322(12) Uani 1 1 d . . . . . N8 N -1.2513(3) -0.1468(2) 0.0207(2) 0.0304(11) Uani 1 1 d . . . . . C1 C -0.8423(4) -0.4042(3) -0.2685(3) 0.0378(16) Uani 1 1 d . . . . . H1 H -0.8008 -0.4354 -0.2656 0.045 Uiso 1 1 calc R U . . . C2 C -0.9211(4) -0.4187(3) -0.2495(3) 0.0424(17) Uani 1 1 d . . . . . H2 H -0.9311 -0.4587 -0.2335 0.051 Uiso 1 1 calc R U . . . C3 C -0.9851(4) -0.3758(2) -0.2535(3) 0.0320(14) Uani 1 1 d . . . . . H3 H -1.0383 -0.3860 -0.2404 0.038 Uiso 1 1 calc R U . . . C4 C -0.9690(3) -0.3168(2) -0.2775(2) 0.0206(12) Uani 1 1 d . . . . . C5 C -0.8859(3) -0.3069(2) -0.2946(2) 0.0214(12) Uani 1 1 d . . . . . C6 C -0.8784(3) -0.2445(2) -0.3119(2) 0.0211(11) Uani 1 1 d . . . . . C7 C -0.9590(3) -0.2169(2) -0.3071(3) 0.0243(11) Uani 1 1 d . . . . . C8 C -0.9627(4) -0.1523(3) -0.3220(3) 0.0369(16) Uani 1 1 d . . . . . H8 H -1.0134 -0.1304 -0.3219 0.044 Uiso 1 1 calc R U . . . C9 C -0.8913(4) -0.1225(3) -0.3365(3) 0.0405(16) Uani 1 1 d . . . . . H9 H -0.8934 -0.0794 -0.3466 0.049 Uiso 1 1 calc R U . . . C10 C -0.8157(4) -0.1531(3) -0.3369(3) 0.0377(15) Uani 1 1 d . . . . . H10 H -0.7680 -0.1296 -0.3458 0.045 Uiso 1 1 calc R U . . . C11 C -1.0143(3) -0.2615(2) -0.2871(2) 0.0218(12) Uani 1 1 d . . . . . C12 C -1.1004(3) -0.2487(3) -0.2691(2) 0.0246(12) Uani 1 1 d . . . . . H12A H -1.1347 -0.2862 -0.2762 0.030 Uiso 1 1 calc R U . . . H12B H -1.1229 -0.2134 -0.2911 0.030 Uiso 1 1 calc R U . . . C13 C -1.1041(3) -0.2322(2) -0.2076(2) 0.0228(12) Uani 1 1 d . . . . . H13A H -1.0727 -0.1928 -0.2027 0.027 Uiso 1 1 calc R U . . . H13B H -1.0734 -0.2654 -0.1876 0.027 Uiso 1 1 calc R U . . . C14 C -1.2499(3) -0.1551(3) -0.2055(3) 0.0274(13) Uani 1 1 d . . . . . C15 C -1.2608(4) -0.1013(3) -0.1736(3) 0.0386(15) Uani 1 1 d . . . . . H15 H -1.2458 -0.1018 -0.1356 0.046 Uiso 1 1 calc R U . . . C16 C -1.2934(4) -0.0469(3) -0.1967(4) 0.052(2) Uani 1 1 d . . . . . H16 H -1.2995 -0.0102 -0.1746 0.062 Uiso 1 1 calc R U . . . C17 C -1.3168(4) -0.0462(3) -0.2518(4) 0.054(2) Uani 1 1 d . . . . . H17 H -1.3388 -0.0090 -0.2676 0.065 Uiso 1 1 calc R U . . . C18 C -1.3081(4) -0.0998(3) -0.2841(3) 0.0472(18) Uani 1 1 d . . . . . H18 H -1.3255 -0.0999 -0.3217 0.057 Uiso 1 1 calc R U . . . C19 C -1.2736(3) -0.1533(3) -0.2607(3) 0.0324(14) Uani 1 1 d . . . . . H19 H -1.2662 -0.1896 -0.2831 0.039 Uiso 1 1 calc R U . . . C20 C -1.2617(4) -0.2903(3) -0.1913(2) 0.0258(13) Uani 1 1 d . . . . . C21 C -1.3435(4) -0.2866(3) -0.2069(3) 0.0328(14) Uani 1 1 d . . . . . H21 H -1.3688 -0.2466 -0.2111 0.039 Uiso 1 1 calc R U . . . C22 C -1.3888(4) -0.3408(3) -0.2163(3) 0.0458(17) Uani 1 1 d . . . . . H22 H -1.4447 -0.3377 -0.2270 0.055 Uiso 1 1 calc R U . . . C23 C -1.3535(5) -0.3989(3) -0.2103(3) 0.0506(19) Uani 1 1 d . . . . . H23 H -1.3849 -0.4357 -0.2167 0.061 Uiso 1 1 calc R U . . . C24 C -1.2725(5) -0.4035(3) -0.1948(3) 0.0442(17) Uani 1 1 d . . . . . H24 H -1.2476 -0.4436 -0.1911 0.053 Uiso 1 1 calc R U . . . C25 C -1.2271(4) -0.3496(3) -0.1847(3) 0.0321(14) Uani 1 1 d . . . . . H25 H -1.1716 -0.3532 -0.1731 0.039 Uiso 1 1 calc R U . . . C26 C -0.6364(3) -0.2943(3) -0.3719(2) 0.0224(12) Uani 1 1 d . . . . . C27 C -0.5561(4) -0.2760(3) -0.4467(3) 0.0401(16) Uani 1 1 d . . . . . H27 H -0.5244 -0.2542 -0.4736 0.048 Uiso 1 1 calc R U . . . C28 C -0.5689(4) -0.3375(3) -0.4446(3) 0.0395(16) Uani 1 1 d . . . . . H28 H -0.5488 -0.3681 -0.4699 0.047 Uiso 1 1 calc R U . . . C29 C -0.5957(4) -0.1842(2) -0.3883(2) 0.0259(13) Uani 1 1 d . . . . . C30 C -0.6427(4) -0.1430(3) -0.4181(2) 0.0303(14) Uani 1 1 d . . . . . C31 C -0.6393(4) -0.0797(3) -0.4037(3) 0.0402(16) Uani 1 1 d . . . . . H31 H -0.6707 -0.0501 -0.4242 0.048 Uiso 1 1 calc R U . . . C32 C -0.5905(4) -0.0589(3) -0.3599(3) 0.0439(17) Uani 1 1 d . . . . . C33 C -0.5441(4) -0.1025(3) -0.3313(3) 0.0384(16) Uani 1 1 d . . . . . H33 H -0.5109 -0.0887 -0.3013 0.046 Uiso 1 1 calc R U . . . C34 C -0.5444(4) -0.1663(3) -0.3450(2) 0.0287(13) Uani 1 1 d . . . . . C35 C -0.6980(4) -0.1652(3) -0.4646(3) 0.0420(16) Uani 1 1 d . . . . . H35A H -0.7346 -0.1981 -0.4507 0.063 Uiso 1 1 calc R U . . . H35B H -0.6644 -0.1821 -0.4948 0.063 Uiso 1 1 calc R U . . . H35C H -0.7307 -0.1299 -0.4783 0.063 Uiso 1 1 calc R U . . . C36 C -0.5885(6) 0.0094(3) -0.3440(4) 0.074(3) Uani 1 1 d . . . . . H36A H -0.5573 0.0330 -0.3718 0.111 Uiso 1 1 calc R U . . . H36B H -0.5621 0.0139 -0.3077 0.111 Uiso 1 1 calc R U . . . H36C H -0.6446 0.0257 -0.3421 0.111 Uiso 1 1 calc R U . . . C37 C -0.4891(4) -0.2116(3) -0.3155(3) 0.0403(16) Uani 1 1 d . . . . . H37A H -0.4519 -0.2313 -0.3423 0.060 Uiso 1 1 calc R U . . . H37B H -0.5222 -0.2441 -0.2974 0.060 Uiso 1 1 calc R U . . . H37C H -0.4570 -0.1891 -0.2874 0.060 Uiso 1 1 calc R U . . . C38 C -0.6412(4) -0.4105(3) -0.3805(2) 0.0268(13) Uani 1 1 d . . . . . C39 C -0.7181(4) -0.4330(3) -0.3947(3) 0.0365(15) Uani 1 1 d . . . . . C40 C -0.7379(4) -0.4938(3) -0.3778(3) 0.0429(16) Uani 1 1 d . . . . . H40 H -0.7909 -0.5100 -0.3859 0.051 Uiso 1 1 calc R U . . . C41 C -0.6827(4) -0.5311(3) -0.3494(3) 0.0405(16) Uani 1 1 d . . . . . C42 C -0.6077(4) -0.5060(3) -0.3361(3) 0.0404(16) Uani 1 1 d . . . . . H42 H -0.5699 -0.5312 -0.3161 0.048 Uiso 1 1 calc R U . . . C43 C -0.5849(4) -0.4461(3) -0.3505(2) 0.0296(13) Uani 1 1 d . . . . . C44 C -0.7039(6) -0.5985(3) -0.3341(3) 0.065(2) Uani 1 1 d . . . . . H44A H -0.6745 -0.6273 -0.3588 0.097 Uiso 1 1 calc R U . . . H44B H -0.7631 -0.6050 -0.3381 0.097 Uiso 1 1 calc R U . . . H44C H -0.6877 -0.6065 -0.2956 0.097 Uiso 1 1 calc R U . . . C45 C -0.7774(5) -0.3940(3) -0.4271(4) 0.060(2) Uani 1 1 d . . . . . H45A H -0.7484 -0.3728 -0.4574 0.090 Uiso 1 1 calc R U . . . H45B H -0.8023 -0.3626 -0.4027 0.090 Uiso 1 1 calc R U . . . H45C H -0.8203 -0.4210 -0.4425 0.090 Uiso 1 1 calc R U . . . C46 C -0.5010(4) -0.4215(3) -0.3357(3) 0.0462(17) Uani 1 1 d . . . . . H46A H -0.5061 -0.3790 -0.3204 0.069 Uiso 1 1 calc R U . . . H46B H -0.4667 -0.4203 -0.3690 0.069 Uiso 1 1 calc R U . . . H46C H -0.4758 -0.4491 -0.3080 0.069 Uiso 1 1 calc R U . . . C47 C -1.0753(4) -0.3506(3) -0.0736(3) 0.0373(15) Uani 1 1 d . . . . . H47 H -1.1230 -0.3751 -0.0674 0.045 Uiso 1 1 calc R U . . . C48 C -0.9998(4) -0.3824(3) -0.0823(3) 0.0385(15) Uani 1 1 d . . . . . H48 H -0.9986 -0.4270 -0.0827 0.046 Uiso 1 1 calc R U . . . C49 C -0.9285(4) -0.3492(3) -0.0901(2) 0.0320(14) Uani 1 1 d . . . . . H49 H -0.8777 -0.3702 -0.0953 0.038 Uiso 1 1 calc R U . . . C50 C -0.9327(3) -0.2839(2) -0.0901(2) 0.0217(12) Uani 1 1 d . . . . . C51 C -1.0124(3) -0.2571(2) -0.0818(2) 0.0217(11) Uani 1 1 d . . . . . C52 C -1.0057(3) -0.1916(2) -0.0889(2) 0.0202(11) Uani 1 1 d . . . . . C53 C -0.9218(3) -0.1782(2) -0.1015(2) 0.0225(12) Uani 1 1 d . . . . . C54 C -0.9042(4) -0.1152(3) -0.1142(3) 0.0360(15) Uani 1 1 d . . . . . H54 H -0.8500 -0.1020 -0.1227 0.043 Uiso 1 1 calc R U . . . C55 C -0.9690(4) -0.0733(3) -0.1137(3) 0.0400(16) Uani 1 1 d . . . . . H55 H -0.9585 -0.0304 -0.1218 0.048 Uiso 1 1 calc R U . . . C56 C -1.0488(4) -0.0915(3) -0.1019(3) 0.0318(14) Uani 1 1 d . . . . . H56 H -1.0910 -0.0608 -0.1032 0.038 Uiso 1 1 calc R U . . . C57 C -0.8762(3) -0.2347(2) -0.1010(2) 0.0195(11) Uani 1 1 d . . . . . C58 C -0.7886(3) -0.2427(3) -0.1193(2) 0.0242(12) Uani 1 1 d . . . . . H58A H -0.7631 -0.2780 -0.0989 0.029 Uiso 1 1 calc R U . . . H58B H -0.7571 -0.2040 -0.1110 0.029 Uiso 1 1 calc R U . . . C59 C -0.7861(3) -0.2558(3) -0.1815(2) 0.0251(12) Uani 1 1 d . . . . . H59A H -0.8159 -0.2211 -0.2000 0.030 Uiso 1 1 calc R U . . . H59B H -0.8184 -0.2945 -0.1880 0.030 Uiso 1 1 calc R U . . . C60 C -0.6400(3) -0.3320(3) -0.1831(2) 0.0241(12) Uani 1 1 d . . . . . C61 C -0.6319(3) -0.3869(3) -0.2141(3) 0.0296(13) Uani 1 1 d . . . . . H61 H -0.6466 -0.3875 -0.2522 0.035 Uiso 1 1 calc R U . . . C62 C -0.6018(4) -0.4413(3) -0.1883(3) 0.0433(17) Uani 1 1 d . . . . . H62 H -0.5968 -0.4789 -0.2092 0.052 Uiso 1 1 calc R U . . . C63 C -0.5801(5) -0.4411(3) -0.1347(3) 0.0494(18) Uani 1 1 d . . . . . H63 H -0.5592 -0.4783 -0.1183 0.059 Uiso 1 1 calc R U . . . C64 C -0.5878(4) -0.3865(3) -0.1027(3) 0.0432(17) Uani 1 1 d . . . . . H64 H -0.5733 -0.3868 -0.0645 0.052 Uiso 1 1 calc R U . . . C65 C -0.6170(3) -0.3314(3) -0.1275(3) 0.0303(14) Uani 1 1 d . . . . . H65 H -0.6212 -0.2938 -0.1064 0.036 Uiso 1 1 calc R U . . . C66 C -0.6304(3) -0.1957(3) -0.1969(2) 0.0259(13) Uani 1 1 d . . . . . C67 C -0.5494(4) -0.1978(3) -0.1789(3) 0.0402(16) Uani 1 1 d . . . . . H67 H -0.5239 -0.2373 -0.1728 0.048 Uiso 1 1 calc R U . . . C68 C -0.5056(5) -0.1433(4) -0.1696(3) 0.057(2) Uani 1 1 d . . . . . H68 H -0.4504 -0.1456 -0.1572 0.069 Uiso 1 1 calc R U . . . C69 C -0.5418(6) -0.0854(4) -0.1783(4) 0.067(2) Uani 1 1 d . . . . . H69 H -0.5113 -0.0479 -0.1724 0.080 Uiso 1 1 calc R U . . . C70 C -0.6220(5) -0.0822(3) -0.1953(3) 0.060(2) Uani 1 1 d . . . . . H70 H -0.6473 -0.0425 -0.2006 0.072 Uiso 1 1 calc R U . . . C71 C -0.6662(4) -0.1371(3) -0.2049(3) 0.0414(17) Uani 1 1 d . . . . . H71 H -0.7215 -0.1345 -0.2170 0.050 Uiso 1 1 calc R U . . . C72 C -1.2405(3) -0.1989(3) -0.0120(2) 0.0259(12) Uani 1 1 d . . . . . C73 C -1.3164(5) -0.2207(3) 0.0656(3) 0.0467(18) Uani 1 1 d . . . . . H73 H -1.3476 -0.2435 0.0921 0.056 Uiso 1 1 calc R U . . . C74 C -1.2965(4) -0.1598(4) 0.0677(3) 0.0471(18) Uani 1 1 d . . . . . H74 H -1.3107 -0.1310 0.0961 0.057 Uiso 1 1 calc R U . . . C75 C -1.2889(4) -0.3077(3) -0.0021(3) 0.0311(14) Uani 1 1 d . . . . . C76 C -1.2346(4) -0.3524(3) 0.0190(3) 0.0408(17) Uani 1 1 d . . . . . C77 C -1.2440(4) -0.4142(3) 0.0006(3) 0.0486(19) Uani 1 1 d . . . . . H77 H -1.2099 -0.4460 0.0158 0.058 Uiso 1 1 calc R U . . . C78 C -1.3015(4) -0.4304(3) -0.0391(3) 0.0446(18) Uani 1 1 d . . . . . C79 C -1.3522(4) -0.3844(3) -0.0593(3) 0.0391(16) Uani 1 1 d . . . . . H79 H -1.3922 -0.3952 -0.0863 0.047 Uiso 1 1 calc R U . . . C80 C -1.3471(4) -0.3226(3) -0.0415(3) 0.0332(14) Uani 1 1 d . . . . . C81 C -1.1676(5) -0.3330(4) 0.0593(3) 0.062(2) Uani 1 1 d . . . . . H81A H -1.1372 -0.3703 0.0714 0.093 Uiso 1 1 calc R U . . . H81B H -1.1923 -0.3125 0.0916 0.093 Uiso 1 1 calc R U . . . H81C H -1.1300 -0.3038 0.0409 0.093 Uiso 1 1 calc R U . . . C82 C -1.3070(5) -0.4977(3) -0.0589(4) 0.071(3) Uani 1 1 d . . . . . H82A H -1.3461 -0.5004 -0.0897 0.106 Uiso 1 1 calc R U . . . H82B H -1.3256 -0.5245 -0.0283 0.106 Uiso 1 1 calc R U . . . H82C H -1.2529 -0.5118 -0.0715 0.106 Uiso 1 1 calc R U . . . C83 C -1.4032(4) -0.2722(3) -0.0650(3) 0.0403(16) Uani 1 1 d . . . . . H83A H -1.4437 -0.2915 -0.0896 0.060 Uiso 1 1 calc R U . . . H83B H -1.3705 -0.2417 -0.0859 0.060 Uiso 1 1 calc R U . . . H83C H -1.4314 -0.2508 -0.0345 0.060 Uiso 1 1 calc R U . . . C84 C -1.2172(4) -0.0861(3) 0.0080(3) 0.0306(13) Uani 1 1 d . . . . . C85 C -1.1364(4) -0.0730(3) 0.0241(3) 0.0371(15) Uani 1 1 d . . . . . C86 C -1.1055(4) -0.0138(3) 0.0122(3) 0.0443(17) Uani 1 1 d . . . . . H86 H -1.0514 -0.0037 0.0236 0.053 Uiso 1 1 calc R U . . . C87 C -1.1509(5) 0.0308(3) -0.0157(3) 0.0466(18) Uani 1 1 d . . . . . C88 C -1.2294(5) 0.0160(3) -0.0311(3) 0.0459(18) Uani 1 1 d . . . . . H88 H -1.2606 0.0465 -0.0505 0.055 Uiso 1 1 calc R U . . . C89 C -1.2655(4) -0.0417(3) -0.0195(3) 0.0405(16) Uani 1 1 d . . . . . C90 C -1.0857(5) -0.1225(4) 0.0513(3) 0.0542(19) Uani 1 1 d . . . . . H90A H -1.0856 -0.1604 0.0282 0.081 Uiso 1 1 calc R U . . . H90B H -1.1089 -0.1325 0.0877 0.081 Uiso 1 1 calc R U . . . H90C H -1.0294 -0.1073 0.0558 0.081 Uiso 1 1 calc R U . . . C91 C -1.1120(6) 0.0939(3) -0.0295(4) 0.070(3) Uani 1 1 d . . . . . H91A H -1.0607 0.0871 -0.0497 0.106 Uiso 1 1 calc R U . . . H91B H -1.1008 0.1169 0.0049 0.106 Uiso 1 1 calc R U . . . H91C H -1.1498 0.1184 -0.0526 0.106 Uiso 1 1 calc R U . . . C92 C -1.3527(5) -0.0566(4) -0.0354(4) 0.059(2) Uani 1 1 d . . . . . H92A H -1.3785 -0.0192 -0.0514 0.088 Uiso 1 1 calc R U . . . H92B H -1.3832 -0.0698 -0.0024 0.088 Uiso 1 1 calc R U . . . H92C H -1.3531 -0.0906 -0.0628 0.088 Uiso 1 1 calc R U . . . O1 O -0.9663(3) -0.3638(3) -0.4687(2) 0.0588(14) Uani 1 1 d . . . . . C93 C -0.9127(5) -0.2579(3) -0.4639(3) 0.057(2) Uani 1 1 d . . . . . H93A H -0.9219 -0.2539 -0.5039 0.086 Uiso 1 1 calc R U . . . H93B H -0.8553 -0.2692 -0.4570 0.086 Uiso 1 1 calc R U . . . H93C H -0.9249 -0.2178 -0.4458 0.086 Uiso 1 1 calc R U . . . C94 C -0.9688(5) -0.3089(4) -0.4404(5) 0.078(3) Uani 1 1 d . . . . . H94A H -0.9531 -0.3170 -0.4014 0.093 Uiso 1 1 calc R U . . . H94B H -1.0259 -0.2931 -0.4404 0.093 Uiso 1 1 calc R U . . . C95 C -1.0107(5) -0.4105(4) -0.4420(3) 0.061(2) Uani 1 1 d . . . . . H95A H -1.0697 -0.3996 -0.4416 0.074 Uiso 1 1 calc R U . . . H95B H -0.9918 -0.4149 -0.4032 0.074 Uiso 1 1 calc R U . . . C96 C -0.9969(6) -0.4743(4) -0.4746(3) 0.068(2) Uani 1 1 d . . . . . H96A H -0.9385 -0.4849 -0.4743 0.102 Uiso 1 1 calc R U . . . H96B H -1.0156 -0.4694 -0.5130 0.102 Uiso 1 1 calc R U . . . H96C H -1.0282 -0.5079 -0.4566 0.102 Uiso 1 1 calc R U . . . 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 Cu1 0.0180(3) 0.0276(3) 0.0238(3) -0.0017(3) 0.0021(3) 0.0041(3) Cu2 0.0157(3) 0.0327(3) 0.0291(4) -0.0045(3) 0.0019(3) -0.0005(3) P1 0.0122(6) 0.0257(7) 0.0226(7) -0.0033(6) 0.0010(6) 0.0025(6) P2 0.0123(7) 0.0240(7) 0.0288(8) -0.0056(6) 0.0007(6) -0.0005(6) N1 0.020(2) 0.030(2) 0.034(3) -0.011(2) -0.011(2) 0.009(2) N2 0.017(2) 0.032(3) 0.031(3) 0.006(2) 0.0028(19) 0.004(2) N3 0.031(3) 0.025(2) 0.025(3) -0.003(2) 0.007(2) 0.006(2) N4 0.032(3) 0.026(2) 0.024(3) -0.003(2) 0.007(2) 0.006(2) N5 0.023(2) 0.027(2) 0.031(3) 0.001(2) -0.001(2) -0.004(2) N6 0.021(2) 0.026(2) 0.031(3) -0.007(2) -0.001(2) 0.0028(19) N7 0.028(3) 0.035(3) 0.033(3) 0.002(2) 0.005(2) 0.000(2) N8 0.026(3) 0.032(3) 0.033(3) -0.004(2) 0.003(2) 0.003(2) C1 0.034(4) 0.022(3) 0.057(4) -0.010(3) -0.016(3) 0.012(3) C2 0.037(4) 0.021(3) 0.069(5) 0.001(3) -0.005(3) 0.003(3) C3 0.026(3) 0.023(3) 0.047(4) -0.001(3) -0.002(3) -0.006(2) C4 0.014(3) 0.023(3) 0.025(3) -0.008(2) -0.004(2) -0.002(2) C5 0.020(3) 0.019(2) 0.025(3) -0.013(2) 0.001(2) 0.000(2) C6 0.013(2) 0.024(2) 0.026(3) -0.005(3) 0.001(2) 0.002(2) C7 0.015(3) 0.030(3) 0.028(3) 0.000(3) 0.002(3) 0.006(2) C8 0.028(3) 0.031(3) 0.052(4) 0.011(3) 0.006(3) 0.006(3) C9 0.034(4) 0.025(3) 0.063(5) 0.012(3) 0.009(3) 0.007(3) C10 0.026(3) 0.031(3) 0.057(4) 0.006(3) 0.007(3) 0.001(3) C11 0.019(3) 0.026(3) 0.020(3) -0.005(2) 0.000(2) 0.003(2) C12 0.013(3) 0.028(3) 0.032(3) -0.002(3) -0.002(2) 0.001(2) C13 0.012(3) 0.023(3) 0.033(3) -0.002(2) -0.002(2) 0.003(2) C14 0.013(3) 0.028(3) 0.041(4) 0.002(3) 0.002(2) -0.003(2) C15 0.032(3) 0.030(3) 0.053(4) -0.003(3) -0.001(3) -0.001(3) C16 0.038(4) 0.030(4) 0.087(6) -0.003(4) -0.001(4) 0.004(3) C17 0.037(4) 0.040(4) 0.086(6) 0.019(4) -0.002(4) -0.001(3) C18 0.027(4) 0.061(5) 0.053(4) 0.018(4) -0.005(3) 0.002(3) C19 0.024(3) 0.037(3) 0.035(3) 0.003(3) 0.000(3) -0.003(3) C20 0.023(3) 0.031(3) 0.023(3) -0.005(2) 0.001(2) 0.000(3) C21 0.020(3) 0.034(3) 0.045(4) -0.004(3) -0.001(3) -0.006(3) C22 0.032(3) 0.046(4) 0.059(4) -0.008(4) -0.008(3) -0.016(3) C23 0.055(5) 0.042(4) 0.055(5) -0.010(3) 0.000(4) -0.024(4) C24 0.053(5) 0.027(3) 0.052(4) 0.000(3) 0.002(4) -0.005(3) C25 0.030(3) 0.030(3) 0.036(4) -0.002(3) 0.004(3) -0.001(3) C26 0.016(3) 0.029(3) 0.022(3) 0.001(2) -0.002(2) 0.006(2) C27 0.047(4) 0.042(4) 0.031(3) 0.000(3) 0.020(3) -0.003(3) C28 0.054(4) 0.040(4) 0.024(3) -0.007(3) 0.017(3) 0.007(3) C29 0.026(3) 0.023(3) 0.028(3) 0.005(2) 0.010(2) -0.001(2) C30 0.026(3) 0.035(3) 0.030(3) 0.008(3) 0.008(3) -0.004(3) C31 0.033(4) 0.032(3) 0.056(4) 0.009(3) 0.005(3) -0.001(3) C32 0.036(4) 0.030(3) 0.065(5) -0.001(3) 0.012(4) -0.006(3) C33 0.035(4) 0.041(4) 0.039(4) -0.010(3) 0.006(3) -0.012(3) C34 0.026(3) 0.035(3) 0.025(3) 0.003(3) 0.004(2) -0.004(3) C35 0.035(4) 0.044(4) 0.046(4) 0.010(3) -0.004(3) 0.001(3) C36 0.086(7) 0.032(4) 0.103(7) -0.011(4) 0.017(5) -0.010(4) C37 0.031(3) 0.050(4) 0.040(4) 0.008(3) -0.003(3) -0.001(3) C38 0.029(3) 0.023(3) 0.028(3) -0.007(2) 0.001(3) 0.005(3) C39 0.032(4) 0.035(3) 0.043(4) -0.013(3) -0.006(3) 0.006(3) C40 0.041(4) 0.040(4) 0.048(4) -0.016(3) 0.003(3) -0.009(3) C41 0.057(4) 0.030(3) 0.034(4) -0.006(3) 0.004(3) -0.003(3) C42 0.054(4) 0.034(3) 0.033(3) -0.001(3) 0.000(3) 0.008(3) C43 0.033(3) 0.034(3) 0.022(3) -0.001(3) -0.001(2) 0.006(3) C44 0.101(7) 0.041(4) 0.052(5) -0.004(4) 0.007(5) -0.013(4) C45 0.052(5) 0.055(5) 0.073(6) -0.016(4) -0.024(4) 0.011(4) C46 0.033(4) 0.050(4) 0.055(4) 0.006(3) -0.009(3) 0.000(3) C47 0.033(3) 0.032(3) 0.047(4) 0.008(3) 0.000(3) -0.011(3) C48 0.046(4) 0.023(3) 0.046(4) 0.004(3) -0.007(3) -0.004(3) C49 0.032(3) 0.027(3) 0.036(4) 0.002(3) -0.003(3) 0.007(3) C50 0.026(3) 0.024(3) 0.015(3) 0.000(2) -0.005(2) 0.004(2) C51 0.020(3) 0.024(2) 0.020(3) 0.001(2) 0.000(3) -0.003(2) C52 0.016(2) 0.026(3) 0.018(3) -0.001(2) -0.002(2) 0.001(2) C53 0.019(3) 0.029(3) 0.019(3) -0.003(2) -0.003(2) -0.002(2) C54 0.020(3) 0.033(3) 0.055(4) -0.005(3) -0.007(3) -0.010(3) C55 0.034(4) 0.019(3) 0.067(5) 0.004(3) -0.010(3) -0.004(3) C56 0.027(3) 0.023(3) 0.045(4) -0.008(3) -0.007(3) 0.005(3) C57 0.011(2) 0.028(3) 0.019(3) -0.004(2) -0.001(2) -0.002(2) C58 0.017(3) 0.033(3) 0.022(3) -0.005(2) 0.000(2) 0.002(2) C59 0.014(3) 0.032(3) 0.029(3) 0.001(2) -0.001(2) 0.002(2) C60 0.013(3) 0.028(3) 0.031(3) -0.002(2) -0.003(2) 0.004(2) C61 0.020(3) 0.031(3) 0.038(3) -0.001(3) -0.004(3) 0.005(2) C62 0.049(4) 0.026(3) 0.054(4) -0.004(3) -0.007(3) 0.006(3) C63 0.053(5) 0.042(4) 0.053(5) 0.016(3) -0.008(4) 0.012(3) C64 0.040(4) 0.054(4) 0.035(4) 0.009(3) -0.005(3) 0.008(3) C65 0.016(3) 0.041(4) 0.035(3) -0.001(3) -0.004(2) 0.006(3) C66 0.020(3) 0.029(3) 0.029(3) -0.007(2) 0.005(2) -0.001(2) C67 0.028(3) 0.046(4) 0.046(4) -0.017(3) 0.001(3) -0.007(3) C68 0.034(4) 0.071(5) 0.067(5) -0.029(4) 0.001(4) -0.026(4) C69 0.075(6) 0.049(5) 0.075(6) -0.028(4) 0.010(5) -0.034(5) C70 0.070(6) 0.029(4) 0.080(6) -0.009(4) 0.023(5) -0.010(4) C71 0.039(4) 0.031(3) 0.053(4) 0.000(3) 0.009(3) -0.005(3) C72 0.015(3) 0.031(3) 0.032(3) -0.002(3) 0.003(2) -0.002(2) C73 0.045(4) 0.062(5) 0.033(4) -0.003(3) 0.014(3) -0.006(4) C74 0.048(4) 0.061(5) 0.032(4) -0.014(3) 0.012(3) -0.001(4) C75 0.025(3) 0.036(3) 0.033(3) 0.007(3) 0.008(3) -0.006(3) C76 0.022(3) 0.049(4) 0.051(4) 0.016(3) 0.003(3) -0.005(3) C77 0.032(4) 0.042(4) 0.072(5) 0.025(4) 0.011(4) 0.003(3) C78 0.029(4) 0.035(3) 0.070(5) 0.000(3) 0.018(3) -0.014(3) C79 0.035(4) 0.041(4) 0.041(4) -0.001(3) 0.003(3) -0.010(3) C80 0.022(3) 0.041(4) 0.036(4) 0.008(3) 0.005(3) -0.005(3) C81 0.043(4) 0.079(6) 0.065(5) 0.027(5) -0.017(4) -0.005(4) C82 0.065(5) 0.038(4) 0.110(7) -0.011(4) 0.028(5) -0.011(4) C83 0.030(4) 0.045(4) 0.046(4) 0.007(3) 0.000(3) 0.002(3) C84 0.029(3) 0.030(3) 0.032(3) -0.008(3) 0.001(3) 0.008(3) C85 0.034(4) 0.038(3) 0.039(4) -0.015(3) 0.000(3) 0.003(3) C86 0.041(4) 0.042(4) 0.050(4) -0.020(3) 0.004(3) -0.004(3) C87 0.051(5) 0.034(3) 0.054(4) -0.018(3) 0.016(4) 0.001(3) C88 0.061(5) 0.033(3) 0.043(4) -0.007(3) 0.005(3) 0.019(4) C89 0.037(4) 0.037(3) 0.047(4) -0.017(3) -0.001(3) 0.010(3) C90 0.042(4) 0.066(5) 0.054(5) -0.004(4) -0.011(4) 0.006(4) C91 0.077(6) 0.037(4) 0.097(7) -0.009(4) 0.034(5) -0.008(4) C92 0.044(4) 0.061(5) 0.072(5) 0.001(4) -0.011(4) 0.020(4) O1 0.054(3) 0.071(4) 0.052(3) -0.002(3) -0.003(3) -0.005(3) C93 0.059(5) 0.050(4) 0.062(5) 0.007(4) -0.011(4) -0.002(4) C94 0.040(4) 0.051(5) 0.142(9) -0.045(5) -0.027(5) 0.008(4) C95 0.061(5) 0.083(6) 0.041(4) 0.029(4) -0.010(4) -0.049(5) C96 0.076(6) 0.081(6) 0.048(5) 0.020(4) 0.006(4) 0.003(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 Cu1 C26 1.947(6) . ? Cu1 N2 2.116(4) . ? Cu1 P1 2.2515(16) . ? Cu1 N1 2.439(5) . ? Cu1 Cu2 9.5541(11) . ? Cu2 C72 1.934(6) . ? Cu2 N6 2.193(4) . ? Cu2 P2 2.2527(17) . ? Cu2 N5 2.290(5) . ? P1 C60 1.826(5) . ? P1 C66 1.831(6) . ? P1 C59 1.835(5) . ? P2 C20 1.824(6) . ? P2 C14 1.829(6) . ? P2 C13 1.837(5) . ? N1 C1 1.333(8) . ? N1 C5 1.369(7) . ? N2 C10 1.352(7) . ? N2 C6 1.357(7) . ? N3 C26 1.359(7) . ? N3 C28 1.386(7) . ? N3 C38 1.439(7) . ? N4 C26 1.359(7) . ? N4 C27 1.380(7) . ? N4 C29 1.441(7) . ? N5 C47 1.317(7) . ? N5 C51 1.348(7) . ? N6 C56 1.339(7) . ? N6 C52 1.349(6) . ? N7 C72 1.364(7) . ? N7 C73 1.405(8) . ? N7 C75 1.428(8) . ? N8 C72 1.373(7) . ? N8 C74 1.380(8) . ? N8 C84 1.440(7) . ? C1 C2 1.399(9) . ? C2 C3 1.391(8) . ? C3 C4 1.407(7) . ? C4 C11 1.410(7) . ? C4 C5 1.432(7) . ? C5 C6 1.399(7) . ? C6 C7 1.445(7) . ? C7 C11 1.397(8) . ? C7 C8 1.422(7) . ? C8 C9 1.372(8) . ? C9 C10 1.394(8) . ? C11 C12 1.494(7) . ? C12 C13 1.525(8) . ? C14 C19 1.386(9) . ? C14 C15 1.390(8) . ? C15 C16 1.392(9) . ? C16 C17 1.383(12) . ? C17 C18 1.389(11) . ? C18 C19 1.391(9) . ? C20 C21 1.388(8) . ? C20 C25 1.393(8) . ? C21 C22 1.390(8) . ? C22 C23 1.371(9) . ? C23 C24 1.376(10) . ? C24 C25 1.388(8) . ? C27 C28 1.328(9) . ? C29 C30 1.369(8) . ? C29 C34 1.392(8) . ? C30 C31 1.393(8) . ? C30 C35 1.514(9) . ? C31 C32 1.394(10) . ? C32 C33 1.385(9) . ? C32 C36 1.504(9) . ? C33 C34 1.398(8) . ? C34 C37 1.501(8) . ? C38 C39 1.385(8) . ? C38 C43 1.394(8) . ? C39 C40 1.396(9) . ? C39 C45 1.496(9) . ? C40 C41 1.381(10) . ? C41 C42 1.373(9) . ? C41 C44 1.522(9) . ? C42 C43 1.372(9) . ? C43 C46 1.507(9) . ? C47 C48 1.421(8) . ? C48 C49 1.374(8) . ? C49 C50 1.394(7) . ? C50 C57 1.420(7) . ? C50 C51 1.433(7) . ? C51 C52 1.410(7) . ? C52 C53 1.430(7) . ? C53 C54 1.406(8) . ? C53 C57 1.415(7) . ? C54 C55 1.384(8) . ? C55 C56 1.388(8) . ? C57 C58 1.505(7) . ? C58 C59 1.526(8) . ? C60 C65 1.393(8) . ? C60 C61 1.393(8) . ? C61 C62 1.404(8) . ? C62 C63 1.339(10) . ? C63 C64 1.403(10) . ? C64 C65 1.401(8) . ? C66 C71 1.391(8) . ? C66 C67 1.391(8) . ? C67 C68 1.382(9) . ? C68 C69 1.384(11) . ? C69 C70 1.372(12) . ? C70 C71 1.393(9) . ? C73 C74 1.338(10) . ? C75 C80 1.380(8) . ? C75 C76 1.396(9) . ? C76 C77 1.398(9) . ? C76 C81 1.521(10) . ? C77 C78 1.383(10) . ? C78 C79 1.373(9) . ? C78 C82 1.513(9) . ? C79 C80 1.385(9) . ? C80 C83 1.521(9) . ? C84 C89 1.399(8) . ? C84 C85 1.402(8) . ? C85 C86 1.388(9) . ? C85 C90 1.492(9) . ? C86 C87 1.379(10) . ? C87 C88 1.370(10) . ? C87 C91 1.525(9) . ? C88 C89 1.391(9) . ? C89 C92 1.506(10) . ? O1 C94 1.355(9) . ? O1 C95 1.389(8) . ? C93 C94 1.530(12) . ? C95 C96 1.584(11) . ? 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 C26 Cu1 N2 116.3(2) . . ? C26 Cu1 P1 133.23(17) . . ? N2 Cu1 P1 102.51(14) . . ? C26 Cu1 N1 119.5(2) . . ? N2 Cu1 N1 81.55(16) . . ? P1 Cu1 N1 90.01(12) . . ? C26 Cu1 Cu2 164.47(16) . . ? N2 Cu1 Cu2 53.33(13) . . ? P1 Cu1 Cu2 62.20(4) . . ? N1 Cu1 Cu2 51.52(11) . . ? C72 Cu2 N6 116.4(2) . . ? C72 Cu2 P2 137.95(18) . . ? N6 Cu2 P2 95.96(13) . . ? C72 Cu2 N5 113.5(2) . . ? N6 Cu2 N5 83.28(16) . . ? P2 Cu2 N5 95.35(14) . . ? C72 Cu2 Cu1 158.43(17) . . ? N6 Cu2 Cu1 51.59(11) . . ? P2 Cu2 Cu1 63.49(4) . . ? N5 Cu2 Cu1 51.94(12) . . ? C60 P1 C66 106.3(3) . . ? C60 P1 C59 104.0(3) . . ? C66 P1 C59 103.0(3) . . ? C60 P1 Cu1 115.41(19) . . ? C66 P1 Cu1 116.22(19) . . ? C59 P1 Cu1 110.56(18) . . ? C20 P2 C14 105.4(3) . . ? C20 P2 C13 103.7(3) . . ? C14 P2 C13 104.1(3) . . ? C20 P2 Cu2 116.71(19) . . ? C14 P2 Cu2 115.9(2) . . ? C13 P2 Cu2 109.62(18) . . ? C1 N1 C5 115.1(5) . . ? C1 N1 Cu1 144.2(4) . . ? C5 N1 Cu1 98.7(3) . . ? C10 N2 C6 114.6(5) . . ? C10 N2 Cu1 136.5(4) . . ? C6 N2 Cu1 108.1(3) . . ? C26 N3 C28 111.3(5) . . ? C26 N3 C38 125.2(5) . . ? C28 N3 C38 123.5(5) . . ? C26 N4 C27 111.5(5) . . ? C26 N4 C29 123.9(4) . . ? C27 N4 C29 124.4(5) . . ? C47 N5 C51 115.1(5) . . ? C47 N5 Cu2 142.6(4) . . ? C51 N5 Cu2 101.3(3) . . ? C56 N6 C52 115.0(5) . . ? C56 N6 Cu2 139.9(4) . . ? C52 N6 Cu2 104.1(3) . . ? C72 N7 C73 111.8(5) . . ? C72 N7 C75 123.5(5) . . ? C73 N7 C75 124.7(5) . . ? C72 N8 C74 112.1(5) . . ? C72 N8 C84 123.6(5) . . ? C74 N8 C84 124.2(5) . . ? N1 C1 C2 123.2(5) . . ? C3 C2 C1 121.4(6) . . ? C2 C3 C4 118.4(5) . . ? C3 C4 C11 135.6(5) . . ? C3 C4 C5 115.2(5) . . ? C11 C4 C5 109.0(5) . . ? N1 C5 C6 125.2(5) . . ? N1 C5 C4 126.7(5) . . ? C6 C5 C4 107.9(5) . . ? N2 C6 C5 125.9(5) . . ? N2 C6 C7 127.3(4) . . ? C5 C6 C7 106.5(4) . . ? C11 C7 C8 135.8(5) . . ? C11 C7 C6 109.8(4) . . ? C8 C7 C6 114.4(5) . . ? C9 C8 C7 118.4(5) . . ? C8 C9 C10 122.4(5) . . ? N2 C10 C9 122.9(6) . . ? C7 C11 C4 106.6(5) . . ? C7 C11 C12 125.6(5) . . ? C4 C11 C12 126.7(5) . . ? C11 C12 C13 111.2(4) . . ? C12 C13 P2 122.1(4) . . ? C19 C14 C15 118.1(6) . . ? C19 C14 P2 125.5(5) . . ? C15 C14 P2 116.3(5) . . ? C14 C15 C16 121.0(7) . . ? C17 C16 C15 119.8(7) . . ? C16 C17 C18 120.2(7) . . ? C17 C18 C19 119.2(7) . . ? C14 C19 C18 121.7(6) . . ? C21 C20 C25 118.2(5) . . ? C21 C20 P2 122.9(4) . . ? C25 C20 P2 118.4(5) . . ? C20 C21 C22 120.5(6) . . ? C23 C22 C21 120.6(6) . . ? C22 C23 C24 119.8(6) . . ? C23 C24 C25 120.0(6) . . ? C24 C25 C20 120.9(6) . . ? N4 C26 N3 103.4(5) . . ? N4 C26 Cu1 125.0(4) . . ? N3 C26 Cu1 131.3(4) . . ? C28 C27 N4 107.0(5) . . ? C27 C28 N3 106.8(5) . . ? C30 C29 C34 123.7(5) . . ? C30 C29 N4 119.2(5) . . ? C34 C29 N4 117.1(5) . . ? C29 C30 C31 117.9(6) . . ? C29 C30 C35 121.4(5) . . ? C31 C30 C35 120.7(6) . . ? C30 C31 C32 121.3(6) . . ? C33 C32 C31 118.5(6) . . ? C33 C32 C36 120.6(7) . . ? C31 C32 C36 120.9(7) . . ? C32 C33 C34 122.2(6) . . ? C29 C34 C33 116.5(6) . . ? C29 C34 C37 122.8(5) . . ? C33 C34 C37 120.7(6) . . ? C39 C38 C43 122.4(5) . . ? C39 C38 N3 119.0(5) . . ? C43 C38 N3 118.5(5) . . ? C38 C39 C40 117.3(6) . . ? C38 C39 C45 121.5(6) . . ? C40 C39 C45 121.2(6) . . ? C41 C40 C39 121.7(6) . . ? C42 C41 C40 118.2(6) . . ? C42 C41 C44 120.8(7) . . ? C40 C41 C44 120.9(7) . . ? C43 C42 C41 123.0(6) . . ? C42 C43 C38 117.2(6) . . ? C42 C43 C46 120.6(6) . . ? C38 C43 C46 122.1(5) . . ? N5 C47 C48 123.8(5) . . ? C49 C48 C47 120.5(5) . . ? C48 C49 C50 118.2(5) . . ? C49 C50 C57 134.8(5) . . ? C49 C50 C51 116.3(5) . . ? C57 C50 C51 108.8(4) . . ? N5 C51 C52 125.7(5) . . ? N5 C51 C50 126.2(4) . . ? C52 C51 C50 107.8(4) . . ? N6 C52 C51 125.5(5) . . ? N6 C52 C53 126.9(5) . . ? C51 C52 C53 107.3(4) . . ? C54 C53 C57 134.9(5) . . ? C54 C53 C52 115.6(5) . . ? C57 C53 C52 109.4(5) . . ? C55 C54 C53 117.2(5) . . ? C54 C55 C56 122.5(5) . . ? N6 C56 C55 122.7(5) . . ? C53 C57 C50 106.7(4) . . ? C53 C57 C58 126.4(5) . . ? C50 C57 C58 126.0(5) . . ? C57 C58 C59 109.5(4) . . ? C58 C59 P1 120.9(4) . . ? C65 C60 C61 119.8(5) . . ? C65 C60 P1 123.5(4) . . ? C61 C60 P1 116.5(4) . . ? C60 C61 C62 119.3(6) . . ? C63 C62 C61 121.1(6) . . ? C62 C63 C64 120.7(6) . . ? C65 C64 C63 119.3(6) . . ? C60 C65 C64 119.8(6) . . ? C71 C66 C67 118.1(6) . . ? C71 C66 P1 118.3(5) . . ? C67 C66 P1 123.3(5) . . ? C68 C67 C66 121.0(7) . . ? C67 C68 C69 120.2(7) . . ? C70 C69 C68 119.7(7) . . ? C69 C70 C71 120.1(7) . . ? C66 C71 C70 120.9(7) . . ? N7 C72 N8 102.7(5) . . ? N7 C72 Cu2 126.7(4) . . ? N8 C72 Cu2 130.5(4) . . ? C74 C73 N7 106.2(6) . . ? C73 C74 N8 107.2(6) . . ? C80 C75 C76 121.9(6) . . ? C80 C75 N7 119.4(5) . . ? C76 C75 N7 118.7(6) . . ? C75 C76 C77 117.2(6) . . ? C75 C76 C81 120.2(6) . . ? C77 C76 C81 122.5(6) . . ? C78 C77 C76 121.9(6) . . ? C79 C78 C77 118.4(6) . . ? C79 C78 C82 121.9(7) . . ? C77 C78 C82 119.7(7) . . ? C78 C79 C80 122.1(6) . . ? C75 C80 C79 118.3(6) . . ? C75 C80 C83 120.4(6) . . ? C79 C80 C83 121.3(6) . . ? C89 C84 C85 121.8(6) . . ? C89 C84 N8 119.3(5) . . ? C85 C84 N8 118.9(5) . . ? C86 C85 C84 117.7(6) . . ? C86 C85 C90 122.2(6) . . ? C84 C85 C90 120.1(6) . . ? C87 C86 C85 122.1(7) . . ? C88 C87 C86 118.4(6) . . ? C88 C87 C91 122.2(7) . . ? C86 C87 C91 119.5(7) . . ? C87 C88 C89 123.0(7) . . ? C88 C89 C84 117.0(6) . . ? C88 C89 C92 122.4(7) . . ? C84 C89 C92 120.6(6) . . ? C94 O1 C95 111.6(7) . . ? O1 C94 C93 114.2(8) . . ? O1 C95 C96 108.1(7) . . ? _refine_diff_density_max 0.857 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.061 _shelxl_version_number 2013-4 _iucr_refine_instructions_details ; TITL 1bEt2O in Pca2(1) CELL 0.71073 16.3089 21.3025 24.1115 90.000 90.000 90.000 ZERR 4.00 0.0015 0.0018 0.0022 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, -Y, Z SYMM 0.5-X, Y, 0.5+Z SFAC C H N P Cu O UNIT 384 392 32 8 8 4 L.S. 10 SIZE 0.5 0.3 0.1 ACTA OMIT -3 50 OMIT 1 2 0 OMIT 0 1 -2 OMIT 1 1 -1 OMIT 1 1 1 OMIT 0 1 2 OMIT 0 0 2 OMIT 0 2 0 OMIT 0 0 -2 OMIT 0 1 0 OMIT 1 2 2 BIND CU1 CU2 BOND TWIN FMAP 2 PLAN 5 TEMP -123.130 WGHT 0.061600 1.861200 BASF 0.27815 FVAR 0.05582 CU1 5 -0.709206 -0.277366 -0.309654 11.00000 0.01803 0.02763 = 0.02381 -0.00166 0.00212 0.00410 CU2 5 -1.177686 -0.210061 -0.079300 11.00000 0.01568 0.03273 = 0.02913 -0.00446 0.00188 -0.00055 P1 4 -0.688236 -0.265409 -0.217964 11.00000 0.01216 0.02570 = 0.02264 -0.00326 0.00100 0.00246 P2 4 -1.201724 -0.221890 -0.170706 11.00000 0.01228 0.02402 = 0.02876 -0.00559 0.00072 -0.00046 N1 3 -0.822520 -0.348856 -0.290536 11.00000 0.02009 0.03042 = 0.03410 -0.01099 -0.01104 0.00868 N2 3 -0.807377 -0.214828 -0.325114 11.00000 0.01705 0.03194 = 0.03135 0.00568 0.00276 0.00413 N3 3 -0.617489 -0.348685 -0.398480 11.00000 0.03143 0.02541 = 0.02515 -0.00336 0.00674 0.00595 N4 3 -0.597468 -0.249851 -0.402474 11.00000 0.03181 0.02588 = 0.02371 -0.00323 0.00702 0.00608 N5 3 -1.082773 -0.289031 -0.073686 11.00000 0.02325 0.02699 = 0.03128 0.00095 -0.00097 -0.00375 N6 3 -1.068782 -0.150595 -0.088760 11.00000 0.02075 0.02580 = 0.03095 -0.00668 -0.00069 0.00281 N7 3 -1.281811 -0.244232 0.016483 11.00000 0.02826 0.03508 = 0.03339 0.00156 0.00530 -0.00004 N8 3 -1.251334 -0.146762 0.020669 11.00000 0.02615 0.03193 = 0.03316 -0.00364 0.00250 0.00255 C1 1 -0.842273 -0.404215 -0.268511 11.00000 0.03437 0.02166 = 0.05735 -0.00980 -0.01564 0.01171 AFIX 43 H1 2 -0.800810 -0.435361 -0.265576 11.00000 -1.20000 AFIX 0 C2 1 -0.921076 -0.418690 -0.249508 11.00000 0.03743 0.02054 = 0.06933 0.00145 -0.00492 0.00339 AFIX 43 H2 2 -0.931108 -0.458714 -0.233510 11.00000 -1.20000 AFIX 0 C3 1 -0.985052 -0.375773 -0.253525 11.00000 0.02564 0.02292 = 0.04743 -0.00066 -0.00190 -0.00638 AFIX 43 H3 2 -1.038319 -0.385994 -0.240382 11.00000 -1.20000 AFIX 0 C4 1 -0.968963 -0.316823 -0.277535 11.00000 0.01373 0.02260 = 0.02539 -0.00832 -0.00377 -0.00152 C5 1 -0.885860 -0.306916 -0.294631 11.00000 0.02014 0.01897 = 0.02502 -0.01280 0.00150 0.00024 C6 1 -0.878381 -0.244474 -0.311868 11.00000 0.01335 0.02425 = 0.02567 -0.00451 0.00103 0.00222 C7 1 -0.958979 -0.216869 -0.307140 11.00000 0.01500 0.02955 = 0.02836 -0.00012 0.00175 0.00551 C8 1 -0.962725 -0.152319 -0.321993 11.00000 0.02826 0.03064 = 0.05168 0.01100 0.00589 0.00620 AFIX 43 H8 2 -1.013450 -0.130395 -0.321906 11.00000 -1.20000 AFIX 0 C9 1 -0.891276 -0.122472 -0.336457 11.00000 0.03386 0.02512 = 0.06253 0.01183 0.00858 0.00679 AFIX 43 H9 2 -0.893378 -0.079398 -0.346561 11.00000 -1.20000 AFIX 0 C10 1 -0.815722 -0.153089 -0.336856 11.00000 0.02552 0.03072 = 0.05689 0.00633 0.00735 0.00124 AFIX 43 H10 2 -0.768030 -0.129553 -0.345765 11.00000 -1.20000 AFIX 0 C11 1 -1.014341 -0.261512 -0.287115 11.00000 0.01934 0.02566 = 0.02035 -0.00462 -0.00015 0.00289 C12 1 -1.100383 -0.248663 -0.269068 11.00000 0.01331 0.02847 = 0.03209 -0.00217 -0.00179 0.00103 AFIX 23 H12A 2 -1.134663 -0.286157 -0.276201 11.00000 -1.20000 H12B 2 -1.122937 -0.213414 -0.291051 11.00000 -1.20000 AFIX 0 C13 1 -1.104069 -0.232227 -0.207554 11.00000 0.01235 0.02332 = 0.03259 -0.00238 -0.00194 0.00296 AFIX 23 H13A 2 -1.072733 -0.192803 -0.202719 11.00000 -1.20000 H13B 2 -1.073370 -0.265356 -0.187605 11.00000 -1.20000 AFIX 0 C14 1 -1.249922 -0.155120 -0.205471 11.00000 0.01270 0.02813 = 0.04125 0.00191 0.00207 -0.00331 C15 1 -1.260826 -0.101345 -0.173639 11.00000 0.03237 0.03015 = 0.05333 -0.00339 -0.00126 -0.00142 AFIX 43 H15 2 -1.245830 -0.101790 -0.135569 11.00000 -1.20000 AFIX 0 C16 1 -1.293378 -0.046860 -0.196688 11.00000 0.03774 0.02991 = 0.08744 -0.00342 -0.00080 0.00356 AFIX 43 H16 2 -1.299516 -0.010225 -0.174608 11.00000 -1.20000 AFIX 0 C17 1 -1.316751 -0.046210 -0.251811 11.00000 0.03708 0.03984 = 0.08643 0.01945 -0.00249 -0.00054 AFIX 43 H17 2 -1.338793 -0.009020 -0.267638 11.00000 -1.20000 AFIX 0 C18 1 -1.308084 -0.099789 -0.284091 11.00000 0.02723 0.06141 = 0.05283 0.01775 -0.00519 0.00211 AFIX 43 H18 2 -1.325460 -0.099881 -0.321697 11.00000 -1.20000 AFIX 0 C19 1 -1.273635 -0.153328 -0.260663 11.00000 0.02436 0.03741 = 0.03533 0.00297 -0.00033 -0.00272 AFIX 43 H19 2 -1.266171 -0.189576 -0.283052 11.00000 -1.20000 AFIX 0 C20 1 -1.261702 -0.290278 -0.191337 11.00000 0.02323 0.03127 = 0.02300 -0.00539 0.00057 -0.00027 C21 1 -1.343521 -0.286557 -0.206870 11.00000 0.01981 0.03352 = 0.04495 -0.00396 -0.00071 -0.00623 AFIX 43 H21 2 -1.368752 -0.246648 -0.211101 11.00000 -1.20000 AFIX 0 C22 1 -1.388809 -0.340826 -0.216280 11.00000 0.03183 0.04638 = 0.05927 -0.00824 -0.00846 -0.01587 AFIX 43 H22 2 -1.444725 -0.337675 -0.226967 11.00000 -1.20000 AFIX 0 C23 1 -1.353503 -0.398851 -0.210274 11.00000 0.05525 0.04192 = 0.05475 -0.00978 -0.00046 -0.02401 AFIX 43 H23 2 -1.384863 -0.435713 -0.216742 11.00000 -1.20000 AFIX 0 C24 1 -1.272493 -0.403505 -0.194847 11.00000 0.05304 0.02722 = 0.05236 0.00015 0.00218 -0.00524 AFIX 43 H24 2 -1.247638 -0.443617 -0.191131 11.00000 -1.20000 AFIX 0 C25 1 -1.227100 -0.349604 -0.184716 11.00000 0.02981 0.03016 = 0.03643 -0.00153 0.00382 -0.00102 AFIX 43 H25 2 -1.171639 -0.353212 -0.173099 11.00000 -1.20000 AFIX 0 C26 1 -0.636409 -0.294327 -0.371858 11.00000 0.01626 0.02875 = 0.02214 0.00135 -0.00183 0.00603 C27 1 -0.556067 -0.276022 -0.446723 11.00000 0.04741 0.04198 = 0.03093 -0.00004 0.01989 -0.00259 AFIX 43 H27 2 -0.524385 -0.254186 -0.473574 11.00000 -1.20000 AFIX 0 C28 1 -0.568946 -0.337543 -0.444625 11.00000 0.05393 0.04002 = 0.02442 -0.00709 0.01743 0.00668 AFIX 43 H28 2 -0.548756 -0.368057 -0.469905 11.00000 -1.20000 AFIX 0 C29 1 -0.595690 -0.184161 -0.388319 11.00000 0.02583 0.02348 = 0.02835 0.00527 0.01036 -0.00145 C30 1 -0.642747 -0.142957 -0.418075 11.00000 0.02591 0.03463 = 0.03046 0.00838 0.00750 -0.00394 C31 1 -0.639288 -0.079667 -0.403736 11.00000 0.03309 0.03154 = 0.05584 0.00930 0.00507 -0.00060 AFIX 43 H31 2 -0.670739 -0.050123 -0.424194 11.00000 -1.20000 AFIX 0 C32 1 -0.590547 -0.058853 -0.359933 11.00000 0.03616 0.03025 = 0.06542 -0.00102 0.01217 -0.00587 C33 1 -0.544072 -0.102510 -0.331253 11.00000 0.03535 0.04054 = 0.03944 -0.00976 0.00594 -0.01188 AFIX 43 H33 2 -0.510899 -0.088678 -0.301259 11.00000 -1.20000 AFIX 0 C34 1 -0.544364 -0.166288 -0.344989 11.00000 0.02631 0.03461 = 0.02503 0.00329 0.00409 -0.00403 C35 1 -0.697988 -0.165207 -0.464566 11.00000 0.03544 0.04425 = 0.04643 0.01004 -0.00419 0.00108 AFIX 137 H35A 2 -0.734634 -0.198094 -0.450660 11.00000 -1.50000 H35B 2 -0.664429 -0.182060 -0.494815 11.00000 -1.50000 H35C 2 -0.730654 -0.129867 -0.478312 11.00000 -1.50000 AFIX 0 C36 1 -0.588450 0.009395 -0.343997 11.00000 0.08565 0.03201 = 0.10340 -0.01148 0.01703 -0.00991 AFIX 137 H36A 2 -0.557311 0.033016 -0.371798 11.00000 -1.50000 H36B 2 -0.562107 0.013924 -0.307687 11.00000 -1.50000 H36C 2 -0.644566 0.025711 -0.342125 11.00000 -1.50000 AFIX 0 C37 1 -0.489065 -0.211616 -0.315460 11.00000 0.03055 0.04995 = 0.04025 0.00825 -0.00292 -0.00066 AFIX 137 H37A 2 -0.451898 -0.231253 -0.342273 11.00000 -1.50000 H37B 2 -0.522219 -0.244079 -0.297391 11.00000 -1.50000 H37C 2 -0.456971 -0.189113 -0.287434 11.00000 -1.50000 AFIX 0 C38 1 -0.641219 -0.410488 -0.380480 11.00000 0.02939 0.02314 = 0.02792 -0.00652 0.00094 0.00511 C39 1 -0.718060 -0.433017 -0.394710 11.00000 0.03214 0.03477 = 0.04259 -0.01266 -0.00552 0.00598 C40 1 -0.737949 -0.493812 -0.377751 11.00000 0.04085 0.03996 = 0.04789 -0.01558 0.00286 -0.00928 AFIX 43 H40 2 -0.790868 -0.509989 -0.385929 11.00000 -1.20000 AFIX 0 C41 1 -0.682731 -0.531051 -0.349404 11.00000 0.05674 0.03048 = 0.03413 -0.00594 0.00418 -0.00259 C42 1 -0.607678 -0.505968 -0.336114 11.00000 0.05408 0.03403 = 0.03309 -0.00137 -0.00033 0.00794 AFIX 43 H42 2 -0.569851 -0.531181 -0.316076 11.00000 -1.20000 AFIX 0 C43 1 -0.584862 -0.446122 -0.350476 11.00000 0.03341 0.03378 = 0.02168 -0.00082 -0.00110 0.00647 C44 1 -0.703864 -0.598459 -0.334096 11.00000 0.10087 0.04077 = 0.05247 -0.00384 0.00679 -0.01260 AFIX 137 H44A 2 -0.674470 -0.627289 -0.358751 11.00000 -1.50000 H44B 2 -0.763052 -0.604997 -0.338078 11.00000 -1.50000 H44C 2 -0.687677 -0.606489 -0.295602 11.00000 -1.50000 AFIX 0 C45 1 -0.777394 -0.393982 -0.427117 11.00000 0.05160 0.05490 = 0.07259 -0.01556 -0.02411 0.01117 AFIX 137 H45A 2 -0.748411 -0.372764 -0.457386 11.00000 -1.50000 H45B 2 -0.802313 -0.362580 -0.402659 11.00000 -1.50000 H45C 2 -0.820323 -0.421033 -0.442532 11.00000 -1.50000 AFIX 0 C46 1 -0.501039 -0.421472 -0.335679 11.00000 0.03298 0.05049 = 0.05504 0.00552 -0.00853 0.00033 AFIX 137 H46A 2 -0.506147 -0.379021 -0.320402 11.00000 -1.50000 H46B 2 -0.466683 -0.420301 -0.369009 11.00000 -1.50000 H46C 2 -0.475787 -0.449068 -0.308006 11.00000 -1.50000 AFIX 0 C47 1 -1.075261 -0.350597 -0.073626 11.00000 0.03347 0.03167 = 0.04671 0.00830 -0.00018 -0.01113 AFIX 43 H47 2 -1.123042 -0.375118 -0.067418 11.00000 -1.20000 AFIX 0 C48 1 -0.999798 -0.382432 -0.082315 11.00000 0.04613 0.02339 = 0.04600 0.00356 -0.00737 -0.00450 AFIX 43 H48 2 -0.998636 -0.427016 -0.082750 11.00000 -1.20000 AFIX 0 C49 1 -0.928461 -0.349224 -0.090096 11.00000 0.03221 0.02747 = 0.03626 0.00191 -0.00261 0.00723 AFIX 43 H49 2 -0.877658 -0.370228 -0.095313 11.00000 -1.20000 AFIX 0 C50 1 -0.932732 -0.283854 -0.090120 11.00000 0.02633 0.02363 = 0.01505 -0.00008 -0.00532 0.00407 C51 1 -1.012436 -0.257088 -0.081828 11.00000 0.02049 0.02426 = 0.02044 0.00143 -0.00024 -0.00263 C52 1 -1.005699 -0.191585 -0.088934 11.00000 0.01649 0.02613 = 0.01797 -0.00087 -0.00207 0.00117 C53 1 -0.921796 -0.178190 -0.101477 11.00000 0.01943 0.02881 = 0.01938 -0.00307 -0.00315 -0.00177 C54 1 -0.904164 -0.115222 -0.114184 11.00000 0.01961 0.03297 = 0.05540 -0.00471 -0.00670 -0.00968 AFIX 43 H54 2 -0.849989 -0.101990 -0.122727 11.00000 -1.20000 AFIX 0 C55 1 -0.969004 -0.073286 -0.113735 11.00000 0.03418 0.01896 = 0.06689 0.00407 -0.00981 -0.00421 AFIX 43 H55 2 -0.958463 -0.030393 -0.121827 11.00000 -1.20000 AFIX 0 C56 1 -1.048800 -0.091498 -0.101919 11.00000 0.02728 0.02295 = 0.04513 -0.00832 -0.00741 0.00467 AFIX 43 H56 2 -1.090973 -0.060771 -0.103222 11.00000 -1.20000 AFIX 0 C57 1 -0.876171 -0.234700 -0.101019 11.00000 0.01128 0.02797 = 0.01919 -0.00366 -0.00054 -0.00226 C58 1 -0.788568 -0.242666 -0.119294 11.00000 0.01738 0.03280 = 0.02246 -0.00471 -0.00032 0.00197 AFIX 23 H58A 2 -0.763100 -0.277966 -0.098887 11.00000 -1.20000 H58B 2 -0.757134 -0.204046 -0.110951 11.00000 -1.20000 AFIX 0 C59 1 -0.786147 -0.255783 -0.181479 11.00000 0.01401 0.03200 = 0.02922 0.00079 -0.00132 0.00179 AFIX 23 H59A 2 -0.815909 -0.221122 -0.199995 11.00000 -1.20000 H59B 2 -0.818412 -0.294458 -0.187964 11.00000 -1.20000 AFIX 0 C60 1 -0.639959 -0.331955 -0.183142 11.00000 0.01319 0.02801 = 0.03114 -0.00155 -0.00341 0.00428 C61 1 -0.631909 -0.386861 -0.214078 11.00000 0.01973 0.03073 = 0.03821 -0.00126 -0.00358 0.00474 AFIX 43 H61 2 -0.646621 -0.387465 -0.252197 11.00000 -1.20000 AFIX 0 C62 1 -0.601811 -0.441291 -0.188291 11.00000 0.04920 0.02623 = 0.05438 -0.00422 -0.00678 0.00632 AFIX 43 H62 2 -0.596793 -0.478895 -0.209198 11.00000 -1.20000 AFIX 0 C63 1 -0.580059 -0.441100 -0.134732 11.00000 0.05270 0.04231 = 0.05311 0.01558 -0.00755 0.01214 AFIX 43 H63 2 -0.559190 -0.478347 -0.118293 11.00000 -1.20000 AFIX 0 C64 1 -0.587764 -0.386492 -0.102652 11.00000 0.04012 0.05409 = 0.03535 0.00859 -0.00550 0.00803 AFIX 43 H64 2 -0.573291 -0.386847 -0.064488 11.00000 -1.20000 AFIX 0 C65 1 -0.617027 -0.331421 -0.127485 11.00000 0.01552 0.04083 = 0.03452 -0.00122 -0.00376 0.00587 AFIX 43 H65 2 -0.621219 -0.293849 -0.106449 11.00000 -1.20000 AFIX 0 C66 1 -0.630383 -0.195683 -0.196938 11.00000 0.01979 0.02920 = 0.02882 -0.00668 0.00528 -0.00122 C67 1 -0.549426 -0.197823 -0.178880 11.00000 0.02837 0.04627 = 0.04592 -0.01698 0.00128 -0.00655 AFIX 43 H67 2 -0.523908 -0.237326 -0.172845 11.00000 -1.20000 AFIX 0 C68 1 -0.505571 -0.143299 -0.169590 11.00000 0.03446 0.07087 = 0.06672 -0.02892 0.00091 -0.02566 AFIX 43 H68 2 -0.450352 -0.145592 -0.157211 11.00000 -1.20000 AFIX 0 C69 1 -0.541830 -0.085359 -0.178259 11.00000 0.07543 0.04928 = 0.07502 -0.02804 0.01040 -0.03401 AFIX 43 H69 2 -0.511338 -0.047940 -0.172425 11.00000 -1.20000 AFIX 0 C70 1 -0.621955 -0.082214 -0.195305 11.00000 0.07030 0.02917 = 0.07960 -0.00912 0.02313 -0.01017 AFIX 43 H70 2 -0.647350 -0.042527 -0.200589 11.00000 -1.20000 AFIX 0 C71 1 -0.666171 -0.137105 -0.204885 11.00000 0.03948 0.03132 = 0.05341 -0.00037 0.00929 -0.00500 AFIX 43 H71 2 -0.721493 -0.134493 -0.217004 11.00000 -1.20000 AFIX 0 C72 1 -1.240492 -0.198882 -0.012006 11.00000 0.01512 0.03086 = 0.03167 -0.00200 0.00320 -0.00231 C73 1 -1.316363 -0.220746 0.065640 11.00000 0.04501 0.06218 = 0.03290 -0.00290 0.01422 -0.00617 AFIX 43 H73 2 -1.347588 -0.243516 0.092128 11.00000 -1.20000 AFIX 0 C74 1 -1.296454 -0.159836 0.067665 11.00000 0.04808 0.06095 = 0.03235 -0.01410 0.01187 -0.00123 AFIX 43 H74 2 -1.310722 -0.131006 0.096134 11.00000 -1.20000 AFIX 0 C75 1 -1.288872 -0.307656 -0.002128 11.00000 0.02457 0.03585 = 0.03303 0.00739 0.00764 -0.00565 C76 1 -1.234647 -0.352385 0.019002 11.00000 0.02155 0.04937 = 0.05142 0.01625 0.00344 -0.00485 C77 1 -1.244009 -0.414222 0.000586 11.00000 0.03150 0.04172 = 0.07248 0.02515 0.01058 0.00337 AFIX 43 H77 2 -1.209882 -0.446020 0.015763 11.00000 -1.20000 AFIX 0 C78 1 -1.301492 -0.430442 -0.039071 11.00000 0.02897 0.03486 = 0.07003 0.00041 0.01751 -0.01448 C79 1 -1.352246 -0.384360 -0.059276 11.00000 0.03507 0.04069 = 0.04149 -0.00088 0.00342 -0.01013 AFIX 43 H79 2 -1.392220 -0.395166 -0.086298 11.00000 -1.20000 AFIX 0 C80 1 -1.347052 -0.322631 -0.041538 11.00000 0.02244 0.04144 = 0.03565 0.00788 0.00468 -0.00486 C81 1 -1.167562 -0.333008 0.059336 11.00000 0.04286 0.07896 = 0.06499 0.02699 -0.01658 -0.00450 AFIX 137 H81A 2 -1.137217 -0.370289 0.071412 11.00000 -1.50000 H81B 2 -1.192283 -0.312475 0.091636 11.00000 -1.50000 H81C 2 -1.129960 -0.303776 0.040949 11.00000 -1.50000 AFIX 0 C82 1 -1.307039 -0.497704 -0.058880 11.00000 0.06460 0.03815 = 0.10971 -0.01052 0.02787 -0.01135 AFIX 137 H82A 2 -1.346128 -0.500396 -0.089657 11.00000 -1.50000 H82B 2 -1.325646 -0.524518 -0.028345 11.00000 -1.50000 H82C 2 -1.252934 -0.511764 -0.071466 11.00000 -1.50000 AFIX 0 C83 1 -1.403167 -0.272155 -0.064964 11.00000 0.02992 0.04547 = 0.04555 0.00657 0.00012 0.00162 AFIX 137 H83A 2 -1.443705 -0.291531 -0.089603 11.00000 -1.50000 H83B 2 -1.370533 -0.241652 -0.085903 11.00000 -1.50000 H83C 2 -1.431424 -0.250755 -0.034481 11.00000 -1.50000 AFIX 0 C84 1 -1.217210 -0.086096 0.007957 11.00000 0.02933 0.03015 = 0.03226 -0.00803 0.00071 0.00815 C85 1 -1.136421 -0.072989 0.024121 11.00000 0.03437 0.03798 = 0.03903 -0.01530 0.00041 0.00265 C86 1 -1.105527 -0.013809 0.012194 11.00000 0.04114 0.04176 = 0.04998 -0.01976 0.00403 -0.00418 AFIX 43 H86 2 -1.051373 -0.003678 0.023619 11.00000 -1.20000 AFIX 0 C87 1 -1.150881 0.030752 -0.015695 11.00000 0.05118 0.03412 = 0.05435 -0.01837 0.01589 0.00126 C88 1 -1.229392 0.015971 -0.031073 11.00000 0.06143 0.03325 = 0.04313 -0.00697 0.00506 0.01861 AFIX 43 H88 2 -1.260588 0.046524 -0.050527 11.00000 -1.20000 AFIX 0 C89 1 -1.265549 -0.041682 -0.019529 11.00000 0.03724 0.03746 = 0.04685 -0.01702 -0.00050 0.00981 C90 1 -1.085743 -0.122522 0.051273 11.00000 0.04248 0.06630 = 0.05377 -0.00363 -0.01080 0.00590 AFIX 137 H90A 2 -1.085615 -0.160359 0.028155 11.00000 -1.50000 H90B 2 -1.108884 -0.132468 0.087739 11.00000 -1.50000 H90C 2 -1.029437 -0.107281 0.055765 11.00000 -1.50000 AFIX 0 C91 1 -1.112045 0.093947 -0.029510 11.00000 0.07721 0.03740 = 0.09686 -0.00901 0.03395 -0.00817 AFIX 137 H91A 2 -1.060655 0.087149 -0.049700 11.00000 -1.50000 H91B 2 -1.100753 0.116879 0.004887 11.00000 -1.50000 H91C 2 -1.149765 0.118434 -0.052597 11.00000 -1.50000 AFIX 0 C92 1 -1.352692 -0.056613 -0.035410 11.00000 0.04420 0.06126 = 0.07151 0.00094 -0.01058 0.01975 AFIX 137 H92A 2 -1.378489 -0.019203 -0.051381 11.00000 -1.50000 H92B 2 -1.383229 -0.069751 -0.002385 11.00000 -1.50000 H92C 2 -1.353069 -0.090603 -0.062798 11.00000 -1.50000 AFIX 0 O1 6 -0.966335 -0.363825 -0.468737 11.00000 0.05355 0.07085 = 0.05204 -0.00241 -0.00305 -0.00529 C93 1 -0.912696 -0.257868 -0.463868 11.00000 0.05942 0.04999 = 0.06183 0.00681 -0.01104 -0.00185 AFIX 137 H93A 2 -0.921891 -0.253943 -0.503884 11.00000 -1.50000 H93B 2 -0.855347 -0.269195 -0.457003 11.00000 -1.50000 H93C 2 -0.924907 -0.217762 -0.445752 11.00000 -1.50000 AFIX 0 C94 1 -0.968809 -0.308927 -0.440394 11.00000 0.03994 0.05068 = 0.14249 -0.04461 -0.02727 0.00813 AFIX 23 H94A 2 -0.953119 -0.317034 -0.401383 11.00000 -1.20000 H94B 2 -1.025903 -0.293140 -0.440416 11.00000 -1.20000 AFIX 0 C95 1 -1.010726 -0.410514 -0.442032 11.00000 0.06101 0.08288 = 0.04054 0.02893 -0.00973 -0.04930 AFIX 23 H95A 2 -1.069737 -0.399627 -0.441644 11.00000 -1.20000 H95B 2 -0.991814 -0.414886 -0.403208 11.00000 -1.20000 AFIX 0 C96 1 -0.996936 -0.474257 -0.474574 11.00000 0.07602 0.08122 = 0.04774 0.02001 0.00627 0.00349 AFIX 137 H96A 2 -0.938491 -0.484940 -0.474267 11.00000 -1.50000 H96B 2 -1.015572 -0.469396 -0.512976 11.00000 -1.50000 H96C 2 -1.028217 -0.507865 -0.456611 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1bEt2O in Pca2(1) REM R1 = 0.0447 for 12125 Fo > 4sig(Fo) and 0.0602 for all 14563 data REM 997 parameters refined using 1 restraints END WGHT 0.0617 1.8639 REM Highest difference peak 0.857, deepest hole -0.331, 1-sigma level 0.061 Q1 1 -0.9540 -0.4368 -0.4594 11.00000 0.05 0.86 Q2 1 -0.6975 -0.2740 -0.2620 11.00000 0.05 0.84 Q3 1 -1.1941 -0.2146 -0.1259 11.00000 0.05 0.80 Q4 1 -0.9474 -0.3098 -0.4805 11.00000 0.05 0.72 Q5 1 -1.3996 -0.2209 -0.0771 11.00000 0.05 0.71 ; _database_code_depnum_ccdc_archive 'CCDC 953911' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2a _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H78 Cu N4 P Pt' _chemical_formula_weight 1337.02 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' Cu Cu 0.3201 1.2651 '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' _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 20.8431(14) _cell_length_b 19.8747(10) _cell_length_c 31.212(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 12929.4(14) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 52878 _cell_measurement_theta_min 1.630 _cell_measurement_theta_max 25.000 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_F_000 5472 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.060 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.010 _exptl_absorpt_coefficient_mu 2.561 _shelx_estimated_absorpt_T_min 0.861 _shelx_estimated_absorpt_T_max 0.975 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.5801 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'Bruker Apex 2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker Kappa Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 52878 _diffrn_reflns_av_unetI/netI 0.1478 _diffrn_reflns_av_R_equivalents 0.1630 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.630 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 0.973 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 0.973 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 0.973 _reflns_number_total 11373 _reflns_number_gt 6110 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker Apex 2 software package' _computing_cell_refinement 'Bruker Apex 2 software package' _computing_data_reduction 'Bruker Apex 2 software package' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'ORTEP and POV-Ray' _computing_publication_material 'SHELXL-2013 (Sheldrick, 2013)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0184P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 11373 _refine_ls_number_parameters 744 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1377 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1003 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.46319(2) 0.27323(2) 0.10541(2) 0.02041(8) Uani 1 1 d . . . . . Cu1 Cu 0.41810(6) 0.28948(5) 0.30226(3) 0.0367(3) Uani 1 1 d . . . . . P1 P 0.44348(10) 0.35183(9) 0.05507(7) 0.0237(5) Uani 1 1 d . . . . . N1 N 0.3646(3) 0.2675(3) 0.24856(18) 0.0220(15) Uani 1 1 d . . . . . N2 N 0.4825(3) 0.3426(3) 0.25835(19) 0.0236(16) Uani 1 1 d . . . . . N3 N 0.3719(3) 0.2471(2) 0.38560(17) 0.0167(15) Uani 1 1 d . . . . . N4 N 0.4517(3) 0.3127(2) 0.39261(19) 0.0176(14) Uani 1 1 d . . . . . C1 C 0.3090(4) 0.2387(3) 0.2386(3) 0.028(2) Uani 1 1 d . . . . . H1 H 0.2868 0.2137 0.2599 0.034 Uiso 1 1 calc R U . . . C2 C 0.2822(4) 0.2441(3) 0.1979(3) 0.027(2) Uani 1 1 d . . . . . H2 H 0.2418 0.2238 0.1924 0.033 Uiso 1 1 calc R U . . . C3 C 0.3135(4) 0.2786(4) 0.1651(2) 0.0255(19) Uani 1 1 d . . . . . H3 H 0.2951 0.2819 0.1373 0.031 Uiso 1 1 calc R U . . . C4 C 0.3722(4) 0.3080(3) 0.1742(2) 0.0201(19) Uani 1 1 d . . . . . C5 C 0.3932(4) 0.3002(3) 0.2163(2) 0.0176(18) Uani 1 1 d . . . . . C6 C 0.4511(4) 0.3373(3) 0.2215(2) 0.0195(19) Uani 1 1 d . . . . . C7 C 0.4666(4) 0.3668(3) 0.1824(2) 0.0217(18) Uani 1 1 d . . . . . C8 C 0.5205(4) 0.4080(4) 0.1825(3) 0.036(2) Uani 1 1 d . . . . . H8 H 0.5334 0.4315 0.1574 0.043 Uiso 1 1 calc R U . . . C9 C 0.5547(4) 0.4136(4) 0.2201(3) 0.042(3) Uani 1 1 d . . . . . H9 H 0.5927 0.4400 0.2205 0.050 Uiso 1 1 calc R U . . . C10 C 0.5350(4) 0.3818(4) 0.2574(3) 0.034(2) Uani 1 1 d . . . . . H10 H 0.5592 0.3879 0.2829 0.041 Uiso 1 1 calc R U . . . C11 C 0.4184(4) 0.3485(3) 0.1492(2) 0.0219(19) Uani 1 1 d . . . . . C12 C 0.3884(4) 0.4066(3) 0.1236(2) 0.028(2) Uani 1 1 d . . . . . H12A H 0.3458 0.3922 0.1129 0.033 Uiso 1 1 calc R U . . . H12B H 0.3817 0.4454 0.1430 0.033 Uiso 1 1 calc R U . . . C13 C 0.4294(4) 0.4289(3) 0.0859(2) 0.027(2) Uani 1 1 d . . . . . H13A H 0.4705 0.4484 0.0959 0.032 Uiso 1 1 calc R U . . . H13B H 0.4066 0.4627 0.0684 0.032 Uiso 1 1 calc R U . . . C14 C 0.5050(4) 0.3747(3) 0.0166(2) 0.022(2) Uani 1 1 d . . . . . C15 C 0.5647(4) 0.3957(4) 0.0330(3) 0.036(2) Uani 1 1 d . . . . . H15 H 0.5698 0.4001 0.0631 0.043 Uiso 1 1 calc R U . . . C16 C 0.6157(4) 0.4099(4) 0.0066(3) 0.038(2) Uani 1 1 d . . . . . H16 H 0.6556 0.4234 0.0185 0.046 Uiso 1 1 calc R U . . . C17 C 0.6086(4) 0.4043(3) -0.0368(3) 0.029(2) Uani 1 1 d . . . . . H17 H 0.6435 0.4145 -0.0552 0.035 Uiso 1 1 calc R U . . . C18 C 0.5505(4) 0.3840(4) -0.0540(3) 0.034(2) Uani 1 1 d . . . . . H18 H 0.5458 0.3799 -0.0841 0.041 Uiso 1 1 calc R U . . . C19 C 0.4992(4) 0.3696(4) -0.0271(3) 0.030(2) Uani 1 1 d . . . . . H19 H 0.4595 0.3560 -0.0392 0.036 Uiso 1 1 calc R U . . . C20 C 0.3693(4) 0.3443(4) 0.0246(2) 0.0232(19) Uani 1 1 d . . . . . C21 C 0.3460(4) 0.3940(4) -0.0038(2) 0.029(2) Uani 1 1 d . . . . . H21 H 0.3709 0.4333 -0.0086 0.034 Uiso 1 1 calc R U . . . C22 C 0.2888(4) 0.3868(4) -0.0243(3) 0.037(2) Uani 1 1 d . . . . . H22 H 0.2751 0.4204 -0.0439 0.045 Uiso 1 1 calc R U . . . C23 C 0.2504(4) 0.3311(4) -0.0171(3) 0.037(2) Uani 1 1 d . . . . . H23 H 0.2108 0.3261 -0.0318 0.045 Uiso 1 1 calc R U . . . C24 C 0.2707(4) 0.2828(4) 0.0119(3) 0.037(2) Uani 1 1 d . . . . . H24 H 0.2440 0.2452 0.0180 0.044 Uiso 1 1 calc R U . . . C25 C 0.3300(4) 0.2891(4) 0.0322(2) 0.032(2) Uani 1 1 d . . . . . H25 H 0.3438 0.2551 0.0515 0.038 Uiso 1 1 calc R U . . . C26 C 0.4971(4) 0.2032(4) 0.0635(2) 0.027(2) Uani 1 1 d . . . . . C27 C 0.5520(4) 0.2103(4) 0.0379(2) 0.031(2) Uani 1 1 d . . . . . H27 H 0.5779 0.2493 0.0412 0.037 Uiso 1 1 calc R U . . . C28 C 0.5695(4) 0.1623(4) 0.0080(3) 0.038(2) Uani 1 1 d . . . . . H28 H 0.6076 0.1686 -0.0082 0.046 Uiso 1 1 calc R U . . . C29 C 0.5328(5) 0.1056(4) 0.0013(3) 0.042(2) Uani 1 1 d . . . . . H29 H 0.5447 0.0736 -0.0199 0.051 Uiso 1 1 calc R U . . . C30 C 0.4785(5) 0.0963(4) 0.0258(3) 0.043(3) Uani 1 1 d . . . . . H30 H 0.4530 0.0571 0.0222 0.051 Uiso 1 1 calc R U . . . C31 C 0.4613(4) 0.1446(3) 0.0557(2) 0.029(2) Uani 1 1 d . . . . . H31 H 0.4232 0.1377 0.0719 0.035 Uiso 1 1 calc R U . . . C32 C 0.4855(4) 0.2087(3) 0.1549(2) 0.026(2) Uani 1 1 d . . . . . C33 C 0.4473(4) 0.1539(4) 0.1666(2) 0.032(2) Uani 1 1 d . . . . . H33 H 0.4097 0.1440 0.1507 0.039 Uiso 1 1 calc R U . . . C34 C 0.4638(5) 0.1138(4) 0.2014(3) 0.045(3) Uani 1 1 d . . . . . H34 H 0.4372 0.0767 0.2086 0.054 Uiso 1 1 calc R U . . . C35 C 0.5173(5) 0.1261(5) 0.2258(3) 0.048(3) Uani 1 1 d . . . . . H35 H 0.5280 0.0980 0.2494 0.058 Uiso 1 1 calc R U . . . C36 C 0.5549(4) 0.1801(5) 0.2150(3) 0.046(3) Uani 1 1 d . . . . . H36 H 0.5920 0.1896 0.2317 0.055 Uiso 1 1 calc R U . . . C37 C 0.5401(4) 0.2216(4) 0.1804(2) 0.0304(18) Uani 1 1 d . . . . . H37 H 0.5670 0.2588 0.1738 0.036 Uiso 1 1 calc R U . . . C38 C 0.4140(3) 0.2839(3) 0.3621(2) 0.0133(16) Uani 1 1 d . . . . . C39 C 0.3821(4) 0.2548(3) 0.4291(2) 0.0225(19) Uani 1 1 d . . . . . H39 H 0.3579 0.2348 0.4515 0.027 Uiso 1 1 calc R U . . . C40 C 0.4329(4) 0.2960(4) 0.4336(2) 0.027(2) Uani 1 1 d . . . . . H40 H 0.4519 0.3106 0.4597 0.032 Uiso 1 1 calc R U . . . C41 C 0.3188(4) 0.2080(3) 0.3682(2) 0.0203(19) Uani 1 1 d . . . . . C42 C 0.3284(4) 0.1405(3) 0.3595(2) 0.0227(19) Uani 1 1 d . . . . . C43 C 0.2752(4) 0.1042(4) 0.3448(3) 0.037(2) Uani 1 1 d . . . . . H43 H 0.2796 0.0578 0.3381 0.044 Uiso 1 1 calc R U . . . C44 C 0.2162(4) 0.1355(4) 0.3399(3) 0.043(3) Uani 1 1 d . . . . . H44 H 0.1805 0.1101 0.3302 0.052 Uiso 1 1 calc R U . . . C45 C 0.2087(4) 0.2026(4) 0.3489(3) 0.036(2) Uani 1 1 d . . . . . H45 H 0.1678 0.2231 0.3455 0.043 Uiso 1 1 calc R U . . . C46 C 0.2603(4) 0.2404(4) 0.3627(2) 0.028(2) Uani 1 1 d . . . . . C47 C 0.3932(4) 0.1070(4) 0.3652(3) 0.034(2) Uani 1 1 d . . . . . H47 H 0.4195 0.1358 0.3847 0.040 Uiso 1 1 calc R U . . . C48 C 0.4279(4) 0.1028(4) 0.3224(3) 0.048(3) Uani 1 1 d . . . . . H48A H 0.4008 0.0789 0.3017 0.071 Uiso 1 1 calc R U . . . H48B H 0.4683 0.0784 0.3261 0.071 Uiso 1 1 calc R U . . . H48C H 0.4368 0.1483 0.3119 0.071 Uiso 1 1 calc R U . . . C49 C 0.3883(4) 0.0371(4) 0.3853(3) 0.045(3) Uani 1 1 d . . . . . H49A H 0.3631 0.0397 0.4117 0.068 Uiso 1 1 calc R U . . . H49B H 0.4314 0.0204 0.3919 0.068 Uiso 1 1 calc R U . . . H49C H 0.3673 0.0063 0.3652 0.068 Uiso 1 1 calc R U . . . C50 C 0.2510(4) 0.3159(4) 0.3713(3) 0.034(2) Uani 1 1 d . . . . . H50 H 0.2927 0.3349 0.3814 0.041 Uiso 1 1 calc R U . . . C51 C 0.2321(5) 0.3522(4) 0.3307(3) 0.070(4) Uani 1 1 d . . . . . H51A H 0.2654 0.3458 0.3089 0.106 Uiso 1 1 calc R U . . . H51B H 0.2273 0.4004 0.3367 0.106 Uiso 1 1 calc R U . . . H51C H 0.1913 0.3342 0.3201 0.106 Uiso 1 1 calc R U . . . C52 C 0.2015(6) 0.3278(5) 0.4056(3) 0.084(4) Uani 1 1 d . . . . . H52A H 0.1596 0.3115 0.3956 0.125 Uiso 1 1 calc R U . . . H52B H 0.1987 0.3761 0.4117 0.125 Uiso 1 1 calc R U . . . H52C H 0.2138 0.3036 0.4316 0.125 Uiso 1 1 calc R U . . . C53 C 0.4986(4) 0.3641(3) 0.3844(2) 0.022(2) Uani 1 1 d . . . . . C54 C 0.5636(4) 0.3458(4) 0.3800(2) 0.025(2) Uani 1 1 d . . . . . C55 C 0.6069(4) 0.3978(4) 0.3746(2) 0.035(2) Uani 1 1 d . . . . . H55 H 0.6511 0.3874 0.3715 0.042 Uiso 1 1 calc R U . . . C56 C 0.5878(4) 0.4645(4) 0.3736(3) 0.040(2) Uani 1 1 d . . . . . H56 H 0.6190 0.4991 0.3708 0.048 Uiso 1 1 calc R U . . . C57 C 0.5233(4) 0.4811(4) 0.3766(3) 0.033(2) Uani 1 1 d . . . . . H57 H 0.5101 0.5268 0.3751 0.040 Uiso 1 1 calc R U . . . C58 C 0.4781(4) 0.4303(4) 0.3820(2) 0.026(2) Uani 1 1 d . . . . . C59 C 0.5841(4) 0.2726(4) 0.3813(2) 0.035(2) Uani 1 1 d . . . . . H59 H 0.5516 0.2474 0.3985 0.042 Uiso 1 1 calc R U . . . C60 C 0.5843(5) 0.2429(4) 0.3361(3) 0.061(3) Uani 1 1 d . . . . . H60A H 0.5408 0.2446 0.3242 0.091 Uiso 1 1 calc R U . . . H60B H 0.5988 0.1960 0.3373 0.091 Uiso 1 1 calc R U . . . H60C H 0.6134 0.2689 0.3179 0.091 Uiso 1 1 calc R U . . . C61 C 0.6500(4) 0.2615(4) 0.4021(3) 0.054(3) Uani 1 1 d . . . . . H61A H 0.6518 0.2855 0.4295 0.080 Uiso 1 1 calc R U . . . H61B H 0.6836 0.2786 0.3830 0.080 Uiso 1 1 calc R U . . . H61C H 0.6566 0.2133 0.4070 0.080 Uiso 1 1 calc R U . . . C62 C 0.4072(4) 0.4501(4) 0.3832(3) 0.035(2) Uani 1 1 d . . . . . H62 H 0.3824 0.4093 0.3918 0.042 Uiso 1 1 calc R U . . . C63 C 0.3850(4) 0.4700(4) 0.3387(3) 0.051(3) Uani 1 1 d . . . . . H63A H 0.4074 0.5109 0.3297 0.077 Uiso 1 1 calc R U . . . H63B H 0.3386 0.4783 0.3392 0.077 Uiso 1 1 calc R U . . . H63C H 0.3945 0.4335 0.3186 0.077 Uiso 1 1 calc R U . . . C64 C 0.3918(4) 0.5053(4) 0.4154(3) 0.055(3) Uani 1 1 d . . . . . H64A H 0.4115 0.5476 0.4061 0.082 Uiso 1 1 calc R U . . . H64B H 0.4089 0.4928 0.4436 0.082 Uiso 1 1 calc R U . . . H64C H 0.3452 0.5111 0.4174 0.082 Uiso 1 1 calc R U . . . C65 C 0.2835(4) 0.1210(4) 0.0785(3) 0.046(3) Uani 1 1 d . . . . . H65A H 0.2913 0.1678 0.0815 0.055 Uiso 1 1 calc R U . . . C66 C 0.2579(4) 0.0849(4) 0.1123(3) 0.044(3) Uani 1 1 d . . . . . H66A H 0.2484 0.1067 0.1387 0.053 Uiso 1 1 calc R U . . . C67 C 0.2462(4) 0.0167(4) 0.1074(3) 0.039(2) Uani 1 1 d . . . . . H67A H 0.2290 -0.0086 0.1305 0.046 Uiso 1 1 calc R U . . . C68 C 0.2596(5) -0.0142(5) 0.0690(3) 0.051(3) Uani 1 1 d . . . . . H68A H 0.2508 -0.0607 0.0653 0.061 Uiso 1 1 calc R U . . . C69 C 0.2858(5) 0.0226(5) 0.0361(3) 0.056(3) Uani 1 1 d . . . . . H69A H 0.2958 0.0011 0.0098 0.067 Uiso 1 1 calc R U . . . C70 C 0.2977(5) 0.0897(5) 0.0408(3) 0.059(3) Uani 1 1 d . . . . . H70A H 0.3158 0.1146 0.0179 0.071 Uiso 1 1 calc R U . . . C71 C 0.1950(4) -0.0485(4) 0.2312(2) 0.080(5) Uani 1 1 d G . . . . H71A H 0.1649 -0.0843 0.2332 0.096 Uiso 1 1 calc R U . . . C72 C 0.2597(4) -0.0626(2) 0.22343(19) 0.079(4) Uani 1 1 d G . . . . H72A H 0.2735 -0.1078 0.2201 0.095 Uiso 1 1 calc R U . . . C73 C 0.3040(3) -0.0100(4) 0.22054(19) 0.053(3) Uani 1 1 d G . . . . H73A H 0.3480 -0.0195 0.2152 0.064 Uiso 1 1 calc R U . . . C74 C 0.2837(3) 0.0566(3) 0.22544(19) 0.057(3) Uani 1 1 d G . . . . H74A H 0.3139 0.0923 0.2235 0.068 Uiso 1 1 calc R U . . . C75 C 0.2191(3) 0.0706(3) 0.23325(19) 0.055(3) Uani 1 1 d G . . . . H75A H 0.2053 0.1159 0.2366 0.066 Uiso 1 1 calc R U . . . C76 C 0.1747(3) 0.0180(4) 0.2361(2) 0.067(3) Uani 1 1 d G . . . . H76A H 0.1308 0.0276 0.2414 0.081 Uiso 1 1 calc R U . . . 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 0.02241(15) 0.02171(13) 0.01710(14) 0.00235(17) 0.00081(19) -0.00007(16) Cu1 0.0564(8) 0.0383(6) 0.0154(5) 0.0028(5) 0.0019(6) 0.0136(5) P1 0.0293(15) 0.0233(11) 0.0184(12) 0.0013(10) -0.0018(11) -0.0028(9) N1 0.024(4) 0.017(3) 0.024(4) -0.005(3) 0.003(3) -0.005(3) N2 0.026(5) 0.028(4) 0.017(4) -0.005(3) 0.003(3) 0.000(3) N3 0.014(4) 0.019(3) 0.017(4) 0.000(3) 0.002(3) 0.001(2) N4 0.018(4) 0.020(3) 0.015(3) 0.001(3) -0.002(4) -0.003(3) C1 0.028(5) 0.020(4) 0.038(5) -0.003(4) 0.003(4) -0.007(4) C2 0.022(5) 0.028(5) 0.031(5) -0.006(4) -0.002(4) -0.002(4) C3 0.032(5) 0.033(4) 0.012(4) 0.001(4) -0.006(4) 0.005(4) C4 0.021(5) 0.013(4) 0.026(5) -0.010(4) -0.005(4) 0.009(3) C5 0.019(5) 0.017(4) 0.017(4) -0.009(3) -0.001(4) 0.004(3) C6 0.024(5) 0.029(4) 0.006(4) 0.000(3) -0.001(4) -0.001(4) C7 0.032(5) 0.014(4) 0.019(4) 0.003(3) 0.009(5) -0.004(4) C8 0.041(7) 0.037(5) 0.030(5) 0.007(4) 0.003(5) -0.003(4) C9 0.034(6) 0.054(6) 0.038(6) 0.018(5) 0.003(5) -0.028(5) C10 0.025(5) 0.044(5) 0.032(5) 0.006(4) -0.013(5) -0.019(5) C11 0.027(5) 0.028(4) 0.011(4) 0.004(4) 0.001(4) 0.002(4) C12 0.030(5) 0.032(4) 0.021(4) 0.003(4) -0.002(4) 0.008(4) C13 0.042(6) 0.021(4) 0.018(4) 0.006(4) -0.011(4) -0.002(4) C14 0.034(6) 0.014(4) 0.018(5) 0.010(4) 0.003(4) 0.002(4) C15 0.031(6) 0.051(6) 0.025(5) 0.005(4) -0.007(5) -0.009(5) C16 0.022(6) 0.044(5) 0.049(7) 0.016(5) -0.003(5) -0.008(4) C17 0.022(5) 0.024(4) 0.042(6) 0.003(4) 0.007(5) 0.001(4) C18 0.043(7) 0.041(5) 0.019(5) 0.006(4) 0.003(5) -0.006(4) C19 0.032(6) 0.037(5) 0.022(5) 0.004(4) 0.001(5) -0.011(4) C20 0.021(5) 0.024(4) 0.025(5) -0.006(4) 0.001(4) 0.003(4) C21 0.028(6) 0.034(5) 0.024(5) 0.000(4) 0.008(5) 0.011(4) C22 0.039(6) 0.043(6) 0.029(6) -0.003(5) -0.005(5) 0.017(5) C23 0.022(5) 0.064(6) 0.025(5) -0.004(5) 0.003(5) 0.011(5) C24 0.016(5) 0.061(6) 0.034(5) -0.009(5) 0.017(4) -0.005(5) C25 0.040(6) 0.040(5) 0.015(4) -0.009(4) -0.002(4) 0.002(4) C26 0.030(6) 0.026(5) 0.025(5) 0.003(4) -0.007(4) 0.008(4) C27 0.034(6) 0.040(5) 0.019(4) -0.002(4) 0.003(4) 0.011(4) C28 0.030(6) 0.059(6) 0.026(5) 0.004(5) 0.008(5) 0.010(5) C29 0.050(7) 0.043(5) 0.034(6) -0.007(4) -0.007(6) 0.019(6) C30 0.063(8) 0.026(5) 0.040(6) -0.001(4) -0.007(6) 0.009(5) C31 0.035(5) 0.024(4) 0.030(5) 0.003(4) 0.002(5) -0.002(4) C32 0.032(5) 0.023(5) 0.022(5) -0.009(4) 0.015(4) 0.008(4) C33 0.043(7) 0.034(5) 0.019(5) 0.005(4) 0.004(5) 0.001(4) C34 0.067(7) 0.031(5) 0.037(6) 0.009(4) 0.022(7) -0.002(5) C35 0.058(8) 0.059(7) 0.027(6) 0.018(5) 0.008(6) 0.023(6) C36 0.022(6) 0.085(7) 0.032(6) 0.005(5) 0.001(5) 0.024(5) C37 0.025(5) 0.038(4) 0.028(4) 0.009(4) 0.009(5) 0.013(5) C38 0.007(4) 0.018(4) 0.015(4) 0.000(3) 0.006(3) 0.003(3) C39 0.023(5) 0.024(4) 0.020(4) 0.007(3) -0.001(4) 0.002(4) C40 0.028(5) 0.038(5) 0.015(4) 0.006(4) -0.002(4) 0.003(4) C41 0.016(5) 0.029(5) 0.016(4) -0.001(4) 0.002(4) -0.013(3) C42 0.028(5) 0.023(4) 0.017(4) -0.002(4) 0.001(4) -0.004(4) C43 0.041(6) 0.027(5) 0.044(6) -0.004(4) -0.008(5) -0.008(4) C44 0.025(6) 0.047(6) 0.058(7) 0.007(5) -0.025(5) -0.015(5) C45 0.007(5) 0.041(5) 0.059(6) 0.006(5) -0.009(5) -0.001(4) C46 0.026(5) 0.024(5) 0.034(5) 0.003(4) 0.000(4) 0.005(4) C47 0.031(6) 0.031(5) 0.039(6) -0.009(4) -0.014(5) 0.002(4) C48 0.041(7) 0.045(5) 0.056(7) -0.001(5) 0.017(6) 0.018(5) C49 0.063(7) 0.039(5) 0.033(6) -0.006(4) 0.009(5) 0.023(5) C50 0.018(5) 0.034(5) 0.050(6) -0.006(5) -0.003(5) 0.008(4) C51 0.100(10) 0.044(6) 0.066(8) 0.013(6) 0.016(8) 0.010(6) C52 0.108(11) 0.060(7) 0.083(9) 0.000(6) 0.038(8) 0.030(7) C53 0.026(5) 0.022(4) 0.019(5) 0.000(4) -0.002(4) -0.009(4) C54 0.019(5) 0.031(4) 0.025(5) 0.010(4) 0.000(4) -0.006(4) C55 0.029(6) 0.047(5) 0.028(5) 0.003(4) -0.008(5) -0.011(4) C56 0.039(6) 0.039(5) 0.042(6) 0.008(5) -0.005(5) -0.028(5) C57 0.033(6) 0.033(5) 0.033(5) 0.001(4) -0.012(5) -0.004(4) C58 0.023(6) 0.026(4) 0.030(5) -0.004(4) -0.008(4) -0.007(3) C59 0.015(4) 0.055(5) 0.037(5) 0.007(5) -0.001(4) 0.004(5) C60 0.058(8) 0.056(6) 0.069(7) -0.015(5) -0.010(6) 0.026(5) C61 0.041(6) 0.070(6) 0.051(7) -0.002(5) -0.003(5) 0.011(5) C62 0.038(6) 0.025(4) 0.041(6) 0.003(4) 0.003(5) 0.000(4) C63 0.040(7) 0.056(6) 0.058(7) 0.000(5) -0.022(6) 0.005(5) C64 0.034(6) 0.066(6) 0.064(7) -0.022(6) 0.001(6) 0.005(5) C65 0.042(7) 0.032(5) 0.065(8) 0.010(5) -0.013(6) -0.010(5) C66 0.035(6) 0.047(6) 0.050(7) -0.003(5) -0.009(6) 0.001(4) C67 0.027(5) 0.052(6) 0.038(5) 0.013(6) -0.010(6) -0.009(4) C68 0.047(7) 0.047(6) 0.058(7) 0.007(6) -0.019(6) -0.006(5) C69 0.048(8) 0.075(8) 0.045(7) -0.019(6) -0.005(6) -0.005(6) C70 0.060(8) 0.061(7) 0.056(8) -0.002(6) 0.006(7) -0.027(6) C71 0.105(12) 0.102(10) 0.032(7) -0.003(7) 0.005(8) -0.076(9) C72 0.159(15) 0.034(6) 0.045(7) 0.008(5) 0.021(9) -0.024(8) C73 0.060(8) 0.070(7) 0.029(6) 0.002(6) -0.010(6) 0.016(6) C74 0.064(8) 0.052(7) 0.054(7) -0.009(5) 0.002(7) -0.009(6) C75 0.058(8) 0.047(6) 0.061(8) 0.006(5) 0.010(7) -0.006(6) C76 0.058(9) 0.095(9) 0.048(7) 0.004(7) 0.007(6) -0.018(7) _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 C26 2.036(8) . ? Pt1 C32 2.061(8) . ? Pt1 C11 2.231(7) . ? Pt1 P1 2.253(2) . ? Cu1 C38 1.872(7) . ? Cu1 N1 2.060(6) . ? Cu1 N2 2.190(6) . ? P1 C14 1.815(8) . ? P1 C20 1.822(8) . ? P1 C13 1.832(7) . ? N1 C1 1.330(8) . ? N1 C5 1.339(9) . ? N2 C6 1.328(8) . ? N2 C10 1.344(9) . ? N3 C38 1.359(8) . ? N3 C39 1.383(8) . ? N3 C41 1.456(8) . ? N4 C38 1.362(8) . ? N4 C40 1.380(8) . ? N4 C53 1.437(8) . ? C1 C2 1.390(10) . ? C2 C3 1.395(9) . ? C3 C4 1.385(10) . ? C4 C5 1.396(9) . ? C4 C11 1.479(10) . ? C5 C6 1.423(10) . ? C6 C7 1.392(9) . ? C7 C8 1.391(10) . ? C7 C11 1.489(10) . ? C8 C9 1.378(10) . ? C9 C10 1.386(10) . ? C11 C12 1.535(9) . ? C12 C13 1.522(9) . ? C14 C19 1.372(10) . ? C14 C15 1.409(10) . ? C15 C16 1.374(11) . ? C16 C17 1.368(10) . ? C17 C18 1.383(10) . ? C18 C19 1.388(10) . ? C20 C25 1.390(10) . ? C20 C21 1.410(10) . ? C21 C22 1.362(11) . ? C22 C23 1.385(11) . ? C23 C24 1.387(10) . ? C24 C25 1.395(10) . ? C26 C31 1.403(10) . ? C26 C27 1.403(10) . ? C27 C28 1.384(10) . ? C28 C29 1.378(11) . ? C29 C30 1.380(11) . ? C30 C31 1.387(10) . ? C32 C33 1.398(10) . ? C32 C37 1.410(10) . ? C33 C34 1.391(10) . ? C34 C35 1.371(12) . ? C35 C36 1.371(12) . ? C36 C37 1.395(10) . ? C39 C40 1.345(10) . ? C41 C42 1.384(9) . ? C41 C46 1.389(10) . ? C42 C43 1.399(10) . ? C42 C47 1.516(10) . ? C43 C44 1.386(11) . ? C44 C45 1.372(10) . ? C45 C46 1.383(10) . ? C46 C50 1.536(9) . ? C47 C48 1.520(10) . ? C47 C49 1.528(10) . ? C50 C52 1.505(11) . ? C50 C51 1.511(11) . ? C53 C58 1.385(9) . ? C53 C54 1.409(10) . ? C54 C55 1.383(10) . ? C54 C59 1.516(10) . ? C55 C56 1.385(10) . ? C56 C57 1.387(11) . ? C57 C58 1.393(10) . ? C58 C62 1.529(11) . ? C59 C60 1.529(10) . ? C59 C61 1.536(10) . ? C62 C63 1.516(10) . ? C62 C64 1.522(10) . ? C65 C70 1.362(12) . ? C65 C66 1.383(11) . ? C66 C67 1.386(10) . ? C67 C68 1.375(11) . ? C68 C69 1.374(12) . ? C69 C70 1.363(11) . ? C71 C72 1.3977 . ? C71 C76 1.3978 . ? C72 C73 1.3978 . ? C73 C74 1.3977 . ? C74 C75 1.3977 . ? C75 C76 1.3979 . ? 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 C26 Pt1 C32 88.7(3) . . ? C26 Pt1 C11 175.5(3) . . ? C32 Pt1 C11 93.0(3) . . ? C26 Pt1 P1 95.1(2) . . ? C32 Pt1 P1 174.3(2) . . ? C11 Pt1 P1 83.42(18) . . ? C38 Cu1 N1 140.7(3) . . ? C38 Cu1 N2 132.9(3) . . ? N1 Cu1 N2 85.7(2) . . ? C14 P1 C20 105.9(4) . . ? C14 P1 C13 104.5(3) . . ? C20 P1 C13 101.9(4) . . ? C14 P1 Pt1 120.5(3) . . ? C20 P1 Pt1 117.5(3) . . ? C13 P1 Pt1 104.0(2) . . ? C1 N1 C5 114.9(7) . . ? C1 N1 Cu1 138.9(6) . . ? C5 N1 Cu1 105.5(5) . . ? C6 N2 C10 115.4(7) . . ? C6 N2 Cu1 101.6(5) . . ? C10 N2 Cu1 142.4(5) . . ? C38 N3 C39 111.8(6) . . ? C38 N3 C41 125.2(6) . . ? C39 N3 C41 122.9(6) . . ? C38 N4 C40 112.6(6) . . ? C38 N4 C53 124.5(6) . . ? C40 N4 C53 122.0(6) . . ? N1 C1 C2 122.1(7) . . ? C1 C2 C3 121.4(8) . . ? C4 C3 C2 118.1(7) . . ? C3 C4 C5 115.0(7) . . ? C3 C4 C11 134.3(7) . . ? C5 C4 C11 110.7(7) . . ? N1 C5 C4 128.5(7) . . ? N1 C5 C6 123.0(7) . . ? C4 C5 C6 108.4(7) . . ? N2 C6 C7 127.7(7) . . ? N2 C6 C5 123.9(7) . . ? C7 C6 C5 108.4(7) . . ? C8 C7 C6 115.7(7) . . ? C8 C7 C11 133.6(7) . . ? C6 C7 C11 110.6(7) . . ? C9 C8 C7 117.8(8) . . ? C8 C9 C10 121.7(8) . . ? N2 C10 C9 121.6(8) . . ? C4 C11 C7 101.8(6) . . ? C4 C11 C12 114.6(7) . . ? C7 C11 C12 117.0(6) . . ? C4 C11 Pt1 103.3(4) . . ? C7 C11 Pt1 107.9(5) . . ? C12 C11 Pt1 110.9(5) . . ? C13 C12 C11 113.0(6) . . ? C12 C13 P1 104.7(5) . . ? C19 C14 C15 117.4(8) . . ? C19 C14 P1 125.3(7) . . ? C15 C14 P1 117.1(6) . . ? C16 C15 C14 121.7(8) . . ? C17 C16 C15 119.6(9) . . ? C16 C17 C18 120.1(8) . . ? C17 C18 C19 120.0(8) . . ? C14 C19 C18 121.2(8) . . ? C25 C20 C21 117.2(8) . . ? C25 C20 P1 118.4(6) . . ? C21 C20 P1 124.2(6) . . ? C22 C21 C20 121.6(8) . . ? C21 C22 C23 120.9(8) . . ? C22 C23 C24 118.9(8) . . ? C23 C24 C25 120.3(8) . . ? C20 C25 C24 121.1(8) . . ? C31 C26 C27 114.7(7) . . ? C31 C26 Pt1 119.6(6) . . ? C27 C26 Pt1 125.4(6) . . ? C28 C27 C26 122.0(8) . . ? C29 C28 C27 121.4(8) . . ? C28 C29 C30 118.7(8) . . ? C29 C30 C31 119.5(8) . . ? C30 C31 C26 123.7(9) . . ? C33 C32 C37 117.0(7) . . ? C33 C32 Pt1 123.5(6) . . ? C37 C32 Pt1 119.5(6) . . ? C34 C33 C32 120.6(9) . . ? C35 C34 C33 122.2(9) . . ? C34 C35 C36 117.9(8) . . ? C35 C36 C37 121.7(9) . . ? C36 C37 C32 120.6(8) . . ? N3 C38 N4 102.8(6) . . ? N3 C38 Cu1 126.9(5) . . ? N4 C38 Cu1 130.3(5) . . ? C40 C39 N3 107.0(7) . . ? C39 C40 N4 105.8(7) . . ? C42 C41 C46 123.5(7) . . ? C42 C41 N3 118.7(7) . . ? C46 C41 N3 117.7(6) . . ? C41 C42 C43 116.7(7) . . ? C41 C42 C47 122.1(7) . . ? C43 C42 C47 121.2(7) . . ? C44 C43 C42 120.5(7) . . ? C45 C44 C43 121.0(8) . . ? C44 C45 C46 120.2(8) . . ? C45 C46 C41 118.0(7) . . ? C45 C46 C50 119.1(7) . . ? C41 C46 C50 122.9(7) . . ? C42 C47 C48 110.2(7) . . ? C42 C47 C49 112.8(7) . . ? C48 C47 C49 110.0(6) . . ? C52 C50 C51 110.0(7) . . ? C52 C50 C46 111.3(7) . . ? C51 C50 C46 110.8(7) . . ? C58 C53 C54 122.5(7) . . ? C58 C53 N4 118.3(7) . . ? C54 C53 N4 119.1(6) . . ? C55 C54 C53 116.5(7) . . ? C55 C54 C59 122.4(8) . . ? C53 C54 C59 121.1(6) . . ? C54 C55 C56 122.1(8) . . ? C55 C56 C57 120.3(7) . . ? C56 C57 C58 119.5(7) . . ? C53 C58 C57 119.1(7) . . ? C53 C58 C62 122.9(7) . . ? C57 C58 C62 118.0(7) . . ? C54 C59 C60 110.4(6) . . ? C54 C59 C61 113.6(7) . . ? C60 C59 C61 109.3(7) . . ? C63 C62 C64 110.7(7) . . ? C63 C62 C58 109.9(7) . . ? C64 C62 C58 114.0(7) . . ? C70 C65 C66 120.4(9) . . ? C65 C66 C67 119.3(9) . . ? C68 C67 C66 120.0(8) . . ? C69 C68 C67 119.5(9) . . ? C70 C69 C68 120.8(9) . . ? C65 C70 C69 120.0(9) . . ? C72 C71 C76 120.0 . . ? C71 C72 C73 120.0 . . ? C74 C73 C72 120.0 . . ? C75 C74 C73 120.0 . . ? C74 C75 C76 120.0 . . ? C71 C76 C75 120.0 . . ? _refine_diff_density_max 1.164 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.136 _shelxl_version_number 2013-4 _iucr_refine_instructions_details ; TITL 2aBenzene in Pbca CELL 0.71073 20.8431 19.8747 31.2115 90.000 90.000 90.000 ZERR 8.00 0.0014 0.0010 0.0020 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N P Cu Pt UNIT 608 624 32 8 8 8 L.S. 10 SIZE 0.06 0.04 0.01 OMIT -3 50 OMIT 1 1 1 BOND BIND cu1 pt1 FMAP 2 PLAN 5 TEMP -123.140 ACTA WGHT 0.018400 FVAR 0.02752 PT1 6 0.463192 0.273228 0.105413 11.00000 0.02241 0.02171 = 0.01710 0.00235 0.00081 -0.00007 CU1 5 0.418101 0.289485 0.302262 11.00000 0.05640 0.03828 = 0.01539 0.00276 0.00191 0.01362 P1 4 0.443481 0.351829 0.055069 11.00000 0.02931 0.02330 = 0.01842 0.00131 -0.00183 -0.00277 N1 3 0.364578 0.267470 0.248561 11.00000 0.02448 0.01695 = 0.02445 -0.00548 0.00349 -0.00451 N2 3 0.482525 0.342582 0.258349 11.00000 0.02627 0.02765 = 0.01673 -0.00513 0.00301 0.00033 N3 3 0.371851 0.247070 0.385600 11.00000 0.01424 0.01934 = 0.01651 0.00023 0.00157 0.00056 N4 3 0.451746 0.312664 0.392612 11.00000 0.01778 0.02035 = 0.01454 0.00078 -0.00232 -0.00294 C1 1 0.308951 0.238723 0.238582 11.00000 0.02759 0.01994 = 0.03763 -0.00341 0.00253 -0.00740 AFIX 43 H1 2 0.286797 0.213737 0.259899 11.00000 -1.20000 AFIX 0 C2 1 0.282196 0.244090 0.197927 11.00000 0.02223 0.02812 = 0.03139 -0.00608 -0.00179 -0.00199 AFIX 43 H2 2 0.241763 0.223821 0.192379 11.00000 -1.20000 AFIX 0 C3 1 0.313491 0.278618 0.165114 11.00000 0.03191 0.03281 = 0.01184 0.00087 -0.00567 0.00526 AFIX 43 H3 2 0.295073 0.281869 0.137349 11.00000 -1.20000 AFIX 0 C4 1 0.372174 0.308025 0.174163 11.00000 0.02110 0.01339 = 0.02583 -0.01049 -0.00464 0.00918 C5 1 0.393222 0.300208 0.216331 11.00000 0.01917 0.01680 = 0.01672 -0.00889 -0.00147 0.00410 C6 1 0.451102 0.337261 0.221498 11.00000 0.02360 0.02912 = 0.00563 -0.00014 -0.00053 -0.00059 C7 1 0.466634 0.366763 0.182406 11.00000 0.03198 0.01445 = 0.01863 0.00296 0.00852 -0.00431 C8 1 0.520530 0.408002 0.182506 11.00000 0.04055 0.03678 = 0.03007 0.00707 0.00348 -0.00270 AFIX 43 H8 2 0.533391 0.431527 0.157440 11.00000 -1.20000 AFIX 0 C9 1 0.554667 0.413636 0.220128 11.00000 0.03366 0.05417 = 0.03795 0.01758 0.00254 -0.02831 AFIX 43 H9 2 0.592674 0.440012 0.220536 11.00000 -1.20000 AFIX 0 C10 1 0.535002 0.381821 0.257407 11.00000 0.02522 0.04425 = 0.03215 0.00631 -0.01316 -0.01926 AFIX 43 H10 2 0.559212 0.387907 0.282903 11.00000 -1.20000 AFIX 0 C11 1 0.418420 0.348542 0.149171 11.00000 0.02674 0.02786 = 0.01096 0.00447 0.00051 0.00212 C12 1 0.388389 0.406553 0.123650 11.00000 0.03031 0.03166 = 0.02071 0.00252 -0.00228 0.00782 AFIX 23 H12A 2 0.345832 0.392233 0.112913 11.00000 -1.20000 H12B 2 0.381731 0.445356 0.143036 11.00000 -1.20000 AFIX 0 C13 1 0.429436 0.428854 0.085888 11.00000 0.04204 0.02065 = 0.01847 0.00588 -0.01113 -0.00209 AFIX 23 H13A 2 0.470477 0.448386 0.095900 11.00000 -1.20000 H13B 2 0.406573 0.462745 0.068360 11.00000 -1.20000 AFIX 0 C14 1 0.504968 0.374735 0.016552 11.00000 0.03365 0.01382 = 0.01768 0.01003 0.00288 0.00223 C15 1 0.564682 0.395678 0.033015 11.00000 0.03112 0.05108 = 0.02504 0.00534 -0.00660 -0.00867 AFIX 43 H15 2 0.569802 0.400100 0.063128 11.00000 -1.20000 AFIX 0 C16 1 0.615675 0.409863 0.006625 11.00000 0.02238 0.04387 = 0.04904 0.01628 -0.00297 -0.00788 AFIX 43 H16 2 0.655628 0.423418 0.018461 11.00000 -1.20000 AFIX 0 C17 1 0.608550 0.404342 -0.036801 11.00000 0.02170 0.02402 = 0.04194 0.00333 0.00695 0.00146 AFIX 43 H17 2 0.643531 0.414494 -0.055213 11.00000 -1.20000 AFIX 0 C18 1 0.550525 0.384012 -0.053957 11.00000 0.04331 0.04053 = 0.01859 0.00576 0.00263 -0.00613 AFIX 43 H18 2 0.545766 0.379896 -0.084115 11.00000 -1.20000 AFIX 0 C19 1 0.499239 0.369620 -0.027104 11.00000 0.03161 0.03746 = 0.02216 0.00434 0.00118 -0.01133 AFIX 43 H19 2 0.459470 0.355987 -0.039178 11.00000 -1.20000 AFIX 0 C20 1 0.369292 0.344349 0.024570 11.00000 0.02080 0.02417 = 0.02459 -0.00577 0.00140 0.00344 C21 1 0.346043 0.393958 -0.003752 11.00000 0.02782 0.03408 = 0.02397 0.00034 0.00751 0.01143 AFIX 43 H21 2 0.370870 0.433317 -0.008589 11.00000 -1.20000 AFIX 0 C22 1 0.288814 0.386775 -0.024344 11.00000 0.03927 0.04340 = 0.02867 -0.00346 -0.00534 0.01715 AFIX 43 H22 2 0.275095 0.420431 -0.043919 11.00000 -1.20000 AFIX 0 C23 1 0.250372 0.331090 -0.017129 11.00000 0.02200 0.06428 = 0.02501 -0.00391 0.00304 0.01126 AFIX 43 H23 2 0.210751 0.326075 -0.031832 11.00000 -1.20000 AFIX 0 C24 1 0.270667 0.282775 0.011909 11.00000 0.01564 0.06080 = 0.03399 -0.00850 0.01667 -0.00522 AFIX 43 H24 2 0.244033 0.245197 0.018033 11.00000 -1.20000 AFIX 0 C25 1 0.330009 0.289090 0.032172 11.00000 0.04050 0.03990 = 0.01452 -0.00907 -0.00210 0.00170 AFIX 43 H25 2 0.343805 0.255085 0.051478 11.00000 -1.20000 AFIX 0 C26 1 0.497078 0.203182 0.063536 11.00000 0.02955 0.02637 = 0.02500 0.00257 -0.00741 0.00817 C27 1 0.552009 0.210335 0.037948 11.00000 0.03432 0.04020 = 0.01899 -0.00240 0.00301 0.01075 AFIX 43 H27 2 0.577945 0.249298 0.041248 11.00000 -1.20000 AFIX 0 C28 1 0.569528 0.162299 0.008037 11.00000 0.02958 0.05945 = 0.02574 0.00396 0.00792 0.01022 AFIX 43 H28 2 0.607650 0.168550 -0.008165 11.00000 -1.20000 AFIX 0 C29 1 0.532839 0.105603 0.001266 11.00000 0.04975 0.04306 = 0.03372 -0.00749 -0.00650 0.01862 AFIX 43 H29 2 0.544724 0.073559 -0.019879 11.00000 -1.20000 AFIX 0 C30 1 0.478491 0.096305 0.025816 11.00000 0.06277 0.02607 = 0.03989 -0.00118 -0.00679 0.00897 AFIX 43 H30 2 0.453014 0.057070 0.022242 11.00000 -1.20000 AFIX 0 C31 1 0.461334 0.144635 0.055736 11.00000 0.03472 0.02388 = 0.02980 0.00265 0.00245 -0.00229 AFIX 43 H31 2 0.423240 0.137716 0.071857 11.00000 -1.20000 AFIX 0 C32 1 0.485544 0.208739 0.154922 11.00000 0.03230 0.02282 = 0.02180 -0.00867 0.01472 0.00805 C33 1 0.447309 0.153939 0.166626 11.00000 0.04350 0.03418 = 0.01921 0.00547 0.00427 0.00147 AFIX 43 H33 2 0.409684 0.144013 0.150652 11.00000 -1.20000 AFIX 0 C34 1 0.463830 0.113815 0.201433 11.00000 0.06680 0.03102 = 0.03674 0.00872 0.02219 -0.00240 AFIX 43 H34 2 0.437179 0.076693 0.208569 11.00000 -1.20000 AFIX 0 C35 1 0.517319 0.126085 0.225782 11.00000 0.05800 0.05917 = 0.02670 0.01838 0.00817 0.02342 AFIX 43 H35 2 0.527999 0.098010 0.249361 11.00000 -1.20000 AFIX 0 C36 1 0.554928 0.180141 0.215047 11.00000 0.02174 0.08452 = 0.03219 0.00470 0.00093 0.02370 AFIX 43 H36 2 0.592044 0.189597 0.231655 11.00000 -1.20000 AFIX 0 C37 1 0.540087 0.221592 0.180373 11.00000 0.02496 0.03824 = 0.02789 0.00886 0.00915 0.01284 AFIX 43 H37 2 0.566961 0.258812 0.173845 11.00000 -1.20000 AFIX 0 C38 1 0.414022 0.283870 0.362076 11.00000 0.00671 0.01784 = 0.01532 0.00026 0.00616 0.00328 C39 1 0.382138 0.254768 0.429095 11.00000 0.02328 0.02418 = 0.01993 0.00708 -0.00134 0.00207 AFIX 43 H39 2 0.357946 0.234757 0.451524 11.00000 -1.20000 AFIX 0 C40 1 0.432896 0.295965 0.433624 11.00000 0.02757 0.03788 = 0.01482 0.00577 -0.00183 0.00269 AFIX 43 H40 2 0.451856 0.310555 0.459697 11.00000 -1.20000 AFIX 0 C41 1 0.318841 0.208039 0.368159 11.00000 0.01593 0.02920 = 0.01589 -0.00148 0.00152 -0.01272 C42 1 0.328386 0.140453 0.359547 11.00000 0.02819 0.02318 = 0.01685 -0.00153 0.00065 -0.00358 C43 1 0.275220 0.104223 0.344834 11.00000 0.04068 0.02672 = 0.04367 -0.00420 -0.00850 -0.00768 AFIX 43 H43 2 0.279586 0.057816 0.338147 11.00000 -1.20000 AFIX 0 C44 1 0.216214 0.135490 0.339933 11.00000 0.02550 0.04706 = 0.05766 0.00742 -0.02484 -0.01548 AFIX 43 H44 2 0.180463 0.110054 0.330234 11.00000 -1.20000 AFIX 0 C45 1 0.208679 0.202594 0.348877 11.00000 0.00697 0.04121 = 0.05944 0.00633 -0.00869 -0.00103 AFIX 43 H45 2 0.167833 0.223146 0.345539 11.00000 -1.20000 AFIX 0 C46 1 0.260342 0.240430 0.362738 11.00000 0.02629 0.02445 = 0.03403 0.00284 -0.00030 0.00532 C47 1 0.393207 0.106981 0.365192 11.00000 0.03121 0.03055 = 0.03905 -0.00948 -0.01389 0.00159 AFIX 13 H47 2 0.419465 0.135823 0.384730 11.00000 -1.20000 AFIX 0 C48 1 0.427863 0.102770 0.322419 11.00000 0.04082 0.04549 = 0.05640 -0.00126 0.01666 0.01773 AFIX 137 H48A 2 0.400832 0.078948 0.301684 11.00000 -1.50000 H48B 2 0.468344 0.078364 0.326102 11.00000 -1.50000 H48C 2 0.436755 0.148282 0.311897 11.00000 -1.50000 AFIX 0 C49 1 0.388318 0.037090 0.385309 11.00000 0.06297 0.03902 = 0.03324 -0.00619 0.00908 0.02286 AFIX 137 H49A 2 0.363083 0.039722 0.411749 11.00000 -1.50000 H49B 2 0.431437 0.020379 0.391907 11.00000 -1.50000 H49C 2 0.367301 0.006337 0.365175 11.00000 -1.50000 AFIX 0 C50 1 0.250966 0.315894 0.371251 11.00000 0.01828 0.03420 = 0.04989 -0.00576 -0.00304 0.00750 AFIX 13 H50 2 0.292730 0.334853 0.381397 11.00000 -1.20000 AFIX 0 C51 1 0.232094 0.352247 0.330662 11.00000 0.10020 0.04448 = 0.06649 0.01314 0.01593 0.01007 AFIX 137 H51A 2 0.265440 0.345765 0.308915 11.00000 -1.50000 H51B 2 0.227278 0.400383 0.336663 11.00000 -1.50000 H51C 2 0.191320 0.334178 0.320075 11.00000 -1.50000 AFIX 0 C52 1 0.201473 0.327810 0.405552 11.00000 0.10802 0.05986 = 0.08293 -0.00044 0.03773 0.02997 AFIX 137 H52A 2 0.159642 0.311540 0.395645 11.00000 -1.50000 H52B 2 0.198746 0.376075 0.411717 11.00000 -1.50000 H52C 2 0.213813 0.303573 0.431625 11.00000 -1.50000 AFIX 0 C53 1 0.498625 0.364090 0.384382 11.00000 0.02571 0.02211 = 0.01930 0.00013 -0.00202 -0.00931 C54 1 0.563578 0.345761 0.380032 11.00000 0.01908 0.03114 = 0.02499 0.00961 0.00003 -0.00577 C55 1 0.606883 0.397788 0.374627 11.00000 0.02879 0.04739 = 0.02821 0.00331 -0.00843 -0.01092 AFIX 43 H55 2 0.651138 0.387435 0.371536 11.00000 -1.20000 AFIX 0 C56 1 0.587774 0.464522 0.373578 11.00000 0.03906 0.03883 = 0.04219 0.00800 -0.00495 -0.02798 AFIX 43 H56 2 0.618976 0.499081 0.370756 11.00000 -1.20000 AFIX 0 C57 1 0.523320 0.481120 0.376627 11.00000 0.03319 0.03260 = 0.03307 0.00131 -0.01195 -0.00355 AFIX 43 H57 2 0.510140 0.526813 0.375085 11.00000 -1.20000 AFIX 0 C58 1 0.478070 0.430259 0.381967 11.00000 0.02294 0.02570 = 0.02992 -0.00350 -0.00834 -0.00694 C59 1 0.584068 0.272620 0.381276 11.00000 0.01477 0.05450 = 0.03657 0.00661 -0.00084 0.00369 AFIX 13 H59 2 0.551627 0.247350 0.398547 11.00000 -1.20000 AFIX 0 C60 1 0.584301 0.242863 0.336100 11.00000 0.05750 0.05607 = 0.06877 -0.01453 -0.01039 0.02616 AFIX 137 H60A 2 0.540838 0.244638 0.324176 11.00000 -1.50000 H60B 2 0.598774 0.195986 0.337303 11.00000 -1.50000 H60C 2 0.613439 0.268892 0.317865 11.00000 -1.50000 AFIX 0 C61 1 0.650004 0.261495 0.402070 11.00000 0.04054 0.06991 = 0.05052 -0.00247 -0.00272 0.01125 AFIX 137 H61A 2 0.651815 0.285476 0.429479 11.00000 -1.50000 H61B 2 0.683619 0.278616 0.383015 11.00000 -1.50000 H61C 2 0.656649 0.213296 0.406984 11.00000 -1.50000 AFIX 0 C62 1 0.407243 0.450137 0.383207 11.00000 0.03838 0.02524 = 0.04083 0.00337 0.00264 0.00034 AFIX 13 H62 2 0.382354 0.409296 0.391805 11.00000 -1.20000 AFIX 0 C63 1 0.384967 0.469978 0.338732 11.00000 0.03998 0.05635 = 0.05806 0.00025 -0.02169 0.00462 AFIX 137 H63A 2 0.407390 0.510933 0.329702 11.00000 -1.50000 H63B 2 0.338632 0.478324 0.339161 11.00000 -1.50000 H63C 2 0.394478 0.433504 0.318579 11.00000 -1.50000 AFIX 0 C64 1 0.391845 0.505316 0.415440 11.00000 0.03437 0.06625 = 0.06394 -0.02187 0.00113 0.00539 AFIX 137 H64A 2 0.411525 0.547628 0.406101 11.00000 -1.50000 H64B 2 0.408863 0.492785 0.443601 11.00000 -1.50000 H64C 2 0.345236 0.511053 0.417366 11.00000 -1.50000 AFIX 0 C65 1 0.283522 0.120962 0.078502 11.00000 0.04168 0.03172 = 0.06534 0.00975 -0.01309 -0.01024 AFIX 43 H65A 2 0.291309 0.167815 0.081549 11.00000 -1.20000 AFIX 0 C66 1 0.257904 0.084949 0.112333 11.00000 0.03469 0.04737 = 0.05032 -0.00269 -0.00946 0.00136 AFIX 43 H66A 2 0.248421 0.106720 0.138679 11.00000 -1.20000 AFIX 0 C67 1 0.246218 0.016746 0.107376 11.00000 0.02671 0.05178 = 0.03758 0.01297 -0.01030 -0.00856 AFIX 43 H67A 2 0.228979 -0.008596 0.130473 11.00000 -1.20000 AFIX 0 C68 1 0.259588 -0.014213 0.069008 11.00000 0.04717 0.04708 = 0.05807 0.00719 -0.01882 -0.00643 AFIX 43 H68A 2 0.250759 -0.060737 0.065260 11.00000 -1.20000 AFIX 0 C69 1 0.285819 0.022627 0.036114 11.00000 0.04767 0.07466 = 0.04499 -0.01853 -0.00451 -0.00476 AFIX 43 H69A 2 0.295821 0.001113 0.009767 11.00000 -1.20000 AFIX 0 C70 1 0.297655 0.089688 0.040849 11.00000 0.05970 0.06126 = 0.05612 -0.00189 0.00596 -0.02716 AFIX 43 H70A 2 0.315774 0.114608 0.017866 11.00000 -1.20000 AFIX 6 C71 1 0.195031 -0.048532 0.231236 11.00000 0.10534 0.10207 = 0.03177 -0.00256 0.00515 -0.07568 AFIX 43 H71A 2 0.164887 -0.084252 0.233203 11.00000 -1.20000 AFIX 5 C72 1 0.259696 -0.062555 0.223434 11.00000 0.15869 0.03376 = 0.04493 0.00779 0.02117 -0.02398 AFIX 43 H72A 2 0.273505 -0.107806 0.220100 11.00000 -1.20000 AFIX 5 C73 1 0.304047 -0.009997 0.220538 11.00000 0.06037 0.07018 = 0.02935 0.00159 -0.00953 0.01557 AFIX 43 H73A 2 0.347998 -0.019531 0.215234 11.00000 -1.20000 AFIX 5 C74 1 0.283739 0.056583 0.225445 11.00000 0.06367 0.05241 = 0.05393 -0.00931 0.00213 -0.00937 AFIX 43 H74A 2 0.313884 0.092301 0.223476 11.00000 -1.20000 AFIX 5 C75 1 0.219075 0.070606 0.233249 11.00000 0.05808 0.04662 = 0.06078 0.00647 0.00974 -0.00628 AFIX 43 H75A 2 0.205269 0.115857 0.236586 11.00000 -1.20000 AFIX 5 C76 1 0.174716 0.018048 0.236144 11.00000 0.05770 0.09550 = 0.04822 0.00431 0.00652 -0.01817 AFIX 43 H76A 2 0.130765 0.027581 0.241447 11.00000 -1.20000 AFIX 0 HKLF 4 REM 2aBenzene in Pbca REM R1 = 0.0526 for 6110 Fo > 4sig(Fo) and 0.1377 for all 11373 data REM 744 parameters refined using 0 restraints END WGHT 0.0183 0.0000 REM Highest difference peak 1.164, deepest hole -0.798, 1-sigma level 0.136 Q1 1 0.4637 0.1827 0.1084 11.00000 0.05 1.16 Q2 1 0.4585 0.3219 0.1066 11.00000 0.05 0.82 Q3 1 0.4631 0.2284 0.1869 11.00000 0.05 0.79 Q4 1 0.4629 0.2117 0.1094 11.00000 0.05 0.69 Q5 1 0.4704 0.2987 0.1395 11.00000 0.05 0.63 ; _vrf_PLAT220_2a ; RESPONSE: The isopropyl carbons have a large range of thermal motions, while the metal-bound carbons have a much smaller range of thermal motions. Consequently, it is reasonable to have a large Ueq(max)/Ueq(min) ratio for carbons. ; _database_code_depnum_ccdc_archive 'CCDC 953912' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2b _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H54 Cu N4 P Pt' _chemical_formula_weight 1096.65 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' Cu Cu 0.3201 1.2651 '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' _space_group_crystal_system tetragonal _space_group_IT_number 96 _space_group_name_H-M_alt 'P 43 21 2' _space_group_name_Hall 'P 4nw 2abw' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 26.3673(5) _cell_length_b 26.3673(5) _cell_length_c 15.2955(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 10634.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 82809 _cell_measurement_theta_min 1.545 _cell_measurement_theta_max 24.999 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_F_000 4416 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_absorpt_coefficient_mu 3.097 _shelx_estimated_absorpt_T_min 0.457 _shelx_estimated_absorpt_T_max 0.747 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.5947 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'Bruker Apex 2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker Kappa Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 82809 _diffrn_reflns_av_unetI/netI 0.0480 _diffrn_reflns_av_R_equivalents 0.0771 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.545 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.970 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.970 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.970 _reflns_number_total 9346 _reflns_number_gt 8281 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.788 _reflns_Friedel_fraction_max 0.999 _reflns_Friedel_fraction_full 0.970 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker Apex 2 software package' _computing_cell_refinement 'Bruker Apex 2 software package' _computing_data_reduction 'Bruker Apex 2 software package' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'ORTEP and POV-Ray' _computing_publication_material 'SHELXL-2013 (Sheldrick, 2013)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0342P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _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 x determined using 3355 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.006(4) _chemical_absolute_configuration ad _refine_ls_number_reflns 9346 _refine_ls_number_parameters 601 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.48306(2) 0.78822(2) 0.50024(2) 0.02130(8) Uani 1 1 d . . . . . Cu1 Cu 0.4751(3) 0.75415(16) 0.8686(4) 0.0410(11) Uani 0.5 1 d . . P A 1 Cu1A Cu 0.4734(3) 0.77597(15) 0.8728(4) 0.0397(11) Uani 0.5 1 d . . P A 2 P1 P 0.53468(7) 0.81741(7) 0.39293(11) 0.0230(4) Uani 1 1 d . . . . . N1 N 0.5199(2) 0.7259(2) 0.7791(3) 0.0288(14) Uani 1 1 d . . . . . N2 N 0.4951(2) 0.8330(2) 0.7945(3) 0.0269(14) Uani 1 1 d . . . . . N3 N 0.4923(2) 0.7487(2) 1.0477(3) 0.0282(14) Uani 1 1 d . . . . . N4 N 0.4119(2) 0.7535(2) 1.0340(3) 0.0257(14) Uani 1 1 d . . . . . C1 C 0.5353(3) 0.6788(3) 0.7622(5) 0.0358(19) Uani 1 1 d . . . . . H1 H 0.5282 0.6528 0.8034 0.043 Uiso 1 1 calc R U . . . C2 C 0.5616(3) 0.6664(3) 0.6864(5) 0.038(2) Uani 1 1 d . . . . . H2 H 0.5732 0.6326 0.6782 0.045 Uiso 1 1 calc R U . . . C3 C 0.5712(3) 0.7022(3) 0.6227(5) 0.0346(18) Uani 1 1 d . . . . . H3 H 0.5887 0.6932 0.5706 0.042 Uiso 1 1 calc R U . . . C4 C 0.5546(3) 0.7523(3) 0.6363(4) 0.0281(17) Uani 1 1 d . . . . . C5 C 0.5312(2) 0.7608(3) 0.7190(4) 0.0246(17) Uani 1 1 d . . . . . C6 C 0.5182(2) 0.8131(3) 0.7247(4) 0.0227(15) Uani 1 1 d . . . . . C7 C 0.5322(2) 0.8371(3) 0.6461(4) 0.0245(16) Uani 1 1 d . . . . . C8 C 0.5225(3) 0.8894(3) 0.6428(5) 0.0292(17) Uani 1 1 d . . . . . H8 H 0.5312 0.9090 0.5928 0.035 Uiso 1 1 calc R U . . . C9 C 0.4999(3) 0.9112(3) 0.7150(5) 0.037(2) Uani 1 1 d . . . . . H9 H 0.4932 0.9466 0.7143 0.044 Uiso 1 1 calc R U . . . C10 C 0.4865(3) 0.8832(3) 0.7890(5) 0.0346(19) Uani 1 1 d . . . . . H10 H 0.4707 0.9001 0.8367 0.042 Uiso 1 1 calc R U . . . C11 C 0.5529(3) 0.7992(3) 0.5845(4) 0.0258(17) Uani 1 1 d . . . . . C12 C 0.5995(3) 0.8108(3) 0.5287(4) 0.0315(19) Uani 1 1 d . . . . . H12A H 0.6250 0.8279 0.5659 0.038 Uiso 1 1 calc R U . . . H12B H 0.6144 0.7783 0.5089 0.038 Uiso 1 1 calc R U . . . C13 C 0.5897(3) 0.8436(3) 0.4493(4) 0.0312(18) Uani 1 1 d . . . . . H13A H 0.6196 0.8434 0.4101 0.037 Uiso 1 1 calc R U . . . H13B H 0.5829 0.8790 0.4673 0.037 Uiso 1 1 calc R U . . . C14 C 0.5610(3) 0.7648(3) 0.3286(4) 0.0245(17) Uani 1 1 d . . . . . C15 C 0.5895(2) 0.7713(2) 0.2519(5) 0.0272(15) Uani 1 1 d . . . . . H15 H 0.5953 0.8045 0.2299 0.033 Uiso 1 1 calc R U . . . C16 C 0.6090(3) 0.7301(3) 0.2081(5) 0.0312(18) Uani 1 1 d . . . . . H16 H 0.6277 0.7351 0.1557 0.037 Uiso 1 1 calc R U . . . C17 C 0.6019(3) 0.6820(3) 0.2393(5) 0.046(2) Uani 1 1 d . . . . . H17 H 0.6155 0.6538 0.2087 0.055 Uiso 1 1 calc R U . . . C18 C 0.5747(4) 0.6745(3) 0.3158(6) 0.053(3) Uani 1 1 d . . . . . H18 H 0.5701 0.6413 0.3383 0.063 Uiso 1 1 calc R U . . . C19 C 0.5544(3) 0.7157(3) 0.3588(5) 0.041(2) Uani 1 1 d . . . . . H19 H 0.5354 0.7103 0.4107 0.049 Uiso 1 1 calc R U . . . C20 C 0.5193(3) 0.8646(3) 0.3089(4) 0.0268(16) Uani 1 1 d . . . . . C21 C 0.5530(3) 0.9032(3) 0.2857(4) 0.0324(18) Uani 1 1 d . . . . . H21 H 0.5846 0.9064 0.3149 0.039 Uiso 1 1 calc R U . . . C22 C 0.5399(3) 0.9369(3) 0.2195(5) 0.041(2) Uani 1 1 d . . . . . H22 H 0.5632 0.9627 0.2032 0.049 Uiso 1 1 calc R U . . . C23 C 0.4951(3) 0.9336(3) 0.1781(5) 0.042(2) Uani 1 1 d . . . . . H23 H 0.4868 0.9571 0.1331 0.051 Uiso 1 1 calc R U . . . C24 C 0.4610(3) 0.8963(3) 0.2011(5) 0.042(2) Uani 1 1 d . . . . . H24 H 0.4294 0.8942 0.1716 0.051 Uiso 1 1 calc R U . . . C25 C 0.4721(3) 0.8616(3) 0.2662(4) 0.0333(19) Uani 1 1 d . . . . . H25 H 0.4482 0.8362 0.2819 0.040 Uiso 1 1 calc R U . . . C26 C 0.4207(3) 0.7749(3) 0.4254(4) 0.0246(16) Uani 1 1 d . . . . . C27 C 0.3786(3) 0.8074(3) 0.4254(5) 0.041(2) Uani 1 1 d . . . . . H27 H 0.3800 0.8377 0.4590 0.049 Uiso 1 1 calc R U . . . C28 C 0.3352(3) 0.7970(4) 0.3784(5) 0.056(3) Uani 1 1 d . . . . . H28 H 0.3076 0.8200 0.3805 0.067 Uiso 1 1 calc R U . . . C29 C 0.3315(3) 0.7551(4) 0.3300(5) 0.057(3) Uani 1 1 d . . . . . H29 H 0.3018 0.7489 0.2965 0.068 Uiso 1 1 calc R U . . . C30 C 0.3722(4) 0.7198(4) 0.3289(5) 0.052(3) Uani 1 1 d . . . . . H30 H 0.3694 0.6893 0.2964 0.063 Uiso 1 1 calc R U . . . C31 C 0.4162(3) 0.7300(3) 0.3755(5) 0.0363(19) Uani 1 1 d . . . . . H31 H 0.4436 0.7066 0.3738 0.044 Uiso 1 1 calc R U . . . C32 C 0.4402(2) 0.7571(3) 0.6004(4) 0.0226(16) Uani 1 1 d . . . . . C33 C 0.4137(3) 0.7879(3) 0.6594(4) 0.0285(16) Uani 1 1 d . . . . . H33 H 0.4137 0.8236 0.6506 0.034 Uiso 1 1 calc R U . . . C34 C 0.3877(3) 0.7685(3) 0.7297(5) 0.037(2) Uani 1 1 d . . . . . H34 H 0.3703 0.7906 0.7685 0.044 Uiso 1 1 calc R U . . . C35 C 0.3869(3) 0.7161(3) 0.7441(5) 0.044(2) Uani 1 1 d . . . . . H35 H 0.3694 0.7021 0.7927 0.053 Uiso 1 1 calc R U . . . C36 C 0.4125(3) 0.6851(3) 0.6851(5) 0.0392(19) Uani 1 1 d . . . . . H36 H 0.4122 0.6494 0.6934 0.047 Uiso 1 1 calc R U . . . C37 C 0.4385(3) 0.7056(3) 0.6141(4) 0.0260(16) Uani 1 1 d . . . . . H37 H 0.4554 0.6835 0.5745 0.031 Uiso 1 1 calc R U . . . C38 C 0.4547(3) 0.7551(3) 0.9867(4) 0.0281(16) Uani 1 1 d . . . . . C39 C 0.4221(3) 0.7475(3) 1.1227(5) 0.034(2) Uani 1 1 d . . . . . H39 H 0.3979 0.7465 1.1687 0.041 Uiso 1 1 calc R U . . . C40 C 0.4725(3) 0.7435(3) 1.1308(5) 0.037(2) Uani 1 1 d . . . . . H40 H 0.4910 0.7381 1.1833 0.044 Uiso 1 1 calc R U . . . C41 C 0.5440(3) 0.7461(3) 1.0199(4) 0.0293(18) Uani 1 1 d . . . . . C42 C 0.5717(2) 0.7894(3) 1.0088(5) 0.0283(16) Uani 1 1 d . . . . . C43 C 0.6185(3) 0.7854(3) 0.9700(5) 0.0373(19) Uani 1 1 d . . . . . H43 H 0.6382 0.8153 0.9623 0.045 Uiso 1 1 calc R U . . . C44 C 0.6382(3) 0.7394(3) 0.9415(5) 0.038(2) Uani 1 1 d . . . . . C45 C 0.6098(3) 0.6959(3) 0.9553(4) 0.0362(19) Uani 1 1 d . . . . . H45 H 0.6231 0.6641 0.9373 0.043 Uiso 1 1 calc R U . . . C46 C 0.5622(3) 0.6976(3) 0.9949(5) 0.0321(16) Uani 1 1 d . . . . . C47 C 0.5507(3) 0.8407(3) 1.0360(5) 0.045(2) Uani 1 1 d . . . . . H47A H 0.5273 0.8530 0.9910 0.068 Uiso 1 1 calc R U . . . H47B H 0.5787 0.8648 1.0428 0.068 Uiso 1 1 calc R U . . . H47C H 0.5326 0.8373 1.0916 0.068 Uiso 1 1 calc R U . . . C48 C 0.6886(3) 0.7362(4) 0.8948(6) 0.053(3) Uani 1 1 d . . . . . H48A H 0.7102 0.7112 0.9239 0.079 Uiso 1 1 calc R U . . . H48B H 0.7052 0.7695 0.8962 0.079 Uiso 1 1 calc R U . . . H48C H 0.6830 0.7260 0.8339 0.079 Uiso 1 1 calc R U . . . C49 C 0.5307(3) 0.6505(3) 1.0070(6) 0.049(2) Uani 1 1 d . . . . . H49A H 0.4963 0.6567 0.9856 0.073 Uiso 1 1 calc R U . . . H49B H 0.5295 0.6417 1.0692 0.073 Uiso 1 1 calc R U . . . H49C H 0.5460 0.6225 0.9742 0.073 Uiso 1 1 calc R U . . . C50 C 0.3615(2) 0.7538(3) 0.9959(5) 0.0291(15) Uani 1 1 d . . . . . C51 C 0.3372(3) 0.7989(3) 0.9767(4) 0.0334(19) Uani 1 1 d . . . . . C52 C 0.2903(3) 0.7959(3) 0.9380(5) 0.040(2) Uani 1 1 d . . . . . H52 H 0.2732 0.8265 0.9236 0.048 Uiso 1 1 calc R U . . . C53 C 0.2668(3) 0.7499(3) 0.9187(5) 0.041(2) Uani 1 1 d . . . . . C54 C 0.2923(3) 0.7059(4) 0.9409(4) 0.0431(19) Uani 1 1 d . . . . . H54 H 0.2763 0.6742 0.9301 0.052 Uiso 1 1 calc R U . . . C55 C 0.3402(3) 0.7064(3) 0.9782(4) 0.0317(18) Uani 1 1 d . . . . . C56 C 0.3610(3) 0.8482(3) 0.9970(7) 0.051(2) Uani 1 1 d . . . . . H56A H 0.3720 0.8485 1.0582 0.076 Uiso 1 1 calc R U . . . H56B H 0.3365 0.8755 0.9874 0.076 Uiso 1 1 calc R U . . . H56C H 0.3905 0.8534 0.9589 0.076 Uiso 1 1 calc R U . . . C57 C 0.2148(3) 0.7468(4) 0.8764(6) 0.059(3) Uani 1 1 d . . . . . H57A H 0.1921 0.7268 0.9136 0.089 Uiso 1 1 calc R U . . . H57B H 0.2178 0.7305 0.8190 0.089 Uiso 1 1 calc R U . . . H57C H 0.2010 0.7810 0.8692 0.089 Uiso 1 1 calc R U . . . C58 C 0.3684(3) 0.6577(3) 0.9981(6) 0.046(2) Uani 1 1 d . . . . . H58A H 0.3977 0.6547 0.9590 0.069 Uiso 1 1 calc R U . . . H58B H 0.3457 0.6287 0.9892 0.069 Uiso 1 1 calc R U . . . H58C H 0.3800 0.6582 1.0589 0.069 Uiso 1 1 calc R U . . . 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 0.01817(13) 0.02724(15) 0.01849(12) 0.00038(14) 0.00238(14) -0.00128(10) Cu1 0.0303(15) 0.073(3) 0.0199(13) 0.007(3) 0.0042(10) 0.006(3) Cu1A 0.0296(16) 0.067(3) 0.0221(15) 0.015(2) 0.0025(11) -0.001(3) P1 0.0206(10) 0.0289(11) 0.0196(9) 0.0000(8) 0.0026(7) -0.0018(8) N1 0.031(3) 0.034(4) 0.021(3) 0.005(3) -0.004(3) 0.001(3) N2 0.028(3) 0.033(4) 0.020(3) -0.002(3) 0.002(3) -0.002(3) N3 0.034(4) 0.033(4) 0.017(3) 0.000(3) 0.005(3) -0.001(3) N4 0.030(3) 0.032(3) 0.016(3) 0.003(3) 0.003(3) 0.001(3) C1 0.041(4) 0.037(4) 0.029(5) 0.004(4) -0.001(4) 0.006(4) C2 0.043(5) 0.033(5) 0.038(5) 0.005(4) -0.002(4) 0.014(4) C3 0.029(4) 0.047(5) 0.028(4) -0.008(4) 0.002(3) 0.012(4) C4 0.021(4) 0.042(5) 0.021(4) 0.001(4) -0.001(3) 0.004(3) C5 0.015(4) 0.039(4) 0.020(3) -0.003(3) -0.001(3) 0.000(3) C6 0.017(3) 0.030(4) 0.021(4) 0.002(3) -0.003(3) 0.000(3) C7 0.014(4) 0.039(5) 0.020(4) 0.004(3) -0.005(3) -0.010(3) C8 0.028(4) 0.031(4) 0.029(4) 0.010(3) -0.003(3) -0.006(3) C9 0.046(5) 0.023(4) 0.041(5) -0.001(4) -0.003(4) -0.005(4) C10 0.038(5) 0.031(5) 0.035(4) -0.006(4) 0.001(4) 0.005(4) C11 0.020(4) 0.037(5) 0.021(4) -0.002(3) 0.002(3) -0.001(3) C12 0.026(4) 0.048(5) 0.021(4) 0.008(3) 0.001(3) -0.001(4) C13 0.023(4) 0.038(5) 0.033(4) -0.003(4) 0.002(3) -0.011(4) C14 0.021(4) 0.032(4) 0.020(4) 0.000(3) -0.003(3) 0.004(3) C15 0.031(4) 0.028(4) 0.023(3) 0.005(4) 0.000(4) -0.002(3) C16 0.029(4) 0.039(5) 0.026(4) 0.001(3) 0.005(3) 0.007(3) C17 0.051(5) 0.036(4) 0.051(5) -0.005(5) 0.017(5) 0.009(4) C18 0.071(7) 0.029(5) 0.059(6) 0.008(4) 0.031(5) 0.009(5) C19 0.045(5) 0.039(5) 0.038(4) 0.011(4) 0.019(4) 0.006(4) C20 0.035(4) 0.023(4) 0.022(4) -0.003(3) 0.010(3) 0.004(4) C21 0.039(5) 0.030(4) 0.028(4) -0.003(3) 0.005(3) 0.000(4) C22 0.061(6) 0.025(4) 0.036(5) 0.000(4) 0.009(4) 0.004(4) C23 0.065(6) 0.036(5) 0.027(4) 0.006(4) 0.007(4) 0.020(5) C24 0.051(6) 0.049(6) 0.027(4) 0.000(4) -0.001(4) 0.017(5) C25 0.038(5) 0.039(4) 0.023(4) -0.002(3) 0.006(3) 0.004(4) C26 0.026(4) 0.031(4) 0.017(4) 0.004(3) -0.001(3) -0.007(3) C27 0.037(5) 0.052(5) 0.033(4) -0.006(4) -0.005(4) 0.013(4) C28 0.033(5) 0.090(8) 0.045(5) -0.012(5) -0.015(4) 0.018(5) C29 0.033(5) 0.102(9) 0.036(5) -0.006(5) -0.006(4) -0.010(6) C30 0.058(6) 0.077(7) 0.021(4) -0.006(4) -0.001(4) -0.035(6) C31 0.034(5) 0.044(5) 0.032(4) -0.002(4) -0.003(4) -0.001(4) C32 0.018(4) 0.031(4) 0.018(3) 0.001(3) -0.005(3) -0.003(3) C33 0.023(4) 0.030(4) 0.032(4) -0.003(4) 0.007(3) 0.001(3) C34 0.030(4) 0.053(5) 0.028(5) -0.007(4) 0.012(3) -0.008(4) C35 0.033(4) 0.070(6) 0.029(4) 0.006(5) 0.007(4) -0.023(4) C36 0.034(5) 0.033(5) 0.050(5) 0.011(4) -0.005(4) -0.006(4) C37 0.026(4) 0.031(4) 0.021(3) 0.002(3) 0.004(3) -0.003(3) C38 0.030(4) 0.034(4) 0.020(4) -0.002(3) 0.002(3) 0.000(3) C39 0.043(5) 0.040(5) 0.020(4) 0.008(3) 0.005(4) -0.007(4) C40 0.049(6) 0.040(5) 0.022(4) 0.004(4) 0.000(4) -0.004(4) C41 0.029(4) 0.046(5) 0.013(4) 0.004(3) -0.001(3) 0.003(4) C42 0.027(4) 0.035(4) 0.022(4) 0.005(4) -0.002(3) -0.001(3) C43 0.037(5) 0.039(5) 0.035(4) 0.010(4) -0.003(4) -0.006(4) C44 0.027(4) 0.059(6) 0.029(4) 0.006(4) 0.000(3) 0.006(4) C45 0.039(5) 0.043(5) 0.026(4) -0.002(4) -0.009(4) 0.018(4) C46 0.036(4) 0.035(4) 0.025(4) 0.002(4) -0.012(4) 0.007(3) C47 0.046(5) 0.040(5) 0.050(5) -0.001(4) 0.008(4) -0.006(4) C48 0.040(5) 0.071(7) 0.046(5) 0.016(5) 0.015(4) 0.012(5) C49 0.050(5) 0.038(5) 0.059(5) 0.005(5) -0.005(5) 0.007(4) C50 0.028(4) 0.041(4) 0.018(3) 0.005(4) 0.007(4) 0.000(3) C51 0.039(4) 0.035(4) 0.026(4) 0.009(3) 0.008(3) 0.004(4) C52 0.035(5) 0.055(6) 0.029(4) 0.011(4) 0.008(4) 0.014(4) C53 0.028(4) 0.065(6) 0.031(4) 0.000(4) 0.005(3) 0.007(5) C54 0.039(5) 0.052(6) 0.038(4) -0.005(4) 0.011(4) -0.012(4) C55 0.027(4) 0.042(5) 0.026(4) 0.000(3) 0.009(3) -0.003(4) C56 0.057(5) 0.043(5) 0.053(5) 0.010(5) -0.002(6) 0.002(4) C57 0.031(5) 0.094(8) 0.053(6) 0.005(5) -0.005(4) 0.005(5) C58 0.042(4) 0.034(4) 0.061(5) 0.000(5) 0.006(5) -0.003(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 C26 2.033(7) . ? Pt1 C32 2.072(6) . ? Pt1 C11 2.266(7) . ? Pt1 P1 2.2670(18) . ? Cu1 C38 1.886(9) . ? Cu1 N1 1.956(9) . ? Cu1 N2 2.427(8) . ? Cu1A C38 1.893(9) . ? Cu1A N2 2.006(8) . ? Cu1A N1 2.302(8) . ? P1 C13 1.823(7) . ? P1 C20 1.835(7) . ? P1 C14 1.836(7) . ? N1 C1 1.332(9) . ? N1 C5 1.334(8) . ? N2 C6 1.337(8) . ? N2 C10 1.346(9) . ? N3 C38 1.372(8) . ? N3 C40 1.381(9) . ? N3 C41 1.431(8) . ? N4 C38 1.340(8) . ? N4 C39 1.391(9) . ? N4 C50 1.452(9) . ? C1 C2 1.391(10) . ? C2 C3 1.381(11) . ? C3 C4 1.408(10) . ? C4 C5 1.426(9) . ? C4 C11 1.467(10) . ? C5 C6 1.424(10) . ? C6 C7 1.407(9) . ? C7 C8 1.403(10) . ? C7 C11 1.478(10) . ? C8 C9 1.381(10) . ? C9 C10 1.397(10) . ? C11 C12 1.528(9) . ? C12 C13 1.514(9) . ? C14 C19 1.385(11) . ? C14 C15 1.404(10) . ? C15 C16 1.377(10) . ? C16 C17 1.368(10) . ? C17 C18 1.385(11) . ? C18 C19 1.379(11) . ? C20 C21 1.396(10) . ? C20 C25 1.407(10) . ? C21 C22 1.390(10) . ? C22 C23 1.345(11) . ? C23 C24 1.378(12) . ? C24 C25 1.383(10) . ? C26 C27 1.402(10) . ? C26 C31 1.414(10) . ? C27 C28 1.378(11) . ? C28 C29 1.333(13) . ? C29 C30 1.422(13) . ? C30 C31 1.387(11) . ? C32 C37 1.377(10) . ? C32 C33 1.402(9) . ? C33 C34 1.374(9) . ? C34 C35 1.398(11) . ? C35 C36 1.392(11) . ? C36 C37 1.393(9) . ? C39 C40 1.341(11) . ? C41 C42 1.365(10) . ? C41 C46 1.417(10) . ? C42 C43 1.376(10) . ? C42 C47 1.518(10) . ? C43 C44 1.390(11) . ? C44 C45 1.385(11) . ? C44 C48 1.511(10) . ? C45 C46 1.394(10) . ? C46 C49 1.505(10) . ? C50 C51 1.381(10) . ? C50 C55 1.397(10) . ? C51 C52 1.372(11) . ? C51 C56 1.478(10) . ? C52 C53 1.394(11) . ? C53 C54 1.384(11) . ? C53 C57 1.517(10) . ? C54 C55 1.388(11) . ? C55 C58 1.514(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 C26 Pt1 C32 84.7(3) . . ? C26 Pt1 C11 177.4(3) . . ? C32 Pt1 C11 94.2(2) . . ? C26 Pt1 P1 97.8(2) . . ? C32 Pt1 P1 175.4(2) . . ? C11 Pt1 P1 83.17(18) . . ? C38 Cu1 N1 148.0(4) . . ? C38 Cu1 N2 119.9(3) . . ? N1 Cu1 N2 82.4(3) . . ? C38 Cu1A N2 147.4(4) . . ? C38 Cu1A N1 123.0(3) . . ? N2 Cu1A N1 84.6(3) . . ? C13 P1 C20 104.5(3) . . ? C13 P1 C14 103.8(3) . . ? C20 P1 C14 102.8(3) . . ? C13 P1 Pt1 105.3(2) . . ? C20 P1 Pt1 127.2(2) . . ? C14 P1 Pt1 111.0(2) . . ? C1 N1 C5 116.2(6) . . ? C1 N1 Cu1 132.5(5) . . ? C5 N1 Cu1 110.7(5) . . ? C1 N1 Cu1A 144.9(5) . . ? C5 N1 Cu1A 98.7(4) . . ? C6 N2 C10 114.4(6) . . ? C6 N2 Cu1A 108.2(5) . . ? C10 N2 Cu1A 136.6(5) . . ? C6 N2 Cu1 97.8(4) . . ? C10 N2 Cu1 146.6(5) . . ? C38 N3 C40 111.4(6) . . ? C38 N3 C41 119.6(5) . . ? C40 N3 C41 128.9(6) . . ? C38 N4 C39 111.6(6) . . ? C38 N4 C50 123.6(5) . . ? C39 N4 C50 124.7(6) . . ? N1 C1 C2 122.2(7) . . ? C3 C2 C1 121.2(7) . . ? C2 C3 C4 118.8(7) . . ? C3 C4 C5 114.3(7) . . ? C3 C4 C11 136.1(6) . . ? C5 C4 C11 109.5(6) . . ? N1 C5 C6 125.0(6) . . ? N1 C5 C4 126.9(7) . . ? C6 C5 C4 108.0(6) . . ? N2 C6 C7 128.7(7) . . ? N2 C6 C5 122.6(6) . . ? C7 C6 C5 108.7(6) . . ? C8 C7 C6 115.2(7) . . ? C8 C7 C11 135.1(6) . . ? C6 C7 C11 109.7(6) . . ? C9 C8 C7 117.3(7) . . ? C8 C9 C10 122.5(7) . . ? N2 C10 C9 121.8(7) . . ? C4 C11 C7 103.7(5) . . ? C4 C11 C12 116.4(6) . . ? C7 C11 C12 121.1(6) . . ? C4 C11 Pt1 103.0(5) . . ? C7 C11 Pt1 98.6(4) . . ? C12 C11 Pt1 111.2(4) . . ? C13 C12 C11 115.2(6) . . ? C12 C13 P1 107.4(5) . . ? C19 C14 C15 117.4(6) . . ? C19 C14 P1 118.7(5) . . ? C15 C14 P1 123.9(5) . . ? C16 C15 C14 120.7(6) . . ? C17 C16 C15 120.6(7) . . ? C16 C17 C18 119.9(7) . . ? C19 C18 C17 119.4(8) . . ? C18 C19 C14 121.9(7) . . ? C21 C20 C25 119.0(7) . . ? C21 C20 P1 122.1(6) . . ? C25 C20 P1 118.9(6) . . ? C22 C21 C20 119.6(8) . . ? C23 C22 C21 121.3(8) . . ? C22 C23 C24 119.9(8) . . ? C23 C24 C25 121.2(8) . . ? C24 C25 C20 119.0(8) . . ? C27 C26 C31 116.4(7) . . ? C27 C26 Pt1 122.3(6) . . ? C31 C26 Pt1 121.1(6) . . ? C28 C27 C26 122.4(8) . . ? C29 C28 C27 121.1(9) . . ? C28 C29 C30 119.5(8) . . ? C31 C30 C29 120.0(9) . . ? C30 C31 C26 120.6(8) . . ? C37 C32 C33 117.2(6) . . ? C37 C32 Pt1 121.5(5) . . ? C33 C32 Pt1 121.3(5) . . ? C34 C33 C32 122.5(7) . . ? C33 C34 C35 120.0(7) . . ? C36 C35 C34 118.1(7) . . ? C35 C36 C37 121.1(7) . . ? C32 C37 C36 121.2(7) . . ? N4 C38 N3 103.7(5) . . ? N4 C38 Cu1 139.2(6) . . ? N3 C38 Cu1 116.3(5) . . ? N4 C38 Cu1A 136.5(6) . . ? N3 C38 Cu1A 118.2(5) . . ? C40 C39 N4 106.9(7) . . ? C39 C40 N3 106.3(7) . . ? C42 C41 C46 122.7(6) . . ? C42 C41 N3 120.3(7) . . ? C46 C41 N3 116.5(6) . . ? C41 C42 C43 118.0(7) . . ? C41 C42 C47 121.1(6) . . ? C43 C42 C47 120.9(7) . . ? C42 C43 C44 122.5(8) . . ? C45 C44 C43 118.3(7) . . ? C45 C44 C48 120.1(8) . . ? C43 C44 C48 121.6(8) . . ? C44 C45 C46 121.7(7) . . ? C45 C46 C41 116.8(7) . . ? C45 C46 C49 121.6(7) . . ? C41 C46 C49 121.6(7) . . ? C51 C50 C55 122.9(7) . . ? C51 C50 N4 120.9(6) . . ? C55 C50 N4 116.1(6) . . ? C52 C51 C50 117.4(7) . . ? C52 C51 C56 121.6(7) . . ? C50 C51 C56 121.0(7) . . ? C51 C52 C53 122.8(7) . . ? C54 C53 C52 117.5(8) . . ? C54 C53 C57 119.8(9) . . ? C52 C53 C57 122.7(8) . . ? C53 C54 C55 122.4(9) . . ? C54 C55 C50 117.0(7) . . ? C54 C55 C58 121.5(7) . . ? C50 C55 C58 121.5(6) . . ? _refine_diff_density_max 0.533 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.072 _shelxl_version_number 2013-4 _iucr_refine_instructions_details ; TITL 2b in P4(3)2(1)2 CELL 0.71073 26.3673 26.3673 15.2955 90.000 90.000 90.000 ZERR 8.00 0.0005 0.0005 0.0004 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5-Y, 0.5+X, 0.75+Z SYMM 0.5+Y, 0.5-X, 0.25+Z SYMM 0.5-X, 0.5+Y, 0.75-Z SYMM 0.5+X, 0.5-Y, 0.25-Z SYMM Y, X, -Z SYMM -Y, -X, 0.5-Z SFAC C H N P Cu Pt UNIT 464 432 32 8 8 8 SIZE 0.3 0.2 0.1 OMIT -3 50 OMIT -1 2 1 OMIT 1 2 1 OMIT 0 1 1 OMIT 0 2 1 OMIT 1 2 0 OMIT 3 3 1 OMIT 1 1 0 OMIT 4 4 1 L.S. 10 ACTA BOND BIND cu1 pt1 FMAP 2 PLAN 5 TEMP -123.140 WGHT 0.034200 FVAR 0.44612 PT1 6 0.483056 0.788225 0.500245 11.00000 0.01817 0.02724 = 0.01849 0.00038 0.00238 -0.00128 PART 1 CU1 5 0.475075 0.754152 0.868583 10.50000 0.03030 0.07280 = 0.01988 0.00692 0.00416 0.00569 PART 2 CU1A 5 0.473409 0.775967 0.872793 10.50000 0.02958 0.06740 = 0.02213 0.01518 0.00249 -0.00091 PART 0 P1 4 0.534677 0.817413 0.392928 11.00000 0.02059 0.02889 = 0.01959 0.00000 0.00259 -0.00181 N1 3 0.519873 0.725870 0.779060 11.00000 0.03123 0.03399 = 0.02104 0.00482 -0.00355 0.00117 N2 3 0.495143 0.833018 0.794497 11.00000 0.02773 0.03254 = 0.02043 -0.00155 0.00206 -0.00249 N3 3 0.492288 0.748710 1.047695 11.00000 0.03400 0.03325 = 0.01733 -0.00007 0.00537 -0.00116 N4 3 0.411895 0.753527 1.034038 11.00000 0.02962 0.03160 = 0.01575 0.00300 0.00284 0.00067 C1 1 0.535330 0.678771 0.762209 11.00000 0.04133 0.03681 = 0.02919 0.00426 -0.00088 0.00635 AFIX 43 H1 2 0.528155 0.652786 0.803417 11.00000 -1.20000 AFIX 0 C2 1 0.561608 0.666354 0.686351 11.00000 0.04315 0.03259 = 0.03795 0.00478 -0.00200 0.01406 AFIX 43 H2 2 0.573170 0.632561 0.678178 11.00000 -1.20000 AFIX 0 C3 1 0.571213 0.702208 0.622685 11.00000 0.02913 0.04674 = 0.02789 -0.00813 0.00204 0.01232 AFIX 43 H3 2 0.588704 0.693208 0.570649 11.00000 -1.20000 AFIX 0 C4 1 0.554626 0.752337 0.636258 11.00000 0.02101 0.04193 = 0.02148 0.00054 -0.00117 0.00414 C5 1 0.531173 0.760772 0.719031 11.00000 0.01486 0.03893 = 0.01996 -0.00333 -0.00134 -0.00022 C6 1 0.518232 0.813089 0.724668 11.00000 0.01676 0.03003 = 0.02145 0.00227 -0.00345 0.00014 C7 1 0.532210 0.837087 0.646140 11.00000 0.01411 0.03888 = 0.02049 0.00427 -0.00545 -0.00981 C8 1 0.522524 0.889364 0.642751 11.00000 0.02811 0.03078 = 0.02869 0.00950 -0.00288 -0.00631 AFIX 43 H8 2 0.531180 0.908953 0.592804 11.00000 -1.20000 AFIX 0 C9 1 0.499899 0.911202 0.714957 11.00000 0.04628 0.02328 = 0.04057 -0.00110 -0.00307 -0.00514 AFIX 43 H9 2 0.493224 0.946605 0.714269 11.00000 -1.20000 AFIX 0 C10 1 0.486452 0.883228 0.788960 11.00000 0.03821 0.03090 = 0.03477 -0.00613 0.00101 0.00523 AFIX 43 H10 2 0.470743 0.900097 0.836695 11.00000 -1.20000 AFIX 0 C11 1 0.552861 0.799167 0.584527 11.00000 0.01955 0.03650 = 0.02149 -0.00187 0.00215 -0.00109 C12 1 0.599459 0.810819 0.528688 11.00000 0.02575 0.04789 = 0.02075 0.00769 0.00064 -0.00110 AFIX 23 H12A 2 0.624965 0.827945 0.565895 11.00000 -1.20000 H12B 2 0.614380 0.778336 0.508881 11.00000 -1.20000 AFIX 0 C13 1 0.589653 0.843627 0.449266 11.00000 0.02259 0.03801 = 0.03292 -0.00306 0.00187 -0.01103 AFIX 23 H13A 2 0.619567 0.843429 0.410150 11.00000 -1.20000 H13B 2 0.582871 0.879038 0.467327 11.00000 -1.20000 AFIX 0 C14 1 0.561032 0.764823 0.328644 11.00000 0.02113 0.03190 = 0.02046 0.00004 -0.00296 0.00445 C15 1 0.589465 0.771323 0.251862 11.00000 0.03092 0.02775 = 0.02290 0.00530 0.00000 -0.00173 AFIX 43 H15 2 0.595266 0.804516 0.229871 11.00000 -1.20000 AFIX 0 C16 1 0.609041 0.730096 0.208077 11.00000 0.02856 0.03890 = 0.02604 0.00102 0.00482 0.00710 AFIX 43 H16 2 0.627704 0.735091 0.155652 11.00000 -1.20000 AFIX 0 C17 1 0.601870 0.682024 0.239347 11.00000 0.05100 0.03576 = 0.05054 -0.00481 0.01715 0.00938 AFIX 43 H17 2 0.615489 0.653815 0.208660 11.00000 -1.20000 AFIX 0 C18 1 0.574738 0.674517 0.315777 11.00000 0.07063 0.02923 = 0.05871 0.00771 0.03052 0.00931 AFIX 43 H18 2 0.570148 0.641264 0.338338 11.00000 -1.20000 AFIX 0 C19 1 0.554444 0.715734 0.358847 11.00000 0.04505 0.03892 = 0.03847 0.01141 0.01855 0.00582 AFIX 43 H19 2 0.535394 0.710309 0.410730 11.00000 -1.20000 AFIX 0 C20 1 0.519264 0.864646 0.308946 11.00000 0.03451 0.02340 = 0.02241 -0.00297 0.00971 0.00357 C21 1 0.552970 0.903185 0.285691 11.00000 0.03904 0.03035 = 0.02794 -0.00340 0.00546 0.00004 AFIX 43 H21 2 0.584606 0.906359 0.314905 11.00000 -1.20000 AFIX 0 C22 1 0.539944 0.936872 0.219533 11.00000 0.06111 0.02464 = 0.03626 0.00036 0.00862 0.00354 AFIX 43 H22 2 0.563204 0.962709 0.203222 11.00000 -1.20000 AFIX 0 C23 1 0.495056 0.933623 0.178129 11.00000 0.06451 0.03609 = 0.02666 0.00638 0.00722 0.02033 AFIX 43 H23 2 0.486828 0.957053 0.133129 11.00000 -1.20000 AFIX 0 C24 1 0.461008 0.896252 0.201080 11.00000 0.05145 0.04897 = 0.02691 -0.00003 -0.00110 0.01693 AFIX 43 H24 2 0.429356 0.894247 0.171611 11.00000 -1.20000 AFIX 0 C25 1 0.472101 0.861635 0.266220 11.00000 0.03812 0.03874 = 0.02297 -0.00169 0.00619 0.00433 AFIX 43 H25 2 0.448250 0.836207 0.281892 11.00000 -1.20000 AFIX 0 C26 1 0.420729 0.774936 0.425377 11.00000 0.02610 0.03075 = 0.01693 0.00421 -0.00067 -0.00709 C27 1 0.378618 0.807401 0.425379 11.00000 0.03658 0.05226 = 0.03317 -0.00612 -0.00543 0.01325 AFIX 43 H27 2 0.380029 0.837675 0.458964 11.00000 -1.20000 AFIX 0 C28 1 0.335243 0.796968 0.378398 11.00000 0.03323 0.08972 = 0.04499 -0.01153 -0.01462 0.01772 AFIX 43 H28 2 0.307577 0.820016 0.380546 11.00000 -1.20000 AFIX 0 C29 1 0.331450 0.755104 0.330014 11.00000 0.03266 0.10184 = 0.03566 -0.00553 -0.00630 -0.01006 AFIX 43 H29 2 0.301753 0.748892 0.296517 11.00000 -1.20000 AFIX 0 C30 1 0.372237 0.719802 0.328946 11.00000 0.05849 0.07692 = 0.02112 -0.00620 -0.00121 -0.03452 AFIX 43 H30 2 0.369350 0.689251 0.296401 11.00000 -1.20000 AFIX 0 C31 1 0.416224 0.730014 0.375451 11.00000 0.03365 0.04365 = 0.03151 -0.00237 -0.00315 -0.00131 AFIX 43 H31 2 0.443595 0.706605 0.373752 11.00000 -1.20000 AFIX 0 C32 1 0.440229 0.757137 0.600351 11.00000 0.01821 0.03126 = 0.01837 0.00145 -0.00489 -0.00255 C33 1 0.413712 0.787920 0.659435 11.00000 0.02331 0.03014 = 0.03207 -0.00257 0.00664 0.00117 AFIX 43 H33 2 0.413707 0.823580 0.650569 11.00000 -1.20000 AFIX 0 C34 1 0.387727 0.768462 0.729693 11.00000 0.02951 0.05339 = 0.02828 -0.00697 0.01226 -0.00769 AFIX 43 H34 2 0.370320 0.790573 0.768478 11.00000 -1.20000 AFIX 0 C35 1 0.386912 0.716103 0.744087 11.00000 0.03341 0.07008 = 0.02937 0.00553 0.00680 -0.02326 AFIX 43 H35 2 0.369408 0.702103 0.792715 11.00000 -1.20000 AFIX 0 C36 1 0.412484 0.685085 0.685115 11.00000 0.03428 0.03341 = 0.04984 0.01106 -0.00548 -0.00631 AFIX 43 H36 2 0.412190 0.649379 0.693401 11.00000 -1.20000 AFIX 0 C37 1 0.438510 0.705560 0.614115 11.00000 0.02585 0.03114 = 0.02098 0.00242 0.00368 -0.00334 AFIX 43 H37 2 0.455375 0.683532 0.574486 11.00000 -1.20000 AFIX 0 C38 1 0.454662 0.755092 0.986728 11.00000 0.02970 0.03414 = 0.02050 -0.00163 0.00155 0.00019 C39 1 0.422058 0.747526 1.122690 11.00000 0.04262 0.03954 = 0.02043 0.00804 0.00534 -0.00723 AFIX 43 H39 2 0.397859 0.746495 1.168671 11.00000 -1.20000 AFIX 0 C40 1 0.472531 0.743474 1.130846 11.00000 0.04904 0.03953 = 0.02161 0.00390 0.00036 -0.00436 AFIX 43 H40 2 0.491015 0.738078 1.183342 11.00000 -1.20000 AFIX 0 C41 1 0.544026 0.746054 1.019896 11.00000 0.02902 0.04569 = 0.01321 0.00367 -0.00146 0.00301 C42 1 0.571662 0.789376 1.008813 11.00000 0.02736 0.03499 = 0.02247 0.00461 -0.00206 -0.00087 C43 1 0.618540 0.785404 0.969957 11.00000 0.03704 0.03934 = 0.03544 0.01016 -0.00285 -0.00597 AFIX 43 H43 2 0.638219 0.815254 0.962271 11.00000 -1.20000 AFIX 0 C44 1 0.638199 0.739367 0.941521 11.00000 0.02746 0.05927 = 0.02868 0.00644 -0.00018 0.00587 C45 1 0.609818 0.695907 0.955297 11.00000 0.03918 0.04316 = 0.02628 -0.00171 -0.00942 0.01806 AFIX 43 H45 2 0.623133 0.664098 0.937297 11.00000 -1.20000 AFIX 0 C46 1 0.562209 0.697596 0.994892 11.00000 0.03563 0.03535 = 0.02541 0.00243 -0.01177 0.00736 C47 1 0.550711 0.840652 1.035957 11.00000 0.04633 0.03952 = 0.04974 -0.00124 0.00822 -0.00570 AFIX 137 H47A 2 0.527280 0.852999 0.991008 11.00000 -1.50000 H47B 2 0.578697 0.864790 1.042750 11.00000 -1.50000 H47C 2 0.532635 0.837261 1.091634 11.00000 -1.50000 AFIX 0 C48 1 0.688577 0.736244 0.894799 11.00000 0.04047 0.07148 = 0.04562 0.01560 0.01466 0.01181 AFIX 137 H48A 2 0.710208 0.711188 0.923938 11.00000 -1.50000 H48B 2 0.705167 0.769494 0.896206 11.00000 -1.50000 H48C 2 0.683040 0.726024 0.833941 11.00000 -1.50000 AFIX 0 C49 1 0.530729 0.650519 1.007025 11.00000 0.05011 0.03776 = 0.05889 0.00525 -0.00526 0.00658 AFIX 137 H49A 2 0.496259 0.656688 0.985551 11.00000 -1.50000 H49B 2 0.529472 0.641737 1.069244 11.00000 -1.50000 H49C 2 0.545952 0.622472 0.974182 11.00000 -1.50000 AFIX 0 C50 1 0.361476 0.753810 0.995861 11.00000 0.02753 0.04125 = 0.01845 0.00472 0.00729 -0.00036 C51 1 0.337191 0.798877 0.976718 11.00000 0.03909 0.03518 = 0.02603 0.00868 0.00798 0.00443 C52 1 0.290339 0.795902 0.937963 11.00000 0.03521 0.05500 = 0.02939 0.01137 0.00846 0.01352 AFIX 43 H52 2 0.273234 0.826504 0.923645 11.00000 -1.20000 AFIX 0 C53 1 0.266772 0.749928 0.918707 11.00000 0.02845 0.06453 = 0.03055 0.00008 0.00503 0.00706 C54 1 0.292253 0.705889 0.940851 11.00000 0.03940 0.05211 = 0.03788 -0.00517 0.01078 -0.01164 AFIX 43 H54 2 0.276340 0.674173 0.930084 11.00000 -1.20000 AFIX 0 C55 1 0.340206 0.706368 0.978216 11.00000 0.02741 0.04165 = 0.02600 -0.00034 0.00916 -0.00258 C56 1 0.361049 0.848226 0.997043 11.00000 0.05685 0.04266 = 0.05314 0.01047 -0.00167 0.00229 AFIX 137 H56A 2 0.372035 0.848508 1.058249 11.00000 -1.50000 H56B 2 0.336452 0.875526 0.987432 11.00000 -1.50000 H56C 2 0.390477 0.853358 0.958920 11.00000 -1.50000 AFIX 0 C57 1 0.214839 0.746792 0.876379 11.00000 0.03129 0.09400 = 0.05275 0.00468 -0.00549 0.00510 AFIX 137 H57A 2 0.192115 0.726817 0.913591 11.00000 -1.50000 H57B 2 0.217828 0.730491 0.819029 11.00000 -1.50000 H57C 2 0.201024 0.781042 0.869170 11.00000 -1.50000 AFIX 0 C58 1 0.368411 0.657716 0.998074 11.00000 0.04232 0.03383 = 0.06129 -0.00034 0.00596 -0.00310 AFIX 137 H58A 2 0.397716 0.654721 0.959004 11.00000 -1.50000 H58B 2 0.345734 0.628727 0.989157 11.00000 -1.50000 H58C 2 0.380046 0.658200 1.058920 11.00000 -1.50000 AFIX 0 HKLF 4 REM 2b in P4(3)2(1)2 REM R1 = 0.0293 for 8281 Fo > 4sig(Fo) and 0.0364 for all 9346 data REM 601 parameters refined using 0 restraints END WGHT 0.0317 0.0000 REM Highest difference peak 0.533, deepest hole -0.358, 1-sigma level 0.072 Q1 1 0.4778 0.7493 0.5013 11.00000 0.05 0.53 Q2 1 0.5675 0.6764 0.7486 11.00000 0.05 0.37 Q3 1 0.4842 0.8314 0.4984 11.00000 0.05 0.33 Q4 1 0.4483 0.7711 0.4989 11.00000 0.05 0.32 Q5 1 0.4575 0.8177 0.4719 11.00000 0.05 0.30 ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.005 734 224 ' ' 2 0.500 0.500 0.254 734 224 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 953913' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2bBenzene _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H57 Cu N4 P Pt' _chemical_formula_weight 1135.70 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' Cu Cu 0.3201 1.2651 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8289(6) _cell_length_b 21.9364(13) _cell_length_c 20.4095(10) _cell_angle_alpha 90 _cell_angle_beta 106.006(2) _cell_angle_gamma 90 _cell_volume 5090.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 39797 _cell_measurement_theta_min 2.305 _cell_measurement_theta_max 24.999 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_F_000 2292 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.270 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 3.238 _shelx_estimated_absorpt_T_min 0.475 _shelx_estimated_absorpt_T_max 0.855 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.6317 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'Bruker Apex 2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker Kappa Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39797 _diffrn_reflns_av_unetI/netI 0.0603 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.305 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.971 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.971 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.971 _reflns_number_total 8942 _reflns_number_gt 6812 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker Apex 2 software package' _computing_cell_refinement 'Bruker Apex 2 software package' _computing_data_reduction 'Bruker Apex 2 software package' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'ORTEP and POV-Ray' _computing_publication_material 'SHELXL-2013 (Sheldrick, 2013)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+3.3269P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8942 _refine_ls_number_parameters 619 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0709 _refine_ls_wR_factor_gt 0.0634 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt -0.09551(2) 1.09072(2) 0.80040(2) 0.01879(6) Uani 1 1 d . . . . . Cu1 Cu 0.15078(5) 0.86962(3) 0.72714(3) 0.02755(15) Uani 1 1 d . . . . . P1 P -0.10412(10) 1.14047(6) 0.89673(6) 0.0195(3) Uani 1 1 d . . . . . N1 N 0.2575(3) 0.9758(2) 0.7896(2) 0.0306(10) Uani 1 1 d . . . . . N2 N 0.0563(3) 0.89085(17) 0.78605(18) 0.0228(9) Uani 1 1 d . . . . . N3 N 0.3450(3) 0.80843(19) 0.69606(19) 0.0284(10) Uani 1 1 d . . . . . N4 N 0.1946(3) 0.80237(19) 0.61037(19) 0.0272(10) Uani 1 1 d . . . . . C1 C 0.3372(4) 1.0208(3) 0.7976(3) 0.0420(15) Uani 1 1 d . . . . . H1 H 0.4021 1.0153 0.7792 0.050 Uiso 1 1 calc R U . . . C2 C 0.3294(4) 1.0748(3) 0.8313(3) 0.0418(15) Uani 1 1 d . . . . . H2 H 0.3884 1.1050 0.8352 0.050 Uiso 1 1 calc R U . . . C3 C 0.2377(4) 1.0854(2) 0.8591(2) 0.0310(12) Uani 1 1 d . . . . . H3 H 0.2327 1.1224 0.8823 0.037 Uiso 1 1 calc R U . . . C4 C 0.1524(4) 1.0401(2) 0.8523(2) 0.0211(11) Uani 1 1 d . . . . . C5 C 0.1695(4) 0.9866(2) 0.8176(2) 0.0212(11) Uani 1 1 d . . . . . C6 C 0.0749(4) 0.9455(2) 0.8168(2) 0.0215(11) Uani 1 1 d . . . . . C7 C 0.0033(4) 0.9726(2) 0.8539(2) 0.0204(11) Uani 1 1 d . . . . . C8 C -0.0898(4) 0.9377(2) 0.8621(2) 0.0254(11) Uani 1 1 d . . . . . H8 H -0.1399 0.9528 0.8876 0.030 Uiso 1 1 calc R U . . . C9 C -0.1082(4) 0.8805(2) 0.8323(2) 0.0292(12) Uani 1 1 d . . . . . H9 H -0.1709 0.8558 0.8379 0.035 Uiso 1 1 calc R U . . . C10 C -0.0360(4) 0.8593(2) 0.7948(2) 0.0298(12) Uani 1 1 d . . . . . H10 H -0.0522 0.8204 0.7739 0.036 Uiso 1 1 calc R U . . . C11 C 0.0432(4) 1.0351(2) 0.8736(2) 0.0207(11) Uani 1 1 d . . . . . C12 C 0.0510(4) 1.0532(2) 0.9472(2) 0.0264(12) Uani 1 1 d . . . . . H12A H -0.0102 1.0306 0.9621 0.032 Uiso 1 1 calc R U . . . H12B H 0.1285 1.0402 0.9768 0.032 Uiso 1 1 calc R U . . . C13 C 0.0358(4) 1.1207(2) 0.9578(2) 0.0238(11) Uani 1 1 d . . . . . H13A H 0.1012 1.1443 0.9487 0.029 Uiso 1 1 calc R U . . . H13B H 0.0332 1.1290 1.0051 0.029 Uiso 1 1 calc R U . . . C14 C -0.1119(4) 1.2231(2) 0.9035(2) 0.0203(10) Uani 1 1 d . . . . . C15 C -0.0424(4) 1.2544(2) 0.9597(2) 0.0256(11) Uani 1 1 d . . . . . H15 H 0.0065 1.2321 0.9968 0.031 Uiso 1 1 calc R U . . . C16 C -0.0434(4) 1.3169(2) 0.9623(2) 0.0316(12) Uani 1 1 d . . . . . H16 H 0.0054 1.3374 1.0008 0.038 Uiso 1 1 calc R U . . . C17 C -0.1150(4) 1.3506(2) 0.9094(3) 0.0333(13) Uani 1 1 d . . . . . H17 H -0.1161 1.3939 0.9116 0.040 Uiso 1 1 calc R U . . . C18 C -0.1846(4) 1.3203(2) 0.8536(3) 0.0361(13) Uani 1 1 d . . . . . H18 H -0.2337 1.3430 0.8170 0.043 Uiso 1 1 calc R U . . . C19 C -0.1839(4) 1.2570(2) 0.8500(2) 0.0267(12) Uani 1 1 d . . . . . H19 H -0.2323 1.2367 0.8112 0.032 Uiso 1 1 calc R U . . . C20 C -0.2103(4) 1.1131(2) 0.9408(2) 0.0206(11) Uani 1 1 d . . . . . C21 C -0.2112(4) 1.1355(2) 1.0049(2) 0.0316(12) Uani 1 1 d . . . . . H21 H -0.1585 1.1671 1.0254 0.038 Uiso 1 1 calc R U . . . C22 C -0.2880(5) 1.1120(3) 1.0384(3) 0.0396(14) Uani 1 1 d . . . . . H22 H -0.2874 1.1271 1.0822 0.047 Uiso 1 1 calc R U . . . C23 C -0.3654(5) 1.0667(3) 1.0085(3) 0.0430(15) Uani 1 1 d . . . . . H23 H -0.4183 1.0507 1.0317 0.052 Uiso 1 1 calc R U . . . C24 C -0.3668(4) 1.0442(3) 0.9453(3) 0.0389(14) Uani 1 1 d . . . . . H24 H -0.4208 1.0131 0.9249 0.047 Uiso 1 1 calc R U . . . C25 C -0.2891(4) 1.0672(2) 0.9116(2) 0.0289(12) Uani 1 1 d . . . . . H25 H -0.2897 1.0514 0.8682 0.035 Uiso 1 1 calc R U . . . C26 C -0.0732(4) 1.0430(2) 0.7186(2) 0.0222(11) Uani 1 1 d . . . . . C27 C 0.0250(4) 1.0509(2) 0.6939(2) 0.0280(12) Uani 1 1 d . . . . . H27 H 0.0778 1.0834 0.7113 0.034 Uiso 1 1 calc R U . . . C28 C 0.0481(5) 1.0125(3) 0.6445(2) 0.0366(14) Uani 1 1 d . . . . . H28 H 0.1169 1.0186 0.6299 0.044 Uiso 1 1 calc R U . . . C29 C -0.0278(5) 0.9662(3) 0.6169(3) 0.0468(16) Uani 1 1 d . . . . . H29 H -0.0116 0.9397 0.5837 0.056 Uiso 1 1 calc R U . . . C30 C -0.1273(5) 0.9586(3) 0.6379(3) 0.0436(15) Uani 1 1 d . . . . . H30 H -0.1818 0.9275 0.6179 0.052 Uiso 1 1 calc R U . . . C31 C -0.1493(4) 0.9955(2) 0.6878(2) 0.0307(12) Uani 1 1 d . . . . . H31 H -0.2185 0.9887 0.7017 0.037 Uiso 1 1 calc R U . . . C32 C -0.2244(4) 1.1389(2) 0.7336(2) 0.0248(11) Uani 1 1 d . . . . . C33 C -0.2003(5) 1.1791(3) 0.6863(2) 0.0367(13) Uani 1 1 d . . . . . H33 H -0.1218 1.1821 0.6833 0.044 Uiso 1 1 calc R U . . . C34 C -0.2859(5) 1.2150(3) 0.6434(3) 0.0483(16) Uani 1 1 d . . . . . H34 H -0.2654 1.2423 0.6123 0.058 Uiso 1 1 calc R U . . . C35 C -0.4001(5) 1.2111(3) 0.6459(3) 0.0473(16) Uani 1 1 d . . . . . H35 H -0.4590 1.2361 0.6173 0.057 Uiso 1 1 calc R U . . . C36 C -0.4288(4) 1.1709(3) 0.6900(3) 0.0418(15) Uani 1 1 d . . . . . H36 H -0.5082 1.1671 0.6913 0.050 Uiso 1 1 calc R U . . . C37 C -0.3420(4) 1.1358(2) 0.7326(2) 0.0349(13) Uani 1 1 d . . . . . H37 H -0.3640 1.1081 0.7628 0.042 Uiso 1 1 calc R U . . . C38 C 0.2312(4) 0.8275(2) 0.6736(2) 0.0245(11) Uani 1 1 d . . . . . C39 C 0.3779(4) 0.7737(2) 0.6487(3) 0.0347(13) Uani 1 1 d . . . . . H39 H 0.4527 0.7556 0.6534 0.042 Uiso 1 1 calc R U . . . C40 C 0.2828(4) 0.7702(3) 0.5940(3) 0.0398(14) Uani 1 1 d . . . . . H40 H 0.2778 0.7496 0.5523 0.048 Uiso 1 1 calc R U . . . C41 C 0.4213(4) 0.8229(2) 0.7629(2) 0.0303(12) Uani 1 1 d . . . . . C42 C 0.4883(4) 0.8756(2) 0.7714(3) 0.0324(13) Uani 1 1 d . . . . . C43 C 0.5608(4) 0.8876(3) 0.8362(3) 0.0375(14) Uani 1 1 d . . . . . H43 H 0.6084 0.9232 0.8437 0.045 Uiso 1 1 calc R U . . . C44 C 0.5649(4) 0.8484(3) 0.8905(3) 0.0408(15) Uani 1 1 d . . . . . C45 C 0.4976(5) 0.7962(3) 0.8789(3) 0.0460(15) Uani 1 1 d . . . . . H45 H 0.5011 0.7692 0.9158 0.055 Uiso 1 1 calc R U . . . C46 C 0.4250(4) 0.7819(3) 0.8150(3) 0.0348(13) Uani 1 1 d . . . . . C47 C 0.4802(5) 0.9189(3) 0.7127(3) 0.0478(16) Uani 1 1 d . . . . . H47A H 0.4960 0.8966 0.6745 0.072 Uiso 1 1 calc R U . . . H47B H 0.5383 0.9515 0.7273 0.072 Uiso 1 1 calc R U . . . H47C H 0.4011 0.9366 0.6983 0.072 Uiso 1 1 calc R U . . . C48 C 0.6440(5) 0.8627(3) 0.9610(3) 0.066(2) Uani 1 1 d . . . . . H48A H 0.7230 0.8466 0.9654 0.099 Uiso 1 1 calc R U . . . H48B H 0.6117 0.8439 0.9955 0.099 Uiso 1 1 calc R U . . . H48C H 0.6483 0.9070 0.9677 0.099 Uiso 1 1 calc R U . . . C49 C 0.3520(5) 0.7246(3) 0.8019(3) 0.0583(18) Uani 1 1 d . . . . . H49A H 0.3689 0.7002 0.8437 0.088 Uiso 1 1 calc R U . . . H49B H 0.3711 0.7010 0.7657 0.088 Uiso 1 1 calc R U . . . H49C H 0.2683 0.7354 0.7880 0.088 Uiso 1 1 calc R U . . . C50 C 0.0775(4) 0.8111(2) 0.5646(2) 0.0244(11) Uani 1 1 d . . . . . C51 C 0.0649(4) 0.8514(2) 0.5106(2) 0.0290(12) Uani 1 1 d . . . . . C52 C -0.0475(4) 0.8595(2) 0.4679(2) 0.0345(13) Uani 1 1 d . . . . . H52 H -0.0584 0.8865 0.4302 0.041 Uiso 1 1 calc R U . . . C53 C -0.1438(4) 0.8299(2) 0.4780(2) 0.0315(13) Uani 1 1 d . . . . . C54 C -0.1262(4) 0.7889(3) 0.5311(2) 0.0339(13) Uani 1 1 d . . . . . H54 H -0.1919 0.7671 0.5374 0.041 Uiso 1 1 calc R U . . . C55 C -0.0163(4) 0.7782(2) 0.5756(2) 0.0275(12) Uani 1 1 d . . . . . C56 C 0.1674(5) 0.8866(3) 0.4991(3) 0.0486(16) Uani 1 1 d . . . . . H56A H 0.2142 0.9038 0.5424 0.073 Uiso 1 1 calc R U . . . H56B H 0.1380 0.9196 0.4665 0.073 Uiso 1 1 calc R U . . . H56C H 0.2167 0.8591 0.4808 0.073 Uiso 1 1 calc R U . . . C57 C -0.2661(4) 0.8416(3) 0.4312(3) 0.0562(19) Uani 1 1 d . . . . . H57A H -0.3025 0.8028 0.4130 0.084 Uiso 1 1 calc R U . . . H57B H -0.2604 0.8680 0.3935 0.084 Uiso 1 1 calc R U . . . H57C H -0.3144 0.8617 0.4569 0.084 Uiso 1 1 calc R U . . . C58 C -0.0003(5) 0.7330(3) 0.6331(3) 0.0451(15) Uani 1 1 d . . . . . H58A H 0.0785 0.7151 0.6430 0.068 Uiso 1 1 calc R U . . . H58B H -0.0595 0.7008 0.6198 0.068 Uiso 1 1 calc R U . . . H58C H -0.0095 0.7539 0.6738 0.068 Uiso 1 1 calc R U . . . C59 C 0.9043(6) 0.5280(3) 0.9574(4) 0.069(2) Uani 1 1 d . . . . . H59 H 0.8382 0.5476 0.9276 0.083 Uiso 1 1 calc R U . . . C60 C 0.8933(7) 0.4991(4) 1.0146(5) 0.079(2) Uani 1 1 d . . . . . H60 H 0.8198 0.4983 1.0250 0.094 Uiso 1 1 calc R U . . . C61 C 1.0096(7) 0.5288(3) 0.9431(4) 0.070(2) Uani 1 1 d . . . . . H61 H 1.0165 0.5489 0.9032 0.084 Uiso 1 1 calc R U . . . 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 0.02022(10) 0.01793(10) 0.01710(9) 0.00019(9) 0.00326(7) 0.00227(9) Cu1 0.0253(3) 0.0294(4) 0.0287(3) -0.0038(3) 0.0086(3) 0.0063(3) P1 0.0199(6) 0.0199(7) 0.0187(6) -0.0004(5) 0.0053(5) 0.0020(5) N1 0.024(2) 0.031(3) 0.041(3) -0.003(2) 0.016(2) 0.004(2) N2 0.022(2) 0.020(2) 0.025(2) -0.0013(17) 0.0037(17) 0.0017(17) N3 0.021(2) 0.036(3) 0.028(2) -0.006(2) 0.0058(18) 0.0035(19) N4 0.023(2) 0.030(3) 0.029(2) -0.0071(19) 0.0089(18) 0.0023(19) C1 0.025(3) 0.044(4) 0.063(4) -0.007(3) 0.021(3) -0.004(3) C2 0.031(3) 0.035(4) 0.064(4) -0.020(3) 0.020(3) -0.014(3) C3 0.029(3) 0.029(3) 0.034(3) -0.009(2) 0.007(2) -0.002(3) C4 0.015(2) 0.022(3) 0.022(2) -0.002(2) -0.0014(19) 0.003(2) C5 0.015(2) 0.018(3) 0.028(3) -0.002(2) 0.004(2) 0.004(2) C6 0.022(3) 0.018(3) 0.019(2) 0.004(2) -0.003(2) 0.006(2) C7 0.020(2) 0.021(3) 0.018(2) 0.007(2) 0.0005(19) 0.008(2) C8 0.025(3) 0.027(3) 0.026(3) 0.004(2) 0.010(2) 0.005(2) C9 0.034(3) 0.019(3) 0.038(3) 0.003(2) 0.015(2) -0.001(2) C10 0.033(3) 0.023(3) 0.033(3) -0.005(2) 0.007(2) -0.004(2) C11 0.019(2) 0.023(3) 0.020(2) 0.001(2) 0.0042(19) 0.007(2) C12 0.027(3) 0.031(3) 0.019(2) -0.001(2) 0.003(2) 0.004(2) C13 0.021(3) 0.030(3) 0.019(2) -0.004(2) 0.003(2) 0.000(2) C14 0.019(2) 0.021(3) 0.023(2) -0.001(2) 0.009(2) 0.001(2) C15 0.026(3) 0.025(3) 0.027(3) -0.002(2) 0.010(2) 0.001(2) C16 0.032(3) 0.030(3) 0.035(3) -0.011(3) 0.013(2) -0.006(2) C17 0.041(3) 0.022(3) 0.041(3) -0.004(3) 0.017(3) 0.000(3) C18 0.039(3) 0.023(3) 0.042(3) 0.006(3) 0.004(3) 0.009(3) C19 0.027(3) 0.023(3) 0.026(3) -0.004(2) 0.003(2) -0.002(2) C20 0.021(2) 0.014(3) 0.025(3) 0.006(2) 0.004(2) 0.005(2) C21 0.030(3) 0.033(3) 0.033(3) 0.001(2) 0.011(2) 0.000(2) C22 0.036(3) 0.053(4) 0.035(3) 0.005(3) 0.019(3) 0.009(3) C23 0.031(3) 0.049(4) 0.055(4) 0.016(3) 0.023(3) -0.002(3) C24 0.029(3) 0.036(4) 0.055(4) 0.002(3) 0.017(3) -0.003(3) C25 0.027(3) 0.025(3) 0.036(3) 0.003(2) 0.012(2) 0.003(2) C26 0.028(3) 0.017(3) 0.019(2) 0.005(2) 0.002(2) 0.007(2) C27 0.038(3) 0.019(3) 0.027(3) 0.005(2) 0.009(2) -0.002(2) C28 0.047(3) 0.041(4) 0.026(3) 0.001(3) 0.018(3) 0.008(3) C29 0.070(4) 0.042(4) 0.027(3) -0.007(3) 0.011(3) 0.020(3) C30 0.056(4) 0.032(4) 0.035(3) -0.014(3) -0.001(3) 0.001(3) C31 0.029(3) 0.031(3) 0.029(3) -0.004(2) 0.004(2) -0.003(2) C32 0.035(3) 0.019(3) 0.016(2) -0.004(2) 0.000(2) 0.008(2) C33 0.041(3) 0.038(4) 0.034(3) 0.011(3) 0.015(3) 0.013(3) C34 0.070(4) 0.041(4) 0.040(3) 0.017(3) 0.024(3) 0.020(3) C35 0.064(4) 0.046(4) 0.025(3) 0.002(3) 0.000(3) 0.030(3) C36 0.022(3) 0.052(4) 0.041(3) -0.003(3) -0.008(3) 0.006(3) C37 0.034(3) 0.030(3) 0.034(3) 0.007(2) -0.003(2) 0.005(3) C38 0.022(3) 0.026(3) 0.028(3) 0.002(2) 0.009(2) 0.000(2) C39 0.021(3) 0.039(4) 0.048(3) -0.012(3) 0.016(2) 0.009(2) C40 0.033(3) 0.049(4) 0.040(3) -0.013(3) 0.015(3) 0.005(3) C41 0.018(3) 0.034(3) 0.038(3) -0.007(3) 0.007(2) 0.003(2) C42 0.026(3) 0.034(4) 0.038(3) -0.008(3) 0.010(2) 0.007(2) C43 0.023(3) 0.031(3) 0.060(4) -0.012(3) 0.013(3) 0.003(2) C44 0.029(3) 0.037(4) 0.047(4) -0.012(3) -0.006(3) 0.007(3) C45 0.041(3) 0.042(4) 0.043(3) 0.009(3) -0.007(3) 0.008(3) C46 0.026(3) 0.033(3) 0.042(3) 0.005(3) 0.003(2) 0.004(2) C47 0.065(4) 0.031(4) 0.057(4) -0.008(3) 0.031(3) -0.008(3) C48 0.053(4) 0.059(5) 0.063(4) -0.012(4) -0.025(3) 0.015(3) C49 0.055(4) 0.049(4) 0.057(4) 0.014(3) -0.008(3) -0.017(3) C50 0.025(3) 0.026(3) 0.022(3) -0.007(2) 0.005(2) 0.003(2) C51 0.034(3) 0.025(3) 0.029(3) -0.008(2) 0.011(2) -0.008(2) C52 0.042(3) 0.038(4) 0.022(3) 0.001(2) 0.007(2) 0.002(3) C53 0.029(3) 0.039(4) 0.026(3) -0.005(2) 0.008(2) 0.002(3) C54 0.028(3) 0.041(4) 0.035(3) -0.001(3) 0.011(2) -0.007(2) C55 0.028(3) 0.025(3) 0.033(3) 0.001(2) 0.013(2) 0.002(2) C56 0.046(4) 0.056(4) 0.044(3) 0.005(3) 0.014(3) -0.016(3) C57 0.026(3) 0.097(6) 0.044(3) 0.012(3) 0.007(3) 0.009(3) C58 0.040(3) 0.040(4) 0.057(4) 0.015(3) 0.015(3) -0.002(3) C59 0.034(4) 0.046(5) 0.110(7) -0.027(5) -0.011(4) 0.004(3) C60 0.059(5) 0.047(5) 0.128(7) -0.025(5) 0.023(5) 0.006(4) C61 0.079(5) 0.035(4) 0.087(5) -0.018(4) 0.008(5) 0.000(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 C32 2.038(4) . ? Pt1 C26 2.049(4) . ? Pt1 C11 2.249(4) . ? Pt1 P1 2.2753(12) . ? Cu1 C38 1.879(5) . ? Cu1 N2 1.911(4) . ? P1 C14 1.823(5) . ? P1 C13 1.829(4) . ? P1 C20 1.835(5) . ? N1 C5 1.340(5) . ? N1 C1 1.343(6) . ? N2 C6 1.344(6) . ? N2 C10 1.345(6) . ? N3 C38 1.362(6) . ? N3 C39 1.369(6) . ? N3 C41 1.448(6) . ? N4 C38 1.359(6) . ? N4 C40 1.374(6) . ? N4 C50 1.454(5) . ? C1 C2 1.385(7) . ? C2 C3 1.376(7) . ? C3 C4 1.395(6) . ? C4 C5 1.414(6) . ? C4 C11 1.476(6) . ? C5 C6 1.434(6) . ? C6 C7 1.412(6) . ? C7 C8 1.389(6) . ? C7 C11 1.470(6) . ? C8 C9 1.384(7) . ? C9 C10 1.377(6) . ? C11 C12 1.533(6) . ? C12 C13 1.515(6) . ? C14 C15 1.394(6) . ? C14 C19 1.398(6) . ? C15 C16 1.373(7) . ? C16 C17 1.388(7) . ? C17 C18 1.378(7) . ? C18 C19 1.392(7) . ? C20 C25 1.390(6) . ? C20 C21 1.399(6) . ? C21 C22 1.379(6) . ? C22 C23 1.374(8) . ? C23 C24 1.377(7) . ? C24 C25 1.386(6) . ? C26 C27 1.399(6) . ? C26 C31 1.406(6) . ? C27 C28 1.396(7) . ? C28 C29 1.371(8) . ? C29 C30 1.369(7) . ? C30 C31 1.381(7) . ? C32 C37 1.388(7) . ? C32 C33 1.394(7) . ? C33 C34 1.387(7) . ? C34 C35 1.368(8) . ? C35 C36 1.368(8) . ? C36 C37 1.383(7) . ? C39 C40 1.352(6) . ? C41 C46 1.383(7) . ? C41 C42 1.385(7) . ? C42 C43 1.389(7) . ? C42 C47 1.511(7) . ? C43 C44 1.392(8) . ? C44 C45 1.377(8) . ? C44 C48 1.518(7) . ? C45 C46 1.386(7) . ? C46 C49 1.507(7) . ? C50 C51 1.388(7) . ? C50 C55 1.393(6) . ? C51 C52 1.387(6) . ? C51 C56 1.510(7) . ? C52 C53 1.376(7) . ? C53 C54 1.380(7) . ? C53 C57 1.520(7) . ? C54 C55 1.385(6) . ? C55 C58 1.507(7) . ? C59 C61 1.354(9) . ? C59 C60 1.367(10) . ? C60 C61 1.375(10) 3_767 ? C61 C60 1.375(10) 3_767 ? 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 C32 Pt1 C26 87.74(17) . . ? C32 Pt1 C11 178.29(18) . . ? C26 Pt1 C11 91.69(16) . . ? C32 Pt1 P1 97.23(13) . . ? C26 Pt1 P1 174.82(12) . . ? C11 Pt1 P1 83.39(11) . . ? C38 Cu1 N2 164.56(19) . . ? C14 P1 C13 103.8(2) . . ? C14 P1 C20 103.4(2) . . ? C13 P1 C20 101.6(2) . . ? C14 P1 Pt1 123.94(14) . . ? C13 P1 Pt1 103.15(15) . . ? C20 P1 Pt1 117.81(16) . . ? C5 N1 C1 114.8(4) . . ? C6 N2 C10 115.6(4) . . ? C6 N2 Cu1 117.5(3) . . ? C10 N2 Cu1 126.5(3) . . ? C38 N3 C39 112.3(4) . . ? C38 N3 C41 123.5(4) . . ? C39 N3 C41 124.2(4) . . ? C38 N4 C40 112.0(4) . . ? C38 N4 C50 123.7(4) . . ? C40 N4 C50 124.3(4) . . ? N1 C1 C2 123.2(5) . . ? C3 C2 C1 121.2(5) . . ? C2 C3 C4 117.9(5) . . ? C3 C4 C5 116.2(4) . . ? C3 C4 C11 133.7(4) . . ? C5 C4 C11 110.0(4) . . ? N1 C5 C4 126.6(4) . . ? N1 C5 C6 125.4(4) . . ? C4 C5 C6 108.0(4) . . ? N2 C6 C7 125.4(4) . . ? N2 C6 C5 126.4(4) . . ? C7 C6 C5 108.1(4) . . ? C8 C7 C6 116.5(4) . . ? C8 C7 C11 133.4(4) . . ? C6 C7 C11 110.1(4) . . ? C9 C8 C7 118.7(4) . . ? C10 C9 C8 120.2(5) . . ? N2 C10 C9 123.4(5) . . ? C7 C11 C4 103.3(4) . . ? C7 C11 C12 115.9(4) . . ? C4 C11 C12 116.7(4) . . ? C7 C11 Pt1 101.8(3) . . ? C4 C11 Pt1 107.5(3) . . ? C12 C11 Pt1 110.3(3) . . ? C13 C12 C11 114.5(4) . . ? C12 C13 P1 104.8(3) . . ? C15 C14 C19 118.4(5) . . ? C15 C14 P1 121.4(4) . . ? C19 C14 P1 120.1(3) . . ? C16 C15 C14 120.9(5) . . ? C15 C16 C17 120.8(5) . . ? C18 C17 C16 118.9(5) . . ? C17 C18 C19 120.9(5) . . ? C18 C19 C14 120.0(4) . . ? C25 C20 C21 118.5(4) . . ? C25 C20 P1 119.7(3) . . ? C21 C20 P1 121.8(4) . . ? C22 C21 C20 120.6(5) . . ? C23 C22 C21 119.9(5) . . ? C22 C23 C24 120.6(5) . . ? C23 C24 C25 119.8(5) . . ? C24 C25 C20 120.6(5) . . ? C27 C26 C31 115.1(4) . . ? C27 C26 Pt1 122.4(3) . . ? C31 C26 Pt1 122.2(3) . . ? C28 C27 C26 122.2(5) . . ? C29 C28 C27 120.5(5) . . ? C30 C29 C28 118.9(5) . . ? C29 C30 C31 120.8(5) . . ? C30 C31 C26 122.5(5) . . ? C37 C32 C33 114.7(4) . . ? C37 C32 Pt1 123.1(4) . . ? C33 C32 Pt1 122.2(4) . . ? C34 C33 C32 122.9(5) . . ? C35 C34 C33 119.7(5) . . ? C36 C35 C34 119.5(5) . . ? C35 C36 C37 119.8(5) . . ? C36 C37 C32 123.3(5) . . ? N4 C38 N3 102.8(4) . . ? N4 C38 Cu1 132.2(3) . . ? N3 C38 Cu1 124.5(3) . . ? C40 C39 N3 106.3(4) . . ? C39 C40 N4 106.5(4) . . ? C46 C41 C42 123.4(5) . . ? C46 C41 N3 117.5(5) . . ? C42 C41 N3 119.1(5) . . ? C41 C42 C43 117.4(5) . . ? C41 C42 C47 121.1(5) . . ? C43 C42 C47 121.5(5) . . ? C42 C43 C44 121.1(5) . . ? C45 C44 C43 119.0(5) . . ? C45 C44 C48 120.7(6) . . ? C43 C44 C48 120.2(5) . . ? C44 C45 C46 121.9(5) . . ? C41 C46 C45 117.1(5) . . ? C41 C46 C49 120.7(5) . . ? C45 C46 C49 122.1(5) . . ? C51 C50 C55 122.8(4) . . ? C51 C50 N4 117.9(4) . . ? C55 C50 N4 119.3(4) . . ? C52 C51 C50 117.2(4) . . ? C52 C51 C56 120.5(5) . . ? C50 C51 C56 122.3(5) . . ? C53 C52 C51 122.3(5) . . ? C52 C53 C54 118.3(5) . . ? C52 C53 C57 120.6(5) . . ? C54 C53 C57 121.1(5) . . ? C53 C54 C55 122.4(5) . . ? C54 C55 C50 116.9(4) . . ? C54 C55 C58 121.0(4) . . ? C50 C55 C58 122.1(4) . . ? C61 C59 C60 119.9(7) . . ? C59 C60 C61 118.8(7) . 3_767 ? C59 C61 C60 121.2(7) . 3_767 ? _refine_diff_density_max 0.891 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.108 _shelxl_version_number 2013-4 _iucr_refine_instructions_details ; TITL 2bBenzene in P2(1)/n CELL 0.71073 11.8289 21.9364 20.4095 90.000 106.006 90.000 ZERR 4.00 0.0006 0.0013 0.0010 0.000 0.002 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N P Cu Pt UNIT 244 228 16 4 4 4 SIZE 0.27 0.22 0.05 L.S. 16 OMIT -3 50 OMIT 0 2 1 OMIT 0 2 0 OMIT -1 1 1 OMIT -1 0 1 OMIT 0 1 1 OMIT 1 1 0 OMIT 0 2 2 BOND BIND cu1 pt1 FMAP 2 ACTA PLAN 5 TEMP -123.150 WGHT 0.026200 3.326900 FVAR 0.08302 PT1 6 -0.095508 1.090724 0.800397 11.00000 0.02022 0.01793 = 0.01710 0.00019 0.00326 0.00227 CU1 5 0.150777 0.869616 0.727136 11.00000 0.02528 0.02944 = 0.02865 -0.00383 0.00862 0.00627 P1 4 -0.104124 1.140472 0.896728 11.00000 0.01995 0.01994 = 0.01874 -0.00044 0.00531 0.00203 N1 3 0.257508 0.975794 0.789564 11.00000 0.02405 0.03131 = 0.04091 -0.00258 0.01637 0.00448 N2 3 0.056282 0.890850 0.786051 11.00000 0.02237 0.01961 = 0.02480 -0.00126 0.00373 0.00168 N3 3 0.345001 0.808430 0.696058 11.00000 0.02081 0.03551 = 0.02823 -0.00560 0.00577 0.00346 N4 3 0.194623 0.802375 0.610368 11.00000 0.02349 0.02951 = 0.02946 -0.00712 0.00891 0.00229 C1 1 0.337191 1.020774 0.797571 11.00000 0.02508 0.04390 = 0.06253 -0.00674 0.02106 -0.00360 AFIX 43 H1 2 0.402086 1.015303 0.779220 11.00000 -1.20000 AFIX 0 C2 1 0.329387 1.074756 0.831277 11.00000 0.03102 0.03470 = 0.06404 -0.01958 0.02019 -0.01359 AFIX 43 H2 2 0.388420 1.104976 0.835238 11.00000 -1.20000 AFIX 0 C3 1 0.237705 1.085419 0.859132 11.00000 0.02854 0.02902 = 0.03444 -0.00935 0.00686 -0.00191 AFIX 43 H3 2 0.232670 1.122441 0.882313 11.00000 -1.20000 AFIX 0 C4 1 0.152404 1.040149 0.852251 11.00000 0.01485 0.02241 = 0.02213 -0.00160 -0.00139 0.00317 C5 1 0.169522 0.986628 0.817595 11.00000 0.01549 0.01847 = 0.02848 -0.00238 0.00405 0.00387 C6 1 0.074902 0.945530 0.816805 11.00000 0.02203 0.01832 = 0.01913 0.00431 -0.00278 0.00602 C7 1 0.003339 0.972558 0.853864 11.00000 0.02023 0.02063 = 0.01766 0.00717 0.00048 0.00774 C8 1 -0.089825 0.937662 0.862057 11.00000 0.02546 0.02682 = 0.02570 0.00450 0.01007 0.00477 AFIX 43 H8 2 -0.139930 0.952753 0.887581 11.00000 -1.20000 AFIX 0 C9 1 -0.108242 0.880512 0.832336 11.00000 0.03382 0.01938 = 0.03757 0.00328 0.01531 -0.00137 AFIX 43 H9 2 -0.170947 0.855821 0.837872 11.00000 -1.20000 AFIX 0 C10 1 -0.036012 0.859291 0.794760 11.00000 0.03306 0.02276 = 0.03273 -0.00515 0.00747 -0.00350 AFIX 43 H10 2 -0.052194 0.820351 0.773908 11.00000 -1.20000 AFIX 0 C11 1 0.043220 1.035107 0.873553 11.00000 0.01851 0.02347 = 0.01958 0.00132 0.00425 0.00718 C12 1 0.050991 1.053176 0.947241 11.00000 0.02740 0.03073 = 0.01887 -0.00080 0.00284 0.00379 AFIX 23 H12A 2 -0.010181 1.030646 0.962064 11.00000 -1.20000 H12B 2 0.128469 1.040241 0.976841 11.00000 -1.20000 AFIX 0 C13 1 0.035823 1.120714 0.957808 11.00000 0.02102 0.03048 = 0.01879 -0.00450 0.00346 0.00020 AFIX 23 H13A 2 0.101197 1.144302 0.948667 11.00000 -1.20000 H13B 2 0.033218 1.129002 1.005052 11.00000 -1.20000 AFIX 0 C14 1 -0.111943 1.223139 0.903547 11.00000 0.01940 0.02062 = 0.02317 -0.00077 0.00949 0.00117 C15 1 -0.042357 1.254389 0.959740 11.00000 0.02647 0.02496 = 0.02681 -0.00177 0.00987 0.00105 AFIX 43 H15 2 0.006485 1.232123 0.996759 11.00000 -1.20000 AFIX 0 C16 1 -0.043438 1.316926 0.962321 11.00000 0.03212 0.03008 = 0.03489 -0.01074 0.01319 -0.00570 AFIX 43 H16 2 0.005428 1.337386 1.000821 11.00000 -1.20000 AFIX 0 C17 1 -0.115018 1.350615 0.909394 11.00000 0.04069 0.02217 = 0.04083 -0.00381 0.01748 -0.00012 AFIX 43 H17 2 -0.116053 1.393863 0.911604 11.00000 -1.20000 AFIX 0 C18 1 -0.184590 1.320333 0.853569 11.00000 0.03914 0.02273 = 0.04181 0.00566 0.00358 0.00884 AFIX 43 H18 2 -0.233697 1.343009 0.817014 11.00000 -1.20000 AFIX 0 C19 1 -0.183872 1.256983 0.850029 11.00000 0.02748 0.02335 = 0.02647 -0.00403 0.00279 -0.00167 AFIX 43 H19 2 -0.232277 1.236717 0.811230 11.00000 -1.20000 AFIX 0 C20 1 -0.210278 1.113132 0.940803 11.00000 0.02148 0.01427 = 0.02495 0.00552 0.00445 0.00468 C21 1 -0.211234 1.135476 1.004867 11.00000 0.02992 0.03312 = 0.03334 0.00137 0.01135 0.00011 AFIX 43 H21 2 -0.158544 1.167130 1.025431 11.00000 -1.20000 AFIX 0 C22 1 -0.287989 1.111957 1.038430 11.00000 0.03638 0.05305 = 0.03469 0.00520 0.01879 0.00873 AFIX 43 H22 2 -0.287375 1.127053 1.082155 11.00000 -1.20000 AFIX 0 C23 1 -0.365361 1.066659 1.008548 11.00000 0.03145 0.04942 = 0.05492 0.01637 0.02337 -0.00177 AFIX 43 H23 2 -0.418336 1.050688 1.031719 11.00000 -1.20000 AFIX 0 C24 1 -0.366756 1.044229 0.945324 11.00000 0.02950 0.03567 = 0.05479 0.00176 0.01702 -0.00331 AFIX 43 H24 2 -0.420805 1.013086 0.924873 11.00000 -1.20000 AFIX 0 C25 1 -0.289087 1.067213 0.911609 11.00000 0.02704 0.02523 = 0.03626 0.00294 0.01193 0.00302 AFIX 43 H25 2 -0.289707 1.051448 0.868158 11.00000 -1.20000 AFIX 0 C26 1 -0.073205 1.042967 0.718561 11.00000 0.02806 0.01724 = 0.01866 0.00514 0.00222 0.00678 C27 1 0.025024 1.050868 0.693906 11.00000 0.03777 0.01948 = 0.02692 0.00458 0.00936 -0.00194 AFIX 43 H27 2 0.077785 1.083387 0.711340 11.00000 -1.20000 AFIX 0 C28 1 0.048115 1.012535 0.644507 11.00000 0.04746 0.04140 = 0.02577 0.00112 0.01804 0.00776 AFIX 43 H28 2 0.116934 1.018632 0.629937 11.00000 -1.20000 AFIX 0 C29 1 -0.027800 0.966166 0.616879 11.00000 0.07047 0.04190 = 0.02699 -0.00707 0.01149 0.01965 AFIX 43 H29 2 -0.011645 0.939746 0.583694 11.00000 -1.20000 AFIX 0 C30 1 -0.127283 0.958554 0.637896 11.00000 0.05644 0.03150 = 0.03491 -0.01386 -0.00089 0.00108 AFIX 43 H30 2 -0.181819 0.927455 0.617945 11.00000 -1.20000 AFIX 0 C31 1 -0.149295 0.995546 0.687751 11.00000 0.02863 0.03146 = 0.02931 -0.00420 0.00356 -0.00338 AFIX 43 H31 2 -0.218463 0.988679 0.701743 11.00000 -1.20000 AFIX 0 C32 1 -0.224405 1.138901 0.733596 11.00000 0.03534 0.01855 = 0.01646 -0.00381 0.00040 0.00800 C33 1 -0.200336 1.179139 0.686299 11.00000 0.04080 0.03818 = 0.03369 0.01114 0.01472 0.01339 AFIX 43 H33 2 -0.121770 1.182110 0.683342 11.00000 -1.20000 AFIX 0 C34 1 -0.285948 1.215030 0.643364 11.00000 0.06987 0.04058 = 0.03965 0.01734 0.02386 0.02016 AFIX 43 H34 2 -0.265418 1.242252 0.612298 11.00000 -1.20000 AFIX 0 C35 1 -0.400090 1.211074 0.645931 11.00000 0.06397 0.04593 = 0.02491 0.00185 0.00031 0.02956 AFIX 43 H35 2 -0.458962 1.236061 0.617296 11.00000 -1.20000 AFIX 0 C36 1 -0.428825 1.170892 0.690012 11.00000 0.02194 0.05195 = 0.04119 -0.00259 -0.00844 0.00636 AFIX 43 H36 2 -0.508166 1.167129 0.691348 11.00000 -1.20000 AFIX 0 C37 1 -0.342007 1.135754 0.732637 11.00000 0.03371 0.03018 = 0.03375 0.00695 -0.00254 0.00548 AFIX 43 H37 2 -0.363991 1.108080 0.762767 11.00000 -1.20000 AFIX 0 C38 1 0.231229 0.827454 0.673582 11.00000 0.02157 0.02569 = 0.02781 0.00224 0.00924 -0.00032 C39 1 0.377902 0.773695 0.648705 11.00000 0.02142 0.03857 = 0.04789 -0.01213 0.01582 0.00914 AFIX 43 H39 2 0.452696 0.755623 0.653374 11.00000 -1.20000 AFIX 0 C40 1 0.282754 0.770234 0.593979 11.00000 0.03251 0.04930 = 0.04047 -0.01293 0.01493 0.00486 AFIX 43 H40 2 0.277782 0.749620 0.552343 11.00000 -1.20000 AFIX 0 C41 1 0.421278 0.822855 0.762895 11.00000 0.01816 0.03400 = 0.03847 -0.00674 0.00727 0.00299 C42 1 0.488257 0.875561 0.771421 11.00000 0.02603 0.03362 = 0.03818 -0.00788 0.00997 0.00680 C43 1 0.560810 0.887601 0.836234 11.00000 0.02308 0.03056 = 0.05989 -0.01230 0.01320 0.00285 AFIX 43 H43 2 0.608388 0.923200 0.843676 11.00000 -1.20000 AFIX 0 C44 1 0.564948 0.848362 0.890458 11.00000 0.02866 0.03677 = 0.04723 -0.01221 -0.00604 0.00701 C45 1 0.497623 0.796198 0.878882 11.00000 0.04142 0.04206 = 0.04342 0.00946 -0.00703 0.00820 AFIX 43 H45 2 0.501065 0.769223 0.915796 11.00000 -1.20000 AFIX 0 C46 1 0.424991 0.781890 0.814969 11.00000 0.02554 0.03302 = 0.04209 0.00470 0.00316 0.00357 C47 1 0.480207 0.918876 0.712714 11.00000 0.06451 0.03076 = 0.05680 -0.00835 0.03103 -0.00774 AFIX 137 H47A 2 0.495985 0.896639 0.674528 11.00000 -1.50000 H47B 2 0.538294 0.951514 0.727269 11.00000 -1.50000 H47C 2 0.401122 0.936558 0.698283 11.00000 -1.50000 AFIX 0 C48 1 0.643987 0.862722 0.961015 11.00000 0.05338 0.05861 = 0.06261 -0.01246 -0.02452 0.01532 AFIX 137 H48A 2 0.722970 0.846580 0.965364 11.00000 -1.50000 H48B 2 0.611673 0.843869 0.995487 11.00000 -1.50000 H48C 2 0.648342 0.906985 0.967744 11.00000 -1.50000 AFIX 0 C49 1 0.351951 0.724604 0.801948 11.00000 0.05463 0.04897 = 0.05734 0.01442 -0.00817 -0.01715 AFIX 137 H49A 2 0.368891 0.700153 0.843718 11.00000 -1.50000 H49B 2 0.371121 0.700986 0.765678 11.00000 -1.50000 H49C 2 0.268328 0.735409 0.787979 11.00000 -1.50000 AFIX 0 C50 1 0.077549 0.811086 0.564622 11.00000 0.02456 0.02615 = 0.02173 -0.00667 0.00514 0.00336 C51 1 0.064938 0.851359 0.510640 11.00000 0.03447 0.02509 = 0.02881 -0.00819 0.01115 -0.00797 C52 1 -0.047498 0.859526 0.467863 11.00000 0.04243 0.03772 = 0.02214 0.00078 0.00710 0.00197 AFIX 43 H52 2 -0.058410 0.886508 0.430223 11.00000 -1.20000 AFIX 0 C53 1 -0.143834 0.829911 0.478027 11.00000 0.02922 0.03924 = 0.02612 -0.00472 0.00787 0.00152 C54 1 -0.126206 0.788860 0.531140 11.00000 0.02777 0.04076 = 0.03471 -0.00074 0.01142 -0.00729 AFIX 43 H54 2 -0.191884 0.767110 0.537417 11.00000 -1.20000 AFIX 0 C55 1 -0.016340 0.778205 0.575612 11.00000 0.02771 0.02460 = 0.03289 0.00139 0.01288 0.00167 C56 1 0.167447 0.886551 0.499081 11.00000 0.04647 0.05596 = 0.04441 0.00470 0.01423 -0.01632 AFIX 137 H56A 2 0.214176 0.903754 0.542410 11.00000 -1.50000 H56B 2 0.137992 0.919600 0.466542 11.00000 -1.50000 H56C 2 0.216709 0.859143 0.480789 11.00000 -1.50000 AFIX 0 C57 1 -0.266149 0.841643 0.431190 11.00000 0.02647 0.09684 = 0.04358 0.01182 0.00665 0.00927 AFIX 137 H57A 2 -0.302518 0.802811 0.413004 11.00000 -1.50000 H57B 2 -0.260363 0.867981 0.393464 11.00000 -1.50000 H57C 2 -0.314421 0.861701 0.456907 11.00000 -1.50000 AFIX 0 C58 1 -0.000318 0.733026 0.633064 11.00000 0.03961 0.04029 = 0.05657 0.01536 0.01541 -0.00232 AFIX 137 H58A 2 0.078467 0.715082 0.642984 11.00000 -1.50000 H58B 2 -0.059522 0.700751 0.619806 11.00000 -1.50000 H58C 2 -0.009480 0.753861 0.673768 11.00000 -1.50000 AFIX 0 C59 1 0.904336 0.528033 0.957366 11.00000 0.03373 0.04562 = 0.10987 -0.02710 -0.01122 0.00408 AFIX 43 H59 2 0.838245 0.547590 0.927592 11.00000 -1.20000 AFIX 0 C60 1 0.893282 0.499114 1.014605 11.00000 0.05949 0.04719 = 0.12766 -0.02454 0.02312 0.00599 AFIX 43 H60 2 0.819816 0.498295 1.025017 11.00000 -1.20000 AFIX 0 C61 1 1.009578 0.528780 0.943142 11.00000 0.07867 0.03535 = 0.08741 -0.01781 0.00795 0.00032 AFIX 43 H61 2 1.016450 0.548948 0.903228 11.00000 -1.20000 AFIX 0 HKLF 4 REM 2bBenzene in P2(1)/n REM R1 = 0.0336 for 6812 Fo > 4sig(Fo) and 0.0564 for all 8942 data REM 619 parameters refined using 0 restraints END WGHT 0.0261 3.3746 REM Highest difference peak 0.891, deepest hole -0.598, 1-sigma level 0.108 Q1 1 -0.1167 1.0891 0.8438 11.00000 0.05 0.89 Q2 1 -0.0917 1.0941 0.7568 11.00000 0.05 0.86 Q3 1 -0.1794 1.0937 0.7982 11.00000 0.05 0.79 Q4 1 -0.1336 1.0946 0.7029 11.00000 0.05 0.70 Q5 1 -0.0507 1.0912 0.8926 11.00000 0.05 0.68 ; _database_code_depnum_ccdc_archive 'CCDC 953914' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H47 N2 Na O6 Pt' _chemical_formula_weight 809.82 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_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 18.3296(11) _cell_length_b 17.6541(10) _cell_length_c 12.0217(8) _cell_angle_alpha 90 _cell_angle_beta 113.916(2) _cell_angle_gamma 90 _cell_volume 3556.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13313 _cell_measurement_theta_min 2.960 _cell_measurement_theta_max 24.997 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_F_000 1632 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 4.002 _shelx_estimated_absorpt_T_min 0.240 _shelx_estimated_absorpt_T_max 0.825 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.4043 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'Bruker Apex 2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker Kappa Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13313 _diffrn_reflns_av_unetI/netI 0.0352 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.960 _diffrn_reflns_theta_max 24.997 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.973 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.973 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.973 _reflns_number_total 3138 _reflns_number_gt 2873 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker Apex 2 software package' _computing_cell_refinement 'Bruker Apex 2 software package' _computing_data_reduction 'Bruker Apex 2 software package' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'ORTEP and POV-Ray' _computing_publication_material 'SHELXL-2013 (Sheldrick, 2013)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+1.5514P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3138 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0494 _refine_ls_wR_factor_gt 0.0479 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.5000 0.17326(2) 0.2500 0.02339(7) Uani 1 2 d S T P . . Na1 Na 0.5000 0.28763(10) 0.7500 0.0265(4) Uani 1 2 d S T P C . O1 O 0.43246(14) 0.18165(12) 0.7754(2) 0.0398(6) Uani 1 1 d . . . . . O2 O 0.45609(14) 0.36701(15) 0.8626(2) 0.0509(7) Uani 1 1 d . . . . . O3 O 0.38945(15) 0.30901(15) 0.5543(2) 0.0470(7) Uani 1 1 d . . . . . N1 N 0.41518(13) 0.26597(14) 0.1913(2) 0.0255(6) Uani 1 1 d . . . . . C1 C 0.33608(16) 0.27583(19) 0.1364(3) 0.0292(7) Uani 1 1 d . . . . . H1 H 0.3020 0.2328 0.1141 0.035 Uiso 1 1 calc R U . . . C2 C 0.30241(17) 0.3491(2) 0.1113(3) 0.0319(8) Uani 1 1 d . . . . . H2 H 0.2461 0.3538 0.0705 0.038 Uiso 1 1 calc R U . . . C3 C 0.34785(17) 0.41394(19) 0.1434(3) 0.0294(7) Uani 1 1 d . . . . . H3 H 0.3235 0.4625 0.1259 0.035 Uiso 1 1 calc R U . . . C4 C 0.43161(17) 0.40650(18) 0.2031(3) 0.0260(7) Uani 1 1 d . . . . . C5 C 0.45847(17) 0.33009(16) 0.2214(3) 0.0226(6) Uani 1 1 d . . . . . C6 C 0.5000 0.4542(3) 0.2500 0.0272(10) Uani 1 2 d S T P . . H6 H 0.5000 0.5080 0.2500 0.033 Uiso 1 2 calc R U P . . C7 C 0.41633(17) 0.09317(17) 0.1920(3) 0.0263(7) Uani 1 1 d . . . . . C8 C 0.36374(18) 0.0801(2) 0.2482(3) 0.0372(8) Uani 1 1 d . . . . . H8 H 0.3682 0.1106 0.3158 0.045 Uiso 1 1 calc R U . . . C9 C 0.30549(19) 0.0244(2) 0.2088(3) 0.0437(9) Uani 1 1 d . . . . . H9 H 0.2718 0.0171 0.2506 0.052 Uiso 1 1 calc R U . . . C10 C 0.29578(19) -0.0203(2) 0.1100(3) 0.0432(9) Uani 1 1 d . . . . . H10 H 0.2556 -0.0582 0.0830 0.052 Uiso 1 1 calc R U . . . C11 C 0.3456(2) -0.0089(2) 0.0510(3) 0.0407(9) Uani 1 1 d . . . . . H11 H 0.3392 -0.0388 -0.0180 0.049 Uiso 1 1 calc R U . . . C12 C 0.40542(18) 0.04613(17) 0.0921(3) 0.0310(7) Uani 1 1 d . . . . . H12 H 0.4398 0.0520 0.0512 0.037 Uiso 1 1 calc R U . . . C13 C 0.48155(18) 0.11591(19) 0.7948(3) 0.0334(8) Uani 1 1 d . . . . . H13A H 0.4489 0.0697 0.7846 0.040 Uiso 1 1 calc R U . C . H13B H 0.5237 0.1163 0.8785 0.040 Uiso 1 1 calc R U . . . C14 C 0.3881(3) 0.1814(2) 0.8500(5) 0.0586(12) Uani 1 1 d . . . . . H14A H 0.3559 0.1352 0.8343 0.088 Uiso 1 1 calc R U . . . H14B H 0.3531 0.2258 0.8307 0.088 Uiso 1 1 calc R U . . . H14C H 0.4252 0.1830 0.9359 0.088 Uiso 1 1 calc R U . . . C15 C 0.3796(3) 0.3976(3) 0.8339(5) 0.0686(13) Uani 1 1 d . . . . . H15A H 0.3585 0.3783 0.8914 0.103 Uiso 1 1 calc R U . . . H15B H 0.3440 0.3828 0.7510 0.103 Uiso 1 1 calc R U . . . H15C H 0.3832 0.4530 0.8395 0.103 Uiso 1 1 calc R U . . . C16 C 0.4858(3) 0.3858(2) 0.5213(3) 0.0663(13) Uani 1 1 d . . . . . H16A H 0.4947 0.4388 0.5029 0.080 Uiso 0.5 1 d R U P A 1 H16B H 0.4931 0.3530 0.4598 0.080 Uiso 0.5 1 d R U P A 1 H16C H 0.4648 0.4349 0.5263 0.080 Uiso 0.5 1 d R U P B 2 H16D H 0.5113 0.3896 0.4658 0.080 Uiso 0.5 1 d R U P B 2 C17A C 0.4144(5) 0.3793(6) 0.5109(8) 0.052(2) Uani 0.5 1 d . . P C 1 H17A H 0.3791 0.3853 0.4236 0.063 Uiso 0.5 1 calc R U P C 1 H17B H 0.4035 0.4225 0.5544 0.063 Uiso 0.5 1 calc R U P C 1 C17B C 0.4126(5) 0.3278(5) 0.4662(7) 0.0437(18) Uani 0.5 1 d . . P C 2 H17C H 0.3679 0.3518 0.3979 0.052 Uiso 0.5 1 calc R U P C 2 H17D H 0.4293 0.2820 0.4351 0.052 Uiso 0.5 1 calc R U P C 2 C18A C 0.3785(5) 0.2508(5) 0.4677(7) 0.055(2) Uani 0.5 1 d . . P C 1 H18A H 0.3345 0.2644 0.3906 0.082 Uiso 0.5 1 calc R U P C 1 H18B H 0.3659 0.2032 0.4979 0.082 Uiso 0.5 1 calc R U P C 1 H18C H 0.4276 0.2445 0.4546 0.082 Uiso 0.5 1 calc R U P C 1 C18B C 0.3210(5) 0.2532(6) 0.5096(8) 0.068(3) Uani 0.5 1 d . . P C 2 H18D H 0.2753 0.2762 0.4433 0.101 Uiso 0.5 1 calc R U P C 2 H18E H 0.3059 0.2400 0.5765 0.101 Uiso 0.5 1 calc R U P C 2 H18F H 0.3375 0.2074 0.4799 0.101 Uiso 0.5 1 calc R U P C 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 0.02686(9) 0.02266(11) 0.02355(10) 0.000 0.01319(7) 0.000 Na1 0.0356(9) 0.0247(10) 0.0253(9) 0.000 0.0185(7) 0.000 O1 0.0502(14) 0.0294(14) 0.0579(16) 0.0116(11) 0.0405(13) 0.0074(10) O2 0.0521(14) 0.0474(17) 0.0692(19) -0.0209(14) 0.0412(14) -0.0026(12) O3 0.0528(15) 0.0583(19) 0.0286(13) 0.0004(12) 0.0151(12) -0.0041(12) N1 0.0275(12) 0.0286(15) 0.0224(13) -0.0012(11) 0.0122(11) -0.0003(11) C1 0.0234(15) 0.037(2) 0.0258(17) -0.0057(15) 0.0088(13) -0.0020(13) C2 0.0228(15) 0.043(2) 0.0278(17) -0.0045(15) 0.0078(13) 0.0033(13) C3 0.0318(16) 0.031(2) 0.0251(17) 0.0008(14) 0.0112(14) 0.0096(14) C4 0.0292(15) 0.0318(19) 0.0186(15) 0.0009(13) 0.0113(13) 0.0045(13) C5 0.0261(14) 0.0254(18) 0.0183(14) -0.0011(12) 0.0111(12) -0.0005(12) C6 0.035(2) 0.023(3) 0.023(2) 0.000 0.0115(19) 0.000 C7 0.0322(16) 0.0212(18) 0.0256(17) 0.0013(13) 0.0117(13) 0.0036(12) C8 0.0395(18) 0.036(2) 0.043(2) -0.0054(16) 0.0234(16) -0.0044(15) C9 0.0383(18) 0.040(2) 0.058(2) 0.0029(19) 0.0254(17) -0.0043(16) C10 0.0340(17) 0.032(2) 0.049(2) 0.0006(18) 0.0012(16) -0.0055(15) C11 0.049(2) 0.029(2) 0.0294(18) -0.0042(15) 0.0012(16) 0.0051(16) C12 0.0397(17) 0.0256(19) 0.0274(17) 0.0033(14) 0.0133(14) 0.0051(13) C13 0.0373(17) 0.0258(19) 0.037(2) 0.0000(15) 0.0147(15) 0.0010(14) C14 0.078(3) 0.038(2) 0.095(4) 0.011(2) 0.071(3) 0.0033(19) C15 0.084(3) 0.053(3) 0.101(4) 0.022(3) 0.071(3) 0.029(2) C16 0.129(4) 0.043(3) 0.034(2) 0.0060(19) 0.041(3) -0.020(3) C17A 0.057(5) 0.069(7) 0.031(5) 0.024(5) 0.017(4) 0.015(5) C17B 0.049(4) 0.050(6) 0.035(4) -0.001(4) 0.020(4) 0.000(4) C18A 0.049(4) 0.063(6) 0.045(5) -0.013(4) 0.012(4) 0.000(4) C18B 0.047(5) 0.097(8) 0.050(5) 0.006(5) 0.010(4) -0.029(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 C7 1.993(3) . ? Pt1 C7 1.993(3) 2_655 ? Pt1 N1 2.169(2) 2_655 ? Pt1 N1 2.169(2) . ? Na1 O2 2.308(3) 2_656 ? Na1 O2 2.308(3) . ? Na1 O1 2.331(3) 2_656 ? Na1 O1 2.331(3) . ? Na1 O3 2.432(2) . ? Na1 O3 2.432(2) 2_656 ? Na1 C17A 3.112(7) 2_656 ? Na1 C17A 3.112(7) . ? Na1 C13 3.121(4) . ? Na1 C13 3.121(4) 2_656 ? O1 C13 1.429(4) . ? O1 C14 1.433(4) . ? O2 C15 1.408(4) . ? O2 C16 1.410(5) 2_656 ? O3 C17B 1.334(8) . ? O3 C18A 1.419(8) . ? O3 C17A 1.488(10) . ? O3 C18B 1.512(8) . ? N1 C1 1.339(3) . ? N1 C5 1.345(4) . ? C1 C2 1.412(5) . ? C2 C3 1.376(5) . ? C3 C4 1.413(4) . ? C4 C5 1.422(4) . ? C4 C6 1.423(4) . ? C5 C5 1.394(6) 2_655 ? C6 C4 1.423(4) 2_655 ? C7 C8 1.403(4) . ? C7 C12 1.406(4) . ? C8 C9 1.386(5) . ? C9 C10 1.376(5) . ? C10 C11 1.379(5) . ? C11 C12 1.397(5) . ? C13 C13 1.485(6) 2_656 ? C16 C17A 1.269(9) . ? C16 O2 1.410(5) 2_656 ? C16 C17B 1.602(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 C7 Pt1 C7 89.60(16) . 2_655 ? C7 Pt1 N1 176.21(10) . 2_655 ? C7 Pt1 N1 94.19(11) 2_655 2_655 ? C7 Pt1 N1 94.19(11) . . ? C7 Pt1 N1 176.21(10) 2_655 . ? N1 Pt1 N1 82.02(13) 2_655 . ? O2 Na1 O2 105.22(15) 2_656 . ? O2 Na1 O1 94.61(9) 2_656 2_656 ? O2 Na1 O1 153.42(10) . 2_656 ? O2 Na1 O1 153.42(10) 2_656 . ? O2 Na1 O1 94.61(9) . . ? O1 Na1 O1 73.23(12) 2_656 . ? O2 Na1 O3 71.97(9) 2_656 . ? O2 Na1 O3 96.95(10) . . ? O1 Na1 O3 106.04(10) 2_656 . ? O1 Na1 O3 88.45(9) . . ? O2 Na1 O3 96.95(10) 2_656 2_656 ? O2 Na1 O3 71.97(9) . 2_656 ? O1 Na1 O3 88.45(9) 2_656 2_656 ? O1 Na1 O3 106.04(10) . 2_656 ? O3 Na1 O3 162.14(15) . 2_656 ? C13 O1 C14 112.0(2) . . ? C13 O1 Na1 109.90(17) . . ? C14 O1 Na1 123.4(2) . . ? C15 O2 C16 115.4(3) . 2_656 ? C15 O2 Na1 129.7(3) . . ? C16 O2 Na1 114.9(2) 2_656 . ? C18A O3 C17A 108.6(6) . . ? C17B O3 C18B 111.4(5) . . ? C17B O3 Na1 113.5(4) . . ? C18A O3 Na1 114.3(4) . . ? C17A O3 Na1 102.4(3) . . ? C18B O3 Na1 119.3(4) . . ? C1 N1 C5 115.2(3) . . ? C1 N1 Pt1 138.5(2) . . ? C5 N1 Pt1 106.30(18) . . ? N1 C1 C2 121.1(3) . . ? C3 C2 C1 122.7(3) . . ? C2 C3 C4 118.3(3) . . ? C3 C4 C5 113.8(3) . . ? C3 C4 C6 138.4(3) . . ? C5 C4 C6 107.8(3) . . ? N1 C5 C5 122.69(16) . 2_655 ? N1 C5 C4 128.8(3) . . ? C5 C5 C4 108.47(16) 2_655 . ? C4 C6 C4 107.5(4) . 2_655 ? C8 C7 C12 115.3(3) . . ? C8 C7 Pt1 122.0(2) . . ? C12 C7 Pt1 122.7(2) . . ? C9 C8 C7 122.5(3) . . ? C10 C9 C8 120.9(3) . . ? C9 C10 C11 118.6(3) . . ? C10 C11 C12 120.5(3) . . ? C11 C12 C7 122.1(3) . . ? O1 C13 C13 108.9(2) . 2_656 ? C17A C16 O2 114.3(5) . 2_656 ? O2 C16 C17B 115.4(4) 2_656 . ? C16 C17A O3 119.5(7) . . ? O3 C17B C16 108.3(6) . . ? _refine_diff_density_max 0.710 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.087 _shelxl_version_number 2013-4 _iucr_refine_instructions_details ; TITL 3 in C2/c CELL 0.71073 18.3296 17.6541 12.0217 90.000 113.916 90.000 ZERR 4.00 0.0011 0.0010 0.0008 0.000 0.002 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O Na Pt UNIT 140 188 8 24 4 4 SIZE 0.5 0.2 0.05 OMIT 1 1 0 OMIT -3 50 L.S. 10 ACTA BOND FMAP 2 PLAN 5 TEMP -123.170 WGHT 0.023300 1.551400 FVAR 0.04898 PT1 6 0.500000 0.173263 0.250000 10.50000 0.02686 0.02266 = 0.02355 0.00000 0.01319 0.00000 NA1 5 0.500000 0.287626 0.750000 10.50000 0.03557 0.02472 = 0.02532 0.00000 0.01850 0.00000 O1 4 0.432461 0.181655 0.775434 11.00000 0.05015 0.02940 = 0.05795 0.01161 0.04051 0.00737 O2 4 0.456094 0.367007 0.862583 11.00000 0.05212 0.04738 = 0.06922 -0.02088 0.04117 -0.00258 O3 4 0.389449 0.309010 0.554340 11.00000 0.05279 0.05834 = 0.02859 0.00044 0.01506 -0.00411 N1 3 0.415175 0.265971 0.191280 11.00000 0.02751 0.02862 = 0.02245 -0.00121 0.01221 -0.00026 C1 1 0.336080 0.275833 0.136441 11.00000 0.02335 0.03726 = 0.02576 -0.00572 0.00881 -0.00202 AFIX 43 H1 2 0.302026 0.232818 0.114073 11.00000 -1.20000 AFIX 0 C2 1 0.302409 0.349097 0.111281 11.00000 0.02275 0.04298 = 0.02778 -0.00453 0.00784 0.00325 AFIX 43 H2 2 0.246091 0.353800 0.070513 11.00000 -1.20000 AFIX 0 C3 1 0.347849 0.413939 0.143408 11.00000 0.03177 0.03104 = 0.02507 0.00082 0.01117 0.00959 AFIX 43 H3 2 0.323512 0.462512 0.125904 11.00000 -1.20000 AFIX 0 C4 1 0.431614 0.406499 0.203085 11.00000 0.02920 0.03182 = 0.01857 0.00095 0.01127 0.00446 C5 1 0.458468 0.330094 0.221359 11.00000 0.02614 0.02539 = 0.01830 -0.00115 0.01113 -0.00046 C6 1 0.500000 0.454155 0.250000 10.50000 0.03520 0.02324 = 0.02305 0.00000 0.01154 0.00000 AFIX 43 H6 2 0.499998 0.507967 0.250001 10.50000 -1.20000 AFIX 0 C7 1 0.416329 0.093173 0.191985 11.00000 0.03223 0.02122 = 0.02558 0.00126 0.01175 0.00360 C8 1 0.363745 0.080107 0.248204 11.00000 0.03948 0.03552 = 0.04301 -0.00545 0.02337 -0.00438 AFIX 43 H8 2 0.368236 0.110564 0.315826 11.00000 -1.20000 AFIX 0 C9 1 0.305494 0.024449 0.208826 11.00000 0.03825 0.04028 = 0.05826 0.00295 0.02538 -0.00431 AFIX 43 H9 2 0.271790 0.017056 0.250603 11.00000 -1.20000 AFIX 0 C10 1 0.295779 -0.020272 0.110041 11.00000 0.03397 0.03188 = 0.04869 0.00059 0.00117 -0.00547 AFIX 43 H10 2 0.255575 -0.058186 0.083035 11.00000 -1.20000 AFIX 0 C11 1 0.345602 -0.008926 0.051044 11.00000 0.04921 0.02921 = 0.02936 -0.00424 0.00120 0.00511 AFIX 43 H11 2 0.339190 -0.038788 -0.018048 11.00000 -1.20000 AFIX 0 C12 1 0.405421 0.046127 0.092074 11.00000 0.03969 0.02560 = 0.02737 0.00330 0.01326 0.00515 AFIX 43 H12 2 0.439847 0.051974 0.051156 11.00000 -1.20000 AFIX 0 C13 1 0.481550 0.115908 0.794766 11.00000 0.03734 0.02585 = 0.03675 -0.00002 0.01471 0.00095 AFIX 23 H13A 2 0.448901 0.069669 0.784592 11.00000 -1.20000 H13B 2 0.523688 0.116265 0.878536 11.00000 -1.20000 AFIX 0 C14 1 0.388139 0.181379 0.849959 11.00000 0.07781 0.03822 = 0.09503 0.01094 0.07123 0.00329 AFIX 137 H14A 2 0.355870 0.135171 0.834259 11.00000 -1.50000 H14B 2 0.353068 0.225773 0.830687 11.00000 -1.50000 H14C 2 0.425162 0.183004 0.935906 11.00000 -1.50000 AFIX 0 C15 1 0.379636 0.397606 0.833937 11.00000 0.08436 0.05295 = 0.10140 0.02169 0.07146 0.02894 AFIX 137 H15A 2 0.358474 0.378317 0.891376 11.00000 -1.50000 H15B 2 0.344009 0.382827 0.751017 11.00000 -1.50000 H15C 2 0.383218 0.452966 0.839482 11.00000 -1.50000 AFIX 0 C16 1 0.485809 0.385780 0.521317 11.00000 0.12877 0.04335 = 0.03438 0.00596 0.04087 -0.01968 AFIX 3 PART 1 H16A 2 0.494689 0.438780 0.502937 10.50000 -1.20000 H16B 2 0.493129 0.352960 0.459847 10.50000 -1.20000 PART 2 H16C 2 0.464849 0.434890 0.526327 10.50000 -1.20000 H16D 2 0.511288 0.389570 0.465757 10.50000 -1.20000 AFIX 0 PART 1 C17A 1 0.414399 0.379276 0.510896 10.50000 0.05688 0.06892 = 0.03101 0.02379 0.01721 0.01488 AFIX 23 H17A 2 0.379104 0.385308 0.423634 10.50000 -1.20000 H17B 2 0.403471 0.422466 0.554409 10.50000 -1.20000 AFIX 0 PART 2 C17B 1 0.412612 0.327835 0.466190 10.50000 0.04898 0.05041 = 0.03473 -0.00102 0.02000 -0.00012 AFIX 23 H17C 2 0.367899 0.351843 0.397873 10.50000 -1.20000 H17D 2 0.429313 0.282013 0.435138 10.50000 -1.20000 AFIX 0 PART 1 C18A 1 0.378501 0.250773 0.467658 10.50000 0.04889 0.06318 = 0.04536 -0.01302 0.01183 0.00043 AFIX 137 H18A 2 0.334498 0.264396 0.390624 10.50000 -1.50000 H18B 2 0.365873 0.203163 0.497898 10.50000 -1.50000 H18C 2 0.427573 0.244540 0.454589 10.50000 -1.50000 AFIX 0 PART 2 C18B 1 0.321003 0.253235 0.509555 10.50000 0.04725 0.09654 = 0.04959 0.00603 0.00999 -0.02937 AFIX 137 H18D 2 0.275261 0.276173 0.443256 10.50000 -1.50000 H18E 2 0.305891 0.239958 0.576513 10.50000 -1.50000 H18F 2 0.337491 0.207418 0.479866 10.50000 -1.50000 PART 0 AFIX 0 HKLF 4 REM 3 in C2/c REM R1 = 0.0224 for 2873 Fo > 4sig(Fo) and 0.0270 for all 3138 data REM 227 parameters refined using 0 restraints END WGHT 0.0233 1.5515 REM Highest difference peak 0.710, deepest hole -0.903, 1-sigma level 0.087 Q1 1 0.5027 0.1765 0.3969 11.00000 0.05 0.71 Q2 1 0.4681 0.1703 0.1609 11.00000 0.05 0.69 Q3 1 0.4683 0.1757 0.3446 11.00000 0.05 0.67 Q4 1 0.4970 0.2259 0.3264 11.00000 0.05 0.67 Q5 1 0.4886 0.1204 0.3285 11.00000 0.05 0.62 ; _database_code_depnum_ccdc_archive 'CCDC 953915' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H61 Cu N4 Pt' _chemical_formula_weight 1060.72 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.1488(8) _cell_length_b 20.0623(14) _cell_length_c 20.5295(16) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5003.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 38782 _cell_measurement_theta_min 1.948 _cell_measurement_theta_max 25.242 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_F_000 2152 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.125 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.070 _exptl_absorpt_coefficient_mu 3.258 _shelx_estimated_absorpt_T_min 0.686 _shelx_estimated_absorpt_T_max 0.804 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.6043 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'Bruker Apex 2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker Kappa Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 38782 _diffrn_reflns_av_unetI/netI 0.0743 _diffrn_reflns_av_R_equivalents 0.0642 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.948 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.973 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.973 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.971 _reflns_number_total 8805 _reflns_number_gt 7254 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.800 _reflns_Friedel_fraction_max 0.999 _reflns_Friedel_fraction_full 0.970 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker Apex 2 software package' _computing_cell_refinement 'Bruker Apex 2 software package' _computing_data_reduction 'Bruker Apex 2 software package' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'ORTEP and POV-Ray' _computing_publication_material 'SHELXL-2013 (Sheldrick, 2013)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0108P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 2819 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.008(5) _chemical_absolute_configuration ad _refine_ls_number_reflns 8805 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0601 _refine_ls_wR_factor_gt 0.0556 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt -0.02806(2) -0.62342(2) -1.12794(2) 0.02868(9) Uani 1 1 d . . . . . Cu1 Cu -0.01291(7) -0.59847(4) -0.85917(4) 0.0268(2) Uani 1 1 d . . . . . N1 N -0.1096(5) -0.4724(3) -0.8141(3) 0.0296(16) Uani 1 1 d . . . . . N2 N -0.2239(5) -0.5524(3) -0.8115(3) 0.0285(16) Uani 1 1 d . . . . . N3 N 0.0940(5) -0.5862(3) -1.0593(3) 0.0270(16) Uani 1 1 d . . . . . N4 N -0.0624(5) -0.6917(3) -1.0496(3) 0.0277(17) Uani 1 1 d . . . . . C1 C -0.1187(6) -0.5383(4) -0.8266(4) 0.0261(19) Uani 1 1 d . . . . . C2 C -0.2783(7) -0.4968(5) -0.7899(4) 0.038(2) Uani 1 1 d . . . . . H2 H -0.3530 -0.4947 -0.7763 0.045 Uiso 1 1 calc R U . . . C3 C -0.2083(6) -0.4467(4) -0.7915(4) 0.035(2) Uani 1 1 d . . . . . H3 H -0.2226 -0.4018 -0.7796 0.042 Uiso 1 1 calc R U . . . C4 C -0.0093(6) -0.4351(4) -0.8233(4) 0.0302(19) Uani 1 1 d . . . . . C5 C 0.0042(5) -0.4005(3) -0.8819(4) 0.036(2) Uani 1 1 d . . . . . C6 C 0.1038(7) -0.3677(5) -0.8906(5) 0.052(3) Uani 1 1 d . . . . . H6 H 0.1170 -0.3440 -0.9299 0.062 Uiso 1 1 calc R U . . . C7 C 0.1840(7) -0.3693(5) -0.8429(5) 0.059(3) Uani 1 1 d . . . . . H7 H 0.2513 -0.3462 -0.8493 0.070 Uiso 1 1 calc R U . . . C8 C 0.1671(7) -0.4036(4) -0.7872(5) 0.047(3) Uani 1 1 d . . . . . H8 H 0.2242 -0.4047 -0.7556 0.056 Uiso 1 1 calc R U . . . C9 C 0.0700(6) -0.4373(4) -0.7743(4) 0.034(2) Uani 1 1 d . . . . . C10 C -0.0833(7) -0.3998(4) -0.9339(4) 0.044(2) Uani 1 1 d . . . . . H10 H -0.1477 -0.4254 -0.9166 0.053 Uiso 1 1 calc R U . . . C11 C -0.0457(8) -0.4343(6) -0.9944(5) 0.090(4) Uani 1 1 d . . . . . H11A H -0.0140 -0.4777 -0.9830 0.135 Uiso 1 1 calc R U . . . H11B H 0.0101 -0.4071 -1.0163 0.135 Uiso 1 1 calc R U . . . H11C H -0.1086 -0.4409 -1.0237 0.135 Uiso 1 1 calc R U . . . C12 C -0.1228(10) -0.3288(6) -0.9471(7) 0.100(5) Uani 1 1 d . . . . . H12A H -0.1761 -0.3291 -0.9829 0.150 Uiso 1 1 calc R U . . . H12B H -0.0598 -0.3008 -0.9589 0.150 Uiso 1 1 calc R U . . . H12C H -0.1578 -0.3108 -0.9078 0.150 Uiso 1 1 calc R U . . . C13 C 0.0561(6) -0.4775(4) -0.7122(4) 0.038(2) Uani 1 1 d . . . . . H13 H -0.0201 -0.4964 -0.7120 0.045 Uiso 1 1 calc R U . . . C14 C 0.1375(7) -0.5360(5) -0.7119(5) 0.055(3) Uani 1 1 d . . . . . H14A H 0.2130 -0.5188 -0.7111 0.083 Uiso 1 1 calc R U . . . H14B H 0.1267 -0.5630 -0.7512 0.083 Uiso 1 1 calc R U . . . H14C H 0.1247 -0.5637 -0.6733 0.083 Uiso 1 1 calc R U . . . C15 C 0.0682(7) -0.4339(5) -0.6523(5) 0.060(3) Uani 1 1 d . . . . . H15A H 0.0120 -0.3989 -0.6531 0.089 Uiso 1 1 calc R U . . . H15B H 0.1415 -0.4135 -0.6521 0.089 Uiso 1 1 calc R U . . . H15C H 0.0590 -0.4612 -0.6131 0.089 Uiso 1 1 calc R U . . . C16 C -0.2681(5) -0.6192(5) -0.8185(4) 0.035(2) Uani 1 1 d . . . . . C17 C -0.3280(5) -0.6335(4) -0.8758(5) 0.043(2) Uani 1 1 d . . . . . C18 C -0.3635(6) -0.6987(5) -0.8820(6) 0.057(3) Uani 1 1 d . . . . . H18 H -0.4036 -0.7111 -0.9199 0.069 Uiso 1 1 calc R U . . . C19 C -0.3431(8) -0.7453(6) -0.8359(7) 0.072(4) Uani 1 1 d . . . . . H19 H -0.3685 -0.7896 -0.8422 0.086 Uiso 1 1 calc R U . . . C20 C -0.2858(8) -0.7295(5) -0.7797(6) 0.060(3) Uani 1 1 d . . . . . H20 H -0.2728 -0.7627 -0.7475 0.072 Uiso 1 1 calc R U . . . C21 C -0.2471(6) -0.6645(4) -0.7705(5) 0.041(2) Uani 1 1 d . . . . . C22 C -0.3480(7) -0.5821(5) -0.9270(5) 0.048(3) Uani 1 1 d . . . . . H22 H -0.3436 -0.5374 -0.9056 0.058 Uiso 1 1 calc R U . . . C23 C -0.4622(7) -0.5876(6) -0.9589(5) 0.087(4) Uani 1 1 d . . . . . H23A H -0.5189 -0.5887 -0.9249 0.131 Uiso 1 1 calc R U . . . H23B H -0.4659 -0.6286 -0.9847 0.131 Uiso 1 1 calc R U . . . H23C H -0.4745 -0.5491 -0.9873 0.131 Uiso 1 1 calc R U . . . C24 C -0.2603(8) -0.5840(6) -0.9801(5) 0.071(3) Uani 1 1 d . . . . . H24A H -0.2650 -0.6264 -1.0036 0.107 Uiso 1 1 calc R U . . . H24B H -0.1873 -0.5797 -0.9602 0.107 Uiso 1 1 calc R U . . . H24C H -0.2723 -0.5470 -1.0105 0.107 Uiso 1 1 calc R U . . . C25 C -0.1853(7) -0.6479(4) -0.7080(5) 0.048(3) Uani 1 1 d . . . . . H25 H -0.1684 -0.5992 -0.7094 0.058 Uiso 1 1 calc R U . . . C26 C -0.2551(8) -0.6597(6) -0.6470(5) 0.075(3) Uani 1 1 d . . . . . H26A H -0.2697 -0.7075 -0.6422 0.112 Uiso 1 1 calc R U . . . H26B H -0.3249 -0.6356 -0.6511 0.112 Uiso 1 1 calc R U . . . H26C H -0.2153 -0.6435 -0.6086 0.112 Uiso 1 1 calc R U . . . C27 C -0.0760(8) -0.6840(5) -0.7046(6) 0.068(3) Uani 1 1 d . . . . . H27A H -0.0305 -0.6713 -0.7420 0.101 Uiso 1 1 calc R U . . . H27B H -0.0887 -0.7322 -0.7054 0.101 Uiso 1 1 calc R U . . . H27C H -0.0380 -0.6719 -0.6642 0.101 Uiso 1 1 calc R U . . . C28 C 0.0903(6) -0.6628(4) -0.8992(4) 0.031(2) Uani 1 1 d . . . . . H28 H 0.1310 -0.6761 -0.8647 0.037 Uiso 1 1 d R U . . . C29 C 0.0080(6) -0.7013(4) -0.9362(4) 0.0281(19) Uani 1 1 d . . . . . C30 C 0.0047(5) -0.6750(4) -0.9999(4) 0.0244(19) Uani 1 1 d . . . . . C31 C 0.0824(5) -0.6237(4) -1.0055(3) 0.0234(16) Uani 1 1 d . . . . . C32 C 0.1378(5) -0.6161(4) -0.9453(3) 0.0247(17) Uani 1 1 d . . . . . C33 C 0.2206(6) -0.5673(4) -0.9452(4) 0.033(2) Uani 1 1 d . . . . . H33 H 0.2644 -0.5595 -0.9077 0.039 Uiso 1 1 calc R U . . . C34 C 0.2362(6) -0.5310(4) -1.0015(5) 0.037(2) Uani 1 1 d . . . . . H34 H 0.2927 -0.4982 -1.0025 0.045 Uiso 1 1 calc R U . . . C35 C 0.1725(6) -0.5406(4) -1.0570(4) 0.034(2) Uani 1 1 d . . . . . H35 H 0.1857 -0.5136 -1.0943 0.041 Uiso 1 1 calc R U . . . C36 C -0.0669(6) -0.7531(4) -0.9254(4) 0.036(2) Uani 1 1 d . . . . . H36 H -0.0713 -0.7744 -0.8842 0.043 Uiso 1 1 calc R U . . . C37 C -0.1340(6) -0.7722(4) -0.9760(4) 0.036(2) Uani 1 1 d . . . . . H37 H -0.1844 -0.8078 -0.9693 0.044 Uiso 1 1 calc R U . . . C38 C -0.1309(6) -0.7415(4) -1.0366(4) 0.034(2) Uani 1 1 d . . . . . H38 H -0.1793 -0.7566 -1.0698 0.041 Uiso 1 1 calc R U . . . C39 C -0.1405(6) -0.6671(4) -1.1839(4) 0.032(2) Uani 1 1 d . . . . . C40 C -0.2519(6) -0.6648(4) -1.1693(4) 0.034(2) Uani 1 1 d . . . . . H40 H -0.2759 -0.6382 -1.1337 0.041 Uiso 1 1 calc R U . . . C41 C -0.3306(7) -0.7009(5) -1.2055(5) 0.044(2) Uani 1 1 d . . . . . H41 H -0.4064 -0.6982 -1.1944 0.053 Uiso 1 1 calc R U . . . C42 C -0.2977(8) -0.7400(5) -1.2567(5) 0.053(3) Uani 1 1 d . . . . . H42 H -0.3503 -0.7647 -1.2810 0.063 Uiso 1 1 calc R U . . . C43 C -0.1876(8) -0.7432(5) -1.2729(5) 0.055(3) Uani 1 1 d . . . . . H43 H -0.1637 -0.7700 -1.3083 0.066 Uiso 1 1 calc R U . . . C44 C -0.1118(7) -0.7066(5) -1.2363(5) 0.046(3) Uani 1 1 d . . . . . H44 H -0.0363 -0.7089 -1.2482 0.056 Uiso 1 1 calc R U . . . C45 C 0.0080(6) -0.5538(4) -1.1938(4) 0.033(2) Uani 1 1 d . . . . . C46 C 0.0455(6) -0.5654(5) -1.2566(4) 0.041(2) Uani 1 1 d . . . . . H46 H 0.0509 -0.6101 -1.2715 0.049 Uiso 1 1 calc R U . . . C47 C 0.0753(7) -0.5140(6) -1.2985(5) 0.052(3) Uani 1 1 d . . . . . H47 H 0.1021 -0.5245 -1.3408 0.062 Uiso 1 1 calc R U . . . C48 C 0.0670(6) -0.4496(5) -1.2801(5) 0.049(3) Uani 1 1 d . . . . . H48 H 0.0853 -0.4148 -1.3097 0.058 Uiso 1 1 calc R U . . . C49 C 0.0317(7) -0.4349(4) -1.2185(5) 0.046(2) Uani 1 1 d . . . . . H49 H 0.0271 -0.3898 -1.2047 0.055 Uiso 1 1 calc R U . . . C50 C 0.0024(5) -0.4863(4) -1.1757(4) 0.038(2) Uani 1 1 d . . . . . H50 H -0.0219 -0.4752 -1.1331 0.046 Uiso 1 1 calc R U . . . C51 C -0.7165(13) -0.3448(6) -1.0595(7) 0.111(5) Uani 1 1 d . . . . . H51A H -0.7455 -0.2992 -1.0589 0.166 Uiso 1 1 calc R U . . . H51B H -0.7742 -0.3759 -1.0457 0.166 Uiso 1 1 calc R U . . . H51C H -0.6927 -0.3560 -1.1038 0.166 Uiso 1 1 calc R U . . . C52 C -0.6141(17) -0.3501(8) -1.0109(10) 0.114(6) Uani 1 1 d . . . . . C53 C -0.5274(18) -0.3916(9) -1.0193(8) 0.135(6) Uani 1 1 d . . . . . H53 H -0.5258 -0.4204 -1.0560 0.162 Uiso 1 1 calc R U . . . C54 C -0.4358(17) -0.3932(12) -0.9727(10) 0.168(10) Uani 1 1 d . . . . . H54 H -0.3763 -0.4226 -0.9814 0.202 Uiso 1 1 calc R U . . . C55 C -0.4309(15) -0.3575(12) -0.9210(10) 0.151(9) Uani 1 1 d . . . . . H55 H -0.3722 -0.3605 -0.8905 0.181 Uiso 1 1 calc R U . . . C56 C -0.5145(17) -0.3162(10) -0.9138(9) 0.155(8) Uani 1 1 d . . . . . H56 H -0.5151 -0.2873 -0.8771 0.186 Uiso 1 1 calc R U . . . C57 C -0.6043(15) -0.3128(11) -0.9586(11) 0.146(7) Uani 1 1 d . . . . . H57 H -0.6608 -0.2813 -0.9500 0.176 Uiso 1 1 calc R U . . . 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 0.02729(14) 0.03608(15) 0.02266(14) -0.00113(18) -0.00218(14) 0.00645(14) Cu1 0.0253(5) 0.0283(5) 0.0269(6) -0.0045(4) 0.0028(4) 0.0033(3) N1 0.026(4) 0.038(4) 0.025(4) -0.007(3) -0.002(3) 0.002(3) N2 0.022(4) 0.037(4) 0.026(4) -0.013(3) -0.001(3) 0.001(3) N3 0.028(4) 0.035(4) 0.018(4) -0.001(3) 0.002(3) 0.001(3) N4 0.024(4) 0.029(4) 0.030(4) -0.012(3) 0.001(3) 0.004(3) C1 0.023(5) 0.031(5) 0.023(5) -0.003(4) -0.004(3) 0.001(3) C2 0.024(5) 0.049(6) 0.040(6) -0.016(5) 0.000(4) 0.008(4) C3 0.024(5) 0.041(6) 0.040(6) -0.022(5) -0.002(4) 0.007(4) C4 0.028(5) 0.027(4) 0.035(5) -0.008(4) 0.006(4) -0.003(3) C5 0.044(5) 0.035(4) 0.029(5) 0.002(4) 0.005(4) 0.006(3) C6 0.058(6) 0.048(6) 0.051(7) 0.005(6) 0.012(5) -0.012(5) C7 0.045(6) 0.061(7) 0.070(8) 0.007(7) 0.004(5) -0.015(5) C8 0.036(5) 0.047(6) 0.057(7) -0.002(5) -0.008(4) -0.013(4) C9 0.024(5) 0.032(5) 0.044(6) -0.004(4) -0.001(4) 0.001(3) C10 0.061(6) 0.041(6) 0.030(6) -0.001(4) 0.001(4) 0.011(4) C11 0.080(8) 0.144(11) 0.046(7) -0.039(8) -0.003(6) 0.030(7) C12 0.115(10) 0.070(9) 0.115(13) 0.009(8) -0.054(9) 0.021(7) C13 0.023(5) 0.048(6) 0.041(6) -0.004(5) -0.006(3) -0.005(4) C14 0.061(7) 0.059(7) 0.046(7) 0.004(6) -0.015(5) 0.015(5) C15 0.069(7) 0.066(7) 0.043(7) -0.013(5) -0.008(5) 0.010(5) C16 0.017(4) 0.038(5) 0.050(6) -0.012(5) 0.005(3) -0.007(4) C17 0.026(4) 0.047(6) 0.055(6) -0.015(7) 0.005(4) -0.001(4) C18 0.044(6) 0.060(7) 0.068(9) -0.032(7) 0.001(5) -0.010(5) C19 0.063(7) 0.058(8) 0.094(11) -0.023(8) 0.013(7) -0.028(6) C20 0.058(7) 0.061(8) 0.060(9) 0.005(6) 0.015(6) -0.015(5) C21 0.037(5) 0.040(6) 0.045(7) -0.004(5) 0.009(4) -0.015(4) C22 0.032(5) 0.065(7) 0.048(7) -0.026(6) -0.013(4) 0.005(4) C23 0.043(6) 0.144(11) 0.076(9) -0.017(8) -0.024(6) 0.007(7) C24 0.059(7) 0.093(9) 0.063(9) 0.009(7) -0.001(6) 0.016(6) C25 0.063(6) 0.037(6) 0.044(7) 0.004(5) 0.004(5) 0.000(4) C26 0.077(7) 0.100(9) 0.047(8) 0.003(6) 0.014(5) 0.009(6) C27 0.062(7) 0.079(9) 0.061(9) 0.008(7) 0.004(6) 0.006(6) C28 0.029(4) 0.035(5) 0.029(5) -0.004(4) -0.004(3) 0.010(3) C29 0.031(5) 0.030(4) 0.024(5) 0.002(4) 0.000(3) 0.010(3) C30 0.027(5) 0.023(4) 0.023(5) -0.007(3) -0.002(3) 0.012(3) C31 0.020(4) 0.026(4) 0.024(4) -0.005(5) 0.002(3) 0.008(4) C32 0.023(4) 0.027(5) 0.024(4) 0.000(4) -0.001(3) 0.012(4) C33 0.021(4) 0.044(6) 0.033(6) -0.004(4) -0.007(4) 0.003(4) C34 0.020(4) 0.050(6) 0.041(6) 0.004(5) 0.000(4) -0.006(4) C35 0.026(5) 0.044(6) 0.032(6) 0.003(4) 0.004(4) -0.007(4) C36 0.051(6) 0.024(5) 0.032(6) 0.009(4) -0.002(4) 0.003(4) C37 0.038(5) 0.027(5) 0.044(6) 0.000(5) -0.009(4) -0.005(4) C38 0.034(5) 0.034(5) 0.034(6) -0.003(4) -0.011(4) 0.000(4) C39 0.033(5) 0.033(5) 0.030(6) 0.009(4) 0.000(4) 0.007(4) C40 0.043(5) 0.032(5) 0.028(5) 0.009(4) 0.003(4) 0.001(4) C41 0.036(5) 0.045(6) 0.051(7) 0.028(5) -0.007(4) -0.011(4) C42 0.069(7) 0.052(7) 0.037(7) -0.005(6) -0.017(5) -0.015(5) C43 0.055(7) 0.068(8) 0.043(7) -0.026(6) -0.003(5) -0.005(5) C44 0.037(5) 0.066(7) 0.037(6) -0.014(5) -0.001(4) 0.003(4) C45 0.018(5) 0.044(5) 0.037(5) -0.001(4) -0.011(3) 0.007(3) C46 0.025(5) 0.063(6) 0.035(6) 0.003(5) 0.004(4) 0.008(4) C47 0.040(6) 0.079(8) 0.037(6) 0.010(6) 0.010(4) 0.008(5) C48 0.026(5) 0.064(7) 0.056(7) 0.033(6) 0.000(4) -0.001(4) C49 0.039(5) 0.044(5) 0.053(7) 0.004(5) -0.007(5) -0.003(5) C50 0.030(6) 0.051(6) 0.033(5) 0.007(4) -0.006(3) 0.001(4) C51 0.196(16) 0.077(10) 0.059(10) 0.007(8) 0.010(10) -0.002(9) C52 0.19(2) 0.038(9) 0.110(17) -0.004(9) 0.033(14) -0.008(10) C53 0.203(18) 0.111(15) 0.090(14) 0.008(11) 0.033(14) -0.035(14) C54 0.19(2) 0.23(3) 0.083(14) -0.013(17) -0.029(13) -0.069(17) C55 0.096(13) 0.23(3) 0.130(18) 0.060(17) -0.034(12) -0.009(13) C56 0.124(16) 0.23(2) 0.108(15) 0.063(14) -0.055(13) -0.015(15) C57 0.126(16) 0.19(2) 0.123(19) 0.048(17) 0.028(13) -0.010(14) _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 C39 1.989(8) . ? Pt1 C45 1.994(8) . ? Pt1 N4 2.153(7) . ? Pt1 N3 2.177(6) . ? Cu1 C1 1.886(7) . ? Cu1 C28 1.979(7) . ? N1 C1 1.350(9) . ? N1 C3 1.385(9) . ? N1 C4 1.443(9) . ? N2 C1 1.346(8) . ? N2 C2 1.371(10) . ? N2 C16 1.450(10) . ? N3 C35 1.323(9) . ? N3 C31 1.344(9) . ? N4 C38 1.328(10) . ? N4 C30 1.348(9) . ? C2 C3 1.317(11) . ? C4 C9 1.394(10) . ? C4 C5 1.398(10) . ? C5 C6 1.388(10) . ? C5 C10 1.507(11) . ? C6 C7 1.382(12) . ? C7 C8 1.349(12) . ? C8 C9 1.386(10) . ? C9 C13 1.518(11) . ? C10 C11 1.494(12) . ? C10 C12 1.528(12) . ? C13 C15 1.515(11) . ? C13 C14 1.535(11) . ? C16 C21 1.365(12) . ? C16 C17 1.412(12) . ? C17 C18 1.382(11) . ? C17 C22 1.494(13) . ? C18 C19 1.354(14) . ? C19 C20 1.384(15) . ? C20 C21 1.401(12) . ? C21 C25 1.523(12) . ? C22 C24 1.523(13) . ? C22 C23 1.538(11) . ? C25 C27 1.515(12) . ? C25 C26 1.531(12) . ? C28 C32 1.451(10) . ? C28 C29 1.473(10) . ? C29 C36 1.399(10) . ? C29 C30 1.409(10) . ? C30 C31 1.403(10) . ? C31 C32 1.415(9) . ? C32 C33 1.404(10) . ? C33 C34 1.379(11) . ? C34 C35 1.391(11) . ? C36 C37 1.375(11) . ? C37 C38 1.388(11) . ? C39 C44 1.380(11) . ? C39 C40 1.387(10) . ? C40 C41 1.412(12) . ? C41 C42 1.371(13) . ? C42 C43 1.379(12) . ? C43 C44 1.398(12) . ? C45 C46 1.387(11) . ? C45 C50 1.406(10) . ? C46 C47 1.391(12) . ? C47 C48 1.351(12) . ? C48 C49 1.368(12) . ? C49 C50 1.400(11) . ? C51 C52 1.60(2) . ? C52 C57 1.31(2) . ? C52 C53 1.35(2) . ? C53 C54 1.47(2) . ? C54 C55 1.28(3) . ? C55 C56 1.32(2) . ? C56 C57 1.43(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 C39 Pt1 C45 93.9(3) . . ? C39 Pt1 N4 91.1(3) . . ? C45 Pt1 N4 174.4(3) . . ? C39 Pt1 N3 173.1(3) . . ? C45 Pt1 N3 92.8(3) . . ? N4 Pt1 N3 82.4(2) . . ? C1 Cu1 C28 175.5(3) . . ? C1 Cu1 Pt1 112.8(2) . . ? C1 N1 C3 110.9(6) . . ? C1 N1 C4 123.6(6) . . ? C3 N1 C4 125.5(7) . . ? C1 N2 C2 111.1(6) . . ? C1 N2 C16 121.6(6) . . ? C2 N2 C16 127.3(6) . . ? C35 N3 C31 115.6(7) . . ? C35 N3 Pt1 138.7(6) . . ? C31 N3 Pt1 105.6(5) . . ? C38 N4 C30 114.4(7) . . ? C38 N4 Pt1 138.6(6) . . ? C30 N4 Pt1 106.9(5) . . ? N2 C1 N1 103.9(6) . . ? N2 C1 Cu1 126.4(6) . . ? N1 C1 Cu1 129.6(5) . . ? C3 C2 N2 107.6(7) . . ? C2 C3 N1 106.5(8) . . ? C9 C4 C5 123.8(7) . . ? C9 C4 N1 118.2(7) . . ? C5 C4 N1 118.0(7) . . ? C6 C5 C4 116.6(7) . . ? C6 C5 C10 121.3(8) . . ? C4 C5 C10 122.0(7) . . ? C7 C6 C5 120.8(9) . . ? C8 C7 C6 120.4(8) . . ? C7 C8 C9 122.7(8) . . ? C8 C9 C4 115.8(8) . . ? C8 C9 C13 121.0(7) . . ? C4 C9 C13 123.2(7) . . ? C11 C10 C5 111.7(7) . . ? C11 C10 C12 112.4(10) . . ? C5 C10 C12 110.8(8) . . ? C15 C13 C9 111.3(7) . . ? C15 C13 C14 112.1(7) . . ? C9 C13 C14 109.8(7) . . ? C21 C16 C17 124.2(8) . . ? C21 C16 N2 118.2(7) . . ? C17 C16 N2 117.6(8) . . ? C18 C17 C16 115.6(9) . . ? C18 C17 C22 122.5(9) . . ? C16 C17 C22 121.9(8) . . ? C19 C18 C17 122.1(10) . . ? C18 C19 C20 121.1(10) . . ? C19 C20 C21 119.6(11) . . ? C16 C21 C20 117.4(9) . . ? C16 C21 C25 123.8(8) . . ? C20 C21 C25 118.8(9) . . ? C17 C22 C24 111.9(7) . . ? C17 C22 C23 113.3(8) . . ? C24 C22 C23 109.0(8) . . ? C27 C25 C21 111.5(8) . . ? C27 C25 C26 112.0(8) . . ? C21 C25 C26 112.5(8) . . ? C32 C28 C29 105.8(7) . . ? C32 C28 Cu1 95.8(5) . . ? C29 C28 Cu1 97.3(5) . . ? C36 C29 C30 113.9(7) . . ? C36 C29 C28 138.4(7) . . ? C30 C29 C28 107.6(6) . . ? N4 C30 C31 121.8(7) . . ? N4 C30 C29 128.8(7) . . ? C31 C30 C29 109.3(7) . . ? N3 C31 C30 123.3(7) . . ? N3 C31 C32 127.5(7) . . ? C30 C31 C32 109.1(7) . . ? C33 C32 C31 114.6(7) . . ? C33 C32 C28 137.3(7) . . ? C31 C32 C28 108.1(7) . . ? C34 C33 C32 117.8(7) . . ? C33 C34 C35 122.5(7) . . ? N3 C35 C34 121.7(8) . . ? C37 C36 C29 118.2(8) . . ? C36 C37 C38 122.4(8) . . ? N4 C38 C37 122.1(8) . . ? C44 C39 C40 115.8(8) . . ? C44 C39 Pt1 121.9(6) . . ? C40 C39 Pt1 122.0(6) . . ? C39 C40 C41 122.0(8) . . ? C42 C41 C40 120.0(8) . . ? C41 C42 C43 119.6(8) . . ? C42 C43 C44 119.0(9) . . ? C39 C44 C43 123.6(8) . . ? C46 C45 C50 115.1(8) . . ? C46 C45 Pt1 125.7(7) . . ? C50 C45 Pt1 119.0(6) . . ? C45 C46 C47 122.3(9) . . ? C48 C47 C46 121.2(9) . . ? C47 C48 C49 119.2(9) . . ? C48 C49 C50 120.2(8) . . ? C49 C50 C45 122.0(8) . . ? C57 C52 C53 113(2) . . ? C57 C52 C51 122.9(18) . . ? C53 C52 C51 124.5(18) . . ? C52 C53 C54 121.3(19) . . ? C55 C54 C53 124(2) . . ? C54 C55 C56 114.0(19) . . ? C55 C56 C57 123(2) . . ? C52 C57 C56 125(2) . . ? _refine_diff_density_max 0.814 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.089 _shelxl_version_number 2013-4 _iucr_refine_instructions_details ; TITL 5toluene in P2(1)2(1)2(1) CELL 0.71073 12.1488 20.0623 20.5295 90.000 90.000 90.000 ZERR 4.00 0.0008 0.0014 0.0016 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N Pt Cu UNIT 228 244 16 4 4 OMIT -3 50 L.S. 10 ACTA SIZE 0.125 0.1 0.07 BOND BIND Cu1 Pt1 FMAP 2 PLAN 5 TEMP -123.150 WGHT 0.010800 FVAR 0.06985 PT1 4 -0.028062 -0.623419 -1.127937 11.00000 0.02729 0.03608 = 0.02266 -0.00113 -0.00218 0.00645 CU1 5 -0.012912 -0.598466 -0.859170 11.00000 0.02535 0.02828 = 0.02692 -0.00449 0.00279 0.00333 N1 3 -0.109572 -0.472437 -0.814105 11.00000 0.02587 0.03833 = 0.02460 -0.00661 -0.00152 0.00197 N2 3 -0.223935 -0.552437 -0.811473 11.00000 0.02236 0.03669 = 0.02647 -0.01334 -0.00108 0.00078 N3 3 0.093955 -0.586178 -1.059342 11.00000 0.02772 0.03513 = 0.01816 -0.00088 0.00215 0.00081 N4 3 -0.062437 -0.691655 -1.049585 11.00000 0.02398 0.02898 = 0.03028 -0.01162 0.00051 0.00443 C1 1 -0.118738 -0.538267 -0.826634 11.00000 0.02348 0.03146 = 0.02331 -0.00315 -0.00367 0.00066 C2 1 -0.278346 -0.496767 -0.789933 11.00000 0.02420 0.04901 = 0.03986 -0.01624 -0.00040 0.00795 AFIX 43 H2 2 -0.353007 -0.494688 -0.776325 11.00000 -1.20000 AFIX 0 C3 1 -0.208264 -0.446687 -0.791537 11.00000 0.02417 0.04135 = 0.03965 -0.02206 -0.00211 0.00710 AFIX 43 H3 2 -0.222581 -0.401772 -0.779576 11.00000 -1.20000 AFIX 0 C4 1 -0.009344 -0.435050 -0.823319 11.00000 0.02834 0.02741 = 0.03470 -0.00772 0.00564 -0.00267 C5 1 0.004211 -0.400476 -0.881898 11.00000 0.04351 0.03488 = 0.02888 0.00208 0.00521 0.00597 C6 1 0.103806 -0.367738 -0.890629 11.00000 0.05755 0.04795 = 0.05059 0.00512 0.01209 -0.01153 AFIX 43 H6 2 0.117013 -0.343963 -0.929878 11.00000 -1.20000 AFIX 0 C7 1 0.183954 -0.369338 -0.842885 11.00000 0.04530 0.06054 = 0.07025 0.00706 0.00442 -0.01502 AFIX 43 H7 2 0.251290 -0.346176 -0.849303 11.00000 -1.20000 AFIX 0 C8 1 0.167142 -0.403603 -0.787201 11.00000 0.03603 0.04720 = 0.05659 -0.00212 -0.00782 -0.01253 AFIX 43 H8 2 0.224223 -0.404682 -0.755591 11.00000 -1.20000 AFIX 0 C9 1 0.069963 -0.437286 -0.774265 11.00000 0.02445 0.03233 = 0.04382 -0.00382 -0.00085 0.00059 C10 1 -0.083322 -0.399802 -0.933886 11.00000 0.06114 0.04114 = 0.03028 -0.00053 0.00093 0.01121 AFIX 13 H10 2 -0.147667 -0.425374 -0.916613 11.00000 -1.20000 AFIX 0 C11 1 -0.045717 -0.434346 -0.994416 11.00000 0.08012 0.14422 = 0.04576 -0.03858 -0.00275 0.02997 AFIX 137 H11A 2 -0.014041 -0.477729 -0.983015 11.00000 -1.50000 H11B 2 0.010105 -0.407079 -1.016267 11.00000 -1.50000 H11C 2 -0.108554 -0.440883 -1.023659 11.00000 -1.50000 AFIX 0 C12 1 -0.122801 -0.328763 -0.947060 11.00000 0.11540 0.06964 = 0.11515 0.00900 -0.05390 0.02114 AFIX 137 H12A 2 -0.176073 -0.329124 -0.982904 11.00000 -1.50000 H12B 2 -0.059803 -0.300774 -0.958926 11.00000 -1.50000 H12C 2 -0.157847 -0.310825 -0.907800 11.00000 -1.50000 AFIX 0 C13 1 0.056105 -0.477522 -0.712168 11.00000 0.02340 0.04847 = 0.04095 -0.00373 -0.00625 -0.00535 AFIX 13 H13 2 -0.020072 -0.496405 -0.712038 11.00000 -1.20000 AFIX 0 C14 1 0.137476 -0.536044 -0.711922 11.00000 0.06086 0.05922 = 0.04591 0.00423 -0.01513 0.01474 AFIX 137 H14A 2 0.212960 -0.518838 -0.711098 11.00000 -1.50000 H14B 2 0.126715 -0.562989 -0.751225 11.00000 -1.50000 H14C 2 0.124708 -0.563669 -0.673284 11.00000 -1.50000 AFIX 0 C15 1 0.068191 -0.433924 -0.652348 11.00000 0.06914 0.06648 = 0.04297 -0.01256 -0.00820 0.01042 AFIX 137 H15A 2 0.011957 -0.398910 -0.653112 11.00000 -1.50000 H15B 2 0.141456 -0.413486 -0.652129 11.00000 -1.50000 H15C 2 0.058977 -0.461170 -0.613104 11.00000 -1.50000 AFIX 0 C16 1 -0.268139 -0.619171 -0.818524 11.00000 0.01708 0.03788 = 0.04971 -0.01163 0.00542 -0.00720 C17 1 -0.328031 -0.633544 -0.875752 11.00000 0.02621 0.04737 = 0.05534 -0.01546 0.00520 -0.00120 C18 1 -0.363528 -0.698654 -0.882008 11.00000 0.04400 0.05995 = 0.06809 -0.03231 0.00059 -0.01032 AFIX 43 H18 2 -0.403550 -0.711089 -0.919860 11.00000 -1.20000 AFIX 0 C19 1 -0.343086 -0.745321 -0.835895 11.00000 0.06340 0.05816 = 0.09383 -0.02311 0.01293 -0.02798 AFIX 43 H19 2 -0.368482 -0.789633 -0.842240 11.00000 -1.20000 AFIX 0 C20 1 -0.285828 -0.729549 -0.779686 11.00000 0.05787 0.06108 = 0.06041 0.00532 0.01519 -0.01514 AFIX 43 H20 2 -0.272840 -0.762686 -0.747536 11.00000 -1.20000 AFIX 0 C21 1 -0.247134 -0.664459 -0.770463 11.00000 0.03653 0.04003 = 0.04530 -0.00366 0.00935 -0.01514 C22 1 -0.347989 -0.582074 -0.927027 11.00000 0.03191 0.06486 = 0.04849 -0.02645 -0.01314 0.00501 AFIX 13 H22 2 -0.343630 -0.537407 -0.905562 11.00000 -1.20000 AFIX 0 C23 1 -0.462172 -0.587634 -0.958885 11.00000 0.04262 0.14411 = 0.07569 -0.01739 -0.02446 0.00749 AFIX 137 H23A 2 -0.518874 -0.588717 -0.924948 11.00000 -1.50000 H23B 2 -0.465945 -0.628644 -0.984724 11.00000 -1.50000 H23C 2 -0.474469 -0.549086 -0.987288 11.00000 -1.50000 AFIX 0 C24 1 -0.260327 -0.583965 -0.980057 11.00000 0.05905 0.09270 = 0.06260 0.00875 -0.00111 0.01597 AFIX 137 H24A 2 -0.265013 -0.626369 -1.003592 11.00000 -1.50000 H24B 2 -0.187309 -0.579707 -0.960200 11.00000 -1.50000 H24C 2 -0.272269 -0.547036 -1.010494 11.00000 -1.50000 AFIX 0 C25 1 -0.185306 -0.647919 -0.707965 11.00000 0.06266 0.03746 = 0.04446 0.00390 0.00387 0.00015 AFIX 13 H25 2 -0.168414 -0.599158 -0.709421 11.00000 -1.20000 AFIX 0 C26 1 -0.255077 -0.659694 -0.646966 11.00000 0.07656 0.10049 = 0.04748 0.00302 0.01434 0.00876 AFIX 137 H26A 2 -0.269697 -0.707484 -0.642184 11.00000 -1.50000 H26B 2 -0.324945 -0.635644 -0.651071 11.00000 -1.50000 H26C 2 -0.215265 -0.643496 -0.608585 11.00000 -1.50000 AFIX 0 C27 1 -0.075963 -0.684015 -0.704577 11.00000 0.06245 0.07944 = 0.06105 0.00771 0.00398 0.00600 AFIX 137 H27A 2 -0.030523 -0.671272 -0.742002 11.00000 -1.50000 H27B 2 -0.088657 -0.732248 -0.705362 11.00000 -1.50000 H27C 2 -0.037957 -0.671881 -0.664176 11.00000 -1.50000 AFIX 0 C28 1 0.090292 -0.662828 -0.899234 11.00000 0.02943 0.03490 = 0.02865 -0.00373 -0.00401 0.01010 AFIX 3 H28 2 0.131012 -0.676128 -0.864744 11.00000 -1.20000 AFIX 0 C29 1 0.008045 -0.701279 -0.936249 11.00000 0.03076 0.02972 = 0.02396 0.00176 -0.00007 0.00992 C30 1 0.004661 -0.675032 -0.999878 11.00000 0.02658 0.02324 = 0.02348 -0.00684 -0.00206 0.01185 C31 1 0.082442 -0.623661 -1.005487 11.00000 0.02008 0.02585 = 0.02440 -0.00540 0.00226 0.00782 C32 1 0.137756 -0.616079 -0.945260 11.00000 0.02280 0.02718 = 0.02409 -0.00047 -0.00100 0.01200 C33 1 0.220607 -0.567276 -0.945232 11.00000 0.02149 0.04358 = 0.03276 -0.00385 -0.00674 0.00269 AFIX 43 H33 2 0.264447 -0.559502 -0.907674 11.00000 -1.20000 AFIX 0 C34 1 0.236216 -0.531004 -1.001545 11.00000 0.02043 0.05013 = 0.04115 0.00441 0.00026 -0.00560 AFIX 43 H34 2 0.292657 -0.498244 -1.002462 11.00000 -1.20000 AFIX 0 C35 1 0.172492 -0.540553 -1.057036 11.00000 0.02576 0.04414 = 0.03245 0.00274 0.00386 -0.00693 AFIX 43 H35 2 0.185701 -0.513603 -1.094273 11.00000 -1.20000 AFIX 0 C36 1 -0.066916 -0.753062 -0.925409 11.00000 0.05113 0.02436 = 0.03220 0.00890 -0.00211 0.00345 AFIX 43 H36 2 -0.071329 -0.774431 -0.884197 11.00000 -1.20000 AFIX 0 C37 1 -0.134036 -0.772192 -0.976023 11.00000 0.03784 0.02688 = 0.04410 0.00015 -0.00879 -0.00481 AFIX 43 H37 2 -0.184405 -0.807752 -0.969287 11.00000 -1.20000 AFIX 0 C38 1 -0.130910 -0.741476 -1.036569 11.00000 0.03372 0.03368 = 0.03411 -0.00336 -0.01140 -0.00040 AFIX 43 H38 2 -0.179331 -0.756588 -1.069768 11.00000 -1.20000 AFIX 0 C39 1 -0.140533 -0.667108 -1.183935 11.00000 0.03347 0.03333 = 0.02983 0.00854 -0.00047 0.00688 C40 1 -0.251895 -0.664847 -1.169256 11.00000 0.04285 0.03249 = 0.02762 0.00853 0.00274 0.00062 AFIX 43 H40 2 -0.275924 -0.638215 -1.133735 11.00000 -1.20000 AFIX 0 C41 1 -0.330634 -0.700938 -1.205519 11.00000 0.03557 0.04549 = 0.05075 0.02751 -0.00731 -0.01060 AFIX 43 H41 2 -0.406418 -0.698165 -1.194438 11.00000 -1.20000 AFIX 0 C42 1 -0.297653 -0.739987 -1.256731 11.00000 0.06935 0.05223 = 0.03662 -0.00475 -0.01740 -0.01533 AFIX 43 H42 2 -0.350333 -0.764676 -1.280967 11.00000 -1.20000 AFIX 0 C43 1 -0.187616 -0.743232 -1.272871 11.00000 0.05484 0.06794 = 0.04315 -0.02634 -0.00253 -0.00508 AFIX 43 H43 2 -0.163705 -0.770000 -1.308324 11.00000 -1.20000 AFIX 0 C44 1 -0.111769 -0.706568 -1.236316 11.00000 0.03672 0.06604 = 0.03657 -0.01383 -0.00075 0.00288 AFIX 43 H44 2 -0.036282 -0.708935 -1.248169 11.00000 -1.20000 AFIX 0 C45 1 0.007958 -0.553758 -1.193841 11.00000 0.01849 0.04421 = 0.03740 -0.00107 -0.01113 0.00687 C46 1 0.045451 -0.565446 -1.256625 11.00000 0.02503 0.06274 = 0.03458 0.00327 0.00450 0.00831 AFIX 43 H46 2 0.050913 -0.610146 -1.271549 11.00000 -1.20000 AFIX 0 C47 1 0.075336 -0.514047 -1.298512 11.00000 0.03986 0.07855 = 0.03690 0.00959 0.01049 0.00783 AFIX 43 H47 2 0.102106 -0.524453 -1.340784 11.00000 -1.20000 AFIX 0 C48 1 0.066960 -0.449569 -1.280133 11.00000 0.02563 0.06433 = 0.05623 0.03262 0.00044 -0.00147 AFIX 43 H48 2 0.085328 -0.414837 -1.309650 11.00000 -1.20000 AFIX 0 C49 1 0.031699 -0.434943 -1.218488 11.00000 0.03933 0.04442 = 0.05308 0.00423 -0.00733 -0.00265 AFIX 43 H49 2 0.027066 -0.389830 -1.204697 11.00000 -1.20000 AFIX 0 C50 1 0.002426 -0.486262 -1.175675 11.00000 0.02981 0.05106 = 0.03301 0.00705 -0.00631 0.00055 AFIX 43 H50 2 -0.021913 -0.475159 -1.133058 11.00000 -1.20000 AFIX 0 C51 1 -0.716549 -0.344785 -1.059523 11.00000 0.19560 0.07666 = 0.05933 0.00662 0.00956 -0.00176 AFIX 137 H51A 2 -0.745524 -0.299202 -1.058903 11.00000 -1.50000 H51B 2 -0.774227 -0.375875 -1.045716 11.00000 -1.50000 H51C 2 -0.692656 -0.356034 -1.103773 11.00000 -1.50000 AFIX 0 C52 1 -0.614137 -0.350081 -1.010861 11.00000 0.19422 0.03778 = 0.11010 -0.00351 0.03349 -0.00785 C53 1 -0.527417 -0.391642 -1.019257 11.00000 0.20281 0.11067 = 0.09040 0.00787 0.03274 -0.03496 AFIX 43 H53 2 -0.525849 -0.420358 -1.056040 11.00000 -1.20000 AFIX 0 C54 1 -0.435838 -0.393192 -0.972663 11.00000 0.18649 0.23496 = 0.08291 -0.01301 -0.02948 -0.06898 AFIX 43 H54 2 -0.376324 -0.422579 -0.981396 11.00000 -1.20000 AFIX 0 C55 1 -0.430871 -0.357499 -0.920953 11.00000 0.09634 0.22626 = 0.12953 0.05955 -0.03384 -0.00889 AFIX 43 H55 2 -0.372206 -0.360530 -0.890500 11.00000 -1.20000 AFIX 0 C56 1 -0.514538 -0.316155 -0.913786 11.00000 0.12437 0.23266 = 0.10842 0.06278 -0.05476 -0.01527 AFIX 43 H56 2 -0.515085 -0.287303 -0.877095 11.00000 -1.20000 AFIX 0 C57 1 -0.604259 -0.312771 -0.958606 11.00000 0.12610 0.18994 = 0.12339 0.04845 0.02849 -0.00984 AFIX 43 H57 2 -0.660840 -0.281289 -0.950017 11.00000 -1.20000 AFIX 0 HKLF 4 REM 5toluene in P2(1)2(1)2(1) REM R1 = 0.0353 for 7254 Fo > 4sig(Fo) and 0.0540 for all 8805 data REM 577 parameters refined using 0 restraints END WGHT 0.0109 0.0000 REM Highest difference peak 0.814, deepest hole -0.408, 1-sigma level 0.089 Q1 1 -0.0417 -0.6775 -1.1269 11.00000 0.05 0.81 Q2 1 0.0203 -0.6668 -1.1279 11.00000 0.05 0.64 Q3 1 -0.0204 -0.6465 -0.8681 11.00000 0.05 0.53 Q4 1 -0.0031 -0.5661 -1.1266 11.00000 0.05 0.52 Q5 1 -0.0721 -0.5779 -1.1287 11.00000 0.05 0.51 ; _vrf_PLAT220_5 ; RESPONSE: The isopropyl carbons have a large range of thermal motions, while the metal-bound carbons have a much smaller range of thermal motions. Consequently, it is reasonable to have a large Ueq(max)/Ueq(min) ratio for carbons. ; _database_code_depnum_ccdc_archive 'CCDC 953916' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_PtLHPh2 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H18 N2 Pt' _chemical_formula_weight 517.48 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.7555(4) _cell_length_b 16.3786(9) _cell_length_c 16.1010(8) _cell_angle_alpha 90 _cell_angle_beta 98.714(3) _cell_angle_gamma 90 _cell_volume 1760.94(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13480 _cell_measurement_theta_min 3.295 _cell_measurement_theta_max 24.994 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.952 _exptl_crystal_F_000 992 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 7.976 _shelx_estimated_absorpt_T_min 0.240 _shelx_estimated_absorpt_T_max 0.796 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.5309 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'Bruker Apex 2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker Kappa Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13480 _diffrn_reflns_av_unetI/netI 0.0311 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.295 _diffrn_reflns_theta_max 24.994 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.966 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.966 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.966 _reflns_number_total 3082 _reflns_number_gt 2673 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker Apex 2 software package' _computing_cell_refinement 'Bruker Apex 2 software package' _computing_data_reduction 'Bruker Apex 2 software package' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'ORTEP and POV-Ray' _computing_publication_material 'SHELXL-2013 (Sheldrick, 2013)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+0.1906P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3082 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0200 _refine_ls_wR_factor_ref 0.0441 _refine_ls_wR_factor_gt 0.0420 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.20874(2) 0.65361(2) 0.88094(2) 0.01830(6) Uani 1 1 d . . . . . N1 N 0.2927(4) 0.64486(18) 1.01547(19) 0.0201(7) Uani 1 1 d . . . . . N2 N 0.1802(4) 0.52271(19) 0.89418(18) 0.0181(7) Uani 1 1 d . . . . . C1 C 0.3395(5) 0.6966(3) 1.0805(2) 0.0235(9) Uani 1 1 d . . . . . H1 H 0.3426 0.7536 1.0699 0.028 Uiso 1 1 calc R U . . . C2 C 0.3835(6) 0.6687(3) 1.1629(3) 0.0294(10) Uani 1 1 d . . . . . H2 H 0.4134 0.7071 1.2073 0.035 Uiso 1 1 calc R U . . . C3 C 0.3845(6) 0.5853(3) 1.1818(2) 0.0299(10) Uani 1 1 d . . . . . H3 H 0.4188 0.5665 1.2379 0.036 Uiso 1 1 calc R U . . . C4 C 0.3340(5) 0.5311(3) 1.1160(2) 0.0224(9) Uani 1 1 d . . . . . C5 C 0.2915(5) 0.5662(2) 1.0367(2) 0.0171(8) Uani 1 1 d . . . . . C6 C 0.2346(5) 0.5042(2) 0.9753(2) 0.0182(8) Uani 1 1 d . . . . . C7 C 0.2412(5) 0.4282(2) 1.0131(2) 0.0214(9) Uani 1 1 d . . . . . C8 C 0.1832(5) 0.3629(2) 0.9598(3) 0.0254(9) Uani 1 1 d . . . . . H8 H 0.1809 0.3088 0.9810 0.030 Uiso 1 1 calc R U . . . C9 C 0.1288(6) 0.3790(3) 0.8750(3) 0.0257(9) Uani 1 1 d . . . . . H9 H 0.0909 0.3351 0.8375 0.031 Uiso 1 1 calc R U . . . C10 C 0.1283(5) 0.4581(2) 0.8435(2) 0.0226(9) Uani 1 1 d . . . . . H10 H 0.0906 0.4669 0.7849 0.027 Uiso 1 1 calc R U . . . C11 C 0.3089(5) 0.4395(3) 1.1062(2) 0.0260(9) Uani 1 1 d . . . . . H11A H 0.4372 0.4108 1.1246 0.031 Uiso 1 1 calc R U . . . H11B H 0.2070 0.4188 1.1392 0.031 Uiso 1 1 calc R U . . . C12 C 0.2545(6) 0.7740(2) 0.8807(2) 0.0227(9) Uani 1 1 d . . . . . C13 C 0.4464(6) 0.8054(3) 0.9026(2) 0.0294(10) Uani 1 1 d . . . . . H13 H 0.5563 0.7686 0.9113 0.035 Uiso 1 1 calc R U . . . C14 C 0.4840(7) 0.8892(3) 0.9124(2) 0.0353(11) Uani 1 1 d . . . . . H14 H 0.6176 0.9082 0.9273 0.042 Uiso 1 1 calc R U . . . C15 C 0.3293(7) 0.9440(3) 0.9007(2) 0.0347(11) Uani 1 1 d . . . . . H15 H 0.3535 1.0008 0.9084 0.042 Uiso 1 1 calc R U . . . C16 C 0.1362(7) 0.9146(3) 0.8773(2) 0.0331(11) Uani 1 1 d . . . . . H16 H 0.0275 0.9520 0.8683 0.040 Uiso 1 1 calc R U . . . C17 C 0.0990(6) 0.8315(2) 0.8670(2) 0.0269(10) Uani 1 1 d . . . . . H17 H -0.0346 0.8132 0.8502 0.032 Uiso 1 1 calc R U . . . C18 C 0.1222(6) 0.6495(2) 0.7572(2) 0.0229(9) Uani 1 1 d . . . . . C19 C -0.0711(6) 0.6718(2) 0.7203(3) 0.0267(9) Uani 1 1 d . . . . . H19 H -0.1588 0.6957 0.7543 0.032 Uiso 1 1 calc R U . . . C20 C -0.1382(7) 0.6598(3) 0.6354(3) 0.0326(10) Uani 1 1 d . . . . . H20 H -0.2723 0.6736 0.6129 0.039 Uiso 1 1 calc R U . . . C21 C -0.0131(7) 0.6281(3) 0.5830(3) 0.0352(11) Uani 1 1 d . . . . . H21 H -0.0581 0.6216 0.5246 0.042 Uiso 1 1 calc R U . . . C22 C 0.1782(7) 0.6062(3) 0.6176(2) 0.0314(10) Uani 1 1 d . . . . . H22 H 0.2657 0.5838 0.5825 0.038 Uiso 1 1 calc R U . . . C23 C 0.2455(6) 0.6161(3) 0.7022(2) 0.0268(9) Uani 1 1 d . . . . . H23 H 0.3782 0.6001 0.7242 0.032 Uiso 1 1 calc R U . . . 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 0.02095(9) 0.01616(9) 0.01766(9) 0.00141(7) 0.00250(6) 0.00277(7) N1 0.0166(16) 0.0204(19) 0.0236(17) 0.0024(14) 0.0044(13) 0.0059(14) N2 0.0145(15) 0.0193(19) 0.0215(17) -0.0008(14) 0.0061(13) 0.0013(13) C1 0.023(2) 0.027(2) 0.021(2) -0.0045(18) 0.0037(17) 0.0018(18) C2 0.023(2) 0.037(3) 0.028(2) -0.010(2) 0.0067(18) 0.0018(19) C3 0.022(2) 0.048(3) 0.019(2) 0.006(2) 0.0019(17) 0.006(2) C4 0.0133(18) 0.030(2) 0.024(2) 0.0043(19) 0.0036(16) 0.0053(17) C5 0.0134(18) 0.020(2) 0.0189(19) 0.0027(16) 0.0056(15) 0.0039(16) C6 0.0105(17) 0.020(2) 0.025(2) 0.0007(17) 0.0049(15) 0.0035(16) C7 0.0126(18) 0.021(2) 0.032(2) 0.0070(18) 0.0072(16) 0.0052(16) C8 0.017(2) 0.018(2) 0.042(3) 0.0062(19) 0.0066(18) 0.0026(17) C9 0.0187(19) 0.020(2) 0.040(3) -0.0034(19) 0.0088(18) 0.0017(18) C10 0.0215(19) 0.025(2) 0.022(2) -0.0027(18) 0.0053(16) 0.0039(18) C11 0.020(2) 0.032(3) 0.026(2) 0.0106(18) 0.0056(17) 0.0067(18) C12 0.035(2) 0.021(2) 0.0133(19) 0.0023(16) 0.0073(18) 0.0032(18) C13 0.032(2) 0.025(2) 0.029(2) 0.0086(19) -0.0016(19) 0.002(2) C14 0.044(3) 0.030(3) 0.029(2) 0.005(2) -0.005(2) -0.007(2) C15 0.066(3) 0.018(2) 0.020(2) -0.0006(18) 0.003(2) -0.002(2) C16 0.051(3) 0.027(3) 0.022(2) 0.0024(18) 0.007(2) 0.015(2) C17 0.034(2) 0.018(2) 0.028(2) 0.0010(17) 0.0016(18) 0.0093(18) C18 0.031(2) 0.013(2) 0.024(2) 0.0037(17) 0.0037(17) -0.0036(18) C19 0.030(2) 0.019(2) 0.031(2) 0.0042(18) 0.0028(19) -0.0032(17) C20 0.036(2) 0.025(3) 0.032(2) 0.004(2) -0.013(2) -0.007(2) C21 0.061(3) 0.023(2) 0.019(2) 0.0013(18) -0.002(2) -0.019(2) C22 0.052(3) 0.021(2) 0.022(2) 0.0026(18) 0.011(2) -0.010(2) C23 0.031(2) 0.023(2) 0.026(2) 0.0045(18) 0.0041(18) -0.0030(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 C18 1.990(4) . ? Pt1 C12 1.996(4) . ? Pt1 N1 2.159(3) . ? Pt1 N2 2.166(3) . ? N1 C5 1.334(4) . ? N1 C1 1.347(5) . ? N2 C6 1.337(4) . ? N2 C10 1.349(5) . ? C1 C2 1.392(6) . ? C2 C3 1.400(6) . ? C3 C4 1.383(5) . ? C4 C5 1.390(5) . ? C4 C11 1.517(6) . ? C5 C6 1.428(5) . ? C6 C7 1.384(5) . ? C7 C8 1.389(5) . ? C7 C11 1.512(5) . ? C8 C9 1.384(5) . ? C9 C10 1.391(5) . ? C12 C13 1.389(5) . ? C12 C17 1.404(5) . ? C13 C14 1.401(6) . ? C14 C15 1.368(6) . ? C15 C16 1.388(6) . ? C16 C17 1.390(6) . ? C18 C19 1.399(6) . ? C18 C23 1.414(5) . ? C19 C20 1.388(5) . ? C20 C21 1.382(6) . ? C21 C22 1.375(6) . ? C22 C23 1.379(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 C18 Pt1 C12 93.08(15) . . ? C18 Pt1 N1 173.99(13) . . ? C12 Pt1 N1 92.86(13) . . ? C18 Pt1 N2 92.76(13) . . ? C12 Pt1 N2 173.77(13) . . ? N1 Pt1 N2 81.33(11) . . ? C5 N1 C1 114.7(3) . . ? C5 N1 Pt1 108.1(2) . . ? C1 N1 Pt1 137.2(3) . . ? C6 N2 C10 114.9(3) . . ? C6 N2 Pt1 107.7(2) . . ? C10 N2 Pt1 137.3(3) . . ? N1 C1 C2 121.8(4) . . ? C1 C2 C3 121.3(4) . . ? C4 C3 C2 117.9(4) . . ? C3 C4 C5 115.5(4) . . ? C3 C4 C11 136.5(4) . . ? C5 C4 C11 108.0(3) . . ? N1 C5 C4 128.8(4) . . ? N1 C5 C6 121.3(3) . . ? C4 C5 C6 109.8(3) . . ? N2 C6 C7 128.2(4) . . ? N2 C6 C5 121.4(3) . . ? C7 C6 C5 110.4(3) . . ? C6 C7 C8 115.7(3) . . ? C6 C7 C11 108.1(3) . . ? C8 C7 C11 136.2(4) . . ? C9 C8 C7 118.0(4) . . ? C8 C9 C10 121.5(4) . . ? N2 C10 C9 121.6(4) . . ? C7 C11 C4 103.7(3) . . ? C13 C12 C17 116.0(4) . . ? C13 C12 Pt1 120.3(3) . . ? C17 C12 Pt1 123.4(3) . . ? C12 C13 C14 122.6(4) . . ? C15 C14 C13 120.3(4) . . ? C14 C15 C16 118.5(4) . . ? C15 C16 C17 121.2(4) . . ? C16 C17 C12 121.4(4) . . ? C19 C18 C23 115.8(4) . . ? C19 C18 Pt1 122.0(3) . . ? C23 C18 Pt1 121.9(3) . . ? C20 C19 C18 121.7(4) . . ? C21 C20 C19 121.0(4) . . ? C22 C21 C20 118.4(4) . . ? C21 C22 C23 121.2(4) . . ? C22 C23 C18 121.8(4) . . ? _refine_diff_density_max 0.638 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.099 _shelxl_version_number 2013-4 _iucr_refine_instructions_details ; TITL Pt(LH)(Ph)2 in P2(1)/c CELL 0.71073 6.7555 16.3786 16.1010 90.000 98.714 90.000 ZERR 4.00 0.0004 0.0009 0.0008 0.000 0.003 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N Pt UNIT 92 72 8 4 L.S. 10 SIZE 0.25 0.25 0.03 ACTA OMIT -3 50 OMIT 0 1 1 BOND FMAP 2 PLAN 5 TEMP -123.150 WGHT 0.019200 0.190600 FVAR 0.07229 PT1 4 0.208737 0.653613 0.880935 11.00000 0.02095 0.01616 = 0.01766 0.00141 0.00250 0.00277 N1 3 0.292670 0.644858 1.015469 11.00000 0.01663 0.02042 = 0.02363 0.00244 0.00436 0.00586 N2 3 0.180169 0.522711 0.894175 11.00000 0.01449 0.01934 = 0.02154 -0.00076 0.00613 0.00127 C1 1 0.339505 0.696570 1.080509 11.00000 0.02306 0.02707 = 0.02057 -0.00449 0.00373 0.00184 AFIX 43 H1 2 0.342602 0.753571 1.069860 11.00000 -1.20000 AFIX 0 C2 1 0.383490 0.668727 1.162911 11.00000 0.02348 0.03722 = 0.02832 -0.01008 0.00667 0.00176 AFIX 43 H2 2 0.413422 0.707131 1.207253 11.00000 -1.20000 AFIX 0 C3 1 0.384518 0.585297 1.181776 11.00000 0.02248 0.04831 = 0.01862 0.00581 0.00189 0.00595 AFIX 43 H3 2 0.418791 0.566464 1.237920 11.00000 -1.20000 AFIX 0 C4 1 0.334030 0.531136 1.116049 11.00000 0.01333 0.03038 = 0.02384 0.00434 0.00365 0.00530 C5 1 0.291463 0.566191 1.036734 11.00000 0.01342 0.01995 = 0.01890 0.00271 0.00560 0.00388 C6 1 0.234584 0.504231 0.975321 11.00000 0.01050 0.01994 = 0.02484 0.00071 0.00488 0.00354 C7 1 0.241154 0.428185 1.013076 11.00000 0.01262 0.02061 = 0.03217 0.00704 0.00722 0.00517 C8 1 0.183182 0.362915 0.959815 11.00000 0.01683 0.01814 = 0.04177 0.00623 0.00657 0.00261 AFIX 43 H8 2 0.180942 0.308825 0.980954 11.00000 -1.20000 AFIX 0 C9 1 0.128774 0.379022 0.875030 11.00000 0.01875 0.02001 = 0.03979 -0.00335 0.00881 0.00168 AFIX 43 H9 2 0.090884 0.335054 0.837494 11.00000 -1.20000 AFIX 0 C10 1 0.128318 0.458143 0.843534 11.00000 0.02153 0.02463 = 0.02216 -0.00270 0.00529 0.00390 AFIX 43 H10 2 0.090576 0.466899 0.784948 11.00000 -1.20000 AFIX 0 C11 1 0.308946 0.439462 1.106247 11.00000 0.02033 0.03224 = 0.02612 0.01059 0.00561 0.00666 AFIX 23 H11A 2 0.437173 0.410841 1.124642 11.00000 -1.20000 H11B 2 0.207042 0.418785 1.139167 11.00000 -1.20000 AFIX 0 C12 1 0.254549 0.773972 0.880745 11.00000 0.03534 0.02056 = 0.01327 0.00225 0.00734 0.00316 C13 1 0.446394 0.805423 0.902615 11.00000 0.03215 0.02474 = 0.02925 0.00859 -0.00159 0.00219 AFIX 43 H13 2 0.556339 0.768649 0.911264 11.00000 -1.20000 AFIX 0 C14 1 0.483973 0.889248 0.912403 11.00000 0.04384 0.02970 = 0.02887 0.00504 -0.00534 -0.00657 AFIX 43 H14 2 0.617570 0.908183 0.927255 11.00000 -1.20000 AFIX 0 C15 1 0.329277 0.943999 0.900685 11.00000 0.06573 0.01773 = 0.01962 -0.00059 0.00334 -0.00188 AFIX 43 H15 2 0.353503 1.000836 0.908354 11.00000 -1.20000 AFIX 0 C16 1 0.136202 0.914619 0.877347 11.00000 0.05133 0.02685 = 0.02155 0.00235 0.00668 0.01479 AFIX 43 H16 2 0.027520 0.951989 0.868297 11.00000 -1.20000 AFIX 0 C17 1 0.098951 0.831488 0.866971 11.00000 0.03412 0.01777 = 0.02782 0.00100 0.00159 0.00928 AFIX 43 H17 2 -0.034590 0.813215 0.850208 11.00000 -1.20000 AFIX 0 C18 1 0.122170 0.649533 0.757217 11.00000 0.03071 0.01350 = 0.02429 0.00367 0.00367 -0.00360 C19 1 -0.071138 0.671786 0.720338 11.00000 0.02990 0.01887 = 0.03091 0.00424 0.00284 -0.00317 AFIX 43 H19 2 -0.158840 0.695747 0.754314 11.00000 -1.20000 AFIX 0 C20 1 -0.138235 0.659784 0.635385 11.00000 0.03609 0.02472 = 0.03151 0.00417 -0.01273 -0.00672 AFIX 43 H20 2 -0.272260 0.673553 0.612881 11.00000 -1.20000 AFIX 0 C21 1 -0.013054 0.628108 0.583029 11.00000 0.06107 0.02265 = 0.01937 0.00132 -0.00175 -0.01857 AFIX 43 H21 2 -0.058106 0.621638 0.524588 11.00000 -1.20000 AFIX 0 C22 1 0.178232 0.606191 0.617581 11.00000 0.05197 0.02143 = 0.02243 0.00261 0.01132 -0.01015 AFIX 43 H22 2 0.265660 0.583820 0.582534 11.00000 -1.20000 AFIX 0 C23 1 0.245450 0.616111 0.702236 11.00000 0.03088 0.02348 = 0.02590 0.00448 0.00406 -0.00296 AFIX 43 H23 2 0.378203 0.600050 0.724210 11.00000 -1.20000 AFIX 0 HKLF 4 REM Pt(LH)(Ph)2 in P2(1)/c REM R1 = 0.0200 for 2673 Fo > 4sig(Fo) and 0.0265 for all 3082 data REM 235 parameters refined using 0 restraints END WGHT 0.0191 0.1902 REM Highest difference peak 0.638, deepest hole -0.363, 1-sigma level 0.099 Q1 1 0.0559 0.6491 0.8782 11.00000 0.05 0.64 Q2 1 0.2757 0.7079 0.9203 11.00000 0.05 0.49 Q3 1 0.1477 0.6976 0.8440 11.00000 0.05 0.46 Q4 1 0.1130 0.6209 0.8617 11.00000 0.05 0.46 Q5 1 0.3605 0.6520 0.8800 11.00000 0.05 0.45 ; _database_code_depnum_ccdc_archive 'CCDC 953917'