# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_IPrCdI2 _database_code_depnum_ccdc_archive 'CCDC 905516' #TrackingRef 'IPrCdI2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C85.50 H108 Cd2 I4 N4' _chemical_formula_weight 1924.16 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.253(3) _cell_length_b 19.437(4) _cell_length_c 15.846(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.39(3) _cell_angle_gamma 90.00 _cell_volume 4507.0(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1914 _exptl_absorpt_coefficient_mu 1.882 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_T_max 0.879 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18865 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9829 _reflns_number_gt 6521 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One fully ordered and occupied molecule of bezene, one fully ordered and 25% site occupied molecule of bezene, and one molecule of benzene disorded over two sites were located in the asymmetric unit. The carbon atoms of the first were refined anisotropically, while those of the other two were refined isotropically. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+5.1017P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9829 _refine_ls_number_parameters 449 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0853 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1489 _refine_ls_wR_factor_gt 0.1284 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.35585(3) 0.504460(19) -0.04736(3) 0.04701(13) Uani 1 1 d . . . I2 I 0.48120(4) 0.39695(2) 0.21136(3) 0.06669(17) Uani 1 1 d . . . Cd1 Cd 0.49293(3) 0.513060(19) 0.11777(3) 0.04070(13) Uani 1 1 d . . . N1 N 0.4199(3) 0.6459(2) 0.2022(3) 0.0359(10) Uani 1 1 d . . . N2 N 0.5667(3) 0.6447(2) 0.2449(3) 0.0367(10) Uani 1 1 d . . . C1 C 0.4934(4) 0.6112(2) 0.1930(3) 0.0336(11) Uani 1 1 d . . . C2 C 0.4475(5) 0.7009(3) 0.2589(3) 0.0442(14) Uani 1 1 d . . . H2 H 0.4088 0.7333 0.2756 0.053 Uiso 1 1 calc R . . C3 C 0.5393(4) 0.6998(3) 0.2857(4) 0.0441(14) Uani 1 1 d . . . H3 H 0.5780 0.7310 0.3254 0.053 Uiso 1 1 calc R . . C4 C 0.3278(4) 0.6340(3) 0.1511(4) 0.0424(13) Uani 1 1 d . . . C5 C 0.2735(5) 0.5876(3) 0.1815(4) 0.0557(16) Uani 1 1 d . . . C6 C 0.1841(5) 0.5790(4) 0.1288(6) 0.074(2) Uani 1 1 d . . . H6 H 0.1445 0.5482 0.1468 0.089 Uiso 1 1 calc R . . C7 C 0.1527(6) 0.6144(5) 0.0515(6) 0.084(3) Uani 1 1 d . . . H7 H 0.0912 0.6080 0.0173 0.101 Uiso 1 1 calc R . . C8 C 0.2077(5) 0.6589(4) 0.0218(5) 0.0678(19) Uani 1 1 d . . . H8 H 0.1843 0.6816 -0.0329 0.081 Uiso 1 1 calc R . . C9 C 0.2967(5) 0.6706(3) 0.0711(4) 0.0536(16) Uani 1 1 d . . . C10 C 0.3100(5) 0.5512(3) 0.2689(4) 0.0635(18) Uani 1 1 d . . . H10 H 0.3769 0.5434 0.2783 0.076 Uiso 1 1 calc R . . C11 C 0.2652(7) 0.4813(4) 0.2720(6) 0.090(3) Uani 1 1 d . . . H11A H 0.1996 0.4875 0.2634 0.136 Uiso 1 1 calc R . . H11B H 0.2926 0.4597 0.3293 0.136 Uiso 1 1 calc R . . H11C H 0.2749 0.4517 0.2253 0.136 Uiso 1 1 calc R . . C12 C 0.2986(9) 0.5959(4) 0.3447(6) 0.113(4) Uani 1 1 d . . . H12A H 0.3426 0.6339 0.3548 0.169 Uiso 1 1 calc R . . H12B H 0.3098 0.5679 0.3981 0.169 Uiso 1 1 calc R . . H12C H 0.2364 0.6144 0.3296 0.169 Uiso 1 1 calc R . . C13 C 0.3578(6) 0.7207(3) 0.0402(4) 0.0671(19) Uani 1 1 d . . . H13 H 0.4222 0.7117 0.0759 0.081 Uiso 1 1 calc R . . C14 C 0.3544(6) 0.7125(4) -0.0558(5) 0.080(2) Uani 1 1 d . . . H14A H 0.2911 0.7174 -0.0924 0.120 Uiso 1 1 calc R . . H14B H 0.3774 0.6669 -0.0651 0.120 Uiso 1 1 calc R . . H14C H 0.3924 0.7480 -0.0720 0.120 Uiso 1 1 calc R . . C15 C 0.3357(9) 0.7940(4) 0.0570(6) 0.118(4) Uani 1 1 d . . . H15A H 0.2706 0.8027 0.0292 0.177 Uiso 1 1 calc R . . H15B H 0.3724 0.8253 0.0322 0.177 Uiso 1 1 calc R . . H15C H 0.3496 0.8018 0.1205 0.177 Uiso 1 1 calc R . . C16 C 0.6611(4) 0.6305(3) 0.2499(4) 0.0480(14) Uani 1 1 d . . . C17 C 0.7084(5) 0.5793(3) 0.3104(4) 0.0583(17) Uani 1 1 d . . . C18 C 0.7971(6) 0.5663(5) 0.3118(6) 0.082(2) Uani 1 1 d . . . H18 H 0.8302 0.5310 0.3486 0.098 Uiso 1 1 calc R . . C19 C 0.8387(6) 0.6042(5) 0.2603(7) 0.091(3) Uani 1 1 d . . . H19 H 0.9008 0.5950 0.2635 0.109 Uiso 1 1 calc R . . C20 C 0.7941(5) 0.6536(4) 0.2058(5) 0.074(2) Uani 1 1 d . . . H20 H 0.8257 0.6783 0.1716 0.089 Uiso 1 1 calc R . . C21 C 0.7020(5) 0.6701(3) 0.1974(4) 0.0608(18) Uani 1 1 d . . . C22 C 0.6619(6) 0.5415(3) 0.3692(4) 0.070(2) Uani 1 1 d . . . H22 H 0.5949 0.5394 0.3387 0.084 Uiso 1 1 calc R . . C23 C 0.6968(7) 0.4683(4) 0.3904(7) 0.115(4) Uani 1 1 d . . . H23A H 0.7048 0.4466 0.3372 0.173 Uiso 1 1 calc R . . H23B H 0.6526 0.4419 0.4116 0.173 Uiso 1 1 calc R . . H23C H 0.7556 0.4694 0.4360 0.173 Uiso 1 1 calc R . . C24 C 0.6756(8) 0.5834(4) 0.4542(5) 0.110(4) Uani 1 1 d . . . H24A H 0.7406 0.5838 0.4868 0.166 Uiso 1 1 calc R . . H24B H 0.6405 0.5624 0.4906 0.166 Uiso 1 1 calc R . . H24C H 0.6546 0.6307 0.4394 0.166 Uiso 1 1 calc R . . C25 C 0.6517(5) 0.7268(3) 0.1377(5) 0.0623(18) Uani 1 1 d U . . H25 H 0.5964 0.7390 0.1567 0.075 Uiso 1 1 calc R . . C26 C 0.6198(6) 0.7026(4) 0.0435(5) 0.083(2) Uani 1 1 d . . . H26A H 0.6729 0.6922 0.0225 0.124 Uiso 1 1 calc R . . H26B H 0.5833 0.7389 0.0069 0.124 Uiso 1 1 calc R . . H26C H 0.5825 0.6611 0.0399 0.124 Uiso 1 1 calc R . . C27 C 0.7098(8) 0.7919(4) 0.1437(7) 0.121(4) Uani 1 1 d . . . H27A H 0.7450 0.7996 0.2050 0.182 Uiso 1 1 calc R . . H27B H 0.6699 0.8314 0.1225 0.182 Uiso 1 1 calc R . . H27C H 0.7518 0.7862 0.1074 0.182 Uiso 1 1 calc R . . C28 C 0.8818(6) 0.6324(5) 0.0125(5) 0.080(2) Uani 1 1 d D . . C29 C 0.8058(7) 0.6270(7) -0.0550(7) 0.117(4) Uani 1 1 d D . . H29 H 0.7730 0.5851 -0.0703 0.140 Uiso 1 1 calc R . . C30 C 0.7807(9) 0.6847(7) -0.0978(9) 0.132(4) Uani 1 1 d D . . H30 H 0.7287 0.6820 -0.1478 0.158 Uiso 1 1 calc R . . C31 C 0.8182(8) 0.7456(6) -0.0805(8) 0.108(3) Uani 1 1 d D . . H31 H 0.7926 0.7840 -0.1162 0.129 Uiso 1 1 calc R . . C32 C 0.9008(10) 0.7544(7) -0.0047(10) 0.170(7) Uani 1 1 d D . . H32 H 0.9303 0.7975 0.0111 0.204 Uiso 1 1 calc R . . C33 C 0.9335(6) 0.6890(5) 0.0447(6) 0.089(3) Uani 1 1 d D . . H33 H 0.9858 0.6872 0.0943 0.107 Uiso 1 1 calc R . . C34 C 0.9079(9) 0.5656(6) 0.0566(9) 0.142(4) Uani 1 1 d DU . . H34A H 0.8642 0.5532 0.0891 0.213 Uiso 1 1 calc R . . H34B H 0.9693 0.5691 0.0976 0.213 Uiso 1 1 calc R . . H34C H 0.9075 0.5302 0.0125 0.213 Uiso 1 1 calc R . . C35 C 0.1314(9) 0.6829(6) -0.2485(10) 0.070(4) Uiso 0.50 1 d PD A 1 C36 C 0.0778(15) 0.7362(6) -0.227(2) 0.138(9) Uiso 0.50 1 d PD A 1 H36 H 0.0915 0.7830 -0.2356 0.165 Uiso 0.50 1 calc PR A 1 C37 C 0.002(2) 0.7187(8) -0.194(3) 0.175(14) Uiso 0.50 1 d PD A 1 H37 H -0.0345 0.7538 -0.1785 0.209 Uiso 0.50 1 calc PR A 1 C38 C -0.0173(11) 0.6477(9) -0.1830(14) 0.112(7) Uiso 0.50 1 d PD A 1 H38 H -0.0723 0.6353 -0.1700 0.135 Uiso 0.50 1 calc PR A 1 C39 C 0.0451(13) 0.5948(7) -0.1918(15) 0.122(8) Uiso 0.50 1 d PD A 1 H39 H 0.0377 0.5491 -0.1739 0.147 Uiso 0.50 1 calc PR A 1 C40 C 0.120(3) 0.6119(7) -0.228(4) 0.185(19) Uiso 0.50 1 d PD A 1 H40 H 0.1597 0.5773 -0.2385 0.222 Uiso 0.50 1 calc PR A 1 C41 C 0.2086(15) 0.7024(10) -0.285(2) 0.163(11) Uiso 0.50 1 d PD A 1 H41A H 0.2078 0.7523 -0.2946 0.244 Uiso 0.50 1 calc PR A 1 H41B H 0.2016 0.6786 -0.3411 0.244 Uiso 0.50 1 calc PR A 1 H41C H 0.2668 0.6892 -0.2434 0.244 Uiso 0.50 1 calc PR A 1 C42 C 0.0423(10) 0.6507(6) -0.2105(12) 0.089(5) Uiso 0.50 1 d PD B 2 C43 C 0.1210(14) 0.6271(6) -0.233(2) 0.095(8) Uiso 0.50 1 d PD B 2 H43 H 0.1372 0.5798 -0.2270 0.114 Uiso 0.50 1 calc PR B 2 C44 C 0.1763(15) 0.6763(8) -0.264(2) 0.160(11) Uiso 0.50 1 d PD B 2 H44 H 0.2259 0.6611 -0.2840 0.193 Uiso 0.50 1 calc PR B 2 C45 C 0.1551(11) 0.7479(7) -0.2631(11) 0.089(5) Uiso 0.50 1 d PD B 2 H45 H 0.1915 0.7803 -0.2829 0.107 Uiso 0.50 1 calc PR B 2 C46 C 0.0804(17) 0.7716(6) -0.233(2) 0.158(10) Uiso 0.50 1 d PD B 2 H46 H 0.0676 0.8195 -0.2329 0.190 Uiso 0.50 1 calc PR B 2 C47 C 0.0242(17) 0.7221(7) -0.204(2) 0.123(9) Uiso 0.50 1 d PD B 2 H47 H -0.0240 0.7369 -0.1815 0.148 Uiso 0.50 1 calc PR B 2 C48 C -0.0207(15) 0.5993(9) -0.188(2) 0.154(10) Uiso 0.50 1 d PD B 2 H48A H -0.0842 0.6136 -0.2141 0.231 Uiso 0.50 1 calc PR B 2 H48B H -0.0083 0.5968 -0.1237 0.231 Uiso 0.50 1 calc PR B 2 H48C H -0.0108 0.5540 -0.2107 0.231 Uiso 0.50 1 calc PR B 2 C49 C 1.0544(11) 0.9260(7) -0.0192(11) 0.072(8) Uiso 0.25 1 d PD C -1 C50 C 1.0092(10) 0.9359(6) 0.0468(9) 0.026(4) Uiso 0.25 1 d PD C -1 H50 H 1.0067 0.8993 0.0858 0.031 Uiso 0.25 1 calc PR C -1 C51 C 0.9674(11) 1.0004(8) 0.0554(9) 0.057(6) Uiso 0.25 1 d PD C -1 H51 H 0.9372 1.0069 0.0996 0.068 Uiso 0.25 1 calc PR C -1 C52 C 0.9718(11) 1.0554(6) -0.0043(11) 0.052(6) Uiso 0.25 1 d PD C -1 H52 H 0.9443 1.0986 0.0003 0.062 Uiso 0.25 1 calc PR C -1 C53 C 1.0172(12) 1.0449(7) -0.0701(10) 0.044(5) Uiso 0.25 1 d PD C -1 H53 H 1.0199 1.0814 -0.1092 0.053 Uiso 0.25 1 calc PR C -1 C54 C 1.0593(12) 0.9800(9) -0.0787(10) 0.061(7) Uiso 0.25 1 d PD C -1 H54 H 1.0896 0.9733 -0.1228 0.073 Uiso 0.25 1 calc PR C -1 C55 C 1.0975(18) 0.8585(9) -0.0268(19) 0.31(5) Uiso 0.25 1 d PD C -1 H55A H 1.1330 0.8430 0.0317 0.469 Uiso 0.25 1 calc PR C -1 H55B H 1.1380 0.8634 -0.0647 0.469 Uiso 0.25 1 calc PR C -1 H55C H 1.0499 0.8246 -0.0524 0.469 Uiso 0.25 1 calc PR C -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0459(2) 0.0469(2) 0.0458(2) -0.01125(16) 0.00901(17) 0.00316(16) I2 0.0992(4) 0.0324(2) 0.0663(3) 0.00807(18) 0.0197(3) -0.0034(2) Cd1 0.0551(3) 0.0273(2) 0.0393(2) -0.00543(15) 0.01273(19) 0.00160(17) N1 0.051(3) 0.027(2) 0.028(2) -0.0036(17) 0.008(2) 0.0039(19) N2 0.046(3) 0.031(2) 0.031(2) -0.0014(18) 0.007(2) 0.0038(19) C1 0.041(3) 0.025(2) 0.030(3) 0.0035(19) 0.002(2) 0.003(2) C2 0.071(4) 0.029(3) 0.034(3) -0.005(2) 0.016(3) 0.002(3) C3 0.062(4) 0.032(3) 0.037(3) -0.009(2) 0.013(3) 0.002(3) C4 0.049(3) 0.038(3) 0.039(3) -0.013(2) 0.012(3) 0.007(2) C5 0.064(4) 0.052(4) 0.057(4) -0.017(3) 0.028(4) -0.003(3) C6 0.049(4) 0.098(6) 0.076(5) -0.023(5) 0.020(4) -0.011(4) C7 0.060(5) 0.101(7) 0.085(6) -0.036(5) 0.008(5) 0.008(5) C8 0.059(5) 0.075(5) 0.060(4) -0.014(4) 0.002(4) 0.016(4) C9 0.069(4) 0.043(3) 0.045(3) -0.005(3) 0.009(3) 0.014(3) C10 0.086(5) 0.052(4) 0.060(4) -0.007(3) 0.032(4) -0.019(3) C11 0.129(8) 0.060(5) 0.102(7) -0.007(4) 0.064(6) -0.018(5) C12 0.225(13) 0.061(5) 0.073(6) -0.010(4) 0.077(7) -0.024(6) C13 0.096(6) 0.047(4) 0.047(4) 0.006(3) 0.001(4) 0.002(4) C14 0.124(7) 0.053(4) 0.062(5) 0.001(3) 0.027(5) 0.011(4) C15 0.211(12) 0.053(5) 0.085(6) -0.012(4) 0.035(7) -0.001(6) C16 0.056(4) 0.040(3) 0.042(3) -0.017(2) 0.003(3) -0.001(3) C17 0.067(4) 0.043(3) 0.052(4) -0.011(3) -0.006(3) 0.010(3) C18 0.057(5) 0.084(6) 0.083(6) -0.017(5) -0.015(4) 0.021(4) C19 0.049(5) 0.095(7) 0.114(8) -0.041(6) 0.000(5) 0.014(5) C20 0.058(5) 0.084(6) 0.085(6) -0.027(4) 0.029(4) -0.019(4) C21 0.083(5) 0.046(4) 0.059(4) -0.015(3) 0.030(4) -0.014(3) C22 0.095(6) 0.048(4) 0.051(4) 0.009(3) -0.006(4) 0.009(4) C23 0.134(9) 0.055(5) 0.123(8) 0.017(5) -0.017(7) 0.013(5) C24 0.199(11) 0.070(5) 0.062(5) 0.007(4) 0.037(6) -0.002(6) C25 0.076(4) 0.058(4) 0.062(4) 0.004(3) 0.034(3) -0.003(3) C26 0.114(7) 0.058(5) 0.069(5) -0.009(4) 0.015(5) 0.010(4) C27 0.184(11) 0.065(5) 0.103(7) -0.004(5) 0.021(7) -0.045(6) C28 0.059(5) 0.112(7) 0.072(5) -0.014(5) 0.020(4) 0.008(5) C29 0.095(8) 0.166(12) 0.100(8) -0.013(8) 0.044(7) 0.000(7) C30 0.158(12) 0.124(10) 0.148(11) 0.025(9) 0.099(10) 0.014(9) C31 0.107(8) 0.095(8) 0.129(9) 0.045(7) 0.046(7) 0.028(6) C32 0.175(14) 0.160(14) 0.241(19) -0.021(12) 0.166(15) -0.016(11) C33 0.091(7) 0.086(6) 0.095(7) -0.005(5) 0.035(5) -0.005(5) C34 0.136(7) 0.135(7) 0.167(7) 0.000(6) 0.060(6) 0.000(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 I1 Cd1 2.8518(9) 3_665 ? I1 Cd1 2.8565(12) . ? I2 Cd1 2.7339(7) . ? Cd1 C1 2.249(5) . ? Cd1 I1 2.8518(8) 3_665 ? N1 C1 1.349(6) . ? N1 C2 1.385(6) . ? N1 C4 1.429(7) . ? N2 C1 1.353(6) . ? N2 C3 1.374(6) . ? N2 C16 1.445(7) . ? C2 C3 1.345(8) . ? C4 C5 1.399(9) . ? C4 C9 1.413(8) . ? C5 C6 1.393(10) . ? C5 C10 1.514(10) . ? C6 C7 1.368(12) . ? C7 C8 1.377(11) . ? C8 C9 1.380(9) . ? C9 C13 1.522(10) . ? C10 C11 1.528(9) . ? C10 C12 1.531(9) . ? C13 C15 1.505(10) . ? C13 C14 1.517(9) . ? C16 C21 1.404(9) . ? C16 C17 1.428(9) . ? C17 C18 1.370(10) . ? C17 C22 1.511(10) . ? C18 C19 1.380(13) . ? C19 C20 1.341(12) . ? C20 C21 1.411(10) . ? C21 C25 1.512(10) . ? C22 C23 1.523(10) . ? C22 C24 1.537(10) . ? C25 C26 1.509(10) . ? C25 C27 1.532(10) . ? C28 C29 1.341(11) . ? C28 C33 1.366(10) . ? C28 C34 1.475(12) . ? C29 C30 1.311(12) . ? C30 C31 1.311(13) . ? C31 C32 1.485(14) . ? C32 C33 1.502(14) . ? C35 C36 1.417(6) . ? C35 C40 1.437(6) . ? C35 C41 1.501(6) . ? C36 C37 1.448(6) . ? C37 C38 1.432(6) . ? C38 C39 1.433(6) . ? C39 C40 1.455(6) . ? C42 C43 1.417(6) . ? C42 C47 1.424(6) . ? C42 C48 1.498(6) . ? C43 C44 1.451(6) . ? C44 C45 1.429(6) . ? C45 C46 1.426(6) . ? C46 C47 1.449(6) . ? C49 C50 1.419(6) . ? C49 C54 1.427(6) . ? C49 C55 1.488(6) . ? C50 C51 1.431(6) . ? C51 C52 1.441(6) . ? C52 C53 1.420(6) . ? C53 C54 1.439(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cd1 I1 Cd1 84.35(3) 3_665 . ? C1 Cd1 I2 113.82(13) . . ? C1 Cd1 I1 115.25(14) . 3_665 ? I2 Cd1 I1 107.31(2) . 3_665 ? C1 Cd1 I1 115.30(12) . . ? I2 Cd1 I1 107.79(2) . . ? I1 Cd1 I1 95.65(3) 3_665 . ? C1 N1 C2 110.3(5) . . ? C1 N1 C4 124.9(4) . . ? C2 N1 C4 124.2(5) . . ? C1 N2 C3 110.6(5) . . ? C1 N2 C16 125.5(4) . . ? C3 N2 C16 123.5(5) . . ? N1 C1 N2 105.3(4) . . ? N1 C1 Cd1 127.0(4) . . ? N2 C1 Cd1 127.5(4) . . ? C3 C2 N1 106.9(5) . . ? C2 C3 N2 107.0(5) . . ? C5 C4 C9 123.5(6) . . ? C5 C4 N1 119.5(5) . . ? C9 C4 N1 117.1(5) . . ? C6 C5 C4 116.4(7) . . ? C6 C5 C10 122.5(7) . . ? C4 C5 C10 121.0(6) . . ? C7 C6 C5 120.8(8) . . ? C6 C7 C8 121.9(8) . . ? C7 C8 C9 120.5(7) . . ? C8 C9 C4 116.9(6) . . ? C8 C9 C13 121.2(6) . . ? C4 C9 C13 122.0(6) . . ? C5 C10 C11 113.1(6) . . ? C5 C10 C12 111.0(6) . . ? C11 C10 C12 109.2(6) . . ? C15 C13 C14 109.3(6) . . ? C15 C13 C9 111.2(7) . . ? C14 C13 C9 113.9(6) . . ? C21 C16 C17 123.7(6) . . ? C21 C16 N2 117.7(5) . . ? C17 C16 N2 118.5(6) . . ? C18 C17 C16 116.6(7) . . ? C18 C17 C22 122.3(7) . . ? C16 C17 C22 121.1(6) . . ? C17 C18 C19 120.7(8) . . ? C20 C19 C18 121.9(8) . . ? C19 C20 C21 122.3(8) . . ? C16 C21 C20 114.7(7) . . ? C16 C21 C25 122.6(6) . . ? C20 C21 C25 122.8(6) . . ? C17 C22 C23 113.2(7) . . ? C17 C22 C24 108.1(6) . . ? C23 C22 C24 110.4(7) . . ? C26 C25 C21 110.9(6) . . ? C26 C25 C27 109.7(6) . . ? C21 C25 C27 112.3(7) . . ? C29 C28 C33 129.7(10) . . ? C29 C28 C34 111.4(10) . . ? C33 C28 C34 118.8(9) . . ? C30 C29 C28 114.0(13) . . ? C31 C30 C29 128.2(15) . . ? C30 C31 C32 119.6(11) . . ? C31 C32 C33 114.0(11) . . ? C28 C33 C32 114.5(10) . . ? C36 C35 C40 122.3(5) . . ? C36 C35 C41 118.2(6) . . ? C40 C35 C41 119.2(6) . . ? C35 C36 C37 119.4(5) . . ? C38 C37 C36 118.7(5) . . ? C37 C38 C39 121.1(6) . . ? C38 C39 C40 119.4(5) . . ? C35 C40 C39 117.8(5) . . ? C43 C42 C47 121.8(5) . . ? C43 C42 C48 119.3(6) . . ? C47 C42 C48 118.8(6) . . ? C42 C43 C44 119.0(5) . . ? C45 C44 C43 119.1(5) . . ? C46 C45 C44 121.3(5) . . ? C45 C46 C47 119.3(5) . . ? C42 C47 C46 118.8(5) . . ? C50 C49 C54 120.9(5) . . ? C50 C49 C55 119.8(6) . . ? C54 C49 C55 119.3(6) . . ? C49 C50 C51 120.8(5) . . ? C50 C51 C52 118.9(5) . . ? C53 C52 C51 119.9(5) . . ? C52 C53 C54 121.2(5) . . ? C49 C54 C53 118.4(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.579 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.115 data_IPrZnBr2 _database_code_depnum_ccdc_archive 'CCDC 905517' #TrackingRef 'IPrZnBr2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H96 Br4 N4 Zn2' _chemical_formula_weight 1539.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.707(2) _cell_length_b 12.313(3) _cell_length_c 16.081(3) _cell_angle_alpha 70.83(3) _cell_angle_beta 88.76(3) _cell_angle_gamma 66.98(3) _cell_volume 1829.2(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 2.884 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.393 _exptl_absorpt_correction_T_max 0.532 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14642 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7964 _reflns_number_gt 5886 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One molecule of benzene, and two half molecules of benzene (sitting on inversion centres) were located in the asymmetric unit. The carbon atoms of these were all refined anisotropically. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+2.2552P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7964 _refine_ls_number_parameters 405 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1226 _refine_ls_wR_factor_gt 0.1103 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.74549(4) 0.00461(4) 0.34814(3) 0.04003(13) Uani 1 1 d . . . Br2 Br 0.44664(4) 0.16680(4) 0.47492(3) 0.03429(12) Uani 1 1 d . . . Zn1 Zn 0.53049(4) 0.01645(4) 0.39359(3) 0.02118(11) Uani 1 1 d . . . N1 N 0.3139(3) 0.1682(2) 0.23144(18) 0.0194(6) Uani 1 1 d . . . N2 N 0.4055(3) -0.0260(3) 0.24344(18) 0.0192(6) Uani 1 1 d . . . C1 C 0.4027(3) 0.0532(3) 0.2864(2) 0.0182(7) Uani 1 1 d . . . C2 C 0.2646(4) 0.1602(3) 0.1559(2) 0.0257(8) Uani 1 1 d . . . H2 H 0.2025 0.2279 0.1077 0.031 Uiso 1 1 calc R . . C3 C 0.3209(4) 0.0393(3) 0.1638(2) 0.0258(8) Uani 1 1 d . . . H3 H 0.3057 0.0044 0.1224 0.031 Uiso 1 1 calc R . . C4 C 0.2629(3) 0.2824(3) 0.2526(2) 0.0212(7) Uani 1 1 d . . . C5 C 0.1432(4) 0.3099(3) 0.2928(2) 0.0248(8) Uani 1 1 d . . . C6 C 0.0948(4) 0.4213(4) 0.3108(3) 0.0321(9) Uani 1 1 d . . . H6 H 0.0139 0.4430 0.3387 0.038 Uiso 1 1 calc R . . C7 C 0.1613(5) 0.5011(4) 0.2892(3) 0.0369(10) Uani 1 1 d . . . H7 H 0.1256 0.5769 0.3019 0.044 Uiso 1 1 calc R . . C8 C 0.2787(4) 0.4715(3) 0.2495(3) 0.0325(9) Uani 1 1 d . . . H8 H 0.3232 0.5274 0.2350 0.039 Uiso 1 1 calc R . . C9 C 0.3346(4) 0.3600(3) 0.2297(2) 0.0251(8) Uani 1 1 d . . . C10 C 0.0718(4) 0.2204(4) 0.3198(2) 0.0281(8) Uani 1 1 d . . . H10 H 0.1000 0.1651 0.2831 0.034 Uiso 1 1 calc R . . C11 C 0.1162(4) 0.1361(4) 0.4173(3) 0.0360(9) Uani 1 1 d . . . H11A H 0.2156 0.0881 0.4268 0.054 Uiso 1 1 calc R . . H11B H 0.0709 0.0780 0.4328 0.054 Uiso 1 1 calc R . . H11C H 0.0907 0.1884 0.4547 0.054 Uiso 1 1 calc R . . C12 C -0.0846(5) 0.2882(5) 0.3044(4) 0.0697(18) Uani 1 1 d . . . H12A H -0.1155 0.3369 0.3440 0.105 Uiso 1 1 calc R . . H12B H -0.1245 0.2260 0.3168 0.105 Uiso 1 1 calc R . . H12C H -0.1138 0.3450 0.2426 0.105 Uiso 1 1 calc R . . C13 C 0.4610(4) 0.3310(4) 0.1828(3) 0.0348(9) Uani 1 1 d . . . H13 H 0.4993 0.2395 0.1910 0.042 Uiso 1 1 calc R . . C14 C 0.5721(5) 0.3572(5) 0.2223(5) 0.0669(17) Uani 1 1 d . . . H14A H 0.5396 0.4477 0.2108 0.100 Uiso 1 1 calc R . . H14B H 0.6557 0.3291 0.1946 0.100 Uiso 1 1 calc R . . H14C H 0.5915 0.3115 0.2864 0.100 Uiso 1 1 calc R . . C15 C 0.4224(5) 0.4057(5) 0.0837(3) 0.0569(14) Uani 1 1 d . . . H15A H 0.3586 0.3812 0.0594 0.085 Uiso 1 1 calc R . . H15B H 0.5050 0.3879 0.0538 0.085 Uiso 1 1 calc R . . H15C H 0.3790 0.4958 0.0743 0.085 Uiso 1 1 calc R . . C16 C 0.4729(4) -0.1625(3) 0.2785(2) 0.0229(7) Uani 1 1 d . . . C17 C 0.4061(4) -0.2277(3) 0.3372(2) 0.0288(8) Uani 1 1 d . . . C18 C 0.4667(5) -0.3588(4) 0.3647(3) 0.0390(10) Uani 1 1 d . . . H18 H 0.4248 -0.4065 0.4045 0.047 Uiso 1 1 calc R . . C19 C 0.5862(5) -0.4200(4) 0.3351(3) 0.0434(11) Uani 1 1 d . . . H19 H 0.6248 -0.5093 0.3537 0.052 Uiso 1 1 calc R . . C20 C 0.6508(4) -0.3537(4) 0.2787(3) 0.0386(10) Uani 1 1 d . . . H20 H 0.7342 -0.3981 0.2599 0.046 Uiso 1 1 calc R . . C21 C 0.5961(4) -0.2227(3) 0.2487(2) 0.0281(8) Uani 1 1 d . . . C22 C 0.2702(4) -0.1603(4) 0.3658(3) 0.0368(10) Uani 1 1 d . . . H22 H 0.2626 -0.0743 0.3595 0.044 Uiso 1 1 calc R . . C23 C 0.2568(5) -0.2258(5) 0.4632(3) 0.0503(12) Uani 1 1 d . . . H23A H 0.2577 -0.3083 0.4705 0.076 Uiso 1 1 calc R . . H23B H 0.1706 -0.1740 0.4791 0.076 Uiso 1 1 calc R . . H23C H 0.3335 -0.2366 0.5018 0.076 Uiso 1 1 calc R . . C24 C 0.1515(5) -0.1440(5) 0.3040(3) 0.0554(13) Uani 1 1 d . . . H24A H 0.1573 -0.0967 0.2428 0.083 Uiso 1 1 calc R . . H24B H 0.0643 -0.0980 0.3220 0.083 Uiso 1 1 calc R . . H24C H 0.1573 -0.2270 0.3077 0.083 Uiso 1 1 calc R . . C25 C 0.6672(4) -0.1504(4) 0.1846(3) 0.0343(9) Uani 1 1 d . . . H25 H 0.6283 -0.0620 0.1844 0.041 Uiso 1 1 calc R . . C26 C 0.8220(4) -0.2070(4) 0.2121(3) 0.0434(11) Uani 1 1 d . . . H26A H 0.8395 -0.2052 0.2711 0.065 Uiso 1 1 calc R . . H26B H 0.8632 -0.1577 0.1692 0.065 Uiso 1 1 calc R . . H26C H 0.8621 -0.2942 0.2136 0.065 Uiso 1 1 calc R . . C27 C 0.6394(5) -0.1459(5) 0.0911(3) 0.0523(13) Uani 1 1 d . . . H27A H 0.6671 -0.2317 0.0910 0.078 Uiso 1 1 calc R . . H27B H 0.6917 -0.1052 0.0517 0.078 Uiso 1 1 calc R . . H27C H 0.5416 -0.0978 0.0702 0.078 Uiso 1 1 calc R . . C28 C 0.1530(7) -0.1932(5) 0.0761(4) 0.0686(17) Uani 1 1 d . . . H28 H 0.1230 -0.2147 0.1329 0.082 Uiso 1 1 calc R . . C29 C 0.0639(7) -0.1513(6) 0.0024(5) 0.0795(19) Uani 1 1 d . . . H29 H -0.0277 -0.1428 0.0073 0.095 Uiso 1 1 calc R . . C30 C 0.1091(7) -0.1212(5) -0.0799(4) 0.0739(18) Uani 1 1 d . . . H30 H 0.0479 -0.0922 -0.1319 0.089 Uiso 1 1 calc R . . C31 C 0.2385(8) -0.1323(5) -0.0872(4) 0.0701(17) Uani 1 1 d . . . H31 H 0.2688 -0.1123 -0.1441 0.084 Uiso 1 1 calc R . . C32 C 0.3252(7) -0.1721(6) -0.0133(5) 0.0764(18) Uani 1 1 d . . . H32 H 0.4160 -0.1778 -0.0184 0.092 Uiso 1 1 calc R . . C33 C 0.2825(7) -0.2049(5) 0.0704(4) 0.0641(16) Uani 1 1 d . . . H33 H 0.3441 -0.2351 0.1225 0.077 Uiso 1 1 calc R . . C34 C 0.0857(7) 0.5574(7) -0.0308(5) 0.086(2) Uani 1 1 d . . . H34 H 0.1449 0.5985 -0.0522 0.103 Uiso 1 1 calc R . . C35 C 0.0299(8) 0.5618(6) 0.0464(5) 0.082(2) Uani 1 1 d . . . H35 H 0.0525 0.6050 0.0788 0.098 Uiso 1 1 calc R . . C36 C -0.0547(8) 0.5071(6) 0.0765(4) 0.0779(19) Uani 1 1 d . . . H36 H -0.0937 0.5124 0.1295 0.094 Uiso 1 1 calc R . . C37 C 0.1163(5) 0.3907(4) 0.5377(3) 0.0374(10) Uani 1 1 d . . . H37 H 0.1964 0.3158 0.5634 0.045 Uiso 1 1 calc R . . C38 C 0.1255(4) 0.5059(4) 0.5014(3) 0.0374(10) Uani 1 1 d . . . H38 H 0.2122 0.5099 0.5025 0.045 Uiso 1 1 calc R . . C39 C 0.0099(5) 0.6143(4) 0.4638(3) 0.0361(10) Uani 1 1 d . . . H39 H 0.0171 0.6927 0.4388 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0253(2) 0.0580(3) 0.0327(2) -0.01195(19) 0.00690(16) -0.01601(19) Br2 0.0390(2) 0.0329(2) 0.0301(2) -0.01179(16) 0.00254(17) -0.01296(18) Zn1 0.0192(2) 0.0254(2) 0.0183(2) -0.00861(16) 0.00113(15) -0.00750(16) N1 0.0200(15) 0.0183(14) 0.0198(14) -0.0074(11) -0.0002(11) -0.0068(12) N2 0.0210(15) 0.0197(14) 0.0179(14) -0.0094(11) 0.0030(11) -0.0071(12) C1 0.0174(16) 0.0192(16) 0.0187(17) -0.0081(13) 0.0048(13) -0.0071(13) C2 0.030(2) 0.0258(19) 0.0179(17) -0.0058(14) -0.0048(15) -0.0089(16) C3 0.029(2) 0.029(2) 0.0169(17) -0.0085(14) -0.0016(15) -0.0085(16) C4 0.0220(17) 0.0178(17) 0.0193(17) -0.0063(13) -0.0020(14) -0.0035(14) C5 0.0244(19) 0.0252(18) 0.0189(17) -0.0050(14) 0.0006(14) -0.0061(15) C6 0.030(2) 0.031(2) 0.030(2) -0.0125(16) 0.0079(17) -0.0053(17) C7 0.050(3) 0.025(2) 0.030(2) -0.0137(16) 0.0035(19) -0.0061(18) C8 0.044(2) 0.0204(19) 0.033(2) -0.0060(16) -0.0007(18) -0.0149(17) C9 0.0257(19) 0.0215(18) 0.0244(18) -0.0056(14) 0.0003(15) -0.0077(15) C10 0.0239(19) 0.034(2) 0.027(2) -0.0111(16) 0.0039(15) -0.0116(16) C11 0.040(2) 0.039(2) 0.031(2) -0.0110(18) 0.0078(18) -0.0197(19) C12 0.029(3) 0.066(4) 0.090(4) 0.005(3) -0.001(3) -0.021(2) C13 0.031(2) 0.031(2) 0.045(2) -0.0119(18) 0.0117(18) -0.0170(18) C14 0.038(3) 0.055(3) 0.122(5) -0.040(3) 0.016(3) -0.027(2) C15 0.059(3) 0.053(3) 0.047(3) -0.008(2) 0.026(3) -0.019(3) C16 0.0286(19) 0.0199(17) 0.0214(18) -0.0107(14) -0.0016(15) -0.0081(15) C17 0.039(2) 0.0256(19) 0.0262(19) -0.0103(15) 0.0005(16) -0.0158(17) C18 0.051(3) 0.027(2) 0.040(2) -0.0094(18) 0.001(2) -0.018(2) C19 0.054(3) 0.019(2) 0.050(3) -0.0106(19) -0.009(2) -0.0079(19) C20 0.036(2) 0.027(2) 0.045(3) -0.0158(18) -0.0040(19) -0.0009(17) C21 0.027(2) 0.0270(19) 0.0254(19) -0.0106(15) -0.0005(15) -0.0048(16) C22 0.047(3) 0.033(2) 0.043(2) -0.0170(18) 0.019(2) -0.026(2) C23 0.062(3) 0.071(3) 0.044(3) -0.026(2) 0.024(2) -0.048(3) C24 0.037(3) 0.064(3) 0.049(3) -0.006(2) 0.007(2) -0.016(2) C25 0.027(2) 0.032(2) 0.032(2) -0.0101(17) 0.0070(17) -0.0007(17) C26 0.032(2) 0.048(3) 0.040(2) -0.015(2) 0.0062(19) -0.006(2) C27 0.044(3) 0.063(3) 0.034(2) -0.012(2) 0.002(2) -0.010(2) C28 0.098(5) 0.056(3) 0.055(4) -0.017(3) 0.023(3) -0.037(3) C29 0.070(4) 0.072(4) 0.089(5) -0.025(4) 0.014(4) -0.024(3) C30 0.087(5) 0.049(3) 0.062(4) -0.014(3) -0.004(3) -0.008(3) C31 0.099(5) 0.055(3) 0.062(4) -0.027(3) 0.033(4) -0.033(3) C32 0.079(4) 0.070(4) 0.105(6) -0.053(4) 0.029(4) -0.039(4) C33 0.087(5) 0.044(3) 0.066(4) -0.027(3) -0.005(3) -0.024(3) C34 0.073(4) 0.080(5) 0.083(5) 0.001(4) -0.019(4) -0.032(4) C35 0.117(6) 0.064(4) 0.054(4) -0.015(3) -0.029(4) -0.030(4) C36 0.093(5) 0.060(4) 0.054(4) -0.015(3) -0.001(4) -0.007(4) C37 0.041(2) 0.037(2) 0.031(2) -0.0149(18) 0.0064(18) -0.0098(19) C38 0.039(2) 0.051(3) 0.032(2) -0.0188(19) 0.0082(18) -0.025(2) C39 0.053(3) 0.035(2) 0.032(2) -0.0185(18) 0.014(2) -0.025(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Zn1 2.3642(8) . ? Br2 Zn1 2.4658(12) 2_656 ? Br2 Zn1 2.4866(9) . ? Zn1 C1 2.039(3) . ? Zn1 Br2 2.4658(12) 2_656 ? N1 C1 1.361(4) . ? N1 C2 1.383(4) . ? N1 C4 1.448(4) . ? N2 C1 1.359(4) . ? N2 C3 1.383(4) . ? N2 C16 1.452(4) . ? C2 C3 1.332(5) . ? C4 C5 1.394(5) . ? C4 C9 1.403(5) . ? C5 C6 1.389(5) . ? C5 C10 1.522(5) . ? C6 C7 1.381(6) . ? C7 C8 1.371(6) . ? C8 C9 1.407(5) . ? C9 C13 1.510(5) . ? C10 C11 1.529(5) . ? C10 C12 1.533(6) . ? C13 C15 1.525(6) . ? C13 C14 1.546(6) . ? C16 C21 1.400(5) . ? C16 C17 1.403(5) . ? C17 C18 1.396(5) . ? C17 C22 1.514(6) . ? C18 C19 1.373(6) . ? C19 C20 1.377(6) . ? C20 C21 1.393(5) . ? C21 C25 1.526(5) . ? C22 C24 1.540(7) . ? C22 C23 1.541(6) . ? C25 C27 1.517(6) . ? C25 C26 1.534(6) . ? C28 C33 1.342(8) . ? C28 C29 1.356(9) . ? C29 C30 1.384(9) . ? C30 C31 1.344(9) . ? C31 C32 1.351(9) . ? C32 C33 1.395(9) . ? C34 C36 1.372(10) 2_565 ? C34 C35 1.373(10) . ? C35 C36 1.325(10) . ? C36 C34 1.372(10) 2_565 ? C37 C39 1.377(6) 2_566 ? C37 C38 1.388(6) . ? C38 C39 1.374(6) . ? C39 C37 1.377(6) 2_566 ? 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 Zn1 Br2 Zn1 86.44(3) 2_656 . ? C1 Zn1 Br1 108.88(9) . . ? C1 Zn1 Br2 116.35(9) . 2_656 ? Br1 Zn1 Br2 111.71(4) . 2_656 ? C1 Zn1 Br2 115.70(10) . . ? Br1 Zn1 Br2 109.92(3) . . ? Br2 Zn1 Br2 93.56(3) 2_656 . ? C1 N1 C2 111.1(3) . . ? C1 N1 C4 125.3(3) . . ? C2 N1 C4 123.1(3) . . ? C1 N2 C3 110.8(3) . . ? C1 N2 C16 126.2(3) . . ? C3 N2 C16 122.6(3) . . ? N2 C1 N1 104.0(3) . . ? N2 C1 Zn1 128.0(2) . . ? N1 C1 Zn1 126.9(2) . . ? C3 C2 N1 106.8(3) . . ? C2 C3 N2 107.4(3) . . ? C5 C4 C9 124.0(3) . . ? C5 C4 N1 117.7(3) . . ? C9 C4 N1 118.3(3) . . ? C6 C5 C4 116.6(3) . . ? C6 C5 C10 121.2(3) . . ? C4 C5 C10 122.2(3) . . ? C7 C6 C5 121.6(4) . . ? C8 C7 C6 120.3(4) . . ? C7 C8 C9 121.4(4) . . ? C4 C9 C8 116.0(3) . . ? C4 C9 C13 123.1(3) . . ? C8 C9 C13 120.8(3) . . ? C5 C10 C11 110.9(3) . . ? C5 C10 C12 113.3(3) . . ? C11 C10 C12 109.0(4) . . ? C9 C13 C15 109.8(3) . . ? C9 C13 C14 111.8(4) . . ? C15 C13 C14 111.2(4) . . ? C21 C16 C17 123.3(3) . . ? C21 C16 N2 119.0(3) . . ? C17 C16 N2 117.6(3) . . ? C18 C17 C16 116.9(4) . . ? C18 C17 C22 120.8(4) . . ? C16 C17 C22 122.2(3) . . ? C19 C18 C17 121.0(4) . . ? C18 C19 C20 120.9(4) . . ? C19 C20 C21 121.2(4) . . ? C20 C21 C16 116.8(4) . . ? C20 C21 C25 120.6(4) . . ? C16 C21 C25 122.6(3) . . ? C17 C22 C24 110.3(4) . . ? C17 C22 C23 113.4(4) . . ? C24 C22 C23 110.2(3) . . ? C27 C25 C21 110.5(4) . . ? C27 C25 C26 109.7(3) . . ? C21 C25 C26 112.3(3) . . ? C33 C28 C29 121.4(6) . . ? C28 C29 C30 118.8(6) . . ? C31 C30 C29 120.9(6) . . ? C30 C31 C32 119.6(6) . . ? C31 C32 C33 120.5(6) . . ? C28 C33 C32 118.9(6) . . ? C36 C34 C35 119.0(7) 2_565 . ? C36 C35 C34 121.4(6) . . ? C35 C36 C34 119.5(7) . 2_565 ? C39 C37 C38 119.4(4) 2_566 . ? C39 C38 C37 120.4(4) . . ? C38 C39 C37 120.1(4) . 2_566 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.700 _refine_diff_density_min -1.186 _refine_diff_density_rms 0.095 data_compound1 _database_code_depnum_ccdc_archive 'CCDC 905518' #TrackingRef 'compound1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H72 Br2 P2 Pt Zn' _chemical_formula_weight 1059.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.7915(8) _cell_length_b 10.9089(17) _cell_length_c 23.5671(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.615(5) _cell_angle_gamma 90.00 _cell_volume 4308.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 5.757 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.161 _exptl_absorpt_correction_T_max 0.327 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19036 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 30.00 _reflns_number_total 6274 _reflns_number_gt 5203 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One molecule of benzene was located in the asymmetric unit, the atomic positions of which were refined at 50% occupancy. The carbon atoms of this molecule were refined anisotropically.One cyclohexyl group in the asymmetric unit was found to be disordered over two sites. This disorder was successfully modelled. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0103P)^2^+18.0097P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6274 _refine_ls_number_parameters 300 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0523 _refine_ls_wR_factor_gt 0.0489 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.5000 0.249040(13) 0.2500 0.01408(4) Uani 1 2 d S . . Br1 Br 0.59577(3) 0.57824(3) 0.305324(16) 0.04823(11) Uani 1 1 d . . . Zn1 Zn 0.5000 0.46941(4) 0.2500 0.03012(12) Uani 1 2 d S . . P1 P 0.45664(4) 0.24227(6) 0.33952(2) 0.01376(11) Uani 1 1 d D . . C2 C 0.35991(15) 0.3177(2) 0.34991(10) 0.0159(5) Uani 1 1 d . A . H2 H 0.3362 0.2784 0.3832 0.019 Uiso 1 1 calc R . . C3 C 0.36832(16) 0.4547(2) 0.36206(13) 0.0229(6) Uani 1 1 d . . . H3A H 0.3959 0.4942 0.3310 0.028 Uiso 1 1 calc R A . H3B H 0.4016 0.4666 0.3978 0.028 Uiso 1 1 calc R . . C4 C 0.28744(18) 0.5164(3) 0.36739(14) 0.0288(7) Uani 1 1 d . A . H4A H 0.2624 0.4837 0.4012 0.035 Uiso 1 1 calc R . . H4B H 0.2954 0.6057 0.3729 0.035 Uiso 1 1 calc R . . C5 C 0.23223(19) 0.4947(3) 0.31490(15) 0.0384(8) Uani 1 1 d . . . H5A H 0.1796 0.5327 0.3202 0.046 Uiso 1 1 calc R A . H5B H 0.2548 0.5335 0.2815 0.046 Uiso 1 1 calc R . . C6 C 0.22192(18) 0.3589(4) 0.30455(14) 0.0357(8) Uani 1 1 d . A . H6A H 0.1867 0.3456 0.2698 0.043 Uiso 1 1 calc R . . H6B H 0.1962 0.3212 0.3370 0.043 Uiso 1 1 calc R . . C7 C 0.30256(17) 0.2977(3) 0.29757(12) 0.0283(6) Uani 1 1 d . . . H7A H 0.3265 0.3317 0.2636 0.034 Uiso 1 1 calc R A . H7B H 0.2945 0.2086 0.2914 0.034 Uiso 1 1 calc R . . C8 C 0.52790(15) 0.3089(2) 0.39352(11) 0.0166(5) Uani 1 1 d . A . H8 H 0.5257 0.3995 0.3873 0.020 Uiso 1 1 calc R . . C9 C 0.50814(18) 0.2887(3) 0.45528(11) 0.0232(6) Uani 1 1 d . . . H9A H 0.4530 0.3169 0.4605 0.028 Uiso 1 1 calc R A . H9B H 0.5111 0.2002 0.4643 0.028 Uiso 1 1 calc R . . C10 C 0.56640(19) 0.3590(3) 0.49546(12) 0.0299(7) Uani 1 1 d . A . H10A H 0.5600 0.4480 0.4886 0.036 Uiso 1 1 calc R . . H10B H 0.5542 0.3423 0.5353 0.036 Uiso 1 1 calc R . . C11 C 0.6519(2) 0.3219(4) 0.48681(17) 0.0488(11) Uani 1 1 d . . . H11A H 0.6886 0.3716 0.5120 0.059 Uiso 1 1 calc R A . H11B H 0.6596 0.2347 0.4973 0.059 Uiso 1 1 calc R . . C12 C 0.67154(19) 0.3402(4) 0.42572(18) 0.0512(12) Uani 1 1 d . A . H12A H 0.7267 0.3115 0.4209 0.061 Uiso 1 1 calc R . . H12B H 0.6692 0.4287 0.4165 0.061 Uiso 1 1 calc R . . C13 C 0.61419(16) 0.2711(3) 0.38454(14) 0.0313(7) Uani 1 1 d . . . H13A H 0.6204 0.1817 0.3908 0.038 Uiso 1 1 calc R A . H13B H 0.6268 0.2894 0.3450 0.038 Uiso 1 1 calc R . . C14 C 0.4360(3) 0.0830(4) 0.3642(3) 0.0155(14) Uani 0.588(4) 1 d PD A 1 H14 H 0.4253 0.0880 0.4053 0.019 Uiso 0.588(4) 1 calc PR A 1 C15 C 0.3633(3) 0.0215(4) 0.3332(2) 0.0214(10) Uani 0.588(4) 1 d PD A 1 H15A H 0.3147 0.0682 0.3409 0.026 Uiso 0.588(4) 1 calc PR A 1 H15B H 0.3695 0.0240 0.2917 0.026 Uiso 0.588(4) 1 calc PR A 1 C16 C 0.3529(3) -0.1119(4) 0.3516(2) 0.0303(13) Uani 0.588(4) 1 d PD A 1 H16A H 0.3408 -0.1139 0.3921 0.036 Uiso 0.588(4) 1 calc PR A 1 H16B H 0.3071 -0.1484 0.3291 0.036 Uiso 0.588(4) 1 calc PR A 1 C17 C 0.4274(4) -0.1887(8) 0.3436(4) 0.033(2) Uani 0.588(4) 1 d PD A 1 H17A H 0.4190 -0.2734 0.3570 0.040 Uiso 0.588(4) 1 calc PR A 1 H17B H 0.4378 -0.1922 0.3027 0.040 Uiso 0.588(4) 1 calc PR A 1 C18 C 0.4986(3) -0.1316(4) 0.3770(3) 0.0363(14) Uani 0.588(4) 1 d PD A 1 H18A H 0.5474 -0.1791 0.3702 0.044 Uiso 0.588(4) 1 calc PR A 1 H18B H 0.4901 -0.1353 0.4182 0.044 Uiso 0.588(4) 1 calc PR A 1 C19 C 0.5102(3) 0.0020(4) 0.3594(3) 0.0300(12) Uani 0.588(4) 1 d PD A 1 H19A H 0.5258 0.0038 0.3196 0.036 Uiso 0.588(4) 1 calc PR A 1 H19B H 0.5548 0.0375 0.3836 0.036 Uiso 0.588(4) 1 calc PR A 1 C20 C 0.8208(5) 0.7739(7) 0.5414(3) 0.054(3) Uani 0.50 1 d PD B -1 H20 H 0.8575 0.8094 0.5690 0.065 Uiso 0.50 1 calc PR B -1 C23 C 0.7125(5) 0.6704(8) 0.4616(4) 0.041(3) Uani 0.50 1 d PD B -1 H23 H 0.6758 0.6354 0.4339 0.049 Uiso 0.50 1 calc PR B -1 C22 C 0.7785(5) 0.6029(6) 0.4826(4) 0.050(2) Uani 0.50 1 d PD B -1 H22 H 0.7864 0.5217 0.4695 0.060 Uiso 0.50 1 calc PR B -1 C21 C 0.8326(4) 0.6545(7) 0.5226(4) 0.057(3) Uani 0.50 1 d PD B -1 H21 H 0.8775 0.6087 0.5372 0.068 Uiso 0.50 1 calc PR B -1 C24 C 0.7004(5) 0.7880(7) 0.4811(4) 0.058(3) Uani 0.50 1 d PD B -1 H24 H 0.6543 0.8326 0.4680 0.070 Uiso 0.50 1 calc PR B -1 C15A C 0.4550(4) 0.0019(5) 0.3019(2) 0.0205(14) Uani 0.412(4) 1 d PD A 2 H15C H 0.4972 0.0298 0.2774 0.025 Uiso 0.412(4) 1 calc PR A 2 H15D H 0.4027 0.0147 0.2810 0.025 Uiso 0.412(4) 1 calc PR A 2 C19A C 0.3940(4) 0.0375(5) 0.3950(3) 0.0202(14) Uani 0.412(4) 1 d PD A 2 H19C H 0.3408 0.0490 0.3751 0.024 Uiso 0.412(4) 1 calc PR A 2 H19D H 0.3965 0.0878 0.4300 0.024 Uiso 0.412(4) 1 calc PR A 2 C18A C 0.4068(5) -0.0975(5) 0.4101(3) 0.0256(16) Uani 0.412(4) 1 d PD A 2 H18C H 0.3649 -0.1251 0.4349 0.031 Uiso 0.412(4) 1 calc PR A 2 H18D H 0.4592 -0.1079 0.4312 0.031 Uiso 0.412(4) 1 calc PR A 2 C16A C 0.4664(5) -0.1342(5) 0.3155(4) 0.0331(19) Uani 0.412(4) 1 d PD A 2 H16C H 0.5206 -0.1482 0.3334 0.040 Uiso 0.412(4) 1 calc PR A 2 H16D H 0.4608 -0.1827 0.2800 0.040 Uiso 0.412(4) 1 calc PR A 2 C17A C 0.4039(7) -0.1752(11) 0.3560(4) 0.028(2) Uani 0.412(4) 1 d PD A 2 H17C H 0.3501 -0.1687 0.3364 0.033 Uiso 0.412(4) 1 calc PR A 2 H17D H 0.4131 -0.2622 0.3663 0.033 Uiso 0.412(4) 1 calc PR A 2 C14A C 0.4590(5) 0.0767(5) 0.3568(3) 0.014(2) Uani 0.412(4) 1 d PD A 2 H14A H 0.5115 0.0591 0.3775 0.016 Uiso 0.412(4) 1 calc PR A 2 C25 C 0.7559(6) 0.8408(7) 0.5199(4) 0.048(3) Uani 0.50 1 d PD B -1 H25 H 0.7492 0.9232 0.5317 0.058 Uiso 0.50 1 calc PR B -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02127(6) 0.00955(6) 0.01121(6) 0.000 -0.00067(4) 0.000 Br1 0.0874(3) 0.02288(16) 0.03653(19) -0.01135(14) 0.02044(19) -0.02421(18) Zn1 0.0584(4) 0.0100(2) 0.0235(2) 0.000 0.0147(2) 0.000 P1 0.0184(3) 0.0115(3) 0.0109(2) -0.0009(2) -0.0027(2) 0.0008(3) C2 0.0174(12) 0.0173(12) 0.0129(11) -0.0008(9) -0.0005(9) -0.0025(10) C3 0.0198(13) 0.0155(12) 0.0329(15) -0.0021(11) -0.0037(11) 0.0008(10) C4 0.0242(15) 0.0221(14) 0.0398(18) -0.0017(13) -0.0005(13) 0.0053(12) C5 0.0258(16) 0.051(2) 0.0375(18) 0.0062(16) -0.0054(14) 0.0145(15) C6 0.0179(14) 0.061(2) 0.0268(15) -0.0121(16) -0.0068(12) 0.0017(14) C7 0.0193(13) 0.0441(18) 0.0208(13) -0.0103(13) -0.0029(11) -0.0007(12) C8 0.0167(12) 0.0159(12) 0.0168(12) -0.0042(10) -0.0013(9) 0.0016(10) C9 0.0292(15) 0.0241(13) 0.0154(12) -0.0025(11) -0.0049(11) 0.0005(11) C10 0.0384(17) 0.0303(16) 0.0191(13) -0.0090(12) -0.0124(12) 0.0039(13) C11 0.037(2) 0.051(2) 0.054(2) -0.0298(19) -0.0293(17) 0.0139(17) C12 0.0170(15) 0.069(3) 0.066(3) -0.046(2) -0.0094(16) -0.0001(16) C13 0.0167(12) 0.0387(19) 0.0380(16) -0.0234(14) -0.0031(11) 0.0013(12) C14 0.016(3) 0.012(2) 0.019(3) -0.0004(19) -0.002(2) 0.0079(19) C15 0.024(2) 0.016(2) 0.024(2) -0.0022(18) -0.0003(18) -0.0064(18) C16 0.046(3) 0.019(2) 0.026(3) -0.002(2) 0.004(2) -0.017(2) C17 0.055(5) 0.012(3) 0.033(4) -0.004(3) 0.005(4) 0.001(4) C18 0.050(4) 0.015(2) 0.044(3) 0.007(2) 0.002(3) 0.005(2) C19 0.031(3) 0.016(2) 0.043(3) 0.005(2) 0.001(2) 0.002(2) C20 0.079(8) 0.056(7) 0.029(4) -0.013(5) 0.016(5) -0.048(6) C23 0.055(8) 0.043(6) 0.025(5) -0.007(5) 0.002(4) -0.021(5) C22 0.060(7) 0.050(6) 0.043(5) -0.008(5) 0.012(5) -0.025(4) C21 0.061(7) 0.064(7) 0.046(5) 0.001(5) 0.004(5) -0.032(5) C24 0.072(8) 0.049(6) 0.057(6) -0.005(5) 0.023(6) -0.023(5) C15A 0.038(4) 0.012(3) 0.012(3) 0.000(2) 0.003(3) -0.003(3) C19A 0.026(3) 0.019(3) 0.015(3) 0.006(3) 0.005(3) -0.006(3) C18A 0.037(4) 0.019(3) 0.021(3) 0.006(3) 0.003(3) -0.009(3) C16A 0.052(5) 0.009(3) 0.039(4) -0.003(3) 0.010(4) -0.004(3) C17A 0.040(6) 0.012(5) 0.032(6) 0.004(4) 0.003(4) -0.004(5) C14A 0.015(5) 0.011(3) 0.014(4) -0.008(3) 0.000(3) 0.005(3) C25 0.063(9) 0.046(7) 0.036(6) -0.015(5) 0.015(5) -0.031(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.2760(6) 2_655 ? Pt1 P1 2.2760(6) . ? Pt1 Zn1 2.4040(6) . ? Br1 Zn1 2.3305(5) . ? Zn1 Br1 2.3305(5) 2_655 ? P1 C8 1.840(3) . ? P1 C2 1.851(3) . ? P1 C14A 1.851(6) . ? P1 C14 1.871(5) . ? C2 C3 1.526(4) . ? C2 C7 1.532(4) . ? C2 H2 1.0000 . ? C3 C4 1.528(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.517(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.510(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.528(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.529(4) . ? C8 C13 1.534(4) . ? C8 H8 1.0000 . ? C9 C10 1.524(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.517(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.510(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.523(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.536(5) . ? C14 C19 1.537(5) . ? C14 H14 1.0000 . ? C15 C16 1.531(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.527(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.523(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.532(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C25 1.381(6) . ? C20 C21 1.394(5) . ? C20 H20 0.9500 . ? C23 C24 1.382(6) . ? C23 C22 1.395(6) . ? C23 H23 0.9500 . ? C22 C21 1.387(5) . ? C22 H22 0.9500 . ? C21 H21 0.9500 . ? C24 C25 1.388(5) . ? C24 H24 0.9500 . ? C15A C14A 1.526(6) . ? C15A C16A 1.529(6) . ? C15A H15C 0.9900 . ? C15A H15D 0.9900 . ? C19A C14A 1.520(6) . ? C19A C18A 1.527(6) . ? C19A H19C 0.9900 . ? C19A H19D 0.9900 . ? C18A C17A 1.529(6) . ? C18A H18C 0.9900 . ? C18A H18D 0.9900 . ? C16A C17A 1.530(6) . ? C16A H16C 0.9900 . ? C16A H16D 0.9900 . ? C17A H17C 0.9900 . ? C17A H17D 0.9900 . ? C14A H14A 1.0000 . ? C25 H25 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P1 176.28(3) 2_655 . ? P1 Pt1 Zn1 91.860(17) 2_655 . ? P1 Pt1 Zn1 91.860(17) . . ? Br1 Zn1 Br1 118.75(3) . 2_655 ? Br1 Zn1 Pt1 120.626(15) . . ? Br1 Zn1 Pt1 120.626(15) 2_655 . ? C8 P1 C2 105.70(11) . . ? C8 P1 C14A 103.2(3) . . ? C2 P1 C14A 114.3(3) . . ? C8 P1 C14 106.1(2) . . ? C2 P1 C14 101.00(19) . . ? C14A P1 C14 13.5(3) . . ? C8 P1 Pt1 113.33(9) . . ? C2 P1 Pt1 116.29(8) . . ? C14A P1 Pt1 103.4(2) . . ? C14 P1 Pt1 113.2(2) . . ? C3 C2 C7 109.7(2) . . ? C3 C2 P1 112.87(18) . . ? C7 C2 P1 110.02(18) . . ? C3 C2 H2 108.0 . . ? C7 C2 H2 108.0 . . ? P1 C2 H2 108.0 . . ? C2 C3 C4 112.0(2) . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 111.4(3) . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C6 C5 C4 110.1(3) . . ? C6 C5 H5A 109.7 . . ? C4 C5 H5A 109.7 . . ? C6 C5 H5B 109.7 . . ? C4 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? C5 C6 C7 110.7(3) . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C6 C7 C2 111.5(2) . . ? C6 C7 H7A 109.3 . . ? C2 C7 H7A 109.3 . . ? C6 C7 H7B 109.3 . . ? C2 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C9 C8 C13 110.9(2) . . ? C9 C8 P1 115.52(19) . . ? C13 C8 P1 112.16(18) . . ? C9 C8 H8 105.8 . . ? C13 C8 H8 105.8 . . ? P1 C8 H8 105.8 . . ? C10 C9 C8 110.5(2) . . ? C10 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? C10 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 111.0(3) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 111.0(3) . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C13 112.0(3) . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C12 C13 C8 110.1(2) . . ? C12 C13 H13A 109.6 . . ? C8 C13 H13A 109.6 . . ? C12 C13 H13B 109.6 . . ? C8 C13 H13B 109.6 . . ? H13A C13 H13B 108.2 . . ? C15 C14 C19 109.8(4) . . ? C15 C14 P1 114.5(4) . . ? C19 C14 P1 110.1(3) . . ? C15 C14 H14 107.4 . . ? C19 C14 H14 107.4 . . ? P1 C14 H14 107.4 . . ? C16 C15 C14 112.4(4) . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? C14 C15 H15B 109.1 . . ? H15A C15 H15B 107.9 . . ? C17 C16 C15 112.2(5) . . ? C17 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? C17 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C18 C17 C16 109.5(5) . . ? C18 C17 H17A 109.8 . . ? C16 C17 H17A 109.8 . . ? C18 C17 H17B 109.8 . . ? C16 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? C17 C18 C19 111.0(6) . . ? C17 C18 H18A 109.4 . . ? C19 C18 H18A 109.4 . . ? C17 C18 H18B 109.4 . . ? C19 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C18 C19 C14 114.2(4) . . ? C18 C19 H19A 108.7 . . ? C14 C19 H19A 108.7 . . ? C18 C19 H19B 108.7 . . ? C14 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C25 C20 C21 120.2(4) . . ? C25 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C24 C23 C22 120.2(4) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C21 C22 C23 119.9(5) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C22 C21 C20 119.7(5) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C23 C24 C25 119.8(5) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C14A C15A C16A 110.1(5) . . ? C14A C15A H15C 109.6 . . ? C16A C15A H15C 109.6 . . ? C14A C15A H15D 109.6 . . ? C16A C15A H15D 109.6 . . ? H15C C15A H15D 108.2 . . ? C14A C19A C18A 108.2(5) . . ? C14A C19A H19C 110.1 . . ? C18A C19A H19C 110.1 . . ? C14A C19A H19D 110.1 . . ? C18A C19A H19D 110.1 . . ? H19C C19A H19D 108.4 . . ? C19A C18A C17A 110.1(7) . . ? C19A C18A H18C 109.6 . . ? C17A C18A H18C 109.6 . . ? C19A C18A H18D 109.6 . . ? C17A C18A H18D 109.6 . . ? H18C C18A H18D 108.1 . . ? C15A C16A C17A 109.4(7) . . ? C15A C16A H16C 109.8 . . ? C17A C16A H16C 109.8 . . ? C15A C16A H16D 109.8 . . ? C17A C16A H16D 109.8 . . ? H16C C16A H16D 108.2 . . ? C18A C17A C16A 111.7(7) . . ? C18A C17A H17C 109.3 . . ? C16A C17A H17C 109.3 . . ? C18A C17A H17D 109.3 . . ? C16A C17A H17D 109.3 . . ? H17C C17A H17D 107.9 . . ? C19A C14A C15A 110.9(6) . . ? C19A C14A P1 113.5(4) . . ? C15A C14A P1 109.6(5) . . ? C19A C14A H14A 107.5 . . ? C15A C14A H14A 107.5 . . ? P1 C14A H14A 107.5 . . ? C20 C25 C24 120.2(5) . . ? C20 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.340 _refine_diff_density_min -1.692 _refine_diff_density_rms 0.102 data_compound2 _database_code_depnum_ccdc_archive 'CCDC 905519' #TrackingRef 'compound2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H74 Cd I2 P2 Pt' _chemical_formula_weight 1214.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 17.011(3) _cell_length_b 11.399(2) _cell_length_c 23.647(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.39(3) _cell_angle_gamma 90.00 _cell_volume 4581.2(16) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 4.959 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.435 _exptl_absorpt_correction_T_max 0.587 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20129 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.00 _reflns_number_total 8275 _reflns_number_gt 7958 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One molecule of toluene was located in the asymmetric unit, the carbon atoms of which were refined anisotropically. The compound was found to be a racemic twin and was refined with the TWIN and BASF commands of Shelxl. Attempts to solve and refine the structure in the centrosymmetric setting, C2/c, were not successful. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0160P)^2^+1.0981P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.486(3) _refine_ls_number_reflns 8275 _refine_ls_number_parameters 444 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0210 _refine_ls_R_factor_gt 0.0192 _refine_ls_wR_factor_ref 0.0413 _refine_ls_wR_factor_gt 0.0404 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.446340(11) 0.260156(10) 0.220310(7) 0.01222(3) Uani 1 1 d . . . I1 I 0.554040(18) 0.61434(3) 0.279461(12) 0.02717(8) Uani 1 1 d . . . I2 I 0.34314(2) 0.59476(3) 0.146296(12) 0.03260(9) Uani 1 1 d . . . Cd1 Cd 0.44778(3) 0.487014(19) 0.217853(15) 0.01816(6) Uani 1 1 d . . . P1 P 0.40084(9) 0.26002(9) 0.30964(5) 0.0133(3) Uani 1 1 d . . . P2 P 0.49157(9) 0.24952(9) 0.13050(5) 0.0134(3) Uani 1 1 d . . . C1 C 0.3076(3) 0.3434(4) 0.31924(18) 0.0164(9) Uani 1 1 d . . . H1 H 0.2792 0.3043 0.3503 0.020 Uiso 1 1 calc R . . C2 C 0.2538(3) 0.3370(4) 0.26517(17) 0.0193(9) Uani 1 1 d . . . H2A H 0.2818 0.3704 0.2330 0.023 Uiso 1 1 calc R . . H2B H 0.2416 0.2539 0.2563 0.023 Uiso 1 1 calc R . . C3 C 0.1772(3) 0.4041(4) 0.27217(19) 0.0257(10) Uani 1 1 d . . . H3A H 0.1447 0.3997 0.2365 0.031 Uiso 1 1 calc R . . H3B H 0.1473 0.3669 0.3024 0.031 Uiso 1 1 calc R . . C4 C 0.1922(3) 0.5316(4) 0.2871(2) 0.0268(11) Uani 1 1 d . . . H4A H 0.2184 0.5708 0.2556 0.032 Uiso 1 1 calc R . . H4B H 0.1415 0.5718 0.2925 0.032 Uiso 1 1 calc R . . C5 C 0.2435(3) 0.5409(4) 0.34038(18) 0.0214(10) Uani 1 1 d . . . H5A H 0.2141 0.5109 0.3726 0.026 Uiso 1 1 calc R . . H5B H 0.2559 0.6245 0.3478 0.026 Uiso 1 1 calc R . . C6 C 0.3211(3) 0.4712(4) 0.33654(18) 0.0197(10) Uani 1 1 d . . . H6A H 0.3545 0.5096 0.3086 0.024 Uiso 1 1 calc R . . H6B H 0.3500 0.4735 0.3738 0.024 Uiso 1 1 calc R . . C7 C 0.4729(3) 0.3209(4) 0.36341(16) 0.0131(9) Uani 1 1 d . . . H7 H 0.4698 0.4080 0.3591 0.016 Uiso 1 1 calc R . . C8 C 0.4522(3) 0.2954(4) 0.42463(17) 0.0192(10) Uani 1 1 d . . . H8A H 0.4551 0.2099 0.4317 0.023 Uiso 1 1 calc R . . H8B H 0.3977 0.3215 0.4308 0.023 Uiso 1 1 calc R . . C9 C 0.5092(3) 0.3594(4) 0.46599(18) 0.0233(11) Uani 1 1 d . . . H9A H 0.5026 0.4452 0.4612 0.028 Uiso 1 1 calc R . . H9B H 0.4966 0.3391 0.5053 0.028 Uiso 1 1 calc R . . C10 C 0.5941(3) 0.3261(4) 0.45596(18) 0.0252(11) Uani 1 1 d . . . H10A H 0.6022 0.2419 0.4645 0.030 Uiso 1 1 calc R . . H10B H 0.6298 0.3719 0.4817 0.030 Uiso 1 1 calc R . . C11 C 0.6141(3) 0.3502(4) 0.39469(17) 0.0205(9) Uani 1 1 d . . . H11A H 0.6687 0.3241 0.3888 0.025 Uiso 1 1 calc R . . H11B H 0.6117 0.4358 0.3877 0.025 Uiso 1 1 calc R . . C12 C 0.5583(3) 0.2879(4) 0.35207(18) 0.0168(9) Uani 1 1 d . . . H12A H 0.5652 0.2019 0.3555 0.020 Uiso 1 1 calc R . . H12B H 0.5708 0.3112 0.3131 0.020 Uiso 1 1 calc R . . C13 C 0.3779(3) 0.1080(4) 0.33425(16) 0.0171(9) Uani 1 1 d . . . H13 H 0.3611 0.1137 0.3742 0.021 Uiso 1 1 calc R . . C14 C 0.4517(3) 0.0301(3) 0.33416(17) 0.0208(8) Uani 1 1 d . . . H14A H 0.4921 0.0627 0.3611 0.025 Uiso 1 1 calc R . . H14B H 0.4733 0.0314 0.2959 0.025 Uiso 1 1 calc R . . C15 C 0.4343(3) -0.0981(4) 0.3507(2) 0.0310(11) Uani 1 1 d . . . H15A H 0.4822 -0.1461 0.3467 0.037 Uiso 1 1 calc R . . H15B H 0.4200 -0.1011 0.3908 0.037 Uiso 1 1 calc R . . C16 C 0.3673(3) -0.1491(4) 0.3135(2) 0.0300(12) Uani 1 1 d . . . H16A H 0.3834 -0.1532 0.2738 0.036 Uiso 1 1 calc R . . H16B H 0.3555 -0.2297 0.3262 0.036 Uiso 1 1 calc R . . C17 C 0.2941(3) -0.0732(4) 0.31680(19) 0.0280(10) Uani 1 1 d . . . H17A H 0.2763 -0.0735 0.3561 0.034 Uiso 1 1 calc R . . H17B H 0.2515 -0.1068 0.2920 0.034 Uiso 1 1 calc R . . C18 C 0.3099(3) 0.0533(4) 0.29863(17) 0.0223(9) Uani 1 1 d . . . H18A H 0.2617 0.1007 0.3028 0.027 Uiso 1 1 calc R . . H18B H 0.3228 0.0544 0.2582 0.027 Uiso 1 1 calc R . . C19 C 0.5862(3) 0.3233(4) 0.11745(17) 0.0154(9) Uani 1 1 d . . . H19 H 0.6080 0.2878 0.0828 0.019 Uiso 1 1 calc R . . C20 C 0.5759(3) 0.4546(4) 0.10702(18) 0.0191(10) Uani 1 1 d . . . H20A H 0.5496 0.4903 0.1394 0.023 Uiso 1 1 calc R . . H20B H 0.5416 0.4669 0.0726 0.023 Uiso 1 1 calc R . . C21 C 0.6548(3) 0.5154(4) 0.0995(2) 0.0231(10) Uani 1 1 d . . . H21A H 0.6783 0.4858 0.0647 0.028 Uiso 1 1 calc R . . H21B H 0.6460 0.6008 0.0949 0.028 Uiso 1 1 calc R . . C22 C 0.7121(3) 0.4944(4) 0.1499(2) 0.0246(10) Uani 1 1 d . . . H22A H 0.7633 0.5319 0.1428 0.030 Uiso 1 1 calc R . . H22B H 0.6911 0.5301 0.1844 0.030 Uiso 1 1 calc R . . C23 C 0.7238(3) 0.3642(4) 0.1590(2) 0.0234(10) Uani 1 1 d . . . H23A H 0.7590 0.3513 0.1928 0.028 Uiso 1 1 calc R . . H23B H 0.7494 0.3303 0.1259 0.028 Uiso 1 1 calc R . . C24 C 0.6449(3) 0.3011(4) 0.16710(18) 0.0197(10) Uani 1 1 d . . . H24A H 0.6544 0.2157 0.1708 0.024 Uiso 1 1 calc R . . H24B H 0.6221 0.3289 0.2025 0.024 Uiso 1 1 calc R . . C25 C 0.4213(3) 0.3022(4) 0.07496(16) 0.0143(9) Uani 1 1 d . . . H25 H 0.4184 0.3892 0.0796 0.017 Uiso 1 1 calc R . . C26 C 0.3383(3) 0.2552(4) 0.08441(19) 0.0202(11) Uani 1 1 d . . . H26A H 0.3231 0.2754 0.1232 0.024 Uiso 1 1 calc R . . H26B H 0.3384 0.1686 0.0810 0.024 Uiso 1 1 calc R . . C27 C 0.2778(3) 0.3071(4) 0.04119(19) 0.0256(10) Uani 1 1 d . . . H27A H 0.2258 0.2707 0.0465 0.031 Uiso 1 1 calc R . . H27B H 0.2728 0.3924 0.0479 0.031 Uiso 1 1 calc R . . C28 C 0.3017(3) 0.2865(4) -0.01912(18) 0.0279(11) Uani 1 1 d . . . H28A H 0.2635 0.3256 -0.0457 0.033 Uiso 1 1 calc R . . H28B H 0.3004 0.2013 -0.0273 0.033 Uiso 1 1 calc R . . C29 C 0.3840(3) 0.3337(4) -0.02845(18) 0.0255(11) Uani 1 1 d . . . H29A H 0.3839 0.4201 -0.0242 0.031 Uiso 1 1 calc R . . H29B H 0.3989 0.3152 -0.0675 0.031 Uiso 1 1 calc R . . C30 C 0.4448(3) 0.2804(4) 0.01384(18) 0.0197(10) Uani 1 1 d . . . H30A H 0.4971 0.3157 0.0081 0.024 Uiso 1 1 calc R . . H30B H 0.4488 0.1949 0.0071 0.024 Uiso 1 1 calc R . . C31 C 0.5026(3) 0.0918(4) 0.11456(16) 0.0177(9) Uani 1 1 d . . . H31 H 0.4534 0.0691 0.0926 0.021 Uiso 1 1 calc R . . C32 C 0.5035(3) 0.0166(4) 0.16876(17) 0.0248(9) Uani 1 1 d . . . H32A H 0.5520 0.0336 0.1919 0.030 Uiso 1 1 calc R . . H32B H 0.4578 0.0379 0.1913 0.030 Uiso 1 1 calc R . . C33 C 0.5002(3) -0.1138(4) 0.1552(2) 0.0364(12) Uani 1 1 d . . . H33A H 0.5054 -0.1590 0.1910 0.044 Uiso 1 1 calc R . . H33B H 0.4484 -0.1326 0.1369 0.044 Uiso 1 1 calc R . . C34 C 0.5646(4) -0.1511(4) 0.1166(2) 0.0411(14) Uani 1 1 d . . . H34A H 0.5564 -0.2341 0.1054 0.049 Uiso 1 1 calc R . . H34B H 0.6162 -0.1453 0.1373 0.049 Uiso 1 1 calc R . . C35 C 0.5654(3) -0.0740(4) 0.06290(19) 0.0327(11) Uani 1 1 d . . . H35A H 0.6111 -0.0958 0.0405 0.039 Uiso 1 1 calc R . . H35B H 0.5170 -0.0887 0.0393 0.039 Uiso 1 1 calc R . . C36 C 0.5703(3) 0.0557(4) 0.07768(17) 0.0243(9) Uani 1 1 d . . . H36A H 0.5683 0.1027 0.0424 0.029 Uiso 1 1 calc R . . H36B H 0.6211 0.0719 0.0982 0.029 Uiso 1 1 calc R . . C37 C 0.7679(3) 0.3233(5) -0.0130(2) 0.0292(11) Uani 1 1 d . . . C38 C 0.7085(4) 0.3714(5) -0.0472(2) 0.0367(15) Uani 1 1 d . . . H38 H 0.7093 0.4530 -0.0555 0.044 Uiso 1 1 calc R . . C39 C 0.6478(4) 0.3028(5) -0.0696(2) 0.0396(15) Uani 1 1 d . . . H39 H 0.6074 0.3372 -0.0930 0.047 Uiso 1 1 calc R . . C40 C 0.6459(4) 0.1845(5) -0.0579(2) 0.0397(15) Uani 1 1 d . . . H40 H 0.6038 0.1373 -0.0727 0.048 Uiso 1 1 calc R . . C41 C 0.7051(4) 0.1354(5) -0.0247(3) 0.0385(15) Uani 1 1 d . . . H41 H 0.7046 0.0534 -0.0174 0.046 Uiso 1 1 calc R . . C42 C 0.7652(3) 0.2035(5) -0.0016(2) 0.0332(13) Uani 1 1 d . . . H42 H 0.8051 0.1685 0.0221 0.040 Uiso 1 1 calc R . . C43 C 0.8323(3) 0.3973(5) 0.0120(2) 0.0518(16) Uani 1 1 d . . . H43A H 0.8565 0.4422 -0.0180 0.078 Uiso 1 1 calc R . . H43B H 0.8721 0.3470 0.0309 0.078 Uiso 1 1 calc R . . H43C H 0.8109 0.4514 0.0396 0.078 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01426(6) 0.01197(6) 0.01041(6) 0.00014(6) 0.00026(4) 0.00054(8) I1 0.0348(2) 0.02050(16) 0.02576(15) -0.00124(11) -0.00369(13) -0.00698(13) I2 0.0447(2) 0.02682(16) 0.02575(15) 0.00262(12) -0.00424(13) 0.01698(16) Cd1 0.02504(14) 0.01270(12) 0.01678(12) 0.00024(13) 0.00157(9) 0.00120(17) P1 0.0115(8) 0.0159(6) 0.0123(6) 0.0000(3) -0.0004(5) -0.0014(4) P2 0.0143(8) 0.0142(6) 0.0116(6) -0.0004(3) 0.0014(5) 0.0019(4) C1 0.013(3) 0.020(2) 0.016(2) -0.0017(15) 0.0004(17) -0.0010(17) C2 0.017(2) 0.020(2) 0.021(2) -0.0012(15) -0.0064(17) 0.0062(18) C3 0.016(3) 0.033(3) 0.027(2) -0.0024(18) -0.0046(18) 0.003(2) C4 0.023(3) 0.025(3) 0.032(2) -0.0033(18) 0.0010(19) 0.012(2) C5 0.023(3) 0.019(2) 0.023(2) -0.0009(16) 0.0065(19) 0.0035(19) C6 0.026(3) 0.014(2) 0.019(2) -0.0032(15) 0.0013(19) 0.0004(19) C7 0.014(3) 0.014(2) 0.0112(19) -0.0003(14) -0.0012(16) -0.0023(17) C8 0.015(3) 0.030(3) 0.013(2) 0.0022(17) -0.0010(17) -0.001(2) C9 0.027(3) 0.030(3) 0.013(2) -0.0006(15) -0.0035(18) -0.005(2) C10 0.021(3) 0.029(3) 0.025(2) 0.0038(17) -0.0094(18) -0.009(2) C11 0.013(2) 0.026(2) 0.022(2) 0.0054(16) -0.0032(16) -0.0045(18) C12 0.011(2) 0.021(2) 0.019(2) 0.0033(15) 0.0030(16) -0.0028(18) C13 0.018(3) 0.020(2) 0.0132(19) 0.0011(15) 0.0005(16) -0.0031(17) C14 0.020(2) 0.016(2) 0.026(2) 0.0030(15) -0.0021(17) -0.0023(17) C15 0.035(3) 0.017(2) 0.040(3) 0.0065(17) -0.007(2) -0.005(2) C16 0.032(3) 0.016(2) 0.041(3) -0.0020(18) -0.003(2) -0.006(2) C17 0.024(3) 0.026(2) 0.033(2) -0.0016(18) 0.0011(19) -0.012(2) C18 0.019(2) 0.022(2) 0.026(2) -0.0014(15) -0.0011(17) -0.0055(17) C19 0.016(3) 0.015(2) 0.015(2) 0.0007(14) 0.0014(16) 0.0020(17) C20 0.016(3) 0.025(2) 0.017(2) 0.0040(16) 0.0000(17) -0.0028(19) C21 0.022(3) 0.021(2) 0.027(2) 0.0013(16) 0.0051(19) 0.0013(19) C22 0.019(3) 0.022(2) 0.033(2) -0.0024(17) 0.0000(19) -0.0028(19) C23 0.018(3) 0.027(3) 0.025(2) 0.0044(16) -0.0004(18) 0.0024(19) C24 0.019(3) 0.021(2) 0.019(2) 0.0039(15) 0.0010(18) 0.0028(18) C25 0.012(3) 0.014(2) 0.017(2) 0.0027(14) -0.0038(16) 0.0010(17) C26 0.020(3) 0.022(2) 0.020(2) 0.0031(15) 0.0037(18) 0.0021(18) C27 0.018(3) 0.026(3) 0.032(3) -0.0005(18) -0.0072(19) -0.004(2) C28 0.025(3) 0.034(3) 0.024(2) 0.0047(18) -0.0106(19) -0.001(2) C29 0.031(3) 0.030(3) 0.014(2) 0.0036(17) -0.0020(19) 0.001(2) C30 0.023(3) 0.023(2) 0.014(2) 0.0016(16) -0.0001(18) 0.002(2) C31 0.020(3) 0.017(2) 0.017(2) -0.0032(15) 0.0010(16) 0.0048(18) C32 0.030(3) 0.021(2) 0.024(2) 0.0024(15) 0.0030(18) 0.0057(19) C33 0.050(4) 0.020(2) 0.038(3) 0.0058(18) -0.003(2) 0.005(2) C34 0.055(4) 0.023(3) 0.044(3) -0.010(2) -0.013(3) 0.016(3) C35 0.032(3) 0.028(3) 0.038(3) -0.0125(19) -0.002(2) 0.011(2) C36 0.023(2) 0.028(2) 0.022(2) -0.0107(16) 0.0002(17) 0.0063(19) C37 0.021(3) 0.045(3) 0.023(2) -0.0053(19) 0.0087(19) 0.010(2) C38 0.047(4) 0.037(3) 0.026(3) 0.007(2) 0.007(2) 0.015(3) C39 0.033(4) 0.061(4) 0.024(3) 0.005(2) -0.002(2) 0.020(3) C40 0.028(4) 0.063(4) 0.029(3) -0.012(2) 0.011(2) -0.005(3) C41 0.048(4) 0.034(3) 0.034(3) 0.007(2) 0.017(3) 0.008(3) C42 0.027(3) 0.055(3) 0.018(2) 0.009(2) 0.006(2) 0.019(3) C43 0.038(4) 0.077(4) 0.041(3) -0.023(3) 0.014(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.2799(13) . ? Pt1 P2 2.2920(13) . ? Pt1 Cd1 2.5867(6) . ? I1 Cd1 2.6974(8) . ? I2 Cd1 2.6997(8) . ? P1 C7 1.863(5) . ? P1 C1 1.871(5) . ? P1 C13 1.874(4) . ? P2 C25 1.839(5) . ? P2 C31 1.848(4) . ? P2 C19 1.853(5) . ? C1 C6 1.529(6) . ? C1 C2 1.543(6) . ? C2 C3 1.526(6) . ? C3 C4 1.514(6) . ? C4 C5 1.506(7) . ? C5 C6 1.547(7) . ? C7 C8 1.532(5) . ? C7 C12 1.536(6) . ? C8 C9 1.533(7) . ? C9 C10 1.522(7) . ? C10 C11 1.527(6) . ? C11 C12 1.530(6) . ? C13 C18 1.536(6) . ? C13 C14 1.537(6) . ? C14 C15 1.544(5) . ? C15 C16 1.525(7) . ? C16 C17 1.521(7) . ? C17 C18 1.531(6) . ? C19 C20 1.526(6) . ? C19 C24 1.531(6) . ? C20 C21 1.528(7) . ? C21 C22 1.526(7) . ? C22 C23 1.512(6) . ? C23 C24 1.541(7) . ? C25 C26 1.535(7) . ? C25 C30 1.536(6) . ? C26 C27 1.539(7) . ? C27 C28 1.518(6) . ? C28 C29 1.524(7) . ? C29 C30 1.534(7) . ? C31 C36 1.531(6) . ? C31 C32 1.541(5) . ? C32 C33 1.521(6) . ? C33 C34 1.516(7) . ? C34 C35 1.545(7) . ? C35 C36 1.520(6) . ? C37 C38 1.382(8) . ? C37 C42 1.393(8) . ? C37 C43 1.486(8) . ? C38 C39 1.383(8) . ? C39 C40 1.377(8) . ? C40 C41 1.370(9) . ? C41 C42 1.379(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 P1 Pt1 P2 176.92(3) . . ? P1 Pt1 Cd1 91.46(3) . . ? P2 Pt1 Cd1 91.62(3) . . ? Pt1 Cd1 I1 122.176(19) . . ? Pt1 Cd1 I2 117.531(19) . . ? I1 Cd1 I2 120.21(2) . . ? C7 P1 C1 105.4(2) . . ? C7 P1 C13 105.8(2) . . ? C1 P1 C13 104.1(2) . . ? C7 P1 Pt1 113.15(14) . . ? C1 P1 Pt1 115.76(14) . . ? C13 P1 Pt1 111.80(13) . . ? C25 P2 C31 103.9(2) . . ? C25 P2 C19 106.0(2) . . ? C31 P2 C19 108.1(2) . . ? C25 P2 Pt1 114.28(15) . . ? C31 P2 Pt1 106.33(13) . . ? C19 P2 Pt1 117.25(14) . . ? C6 C1 C2 110.1(4) . . ? C6 C1 P1 113.4(3) . . ? C2 C1 P1 110.6(3) . . ? C3 C2 C1 111.5(3) . . ? C4 C3 C2 111.7(4) . . ? C5 C4 C3 110.4(4) . . ? C4 C5 C6 112.4(4) . . ? C1 C6 C5 112.6(4) . . ? C8 C7 C12 112.0(4) . . ? C8 C7 P1 113.8(3) . . ? C12 C7 P1 113.0(3) . . ? C7 C8 C9 110.4(4) . . ? C10 C9 C8 111.2(4) . . ? C9 C10 C11 110.7(4) . . ? C10 C11 C12 112.7(4) . . ? C11 C12 C7 109.7(4) . . ? C18 C13 C14 111.2(3) . . ? C18 C13 P1 111.5(3) . . ? C14 C13 P1 110.7(3) . . ? C13 C14 C15 112.4(4) . . ? C16 C15 C14 111.2(4) . . ? C17 C16 C15 110.3(4) . . ? C16 C17 C18 111.6(4) . . ? C17 C18 C13 111.4(3) . . ? C20 C19 C24 110.7(4) . . ? C20 C19 P2 112.2(3) . . ? C24 C19 P2 109.9(3) . . ? C19 C20 C21 111.6(4) . . ? C22 C21 C20 112.0(4) . . ? C23 C22 C21 109.9(4) . . ? C22 C23 C24 111.5(4) . . ? C19 C24 C23 111.8(4) . . ? C26 C25 C30 111.0(4) . . ? C26 C25 P2 110.9(3) . . ? C30 C25 P2 115.6(3) . . ? C25 C26 C27 111.3(4) . . ? C28 C27 C26 111.5(4) . . ? C27 C28 C29 111.4(4) . . ? C28 C29 C30 111.3(4) . . ? C29 C30 C25 110.7(4) . . ? C36 C31 C32 110.0(4) . . ? C36 C31 P2 117.6(3) . . ? C32 C31 P2 111.6(3) . . ? C33 C32 C31 111.7(3) . . ? C34 C33 C32 112.3(4) . . ? C33 C34 C35 111.5(4) . . ? C36 C35 C34 111.5(4) . . ? C35 C36 C31 110.9(4) . . ? C38 C37 C42 118.3(5) . . ? C38 C37 C43 121.1(5) . . ? C42 C37 C43 120.6(5) . . ? C37 C38 C39 121.0(5) . . ? C40 C39 C38 120.1(5) . . ? C41 C40 C39 119.5(6) . . ? C40 C41 C42 120.8(5) . . ? C41 C42 C37 120.3(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.935 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.085 data_compound3 _database_code_depnum_ccdc_archive 'CCDC 905520' #TrackingRef 'CCDC905520.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H66 Hg I2 P2 Pt' _chemical_formula_weight 1210.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.4975(5) _cell_length_b 13.4310(3) _cell_length_c 23.4845(8) _cell_angle_alpha 90.00 _cell_angle_beta 107.180(3) _cell_angle_gamma 90.00 _cell_volume 4067.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.976 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 8.825 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.352 _exptl_absorpt_correction_T_max 0.472 _exptl_absorpt_process_details 'SCALE3 ABSPACK' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini Ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26184 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7991 _reflns_number_gt 6970 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One cyclohexyl group in the asymmetric unit was found to be disordered over two sites. This disorder was successfully modelled with the carbon atoms of both sets refined anisotropically. The C-C distances within both disordered sets were fixed at 1.52 ang. using the DFIX command of Shelxl. The iodine atom, I2, was also found to be disordered over two sites. This disorder was successfully modelled. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0140P)^2^+7.7957P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7991 _refine_ls_number_parameters 425 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0481 _refine_ls_wR_factor_gt 0.0450 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.371361(13) 0.794543(11) 0.355621(8) 0.02456(5) Uani 1 1 d . . . Pt1 Pt 0.285520(11) 0.641502(10) 0.382008(7) 0.01313(4) Uani 1 1 d . A . I1 I 0.19880(2) 0.479743(18) 0.411417(14) 0.02621(7) Uani 1 1 d . . . I2 I 0.44031(13) 0.96134(12) 0.31779(7) 0.0553(4) Uani 0.50 1 d P A 1 I2A I 0.47709(12) 0.95164(12) 0.34136(5) 0.0365(3) Uani 0.50 1 d P A 2 P1 P 0.39518(8) 0.55102(7) 0.34110(4) 0.0136(2) Uani 1 1 d . . . P2 P 0.16517(8) 0.74893(7) 0.40388(5) 0.0146(2) Uani 1 1 d . . . C1 C 0.3375(3) 0.5445(3) 0.25936(17) 0.0150(8) Uani 1 1 d . A . H1 H 0.3892 0.5109 0.2429 0.018 Uiso 1 1 calc R . . C2 C 0.2387(3) 0.4809(3) 0.24180(19) 0.0223(9) Uani 1 1 d . . . H2A H 0.2535 0.4149 0.2612 0.027 Uiso 1 1 calc R A . H2B H 0.1845 0.5135 0.2559 0.027 Uiso 1 1 calc R . . C3 C 0.1990(3) 0.4673(3) 0.1742(2) 0.0281(10) Uani 1 1 d . A . H3A H 0.2515 0.4309 0.1605 0.034 Uiso 1 1 calc R . . H3B H 0.1348 0.4269 0.1639 0.034 Uiso 1 1 calc R . . C4 C 0.1768(3) 0.5670(3) 0.1421(2) 0.0277(10) Uani 1 1 d . . . H4A H 0.1182 0.6000 0.1519 0.033 Uiso 1 1 calc R A . H4B H 0.1564 0.5560 0.0985 0.033 Uiso 1 1 calc R . . C5 C 0.2719(3) 0.6341(3) 0.16043(19) 0.0239(9) Uani 1 1 d . A . H5A H 0.2539 0.7004 0.1418 0.029 Uiso 1 1 calc R . . H5B H 0.3272 0.6054 0.1457 0.029 Uiso 1 1 calc R . . C6 C 0.3124(3) 0.6462(3) 0.22805(18) 0.0217(9) Uani 1 1 d . . . H6A H 0.2595 0.6807 0.2424 0.026 Uiso 1 1 calc R A . H6B H 0.3757 0.6879 0.2384 0.026 Uiso 1 1 calc R . . C7 C 0.4139(3) 0.4182(3) 0.36251(17) 0.0180(9) Uani 1 1 d . A . H7 H 0.3429 0.3927 0.3596 0.022 Uiso 1 1 calc R . . C8 C 0.4550(3) 0.3485(3) 0.32269(18) 0.0197(9) Uani 1 1 d . . . H8A H 0.4138 0.3575 0.2805 0.024 Uiso 1 1 calc R A . H8B H 0.5281 0.3652 0.3265 0.024 Uiso 1 1 calc R . . C9 C 0.4476(3) 0.2411(3) 0.34120(18) 0.0226(9) Uani 1 1 d . A . H9A H 0.4758 0.1968 0.3161 0.027 Uiso 1 1 calc R . . H9B H 0.3739 0.2235 0.3346 0.027 Uiso 1 1 calc R . . C10 C 0.5075(4) 0.2250(3) 0.40662(19) 0.0242(10) Uani 1 1 d . . . H10A H 0.4973 0.1556 0.4179 0.029 Uiso 1 1 calc R A . H10B H 0.5824 0.2348 0.4121 0.029 Uiso 1 1 calc R . . C11 C 0.4724(4) 0.2960(3) 0.44713(19) 0.0281(10) Uani 1 1 d . A . H11A H 0.5176 0.2879 0.4886 0.034 Uiso 1 1 calc R . . H11B H 0.4006 0.2794 0.4463 0.034 Uiso 1 1 calc R . . C12 C 0.4765(4) 0.4038(3) 0.42788(18) 0.0240(10) Uani 1 1 d . . . H12A H 0.5495 0.4232 0.4334 0.029 Uiso 1 1 calc R A . H12B H 0.4483 0.4477 0.4533 0.029 Uiso 1 1 calc R . . C13 C 0.5288(3) 0.5971(3) 0.35334(17) 0.0254(11) Uani 0.515(6) 1 d PD A 1 H13 H 0.5680 0.5340 0.3531 0.030 Uiso 0.515(6) 1 calc PR A 1 C14 C 0.5811(3) 0.6374(3) 0.41550(18) 0.0273(11) Uani 0.515(6) 1 d PD A 1 H14A H 0.5521 0.7042 0.4186 0.033 Uiso 0.515(6) 1 calc PR A 1 H14B H 0.5620 0.5938 0.4446 0.033 Uiso 0.515(6) 1 calc PR A 1 C15 C 0.6971(5) 0.6461(7) 0.4338(4) 0.027(2) Uani 0.515(6) 1 d PD A 1 H15A H 0.7299 0.5804 0.4329 0.032 Uiso 0.515(6) 1 calc PR A 1 H15B H 0.7240 0.6748 0.4742 0.032 Uiso 0.515(6) 1 calc PR A 1 C15' C 0.6762(7) 0.7015(9) 0.4132(6) 0.043(4) Uani 0.485(6) 1 d PD A 2 H15C H 0.6499 0.7652 0.3934 0.052 Uiso 0.485(6) 1 calc PR A 2 H15D H 0.7170 0.7172 0.4547 0.052 Uiso 0.485(6) 1 calc PR A 2 C16 C 0.7162(8) 0.7156(7) 0.3871(3) 0.028(2) Uani 0.515(6) 1 d PD A 1 H16A H 0.7917 0.7269 0.3957 0.034 Uiso 0.515(6) 1 calc PR A 1 H16B H 0.6830 0.7807 0.3893 0.034 Uiso 0.515(6) 1 calc PR A 1 C16' C 0.7493(7) 0.6565(9) 0.3819(4) 0.036(3) Uani 0.485(6) 1 d PD A 2 H16C H 0.7885 0.6012 0.4063 0.043 Uiso 0.485(6) 1 calc PR A 2 H16D H 0.7997 0.7076 0.3781 0.043 Uiso 0.485(6) 1 calc PR A 2 C17 C 0.6731(5) 0.6735(7) 0.3242(4) 0.023(2) Uani 0.515(6) 1 d PD A 1 H17A H 0.6884 0.7202 0.2953 0.028 Uiso 0.515(6) 1 calc PR A 1 H17B H 0.7079 0.6095 0.3216 0.028 Uiso 0.515(6) 1 calc PR A 1 C17' C 0.6911(7) 0.6174(8) 0.3202(4) 0.032(3) Uani 0.485(6) 1 d PD A 2 H17C H 0.7393 0.5790 0.3040 0.038 Uiso 0.485(6) 1 calc PR A 2 H17D H 0.6644 0.6742 0.2932 0.038 Uiso 0.485(6) 1 calc PR A 2 C18 C 0.5567(5) 0.6569(5) 0.3081(3) 0.0139(17) Uani 0.515(6) 1 d PD A 1 H18A H 0.5211 0.7221 0.3041 0.017 Uiso 0.515(6) 1 calc PR A 1 H18B H 0.5327 0.6225 0.2691 0.017 Uiso 0.515(6) 1 calc PR A 1 C18' C 0.6009(6) 0.5509(6) 0.3227(4) 0.028(2) Uani 0.485(6) 1 d PD A 2 H18C H 0.5605 0.5331 0.2814 0.033 Uiso 0.485(6) 1 calc PR A 2 H18D H 0.6292 0.4884 0.3436 0.033 Uiso 0.485(6) 1 calc PR A 2 C19 C 0.2066(3) 0.8811(3) 0.42216(18) 0.0178(9) Uani 1 1 d . A . H19 H 0.2343 0.9023 0.3890 0.021 Uiso 1 1 calc R . . C20 C 0.2980(4) 0.8929(3) 0.4780(2) 0.0287(10) Uani 1 1 d . . . H20A H 0.3527 0.8444 0.4770 0.034 Uiso 1 1 calc R A . H20B H 0.2753 0.8783 0.5136 0.034 Uiso 1 1 calc R . . C21 C 0.3421(4) 0.9983(3) 0.4827(2) 0.0379(12) Uani 1 1 d . A . H21A H 0.3986 1.0052 0.5206 0.046 Uiso 1 1 calc R . . H21B H 0.3719 1.0102 0.4495 0.046 Uiso 1 1 calc R . . C22 C 0.2581(5) 1.0756(3) 0.4805(3) 0.0451(14) Uani 1 1 d . . . H22A H 0.2341 1.0684 0.5163 0.054 Uiso 1 1 calc R A . H22B H 0.2876 1.1432 0.4811 0.054 Uiso 1 1 calc R . . C23 C 0.1673(4) 1.0637(3) 0.4254(3) 0.0394(13) Uani 1 1 d . A . H23A H 0.1900 1.0770 0.3897 0.047 Uiso 1 1 calc R . . H23B H 0.1132 1.1130 0.4262 0.047 Uiso 1 1 calc R . . C24 C 0.1211(4) 0.9580(3) 0.4212(2) 0.0333(11) Uani 1 1 d . . . H24A H 0.0635 0.9511 0.3838 0.040 Uiso 1 1 calc R A . H24B H 0.0933 0.9460 0.4551 0.040 Uiso 1 1 calc R . . C25 C 0.1091(3) 0.7019(3) 0.46129(17) 0.0151(8) Uani 1 1 d . A . H25 H 0.0788 0.6357 0.4459 0.018 Uiso 1 1 calc R . . C26 C 0.1910(3) 0.6781(3) 0.52068(18) 0.0227(9) Uani 1 1 d . . . H26A H 0.2487 0.6403 0.5130 0.027 Uiso 1 1 calc R A . H26B H 0.2196 0.7410 0.5410 0.027 Uiso 1 1 calc R . . C27 C 0.1434(4) 0.6174(3) 0.5606(2) 0.0289(10) Uani 1 1 d . A . H27A H 0.1218 0.5517 0.5420 0.035 Uiso 1 1 calc R . . H27B H 0.1964 0.6060 0.5995 0.035 Uiso 1 1 calc R . . C28 C 0.0504(4) 0.6692(3) 0.5709(2) 0.0288(10) Uani 1 1 d . . . H28A H 0.0737 0.7304 0.5947 0.035 Uiso 1 1 calc R A . H28B H 0.0182 0.6249 0.5941 0.035 Uiso 1 1 calc R . . C29 C -0.0295(3) 0.6966(3) 0.5126(2) 0.0252(10) Uani 1 1 d . A . H29A H -0.0866 0.7343 0.5210 0.030 Uiso 1 1 calc R . . H29B H -0.0591 0.6350 0.4910 0.030 Uiso 1 1 calc R . . C30 C 0.0188(3) 0.7593(3) 0.47351(19) 0.0215(9) Uani 1 1 d . . . H30A H 0.0445 0.8229 0.4938 0.026 Uiso 1 1 calc R A . H30B H -0.0343 0.7749 0.4353 0.026 Uiso 1 1 calc R . . C31 C 0.0532(3) 0.7635(3) 0.33616(18) 0.0202(9) Uani 1 1 d . A . H31 H 0.0017 0.8074 0.3469 0.024 Uiso 1 1 calc R . . C32 C -0.0021(4) 0.6656(3) 0.3126(2) 0.0304(11) Uani 1 1 d . . . H32A H 0.0472 0.6198 0.3020 0.037 Uiso 1 1 calc R A . H32B H -0.0258 0.6337 0.3443 0.037 Uiso 1 1 calc R . . C33 C -0.0948(4) 0.6833(4) 0.2581(2) 0.0387(12) Uani 1 1 d . A . H33A H -0.1474 0.7233 0.2697 0.046 Uiso 1 1 calc R . . H33B H -0.1267 0.6186 0.2426 0.046 Uiso 1 1 calc R . . C34 C -0.0634(4) 0.7377(4) 0.2089(2) 0.0436(14) Uani 1 1 d . . . H34A H -0.0180 0.6940 0.1935 0.052 Uiso 1 1 calc R A . H34B H -0.1261 0.7527 0.1755 0.052 Uiso 1 1 calc R . . C35 C -0.0070(4) 0.8332(4) 0.2317(2) 0.0354(12) Uani 1 1 d . A . H35A H -0.0555 0.8802 0.2420 0.043 Uiso 1 1 calc R . . H35B H 0.0170 0.8639 0.1998 0.043 Uiso 1 1 calc R . . C36 C 0.0856(3) 0.8162(4) 0.28620(18) 0.0279(10) Uani 1 1 d . . . H36A H 0.1180 0.8811 0.3010 0.034 Uiso 1 1 calc R A . H36B H 0.1378 0.7752 0.2749 0.034 Uiso 1 1 calc R . . C14' C 0.5811(3) 0.6374(3) 0.41550(18) 0.0273(11) Uani 0.48 1 d PD A 2 H14C H 0.6042 0.5816 0.4439 0.033 Uiso 0.485(6) 1 calc PR A 2 H14D H 0.5316 0.6787 0.4291 0.033 Uiso 0.485(6) 1 calc PR A 2 C13' C 0.5288(3) 0.5971(3) 0.35334(17) 0.0254(11) Uani 0.48 1 d PD A 2 H13' H 0.5134 0.6613 0.3309 0.030 Uiso 0.485(6) 1 calc PR A 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 Hg1 0.02785(10) 0.01451(8) 0.03964(11) -0.00154(7) 0.02283(8) -0.00231(6) Pt1 0.01194(8) 0.01279(8) 0.01566(8) 0.00003(6) 0.00560(6) 0.00083(5) I1 0.02828(17) 0.01594(13) 0.04288(18) 0.00050(12) 0.02360(14) -0.00140(11) I2 0.0932(13) 0.0183(4) 0.0822(11) 0.0000(7) 0.0690(9) -0.0114(7) I2A 0.0564(8) 0.0210(5) 0.0415(7) -0.0016(5) 0.0292(5) -0.0163(5) P1 0.0131(5) 0.0140(5) 0.0141(5) -0.0001(4) 0.0046(4) 0.0015(4) P2 0.0125(5) 0.0176(5) 0.0137(5) -0.0002(4) 0.0038(4) 0.0024(4) C1 0.015(2) 0.0177(19) 0.012(2) 0.0012(16) 0.0030(16) 0.0007(15) C2 0.017(2) 0.029(2) 0.021(2) 0.0035(18) 0.0050(18) -0.0048(17) C3 0.021(2) 0.035(3) 0.024(2) -0.002(2) 0.000(2) -0.0099(19) C4 0.020(2) 0.042(3) 0.019(2) 0.006(2) 0.0020(19) 0.0042(19) C5 0.025(2) 0.027(2) 0.019(2) 0.0078(18) 0.0061(19) 0.0048(18) C6 0.025(2) 0.020(2) 0.018(2) 0.0024(17) 0.0039(18) 0.0030(17) C7 0.021(2) 0.016(2) 0.017(2) 0.0027(16) 0.0060(18) 0.0034(16) C8 0.024(2) 0.017(2) 0.019(2) 0.0003(17) 0.0089(18) 0.0060(16) C9 0.033(3) 0.015(2) 0.021(2) -0.0027(17) 0.008(2) 0.0035(17) C10 0.037(3) 0.014(2) 0.022(2) 0.0029(17) 0.009(2) 0.0072(18) C11 0.046(3) 0.024(2) 0.015(2) 0.0055(18) 0.010(2) 0.008(2) C12 0.036(3) 0.020(2) 0.015(2) -0.0012(17) 0.006(2) 0.0106(18) C13 0.015(2) 0.037(3) 0.025(2) -0.013(2) 0.0067(19) -0.0039(18) C14 0.024(3) 0.029(2) 0.024(2) -0.0078(19) 0.000(2) -0.0017(18) C15 0.022(5) 0.027(5) 0.025(5) 0.010(4) -0.004(4) 0.004(4) C15' 0.012(6) 0.065(9) 0.052(9) -0.041(8) 0.008(6) -0.010(6) C16 0.011(5) 0.027(5) 0.034(6) 0.003(5) -0.012(4) -0.008(4) C16' 0.024(6) 0.041(7) 0.035(6) -0.002(5) -0.002(5) -0.012(5) C17 0.015(5) 0.025(5) 0.030(5) 0.008(4) 0.010(4) -0.001(4) C17' 0.020(6) 0.045(7) 0.033(6) -0.006(6) 0.010(5) -0.007(5) C18 0.015(4) 0.016(4) 0.013(4) -0.002(3) 0.007(3) 0.001(3) C18' 0.020(5) 0.035(5) 0.028(5) -0.012(4) 0.007(4) -0.001(4) C19 0.022(2) 0.0118(19) 0.023(2) -0.0030(16) 0.0117(18) 0.0017(15) C20 0.038(3) 0.017(2) 0.025(2) 0.0005(18) 0.001(2) -0.0029(19) C21 0.045(3) 0.025(2) 0.037(3) -0.004(2) 0.001(2) -0.014(2) C22 0.073(4) 0.020(2) 0.049(3) -0.009(2) 0.028(3) -0.009(2) C23 0.048(3) 0.017(2) 0.058(4) 0.002(2) 0.023(3) 0.007(2) C24 0.039(3) 0.020(2) 0.046(3) -0.001(2) 0.020(3) 0.0077(19) C25 0.013(2) 0.019(2) 0.013(2) -0.0048(16) 0.0035(16) -0.0034(15) C26 0.018(2) 0.031(2) 0.019(2) 0.0022(18) 0.0037(18) -0.0016(17) C27 0.029(3) 0.036(3) 0.020(2) 0.004(2) 0.003(2) -0.005(2) C28 0.033(3) 0.035(3) 0.023(2) -0.006(2) 0.015(2) -0.014(2) C29 0.018(2) 0.032(2) 0.029(3) -0.006(2) 0.011(2) -0.0059(18) C30 0.018(2) 0.026(2) 0.022(2) -0.0065(18) 0.0081(19) 0.0003(17) C31 0.014(2) 0.032(2) 0.013(2) -0.0012(17) 0.0027(17) 0.0050(17) C32 0.026(3) 0.036(3) 0.025(3) -0.006(2) 0.001(2) 0.000(2) C33 0.027(3) 0.051(3) 0.029(3) -0.009(2) -0.005(2) 0.002(2) C34 0.029(3) 0.078(4) 0.017(3) -0.006(2) -0.003(2) 0.016(3) C35 0.025(3) 0.062(3) 0.017(2) 0.008(2) 0.003(2) 0.010(2) C36 0.022(2) 0.049(3) 0.013(2) 0.006(2) 0.0061(19) 0.009(2) C14' 0.024(3) 0.029(2) 0.024(2) -0.0078(19) 0.000(2) -0.0017(18) C13' 0.015(2) 0.037(3) 0.025(2) -0.013(2) 0.0067(19) -0.0039(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Hg1 Pt1 2.5250(2) . ? Hg1 I2A 2.6236(16) . ? Hg1 I2 2.6764(16) . ? Pt1 P1 2.3304(10) . ? Pt1 P2 2.3403(10) . ? Pt1 I1 2.6542(3) . ? P1 C13 1.847(4) . ? P1 C1 1.848(4) . ? P1 C7 1.851(4) . ? P2 C25 1.842(4) . ? P2 C31 1.853(4) . ? P2 C19 1.872(4) . ? C1 C2 1.535(5) . ? C1 C6 1.541(5) . ? C2 C3 1.529(6) . ? C3 C4 1.522(6) . ? C4 C5 1.523(6) . ? C5 C6 1.528(6) . ? C7 C12 1.530(5) . ? C7 C8 1.537(5) . ? C8 C9 1.518(5) . ? C9 C10 1.526(6) . ? C10 C11 1.519(6) . ? C11 C12 1.523(6) . ? C13 C18 1.467(6) . ? C13 C14 1.521(4) . ? C14 C15 1.501(6) . ? C15 C16 1.519(7) . ? C15' C16' 1.520(7) . ? C16 C17 1.527(7) . ? C16' C17' 1.522(7) . ? C17 C18 1.520(7) . ? C17' C18' 1.525(7) . ? C19 C20 1.520(6) . ? C19 C24 1.543(5) . ? C20 C21 1.528(6) . ? C21 C22 1.527(7) . ? C22 C23 1.506(8) . ? C23 C24 1.542(6) . ? C25 C26 1.536(5) . ? C25 C30 1.540(5) . ? C26 C27 1.521(6) . ? C27 C28 1.516(6) . ? C28 C29 1.517(6) . ? C29 C30 1.527(6) . ? C31 C32 1.532(6) . ? C31 C36 1.541(6) . ? C32 C33 1.523(6) . ? C33 C34 1.529(7) . ? C34 C35 1.506(7) . ? C35 C36 1.519(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Pt1 Hg1 I2A 172.91(3) . . ? Pt1 Hg1 I2 173.05(3) . . ? I2A Hg1 I2 13.79(4) . . ? P1 Pt1 P2 168.10(4) . . ? P1 Pt1 Hg1 85.99(2) . . ? P2 Pt1 Hg1 87.17(3) . . ? P1 Pt1 I1 93.61(2) . . ? P2 Pt1 I1 93.41(3) . . ? Hg1 Pt1 I1 178.850(11) . . ? C13 P1 C1 105.65(17) . . ? C13 P1 C7 103.43(19) . . ? C1 P1 C7 102.61(17) . . ? C13 P1 Pt1 118.09(13) . . ? C1 P1 Pt1 109.21(13) . . ? C7 P1 Pt1 116.30(13) . . ? C25 P2 C31 104.90(18) . . ? C25 P2 C19 108.48(17) . . ? C31 P2 C19 102.08(19) . . ? C25 P2 Pt1 114.27(12) . . ? C31 P2 Pt1 108.66(13) . . ? C19 P2 Pt1 117.08(13) . . ? C2 C1 C6 108.3(3) . . ? C2 C1 P1 111.8(3) . . ? C6 C1 P1 114.8(3) . . ? C3 C2 C1 110.8(3) . . ? C4 C3 C2 111.5(4) . . ? C3 C4 C5 110.8(4) . . ? C4 C5 C6 111.6(3) . . ? C5 C6 C1 111.3(3) . . ? C12 C7 C8 110.0(3) . . ? C12 C7 P1 112.6(3) . . ? C8 C7 P1 117.8(3) . . ? C9 C8 C7 109.7(3) . . ? C8 C9 C10 111.3(3) . . ? C11 C10 C9 111.8(3) . . ? C10 C11 C12 111.5(3) . . ? C11 C12 C7 111.1(3) . . ? C18 C13 C14 110.8(4) . . ? C18 C13 P1 121.2(4) . . ? C14 C13 P1 115.1(3) . . ? C15 C14 C13 116.8(5) . . ? C14 C15 C16 103.1(6) . . ? C15 C16 C17 111.9(7) . . ? C15' C16' C17' 111.8(9) . . ? C18 C17 C16 111.4(7) . . ? C16' C17' C18' 111.1(8) . . ? C13 C18 C17 111.6(5) . . ? C20 C19 C24 110.9(4) . . ? C20 C19 P2 114.1(3) . . ? C24 C19 P2 117.4(3) . . ? C19 C20 C21 111.0(4) . . ? C22 C21 C20 111.0(4) . . ? C23 C22 C21 111.4(4) . . ? C22 C23 C24 111.4(4) . . ? C23 C24 C19 109.2(4) . . ? C26 C25 C30 109.4(3) . . ? C26 C25 P2 113.2(3) . . ? C30 C25 P2 118.9(3) . . ? C27 C26 C25 110.4(3) . . ? C28 C27 C26 111.9(4) . . ? C27 C28 C29 111.6(4) . . ? C28 C29 C30 111.2(3) . . ? C29 C30 C25 109.7(3) . . ? C32 C31 C36 109.7(4) . . ? C32 C31 P2 113.9(3) . . ? C36 C31 P2 111.0(3) . . ? C33 C32 C31 111.2(4) . . ? C32 C33 C34 111.6(4) . . ? C35 C34 C33 111.2(4) . . ? C34 C35 C36 112.0(4) . . ? C35 C36 C31 111.2(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.464 _refine_diff_density_min -1.803 _refine_diff_density_rms 0.120