# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Chen-Yu Yeh' _publ_contact_author_address ; Department of Chemistry National Chung Hsing University Taichung 402 TAIWAN ; _publ_contact_author_email cyyeh@dragon.nchu.edu.tw _publ_section_title ; Porphyrin Dimers Bridged by a Platinum-diacetylide Unit ; loop_ _publ_author_name 'Chen-Yu Yeh' 'Yi-Jen Chen' 'Szu-Shuo Chen' 'Shang-Shih Lo' data_dinickel_complex _database_code_depnum_ccdc_archive 'CCDC 285537' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C146 H178 Cl18 N8 Ni2 P2 Pt' _chemical_formula_weight 3057.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7645(1) _cell_length_b 19.8365(2) _cell_length_c 22.0587(2) _cell_angle_alpha 68.4657(6) _cell_angle_beta 80.3541(6) _cell_angle_gamma 89.0879(6) _cell_volume 3913.36(7) _cell_formula_units_Z 1 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1580 _exptl_absorpt_coefficient_mu 1.505 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.629 _exptl_absorpt_correction_T_max 0.899 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69469 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 27.50 _reflns_number_total 17970 _reflns_number_gt 15136 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1340P)^2^+5.3118P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0046(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 17970 _refine_ls_number_parameters 814 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.2037 _refine_ls_wR_factor_gt 0.1922 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.012 _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 Pt Pt 0.0000 0.0000 0.0000 0.02831(11) Uani 1 2 d S . . Ni Ni 0.68706(6) 0.17858(3) -0.26460(3) 0.02463(14) Uani 1 1 d . . . P1 P -0.14037(15) 0.07587(9) -0.06538(7) 0.0476(4) Uani 1 1 d . C . N1 N 0.5968(4) 0.0836(2) -0.23328(19) 0.0275(8) Uani 1 1 d . . . N2 N 0.5723(4) 0.1995(2) -0.19470(18) 0.0265(8) Uani 1 1 d . . . N3 N 0.7774(4) 0.2732(2) -0.29662(19) 0.0282(8) Uani 1 1 d . . . N4 N 0.8040(4) 0.1571(2) -0.33343(19) 0.0303(8) Uani 1 1 d . . . C1 C 0.4713(5) 0.0594(3) -0.1907(2) 0.0304(10) Uani 1 1 d . . . C2 C 0.4373(5) -0.0141(3) -0.1817(3) 0.0364(11) Uani 1 1 d . . . H2A H 0.3544 -0.0418 -0.1567 0.044 Uiso 1 1 calc R . . C3 C 0.5453(6) -0.0366(3) -0.2153(3) 0.0391(11) Uani 1 1 d . . . H3A H 0.5546 -0.0837 -0.2169 0.047 Uiso 1 1 calc R . . C4 C 0.6435(5) 0.0244(3) -0.2481(2) 0.0306(10) Uani 1 1 d . . . C5 C 0.7644(5) 0.0247(3) -0.2920(2) 0.0333(10) Uani 1 1 d . . . C6 C 0.8341(5) 0.0892(3) -0.3345(2) 0.0338(10) Uani 1 1 d . . . C7 C 0.9360(6) 0.0959(3) -0.3921(3) 0.0457(13) Uani 1 1 d . . . H7A H 0.9775 0.0572 -0.4030 0.055 Uiso 1 1 calc R . . C8 C 0.9609(6) 0.1672(3) -0.4275(3) 0.0447(13) Uani 1 1 d . . . H8A H 1.0200 0.1883 -0.4692 0.054 Uiso 1 1 calc R . . C9 C 0.8814(5) 0.2061(3) -0.3903(2) 0.0326(10) Uani 1 1 d . . . C10 C 0.8980(5) 0.2797(3) -0.4059(2) 0.0307(10) Uani 1 1 d . . . C11 C 0.8548(5) 0.3102(3) -0.3590(2) 0.0303(10) Uani 1 1 d . . . C12 C 0.8987(6) 0.3808(3) -0.3640(3) 0.0373(11) Uani 1 1 d . . . H12A H 0.9505 0.4170 -0.4020 0.045 Uiso 1 1 calc R . . C13 C 0.8537(6) 0.3868(3) -0.3054(3) 0.0379(11) Uani 1 1 d . . . H13A H 0.8705 0.4270 -0.2937 0.045 Uiso 1 1 calc R . . C14 C 0.7754(5) 0.3208(3) -0.2640(2) 0.0298(9) Uani 1 1 d . . . C15 C 0.6942(5) 0.3114(3) -0.2034(2) 0.0311(10) Uani 1 1 d . . . C16 C 0.5926(5) 0.2556(3) -0.1724(2) 0.0299(9) Uani 1 1 d . . . C17 C 0.4883(6) 0.2500(3) -0.1174(3) 0.0379(11) Uani 1 1 d . . . H17A H 0.4818 0.2804 -0.0924 0.045 Uiso 1 1 calc R . . C18 C 0.3999(5) 0.1935(3) -0.1069(3) 0.0369(11) Uani 1 1 d . . . H18A H 0.3177 0.1782 -0.0745 0.044 Uiso 1 1 calc R . . C19 C 0.4534(5) 0.1612(3) -0.1536(2) 0.0285(9) Uani 1 1 d . . . C20 C 0.3987(5) 0.0969(3) -0.1540(2) 0.0290(9) Uani 1 1 d . . . C21 C 0.2732(5) 0.0642(3) -0.1091(2) 0.0316(10) Uani 1 1 d . . . C22 C 0.1691(5) 0.0400(3) -0.0689(2) 0.0322(10) Uani 1 1 d . . . C23 C 0.8140(6) -0.0451(3) -0.2962(3) 0.0390(11) Uani 1 1 d . . . C24 C 0.9227(7) -0.0770(4) -0.2644(3) 0.0508(15) Uani 1 1 d . . . H24A H 0.9618 -0.0541 -0.2398 0.061 Uiso 1 1 calc R . . C25 C 0.9763(8) -0.1407(4) -0.2672(4) 0.0612(18) Uani 1 1 d . A . C26 C 0.9146(7) -0.1731(3) -0.3041(3) 0.0514(15) Uani 1 1 d . . . H26A H 0.9487 -0.2174 -0.3064 0.062 Uiso 1 1 calc R . . C27 C 0.8050(6) -0.1425(3) -0.3374(3) 0.0454(13) Uani 1 1 d . . . C28 C 0.7565(6) -0.0784(3) -0.3326(3) 0.0417(12) Uani 1 1 d . . . H28A H 0.6822 -0.0566 -0.3545 0.050 Uiso 1 1 calc R . . C29 C 1.0929(11) -0.1779(5) -0.2307(4) 0.094(3) Uani 1 1 d D . . C30 C 1.129(2) -0.1455(10) -0.1833(8) 0.073(4) Uiso 0.50 1 d PD A 1 H30A H 1.2061 -0.1711 -0.1627 0.110 Uiso 0.50 1 calc PR A 1 H30B H 1.0480 -0.1502 -0.1490 0.110 Uiso 0.50 1 calc PR A 1 H30C H 1.1574 -0.0941 -0.2074 0.110 Uiso 0.50 1 calc PR A 1 C31 C 1.209(2) -0.1797(15) -0.2844(10) 0.110(7) Uiso 0.50 1 d PD A 1 H31A H 1.2893 -0.2020 -0.2647 0.166 Uiso 0.50 1 calc PR A 1 H31B H 1.2359 -0.1301 -0.3156 0.166 Uiso 0.50 1 calc PR A 1 H31C H 1.1774 -0.2082 -0.3080 0.166 Uiso 0.50 1 calc PR A 1 C32 C 1.058(2) -0.2594(7) -0.1948(10) 0.085(5) Uiso 0.50 1 d PD A 1 H32A H 1.1341 -0.2823 -0.1720 0.127 Uiso 0.50 1 calc PR A 1 H32B H 1.0452 -0.2811 -0.2270 0.127 Uiso 0.50 1 calc PR A 1 H32C H 0.9720 -0.2671 -0.1624 0.127 Uiso 0.50 1 calc PR A 1 C30' C 1.081(2) -0.1725(10) -0.1635(6) 0.070(4) Uiso 0.50 1 d PD A 2 H30D H 1.1587 -0.1958 -0.1425 0.105 Uiso 0.50 1 calc PR A 2 H30E H 0.9930 -0.1968 -0.1358 0.105 Uiso 0.50 1 calc PR A 2 H30F H 1.0822 -0.1212 -0.1686 0.105 Uiso 0.50 1 calc PR A 2 C31' C 1.216(4) -0.124(3) -0.261(3) 0.15(3) Uiso 0.50 1 d PD A 2 H31D H 1.2964 -0.1436 -0.2407 0.233 Uiso 0.50 1 calc PR A 2 H31E H 1.1926 -0.0784 -0.2545 0.233 Uiso 0.50 1 calc PR A 2 H31F H 1.2384 -0.1138 -0.3090 0.233 Uiso 0.50 1 calc PR A 2 C32' C 1.155(4) -0.2469(12) -0.2305(19) 0.156(12) Uiso 0.50 1 d PD A 2 H32D H 1.2273 -0.2586 -0.2027 0.234 Uiso 0.50 1 calc PR A 2 H32E H 1.1965 -0.2414 -0.2758 0.234 Uiso 0.50 1 calc PR A 2 H32F H 1.0827 -0.2861 -0.2128 0.234 Uiso 0.50 1 calc PR A 2 C33 C 0.7409(8) -0.1749(4) -0.3810(4) 0.0627(18) Uani 1 1 d . . . C34 C 0.8107(10) -0.2438(5) -0.3830(5) 0.077(2) Uani 1 1 d . . . H34A H 0.7935 -0.2817 -0.3386 0.116 Uiso 1 1 calc R . . H34B H 0.9110 -0.2334 -0.3980 0.116 Uiso 1 1 calc R . . H34C H 0.7722 -0.2605 -0.4136 0.116 Uiso 1 1 calc R . . C35 C 0.5865(10) -0.1890(6) -0.3564(6) 0.095(3) Uani 1 1 d . . . H35A H 0.5445 -0.1440 -0.3558 0.142 Uiso 1 1 calc R . . H35B H 0.5700 -0.2259 -0.3115 0.142 Uiso 1 1 calc R . . H35C H 0.5448 -0.2062 -0.3858 0.142 Uiso 1 1 calc R . . C36 C 0.7664(11) -0.1192(5) -0.4528(4) 0.083(3) Uani 1 1 d . . . H36A H 0.7129 -0.0764 -0.4551 0.124 Uiso 1 1 calc R . . H36B H 0.7369 -0.1410 -0.4821 0.124 Uiso 1 1 calc R . . H36C H 0.8657 -0.1047 -0.4668 0.124 Uiso 1 1 calc R . . C37 C 0.9718(5) 0.3261(3) -0.4730(2) 0.0317(10) Uani 1 1 d . . . C38 C 0.9039(5) 0.3418(3) -0.5270(2) 0.0317(10) Uani 1 1 d . . . H38A H 0.8115 0.3228 -0.5201 0.038 Uiso 1 1 calc R . . C39 C 0.9682(5) 0.3846(3) -0.5906(2) 0.0311(10) Uani 1 1 d . . . C40 C 1.1056(5) 0.4106(3) -0.5986(2) 0.0316(10) Uani 1 1 d . . . H40A H 1.1519 0.4392 -0.6418 0.038 Uiso 1 1 calc R . . C41 C 1.1763(5) 0.3966(3) -0.5465(2) 0.0338(10) Uani 1 1 d . . . C42 C 1.1076(5) 0.3537(3) -0.4829(2) 0.0346(10) Uani 1 1 d . . . H42A H 1.1542 0.3433 -0.4462 0.042 Uiso 1 1 calc R . . C43 C 0.8898(5) 0.4045(3) -0.6490(3) 0.0362(11) Uani 1 1 d . . . C44 C 0.7850(7) 0.3448(4) -0.6407(3) 0.0539(16) Uani 1 1 d . . . H44A H 0.8329 0.2999 -0.6363 0.081 Uiso 1 1 calc R . . H44B H 0.7391 0.3590 -0.6795 0.081 Uiso 1 1 calc R . . H44C H 0.7152 0.3369 -0.6009 0.081 Uiso 1 1 calc R . . C45 C 0.8125(6) 0.4733(3) -0.6520(3) 0.0485(14) Uani 1 1 d . . . H45A H 0.8793 0.5120 -0.6568 0.073 Uiso 1 1 calc R . . H45B H 0.7448 0.4631 -0.6112 0.073 Uiso 1 1 calc R . . H45C H 0.7639 0.4886 -0.6900 0.073 Uiso 1 1 calc R . . C46 C 0.9879(7) 0.4203(4) -0.7148(3) 0.0570(17) Uani 1 1 d . . . H46A H 1.0474 0.4637 -0.7247 0.086 Uiso 1 1 calc R . . H46B H 0.9332 0.4286 -0.7501 0.086 Uiso 1 1 calc R . . H46C H 1.0459 0.3788 -0.7119 0.086 Uiso 1 1 calc R . . C47 C 1.3241(6) 0.4275(3) -0.5549(3) 0.0451(13) Uani 1 1 d . . . C48 C 1.4147(7) 0.3661(4) -0.5207(4) 0.064(2) Uani 1 1 d . . . H48A H 1.4209 0.3304 -0.5420 0.096 Uiso 1 1 calc R . . H48B H 1.3731 0.3425 -0.4739 0.096 Uiso 1 1 calc R . . H48C H 1.5081 0.3861 -0.5242 0.096 Uiso 1 1 calc R . . C49 C 1.3192(7) 0.4842(5) -0.5224(4) 0.066(2) Uani 1 1 d . . . H49A H 1.4104 0.5098 -0.5338 0.099 Uiso 1 1 calc R . . H49B H 1.2951 0.4599 -0.4742 0.099 Uiso 1 1 calc R . . H49C H 1.2489 0.5190 -0.5384 0.099 Uiso 1 1 calc R . . C50 C 1.3910(7) 0.4626(5) -0.6277(3) 0.064(2) Uani 1 1 d . . . H50A H 1.3852 0.4280 -0.6497 0.096 Uiso 1 1 calc R . . H50B H 1.4888 0.4762 -0.6310 0.096 Uiso 1 1 calc R . . H50C H 1.3418 0.5060 -0.6492 0.096 Uiso 1 1 calc R . . C51 C 0.7042(5) 0.3675(3) -0.1733(2) 0.0347(11) Uani 1 1 d . . . C52 C 0.8139(6) 0.3687(3) -0.1414(3) 0.0401(12) Uani 1 1 d . . . H52A H 0.8823 0.3336 -0.1382 0.048 Uiso 1 1 calc R . . C53 C 0.8254(7) 0.4215(3) -0.1137(3) 0.0487(14) Uani 1 1 d . . . C54 C 0.7234(8) 0.4718(4) -0.1200(3) 0.0540(16) Uani 1 1 d . . . H54A H 0.7294 0.5074 -0.1011 0.065 Uiso 1 1 calc R . . C55 C 0.6128(7) 0.4729(3) -0.1526(3) 0.0479(14) Uani 1 1 d . . . C56 C 0.6039(6) 0.4199(3) -0.1796(3) 0.0399(12) Uani 1 1 d . . . H56A H 0.5296 0.4193 -0.2022 0.048 Uiso 1 1 calc R . . C57 C 0.9432(8) 0.4210(4) -0.0751(3) 0.0619(18) Uani 1 1 d . . . C58 C 1.0673(9) 0.3856(7) -0.0975(6) 0.095(3) Uani 1 1 d . . . H58A H 1.1492 0.3997 -0.0837 0.143 Uiso 1 1 calc R . . H58B H 1.0830 0.4013 -0.1458 0.143 Uiso 1 1 calc R . . H58C H 1.0512 0.3328 -0.0776 0.143 Uiso 1 1 calc R . . C59 C 0.9899(11) 0.4973(5) -0.0851(4) 0.089(3) Uani 1 1 d . . . H59A H 1.0736 0.4957 -0.0657 0.133 Uiso 1 1 calc R . . H59B H 0.9157 0.5190 -0.0636 0.133 Uiso 1 1 calc R . . H59C H 1.0105 0.5265 -0.1326 0.133 Uiso 1 1 calc R . . C60 C 0.8871(10) 0.3789(5) -0.0011(4) 0.074(2) Uani 1 1 d . . . H60A H 0.9625 0.3739 0.0243 0.111 Uiso 1 1 calc R . . H60B H 0.8508 0.3306 0.0050 0.111 Uiso 1 1 calc R . . H60C H 0.8125 0.4053 0.0144 0.111 Uiso 1 1 calc R . . C61 C 0.5063(8) 0.5324(4) -0.1597(4) 0.0614(18) Uani 1 1 d . . . C62 C 0.5805(12) 0.6085(4) -0.2017(6) 0.104(4) Uani 1 1 d . . . H62A H 0.6270 0.6086 -0.2447 0.156 Uiso 1 1 calc R . . H62B H 0.6496 0.6187 -0.1783 0.156 Uiso 1 1 calc R . . H62C H 0.5115 0.6458 -0.2084 0.156 Uiso 1 1 calc R . . C63 C 0.4385(12) 0.5276(7) -0.0905(5) 0.110(4) Uani 1 1 d . . . H63A H 0.3893 0.4801 -0.0665 0.165 Uiso 1 1 calc R . . H63B H 0.3723 0.5660 -0.0942 0.165 Uiso 1 1 calc R . . H63C H 0.5103 0.5336 -0.0665 0.165 Uiso 1 1 calc R . . C64 C 0.3921(8) 0.5245(5) -0.1959(4) 0.070(2) Uani 1 1 d . . . H64A H 0.3375 0.4790 -0.1700 0.104 Uiso 1 1 calc R . . H64B H 0.4337 0.5241 -0.2393 0.104 Uiso 1 1 calc R . . H64C H 0.3314 0.5654 -0.2016 0.104 Uiso 1 1 calc R . . C65 C -0.0639(7) 0.1282(4) -0.1510(3) 0.0584(17) Uani 1 1 d . . . H65A H -0.1313 0.1634 -0.1716 0.070 Uiso 1 1 calc R . . H65B H 0.0198 0.1562 -0.1517 0.070 Uiso 1 1 calc R . . C66 C -0.0238(8) 0.0827(6) -0.1918(4) 0.077(3) Uani 1 1 d . . . H66A H 0.0355 0.1121 -0.2335 0.115 Uiso 1 1 calc R . . H66B H -0.1077 0.0648 -0.2011 0.115 Uiso 1 1 calc R . . H66C H 0.0272 0.0415 -0.1673 0.115 Uiso 1 1 calc R . . C67 C -0.3013(9) 0.0339(8) -0.0672(5) 0.126(6) Uani 1 1 d . . . H67A H -0.3667 0.0275 -0.0258 0.151 Uiso 1 1 calc R . . H67B H -0.3428 0.0671 -0.1045 0.151 Uiso 1 1 calc R . . C68 C -0.2863(15) -0.0391(8) -0.0745(5) 0.159(8) Uani 1 1 d . . . H68A H -0.3781 -0.0588 -0.0740 0.239 Uiso 1 1 calc R . . H68B H -0.2458 -0.0726 -0.0377 0.239 Uiso 1 1 calc R . . H68C H -0.2255 -0.0331 -0.1164 0.239 Uiso 1 1 calc R . . C69 C -0.1962(19) 0.1466(8) -0.0342(7) 0.157(7) Uani 1 1 d D . . H69A H -0.2369 0.1849 -0.0687 0.188 Uiso 0.67 1 calc PR B 1 H69B H -0.2709 0.1257 0.0047 0.188 Uiso 0.67 1 calc PR B 1 H69C H -0.1242 0.1847 -0.0578 0.188 Uiso 0.33 1 d PR B 2 H69D H -0.2771 0.1640 -0.0546 0.188 Uiso 0.33 1 d PR B 2 C70 C -0.089(2) 0.1799(12) -0.0154(12) 0.132(7) Uiso 0.67 1 d P C 1 H70A H -0.1290 0.2170 0.0009 0.198 Uiso 0.67 1 calc PR C 1 H70B H -0.0158 0.2026 -0.0539 0.198 Uiso 0.67 1 calc PR C 1 H70C H -0.0493 0.1429 0.0196 0.198 Uiso 0.67 1 calc PR C 1 C70' C -0.225(5) 0.159(2) 0.0291(13) 0.128(13) Uiso 0.33 1 d PD C 2 H70D H -0.2531 0.2091 0.0205 0.192 Uiso 0.33 1 calc PR C 2 H70E H -0.1408 0.1517 0.0491 0.192 Uiso 0.33 1 calc PR C 2 H70F H -0.2999 0.1252 0.0596 0.192 Uiso 0.33 1 calc PR C 2 C71 C 0.6904(10) -0.2888(5) -0.7235(4) 0.077(2) Uani 1 1 d . . . H71A H 0.6392 -0.2476 -0.7504 0.092 Uiso 0.50 1 calc PR D 1 H71B H 0.6599 -0.2665 -0.7653 0.092 Uiso 0.50 1 d PR D 2 Cl1 Cl 0.5736(3) -0.35845(19) -0.67097(18) 0.1264(12) Uani 1 1 d . E . Cl2 Cl 0.7931(11) -0.3295(4) -0.7773(3) 0.136(3) Uani 0.50 1 d P E 1 Cl3 Cl 0.8106(9) -0.2566(5) -0.6914(3) 0.126(3) Uani 0.50 1 d P E 1 Cl2' Cl 0.8506(6) -0.3122(4) -0.7347(6) 0.152(4) Uani 0.50 1 d P E 2 Cl3' Cl 0.6801(13) -0.2280(4) -0.6814(4) 0.141(3) Uani 0.50 1 d P E 2 C72 C 0.4091(12) -0.1098(5) -0.5711(6) 0.203(9) Uiso 1 1 d D . . H72A H 0.3273 -0.1023 -0.5943 0.244 Uiso 0.50 1 calc PR F 1 H72B H 0.3445 -0.0958 -0.6039 0.244 Uiso 0.50 1 calc PR F 2 Cl4 Cl 0.4453(9) -0.2015(4) -0.5321(4) 0.133(2) Uiso 0.50 1 d PD G 1 Cl5 Cl 0.5698(14) -0.0737(7) -0.6240(7) 0.253(7) Uiso 0.50 1 d PD G 1 Cl6 Cl 0.398(3) -0.0715(9) -0.5125(10) 0.49(2) Uiso 0.50 1 d PD G 1 Cl4' Cl 0.5007(17) -0.1820(6) -0.5741(9) 0.277(8) Uiso 0.50 1 d PD G 2 Cl5' Cl 0.5241(10) -0.0387(4) -0.5836(5) 0.156(3) Uiso 0.50 1 d PD G 2 Cl6' Cl 0.3200(19) -0.1286(10) -0.4908(8) 0.350 Uiso 0.50 1 d PD G 2 C73 C 1.4070(10) 0.2385(8) 0.0748(4) 0.159(6) Uiso 1 1 d D . . H73A H 1.4418 0.1902 0.0767 0.191 Uiso 0.67 1 calc PR H 1 H73B H 1.4188 0.2037 0.0537 0.191 Uiso 0.33 1 d PR H 2 Cl7 Cl 1.2610(8) 0.2518(4) 0.0365(4) 0.165(2) Uiso 0.67 1 d PD I 1 Cl8 Cl 1.3527(6) 0.2316(3) 0.1562(3) 0.1178(15) Uiso 0.67 1 d PD I 1 Cl9 Cl 1.5399(10) 0.3024(5) 0.0285(5) 0.198(3) Uiso 0.67 1 d PD I 1 Cl7' Cl 1.2618(13) 0.2298(12) 0.1354(9) 0.221(8) Uiso 0.33 1 d PD I 2 Cl8' Cl 1.5218(13) 0.2447(9) 0.1260(7) 0.176(5) Uiso 0.33 1 d PD I 2 Cl9' Cl 1.369(3) 0.3295(9) 0.0295(11) 0.247(9) Uiso 0.33 1 d PD I 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 Pt 0.02033(14) 0.03232(16) 0.02548(15) -0.00385(10) -0.00159(9) 0.00192(9) Ni 0.0222(3) 0.0272(3) 0.0210(3) -0.0063(2) -0.0001(2) 0.0014(2) P1 0.0342(7) 0.0602(9) 0.0345(7) -0.0022(7) -0.0051(6) 0.0157(7) N1 0.0254(18) 0.031(2) 0.0239(18) -0.0089(16) -0.0005(15) 0.0002(15) N2 0.0229(18) 0.0276(19) 0.0250(18) -0.0058(15) -0.0023(14) 0.0024(14) N3 0.0269(19) 0.031(2) 0.0231(18) -0.0071(16) -0.0016(15) 0.0026(15) N4 0.030(2) 0.032(2) 0.0248(19) -0.0082(16) 0.0020(15) 0.0023(16) C1 0.026(2) 0.034(2) 0.028(2) -0.0075(19) -0.0037(18) 0.0003(18) C2 0.034(3) 0.037(3) 0.034(3) -0.010(2) 0.000(2) -0.005(2) C3 0.041(3) 0.037(3) 0.039(3) -0.017(2) 0.001(2) -0.003(2) C4 0.034(2) 0.028(2) 0.027(2) -0.0086(19) -0.0038(19) 0.0028(19) C5 0.034(2) 0.037(3) 0.029(2) -0.013(2) -0.0020(19) 0.003(2) C6 0.036(3) 0.034(2) 0.029(2) -0.011(2) 0.001(2) 0.003(2) C7 0.049(3) 0.043(3) 0.039(3) -0.017(2) 0.012(2) 0.006(2) C8 0.050(3) 0.041(3) 0.035(3) -0.013(2) 0.014(2) -0.001(2) C9 0.033(2) 0.036(2) 0.024(2) -0.0081(19) 0.0024(18) -0.001(2) C10 0.026(2) 0.035(2) 0.027(2) -0.008(2) -0.0023(18) 0.0019(18) C11 0.027(2) 0.032(2) 0.025(2) -0.0033(19) 0.0003(17) -0.0005(18) C12 0.039(3) 0.032(2) 0.032(3) -0.005(2) 0.002(2) -0.002(2) C13 0.040(3) 0.033(3) 0.037(3) -0.010(2) -0.001(2) -0.003(2) C14 0.029(2) 0.030(2) 0.029(2) -0.0086(19) -0.0031(18) 0.0006(18) C15 0.030(2) 0.029(2) 0.034(2) -0.012(2) -0.0044(19) 0.0030(18) C16 0.029(2) 0.033(2) 0.027(2) -0.0107(19) -0.0040(18) 0.0039(18) C17 0.040(3) 0.039(3) 0.032(3) -0.015(2) 0.002(2) 0.006(2) C18 0.035(3) 0.042(3) 0.030(2) -0.012(2) 0.004(2) 0.003(2) C19 0.021(2) 0.033(2) 0.024(2) -0.0034(18) -0.0015(17) 0.0061(17) C20 0.024(2) 0.034(2) 0.022(2) -0.0031(18) -0.0031(17) 0.0023(18) C21 0.024(2) 0.034(2) 0.031(2) -0.007(2) -0.0033(19) 0.0033(18) C22 0.024(2) 0.037(3) 0.032(2) -0.009(2) -0.0039(19) 0.0047(19) C23 0.039(3) 0.039(3) 0.036(3) -0.014(2) 0.004(2) 0.005(2) C24 0.058(4) 0.059(4) 0.047(3) -0.030(3) -0.016(3) 0.021(3) C25 0.063(4) 0.072(5) 0.058(4) -0.034(4) -0.015(3) 0.029(4) C26 0.061(4) 0.044(3) 0.053(4) -0.024(3) -0.009(3) 0.018(3) C27 0.048(3) 0.041(3) 0.047(3) -0.020(3) -0.002(3) 0.007(2) C28 0.043(3) 0.039(3) 0.043(3) -0.016(2) -0.004(2) 0.008(2) C29 0.105(7) 0.112(8) 0.096(7) -0.067(6) -0.047(6) 0.069(6) C33 0.064(4) 0.061(4) 0.084(5) -0.048(4) -0.018(4) 0.016(3) C34 0.098(6) 0.067(5) 0.094(6) -0.055(5) -0.035(5) 0.030(4) C35 0.075(6) 0.091(6) 0.155(10) -0.082(7) -0.036(6) 0.014(5) C36 0.122(8) 0.081(6) 0.069(5) -0.046(5) -0.042(5) 0.044(5) C37 0.029(2) 0.034(2) 0.027(2) -0.008(2) 0.0019(18) 0.0006(19) C38 0.027(2) 0.033(2) 0.030(2) -0.009(2) 0.0022(18) -0.0025(19) C39 0.034(2) 0.031(2) 0.027(2) -0.0093(19) -0.0033(19) 0.0045(19) C40 0.028(2) 0.034(2) 0.025(2) -0.0052(19) 0.0042(18) -0.0013(19) C41 0.025(2) 0.038(3) 0.032(2) -0.008(2) -0.0007(19) -0.0002(19) C42 0.030(2) 0.042(3) 0.027(2) -0.009(2) -0.0030(19) 0.001(2) C43 0.033(3) 0.040(3) 0.032(3) -0.009(2) -0.008(2) 0.004(2) C44 0.058(4) 0.057(4) 0.046(3) -0.014(3) -0.019(3) -0.011(3) C45 0.045(3) 0.050(3) 0.048(3) -0.012(3) -0.018(3) 0.007(3) C46 0.046(3) 0.090(5) 0.031(3) -0.017(3) -0.007(2) 0.002(3) C47 0.027(3) 0.059(4) 0.038(3) -0.007(3) -0.002(2) -0.005(2) C48 0.034(3) 0.085(5) 0.050(4) 0.001(3) -0.004(3) 0.009(3) C49 0.047(4) 0.083(5) 0.071(5) -0.027(4) -0.019(3) -0.014(3) C50 0.035(3) 0.090(5) 0.046(4) -0.003(3) -0.001(3) -0.017(3) C51 0.040(3) 0.034(3) 0.028(2) -0.013(2) 0.000(2) -0.004(2) C52 0.045(3) 0.045(3) 0.029(3) -0.012(2) -0.006(2) 0.001(2) C53 0.061(4) 0.052(3) 0.034(3) -0.016(3) -0.008(3) -0.010(3) C54 0.073(4) 0.056(4) 0.042(3) -0.031(3) -0.002(3) -0.003(3) C55 0.056(4) 0.046(3) 0.044(3) -0.024(3) 0.000(3) 0.002(3) C56 0.043(3) 0.041(3) 0.034(3) -0.014(2) -0.001(2) 0.001(2) C57 0.067(4) 0.081(5) 0.047(4) -0.031(4) -0.015(3) -0.011(4) C58 0.060(5) 0.142(9) 0.106(7) -0.065(7) -0.030(5) -0.015(5) C59 0.121(8) 0.090(6) 0.055(4) -0.018(4) -0.028(5) -0.047(6) C60 0.101(6) 0.067(5) 0.050(4) -0.009(3) -0.030(4) -0.012(4) C61 0.070(5) 0.059(4) 0.064(4) -0.035(4) -0.008(4) 0.015(3) C62 0.116(8) 0.044(4) 0.151(10) -0.033(5) -0.027(7) 0.011(5) C63 0.109(8) 0.167(11) 0.091(7) -0.090(8) -0.026(6) 0.071(8) C64 0.064(5) 0.072(5) 0.075(5) -0.032(4) -0.008(4) 0.026(4) C65 0.048(3) 0.060(4) 0.044(3) 0.011(3) -0.016(3) 0.002(3) C66 0.051(4) 0.138(8) 0.044(4) -0.035(5) -0.010(3) 0.002(4) C67 0.042(4) 0.192(14) 0.072(6) 0.043(7) -0.028(4) -0.029(6) C68 0.192(14) 0.158(12) 0.081(7) 0.042(7) -0.082(8) -0.122(11) C69 0.221(16) 0.163(12) 0.108(9) -0.064(9) -0.071(10) 0.158(13) C71 0.083(6) 0.068(5) 0.070(5) -0.004(4) -0.039(4) 0.022(4) Cl1 0.0883(18) 0.114(2) 0.132(3) 0.0096(19) -0.0248(17) -0.0125(16) Cl2 0.189(8) 0.129(5) 0.082(4) -0.033(4) -0.020(4) 0.080(6) Cl3 0.126(5) 0.132(6) 0.093(4) 0.000(4) -0.041(4) -0.037(5) Cl2' 0.067(3) 0.093(4) 0.258(11) -0.024(6) -0.019(5) 0.017(3) Cl3' 0.237(10) 0.081(4) 0.106(5) -0.018(3) -0.067(6) -0.006(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 Pt C22 1.995(5) 2 ? Pt C22 1.995(5) . ? Pt P1 2.2863(14) . ? Pt P1 2.2863(14) 2 ? Ni N4 1.915(4) . ? Ni N3 1.916(4) . ? Ni N2 1.919(4) . ? Ni N1 1.924(4) . ? P1 C67 1.803(10) . ? P1 C69 1.815(11) . ? P1 C65 1.821(6) . ? N1 C4 1.381(6) . ? N1 C1 1.384(6) . ? N2 C19 1.384(6) . ? N2 C16 1.400(6) . ? N3 C14 1.379(6) . ? N3 C11 1.390(6) . ? N4 C9 1.378(6) . ? N4 C6 1.382(6) . ? C1 C20 1.394(7) . ? C1 C2 1.434(7) . ? C2 C3 1.353(8) . ? C3 C4 1.438(7) . ? C4 C5 1.394(7) . ? C5 C6 1.383(7) . ? C5 C23 1.489(7) . ? C6 C7 1.442(7) . ? C7 C8 1.345(8) . ? C8 C9 1.449(7) . ? C9 C10 1.378(7) . ? C10 C11 1.384(7) . ? C10 C37 1.489(6) . ? C11 C12 1.432(7) . ? C12 C13 1.340(7) . ? C13 C14 1.432(7) . ? C14 C15 1.385(7) . ? C15 C16 1.389(7) . ? C15 C51 1.501(7) . ? C16 C17 1.419(7) . ? C17 C18 1.352(8) . ? C18 C19 1.428(7) . ? C19 C20 1.395(7) . ? C20 C21 1.432(7) . ? C21 C22 1.204(7) . ? C23 C24 1.386(9) . ? C23 C28 1.395(8) . ? C24 C25 1.378(9) . ? C25 C26 1.414(10) . ? C25 C29 1.528(11) . ? C26 C27 1.403(9) . ? C27 C28 1.384(8) . ? C27 C33 1.550(9) . ? C29 C32' 1.487(10) . ? C29 C30 1.501(9) . ? C29 C31 1.507(10) . ? C29 C30' 1.509(9) . ? C29 C31' 1.515(10) . ? C29 C32 1.532(9) . ? C33 C35 1.507(12) . ? C33 C34 1.529(9) . ? C33 C36 1.544(12) . ? C37 C38 1.393(7) . ? C37 C42 1.394(7) . ? C38 C39 1.390(7) . ? C39 C40 1.404(7) . ? C39 C43 1.532(7) . ? C40 C41 1.378(7) . ? C41 C42 1.403(7) . ? C41 C47 1.532(7) . ? C43 C44 1.518(8) . ? C43 C46 1.528(8) . ? C43 C45 1.533(8) . ? C47 C50 1.528(8) . ? C47 C48 1.532(9) . ? C47 C49 1.537(10) . ? C51 C52 1.382(8) . ? C51 C56 1.403(8) . ? C52 C53 1.405(8) . ? C53 C54 1.387(10) . ? C53 C57 1.540(9) . ? C54 C55 1.390(10) . ? C55 C56 1.394(8) . ? C55 C61 1.542(10) . ? C57 C58 1.494(13) . ? C57 C59 1.513(11) . ? C57 C60 1.540(10) . ? C61 C64 1.516(11) . ? C61 C63 1.527(11) . ? C61 C62 1.563(12) . ? C65 C66 1.497(11) . ? C67 C68 1.52(2) . ? C69 C70 1.44(3) . ? C69 C70' 1.490(7) . ? C71 Cl2' 1.629(11) . ? C71 Cl3 1.709(11) . ? C71 Cl1 1.728(10) . ? C71 Cl3' 1.765(12) . ? C71 Cl2 1.829(11) . ? C72 Cl4' 1.691(9) . ? C72 Cl6 1.712(9) . ? C72 Cl5' 1.729(9) . ? C72 Cl6' 1.744(9) . ? C72 Cl4 1.761(9) . ? C72 Cl5 1.774(9) . ? C73 Cl9 1.730(9) . ? C73 Cl8 1.738(8) . ? C73 Cl7' 1.740(9) . ? C73 Cl7 1.745(8) . ? C73 Cl8' 1.754(9) . ? C73 Cl9' 1.781(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C22 Pt C22 180. 2 . ? C22 Pt P1 87.92(14) 2 . ? C22 Pt P1 92.08(14) . . ? C22 Pt P1 92.08(14) 2 2 ? C22 Pt P1 87.92(14) . 2 ? P1 Pt P1 180. 2 . ? N4 Ni N3 89.78(17) . . ? N4 Ni N2 179.02(17) . . ? N3 Ni N2 90.18(16) . . ? N4 Ni N1 89.73(17) . . ? N3 Ni N1 179.45(16) . . ? N2 Ni N1 90.32(16) . . ? C67 P1 C69 103.7(8) . . ? C67 P1 C65 106.7(4) . . ? C69 P1 C65 102.1(6) . . ? C67 P1 Pt 115.1(4) . . ? C69 P1 Pt 110.2(4) . . ? C65 P1 Pt 117.5(2) . . ? C4 N1 C1 104.9(4) . . ? C4 N1 Ni 127.5(3) . . ? C1 N1 Ni 127.5(3) . . ? C19 N2 C16 104.5(4) . . ? C19 N2 Ni 127.8(3) . . ? C16 N2 Ni 127.7(3) . . ? C14 N3 C11 104.8(4) . . ? C14 N3 Ni 127.8(3) . . ? C11 N3 Ni 127.4(3) . . ? C9 N4 C6 105.9(4) . . ? C9 N4 Ni 127.1(3) . . ? C6 N4 Ni 127.0(3) . . ? N1 C1 C20 124.8(4) . . ? N1 C1 C2 110.4(4) . . ? C20 C1 C2 124.1(4) . . ? C3 C2 C1 107.2(4) . . ? C2 C3 C4 106.8(5) . . ? N1 C4 C5 125.0(4) . . ? N1 C4 C3 110.5(4) . . ? C5 C4 C3 124.4(5) . . ? C6 C5 C4 120.9(5) . . ? C6 C5 C23 119.5(4) . . ? C4 C5 C23 119.5(4) . . ? N4 C6 C5 125.4(4) . . ? N4 C6 C7 110.0(4) . . ? C5 C6 C7 124.0(5) . . ? C8 C7 C6 106.9(5) . . ? C7 C8 C9 107.6(5) . . ? C10 C9 N4 126.1(4) . . ? C10 C9 C8 123.8(4) . . ? N4 C9 C8 109.5(4) . . ? C9 C10 C11 121.0(4) . . ? C9 C10 C37 119.0(4) . . ? C11 C10 C37 119.9(4) . . ? C10 C11 N3 124.7(4) . . ? C10 C11 C12 124.9(4) . . ? N3 C11 C12 109.8(4) . . ? C13 C12 C11 107.8(4) . . ? C12 C13 C14 106.8(5) . . ? N3 C14 C15 125.3(4) . . ? N3 C14 C13 110.7(4) . . ? C15 C14 C13 123.4(5) . . ? C14 C15 C16 122.0(4) . . ? C14 C15 C51 119.5(4) . . ? C16 C15 C51 118.2(4) . . ? C15 C16 N2 124.2(4) . . ? C15 C16 C17 125.4(5) . . ? N2 C16 C17 110.2(4) . . ? C18 C17 C16 107.6(4) . . ? C17 C18 C19 107.0(4) . . ? N2 C19 C20 125.1(4) . . ? N2 C19 C18 110.6(4) . . ? C20 C19 C18 124.1(4) . . ? C1 C20 C19 121.7(4) . . ? C1 C20 C21 119.3(5) . . ? C19 C20 C21 118.5(4) . . ? C22 C21 C20 175.3(6) . . ? C21 C22 Pt 178.1(5) . . ? C24 C23 C28 119.0(5) . . ? C24 C23 C5 119.1(5) . . ? C28 C23 C5 121.9(5) . . ? C25 C24 C23 122.5(6) . . ? C24 C25 C26 116.9(6) . . ? C24 C25 C29 123.2(6) . . ? C26 C25 C29 119.9(6) . . ? C27 C26 C25 122.6(6) . . ? C28 C27 C26 117.5(6) . . ? C28 C27 C33 119.0(6) . . ? C26 C27 C33 123.5(5) . . ? C27 C28 C23 121.6(6) . . ? C32' C29 C30 118.9(17) . . ? C32' C29 C31 58.2(16) . . ? C30 C29 C31 116.6(14) . . ? C32' C29 C30' 111.0(17) . . ? C30 C29 C30' 26.3(8) . . ? C31 C29 C30' 136.7(14) . . ? C32' C29 C31' 103(3) . . ? C30 C29 C31' 68(3) . . ? C31 C29 C31' 55(2) . . ? C30' C29 C31' 94(3) . . ? C32' C29 C25 126.5(15) . . ? C30 C29 C25 114.0(9) . . ? C31 C29 C25 104.7(12) . . ? C30' C29 C25 112.3(9) . . ? C31' C29 C25 104(3) . . ? C32' C29 C32 42.5(15) . . ? C30 C29 C32 110.2(12) . . ? C31 C29 C32 99.6(13) . . ? C30' C29 C32 87.7(12) . . ? C31' C29 C32 141(3) . . ? C25 C29 C32 110.7(11) . . ? C35 C33 C34 111.2(7) . . ? C35 C33 C36 109.2(8) . . ? C34 C33 C36 106.6(6) . . ? C35 C33 C27 109.4(6) . . ? C34 C33 C27 112.0(6) . . ? C36 C33 C27 108.3(6) . . ? C38 C37 C42 119.3(4) . . ? C38 C37 C10 119.3(4) . . ? C42 C37 C10 121.4(4) . . ? C39 C38 C37 121.6(4) . . ? C38 C39 C40 117.3(5) . . ? C38 C39 C43 121.0(4) . . ? C40 C39 C43 121.7(4) . . ? C41 C40 C39 123.0(4) . . ? C40 C41 C42 118.1(4) . . ? C40 C41 C47 122.9(4) . . ? C42 C41 C47 119.0(5) . . ? C37 C42 C41 120.7(5) . . ? C44 C43 C46 107.8(5) . . ? C44 C43 C39 112.0(5) . . ? C46 C43 C39 112.2(4) . . ? C44 C43 C45 108.9(5) . . ? C46 C43 C45 108.5(5) . . ? C39 C43 C45 107.3(4) . . ? C50 C47 C41 111.8(5) . . ? C50 C47 C48 108.2(5) . . ? C41 C47 C48 109.4(5) . . ? C50 C47 C49 109.4(6) . . ? C41 C47 C49 109.1(5) . . ? C48 C47 C49 108.9(6) . . ? C52 C51 C56 120.2(5) . . ? C52 C51 C15 120.2(5) . . ? C56 C51 C15 119.6(5) . . ? C51 C52 C53 120.8(6) . . ? C54 C53 C52 117.5(6) . . ? C54 C53 C57 121.4(6) . . ? C52 C53 C57 121.1(6) . . ? C53 C54 C55 123.4(5) . . ? C54 C55 C56 117.9(6) . . ? C54 C55 C61 120.3(6) . . ? C56 C55 C61 121.8(6) . . ? C55 C56 C51 120.3(6) . . ? C58 C57 C59 107.4(8) . . ? C58 C57 C53 111.1(6) . . ? C59 C57 C53 111.3(7) . . ? C58 C57 C60 110.0(8) . . ? C59 C57 C60 109.4(6) . . ? C53 C57 C60 107.8(6) . . ? C64 C61 C63 108.0(7) . . ? C64 C61 C55 113.0(6) . . ? C63 C61 C55 108.4(7) . . ? C64 C61 C62 105.8(7) . . ? C63 C61 C62 111.9(8) . . ? C55 C61 C62 109.8(7) . . ? C66 C65 P1 113.7(5) . . ? C68 C67 P1 114.4(8) . . ? C70 C69 C70' 60.5(19) . . ? C70 C69 P1 115.4(13) . . ? C70' C69 P1 140.3(19) . . ? Cl2' C71 Cl3 61.5(6) . . ? Cl2' C71 Cl1 114.7(5) . . ? Cl3 C71 Cl1 119.0(5) . . ? Cl2' C71 Cl3' 109.0(8) . . ? Cl3 C71 Cl3' 47.6(5) . . ? Cl1 C71 Cl3' 102.3(6) . . ? Cl2' C71 Cl2 44.3(5) . . ? Cl3 C71 Cl2 104.6(7) . . ? Cl1 C71 Cl2 103.4(6) . . ? Cl3' C71 Cl2 149.5(8) . . ? Cl4' C72 Cl6 127.5(11) . . ? Cl4' C72 Cl5' 108.9(7) . . ? Cl6 C72 Cl5' 60.8(7) . . ? Cl4' C72 Cl6' 109.7(7) . . ? Cl6 C72 Cl6' 42.9(8) . . ? Cl5' C72 Cl6' 103.2(7) . . ? Cl4' C72 Cl4 31.4(6) . . ? Cl6 C72 Cl4 106.7(8) . . ? Cl5' C72 Cl4 122.9(8) . . ? Cl6' C72 Cl4 78.8(8) . . ? Cl4' C72 Cl5 73.9(7) . . ? Cl6 C72 Cl5 104.2(7) . . ? Cl5' C72 Cl5 44.8(6) . . ? Cl6' C72 Cl5 142.6(10) . . ? Cl4 C72 Cl5 101.6(6) . . ? Cl9 C73 Cl8 116.5(7) . . ? Cl9 C73 Cl7' 138.0(11) . . ? Cl8 C73 Cl7' 35.9(6) . . ? Cl9 C73 Cl7 111.5(7) . . ? Cl8 C73 Cl7 107.9(6) . . ? Cl7' C73 Cl7 72.5(8) . . ? Cl9 C73 Cl8' 70.5(7) . . ? Cl8 C73 Cl8' 56.7(5) . . ? Cl7' C73 Cl8' 92.6(6) . . ? Cl7 C73 Cl8' 160.0(10) . . ? Cl9 C73 Cl9' 59.6(9) . . ? Cl8 C73 Cl9' 102.0(11) . . ? Cl7' C73 Cl9' 91.0(13) . . ? Cl7 C73 Cl9' 62.3(9) . . ? Cl8' C73 Cl9' 105.8(12) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.581 _refine_diff_density_min -1.317 _refine_diff_density_rms 0.184 #===END data_dizinc_complex _database_code_depnum_ccdc_archive 'CCDC 285538' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C134 H162 Cl4 N8 O4 Zn2' _chemical_formula_weight 2221.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _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 13.8674(2) _cell_length_b 14.9588(2) _cell_length_c 16.0677(2) _cell_angle_alpha 85.2430(8) _cell_angle_beta 87.9895(9) _cell_angle_gamma 68.9350(9) _cell_volume 3099.58(7) _cell_formula_units_Z 1 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1182 _exptl_absorpt_coefficient_mu 0.528 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.876 _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64819 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14190 _reflns_number_gt 10183 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1015P)^2^+1.6046P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0060(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 14190 _refine_ls_number_parameters 707 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1760 _refine_ls_wR_factor_gt 0.1551 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.57221(2) 0.34476(2) 0.706848(19) 0.02836(11) Uani 1 1 d . . . O1 O 0.61100(16) 0.40971(15) 0.59185(12) 0.0405(5) Uani 1 1 d . . . H1A H 0.5978 0.3973 0.5377 0.061 Uiso 1 1 d . . . N1 N 0.65139(16) 0.20060(15) 0.69361(14) 0.0294(5) Uani 1 1 d . . . N2 N 0.69092(17) 0.34411(15) 0.78097(14) 0.0298(5) Uani 1 1 d . . . N3 N 0.48081(16) 0.47503(15) 0.74732(14) 0.0299(5) Uani 1 1 d . . . N4 N 0.44331(16) 0.33206(15) 0.65667(13) 0.0277(4) Uani 1 1 d . . . C1 C 0.6215(2) 0.14351(17) 0.64632(16) 0.0293(5) Uani 1 1 d . . . C2 C 0.7041(2) 0.05304(19) 0.63876(18) 0.0337(6) Uani 1 1 d . . . H2A H 0.7027 0.0014 0.6088 0.040 Uiso 1 1 calc R . . C3 C 0.7844(2) 0.05571(19) 0.68249(17) 0.0329(6) Uani 1 1 d . . . H3A H 0.8502 0.0060 0.6891 0.039 Uiso 1 1 calc R . . C4 C 0.7520(2) 0.14727(18) 0.71702(16) 0.0297(5) Uani 1 1 d . . . C5 C 0.8146(2) 0.17876(19) 0.76432(16) 0.0303(5) Uani 1 1 d . . . C6 C 0.7855(2) 0.27165(19) 0.79292(16) 0.0311(6) Uani 1 1 d . . . C7 C 0.8507(2) 0.3049(2) 0.84011(18) 0.0355(6) Uani 1 1 d . . . H7A H 0.9193 0.2685 0.8577 0.043 Uiso 1 1 calc R . . C8 C 0.7970(2) 0.3964(2) 0.85465(18) 0.0357(6) Uani 1 1 d . . . H8A H 0.8212 0.4375 0.8829 0.043 Uiso 1 1 calc R . . C9 C 0.6954(2) 0.42138(18) 0.81947(16) 0.0308(6) Uani 1 1 d . . . C10 C 0.6122(2) 0.50901(18) 0.82738(16) 0.0299(5) Uani 1 1 d . . . C11 C 0.5113(2) 0.53055(18) 0.79771(17) 0.0307(6) Uani 1 1 d . . . C12 C 0.4229(2) 0.61419(19) 0.81600(18) 0.0342(6) Uani 1 1 d . . . H12A H 0.4221 0.6630 0.8506 0.041 Uiso 1 1 calc R . . C13 C 0.3414(2) 0.60993(19) 0.77445(17) 0.0325(6) Uani 1 1 d . . . H13A H 0.2729 0.6556 0.7741 0.039 Uiso 1 1 calc R . . C14 C 0.3779(2) 0.52336(18) 0.73102(16) 0.0289(5) Uani 1 1 d . . . C15 C 0.31636(19) 0.49359(18) 0.67977(16) 0.0274(5) Uani 1 1 d . . . C16 C 0.34823(19) 0.40461(18) 0.64389(16) 0.0274(5) Uani 1 1 d . . . C17 C 0.2878(2) 0.37467(19) 0.58878(17) 0.0308(6) Uani 1 1 d . . . H17A H 0.2202 0.4116 0.5691 0.037 Uiso 1 1 calc R . . C18 C 0.3450(2) 0.28452(19) 0.57047(17) 0.0316(6) Uani 1 1 d . . . H18A H 0.3249 0.2457 0.5359 0.038 Uiso 1 1 calc R . . C19 C 0.44158(19) 0.25799(18) 0.61285(16) 0.0284(5) Uani 1 1 d . . . C20 C 0.5237(2) 0.16972(18) 0.60857(17) 0.0304(5) Uani 1 1 d . . . C21 C 0.5092(2) 0.09925(19) 0.56093(18) 0.0337(6) Uani 1 1 d . . . C22 C 0.5029(2) 0.03623(19) 0.52210(19) 0.0361(6) Uani 1 1 d . . . C23 C 0.9208(2) 0.10840(19) 0.78575(17) 0.0325(6) Uani 1 1 d . . . C24 C 0.9330(2) 0.02177(19) 0.83098(17) 0.0325(6) Uani 1 1 d . . . H24A H 0.8735 0.0082 0.8490 0.039 Uiso 1 1 calc R . . C25 C 1.0309(2) -0.04587(19) 0.85053(18) 0.0341(6) Uani 1 1 d . . . C26 C 1.1163(2) -0.0222(2) 0.82314(19) 0.0392(7) Uani 1 1 d . . . H26A H 1.1836 -0.0670 0.8358 0.047 Uiso 1 1 calc R . . C27 C 1.1068(2) 0.0644(2) 0.77804(19) 0.0385(6) Uani 1 1 d . . . C28 C 1.0077(2) 0.1288(2) 0.75936(18) 0.0358(6) Uani 1 1 d . . . H28A H 0.9993 0.1878 0.7280 0.043 Uiso 1 1 calc R . . C29 C 1.0418(2) -0.1429(2) 0.89722(19) 0.0376(6) Uani 1 1 d . . . C30 C 0.9672(3) -0.1286(2) 0.9716(2) 0.0514(8) Uani 1 1 d . . . H30A H 0.8961 -0.0970 0.9517 0.077 Uiso 1 1 calc R . . H30B H 0.9828 -0.0886 1.0104 0.077 Uiso 1 1 calc R . . H30C H 0.9749 -0.1912 1.0002 0.077 Uiso 1 1 calc R . . C31 C 1.0170(3) -0.2056(2) 0.8364(2) 0.0534(8) Uani 1 1 d . . . H31A H 0.9476 -0.1718 0.8136 0.080 Uiso 1 1 calc R . . H31B H 1.0199 -0.2664 0.8661 0.080 Uiso 1 1 calc R . . H31C H 1.0677 -0.2185 0.7907 0.080 Uiso 1 1 calc R . . C32 C 1.1509(3) -0.1968(2) 0.9302(2) 0.0551(9) Uani 1 1 d . . . H32A H 1.1696 -0.1568 0.9672 0.083 Uiso 1 1 calc R . . H32B H 1.1997 -0.2114 0.8832 0.083 Uiso 1 1 calc R . . H32C H 1.1535 -0.2568 0.9613 0.083 Uiso 1 1 calc R . . C33 C 1.2034(2) 0.0860(3) 0.7508(2) 0.0524(8) Uani 1 1 d . . . C34 C 1.2654(4) 0.0148(4) 0.6904(4) 0.0993(18) Uani 1 1 d . . . H34A H 1.2229 0.0190 0.6417 0.149 Uiso 1 1 calc R . . H34B H 1.2869 -0.0503 0.7178 0.149 Uiso 1 1 calc R . . H34C H 1.3267 0.0294 0.6723 0.149 Uiso 1 1 calc R . . C35 C 1.2690(3) 0.0790(3) 0.8282(3) 0.0818(14) Uani 1 1 d . . . H35A H 1.2912 0.0135 0.8546 0.123 Uiso 1 1 calc R . . H35B H 1.2276 0.1241 0.8679 0.123 Uiso 1 1 calc R . . H35C H 1.3298 0.0950 0.8111 0.123 Uiso 1 1 calc R . . C36 C 1.1775(3) 0.1887(3) 0.7116(3) 0.0714(12) Uani 1 1 d . . . H36A H 1.1414 0.1960 0.6587 0.107 Uiso 1 1 calc R . . H36B H 1.2415 0.2017 0.7012 0.107 Uiso 1 1 calc R . . H36C H 1.1331 0.2342 0.7497 0.107 Uiso 1 1 calc R . . C37 C 0.6343(2) 0.58515(18) 0.86956(17) 0.0307(6) Uani 1 1 d . . . C38 C 0.6788(2) 0.56598(19) 0.94851(17) 0.0334(6) Uani 1 1 d . . . H38A H 0.6884 0.5060 0.9785 0.040 Uiso 1 1 calc R . . C39 C 0.7096(2) 0.6333(2) 0.98443(17) 0.0352(6) Uani 1 1 d . . . C40 C 0.6866(2) 0.7232(2) 0.94129(18) 0.0363(6) Uani 1 1 d . . . H40A H 0.7047 0.7706 0.9659 0.044 Uiso 1 1 calc R . . C41 C 0.6382(2) 0.74679(19) 0.86378(19) 0.0355(6) Uani 1 1 d . . . C42 C 0.6141(2) 0.67570(19) 0.82757(17) 0.0321(6) Uani 1 1 d . . . H42A H 0.5837 0.6890 0.7737 0.039 Uiso 1 1 calc R . . C43 C 0.7672(3) 0.6103(2) 1.06772(19) 0.0432(7) Uani 1 1 d . . . C44 C 0.8059(3) 0.5022(2) 1.0941(2) 0.0549(9) Uani 1 1 d . . . H44A H 0.8517 0.4668 1.0506 0.082 Uiso 1 1 calc R . . H44B H 0.7468 0.4811 1.1019 0.082 Uiso 1 1 calc R . . H44C H 0.8440 0.4899 1.1466 0.082 Uiso 1 1 calc R . . C45 C 0.8627(3) 0.6400(3) 1.0590(2) 0.0614(10) Uani 1 1 d . . . H45A H 0.8406 0.7094 1.0451 0.092 Uiso 1 1 calc R . . H45B H 0.9077 0.6060 1.0145 0.092 Uiso 1 1 calc R . . H45C H 0.9005 0.6234 1.1118 0.092 Uiso 1 1 calc R . . C46 C 0.6941(3) 0.6658(3) 1.1356(2) 0.0577(9) Uani 1 1 d . . . H46A H 0.6713 0.7349 1.1197 0.087 Uiso 1 1 calc R . . H46B H 0.7307 0.6516 1.1889 0.087 Uiso 1 1 calc R . . H46C H 0.6339 0.6461 1.1412 0.087 Uiso 1 1 calc R . . C47 C 0.6152(2) 0.8474(2) 0.8212(2) 0.0439(7) Uani 1 1 d . . . C48 C 0.7155(3) 0.8682(3) 0.8112(3) 0.0577(9) Uani 1 1 d . . . H48A H 0.7635 0.8224 0.7751 0.087 Uiso 1 1 calc R . . H48B H 0.7469 0.8620 0.8661 0.087 Uiso 1 1 calc R . . H48C H 0.7002 0.9337 0.7859 0.087 Uiso 1 1 calc R . . C49 C 0.5406(3) 0.9208(2) 0.8778(3) 0.0664(11) Uani 1 1 d . . . H49A H 0.4756 0.9089 0.8842 0.100 Uiso 1 1 calc R . . H49B H 0.5268 0.9860 0.8524 0.100 Uiso 1 1 calc R . . H49C H 0.5721 0.9140 0.9328 0.100 Uiso 1 1 calc R . . C50 C 0.5672(3) 0.8594(3) 0.7353(3) 0.0653(11) Uani 1 1 d . . . H50A H 0.6141 0.8121 0.6996 0.098 Uiso 1 1 calc R . . H50B H 0.5556 0.9243 0.7102 0.098 Uiso 1 1 calc R . . H50C H 0.5012 0.8493 0.7408 0.098 Uiso 1 1 calc R . . C51 C 0.2098(2) 0.56203(18) 0.65917(16) 0.0290(5) Uani 1 1 d . . . C52 C 0.1972(2) 0.65165(19) 0.61788(17) 0.0335(6) Uani 1 1 d . . . H52A H 0.2559 0.6694 0.6065 0.040 Uiso 1 1 calc R . . C53 C 0.1001(2) 0.7148(2) 0.59347(18) 0.0382(6) Uani 1 1 d . . . C54 C 0.0156(2) 0.6868(2) 0.61131(19) 0.0434(7) Uani 1 1 d . . . H54A H -0.0510 0.7295 0.5940 0.052 Uiso 1 1 calc R . . C55 C 0.0244(2) 0.5992(2) 0.65329(19) 0.0380(6) Uani 1 1 d . . . C56 C 0.1236(2) 0.53735(19) 0.67720(17) 0.0320(6) Uani 1 1 d . . . H56A H 0.1321 0.4772 0.7064 0.038 Uiso 1 1 calc R . . C57 C 0.0848(3) 0.8128(2) 0.5467(2) 0.0508(8) Uani 1 1 d . . . C58 C 0.1893(4) 0.8317(3) 0.5357(3) 0.0811(13) Uani 1 1 d . . . H58A H 0.2368 0.7843 0.5006 0.122 Uiso 1 1 calc R . . H58B H 0.2206 0.8263 0.5905 0.122 Uiso 1 1 calc R . . H58C H 0.1756 0.8964 0.5091 0.122 Uiso 1 1 calc R . . C59 C 0.0131(4) 0.8916(3) 0.5959(3) 0.0846(15) Uani 1 1 d . . . H59A H -0.0529 0.8820 0.6049 0.127 Uiso 1 1 calc R . . H59B H 0.0012 0.9539 0.5649 0.127 Uiso 1 1 calc R . . H59C H 0.0442 0.8904 0.6500 0.127 Uiso 1 1 calc R . . C60 C 0.0458(5) 0.8159(3) 0.4602(3) 0.0940(17) Uani 1 1 d . . . H60A H -0.0205 0.8063 0.4635 0.141 Uiso 1 1 calc R . . H60B H 0.0960 0.7649 0.4298 0.141 Uiso 1 1 calc R . . H60C H 0.0366 0.8784 0.4308 0.141 Uiso 1 1 calc R . . C61 C -0.0691(2) 0.5701(2) 0.6769(3) 0.0549(9) Uani 1 1 d . . . C62 C -0.0492(3) 0.4682(3) 0.6545(4) 0.0965(18) Uani 1 1 d . . . H62A H 0.0122 0.4239 0.6840 0.145 Uiso 1 1 calc R . . H62B H -0.0379 0.4646 0.5941 0.145 Uiso 1 1 calc R . . H62C H -0.1091 0.4505 0.6709 0.145 Uiso 1 1 calc R . . C63 C -0.1669(3) 0.6375(3) 0.6308(3) 0.0759(13) Uani 1 1 d . . . H63A H -0.1577 0.6304 0.5707 0.114 Uiso 1 1 calc R . . H63B H -0.1789 0.7041 0.6418 0.114 Uiso 1 1 calc R . . H63C H -0.2264 0.6208 0.6506 0.114 Uiso 1 1 calc R . . C64 C -0.0894(3) 0.5796(3) 0.7719(3) 0.0711(11) Uani 1 1 d . . . H64A H -0.0308 0.5331 0.8031 0.107 Uiso 1 1 calc R . . H64B H -0.1525 0.5668 0.7875 0.107 Uiso 1 1 calc R . . H64C H -0.0978 0.6448 0.7851 0.107 Uiso 1 1 calc R . . C65 C 0.6995(2) 0.4368(3) 0.5831(2) 0.0472(7) Uani 1 1 d . . . H65A H 0.6909 0.4830 0.5344 0.071 Uiso 1 1 calc R . . H65B H 0.7611 0.3797 0.5753 0.071 Uiso 1 1 calc R . . H65C H 0.7073 0.4663 0.6334 0.071 Uiso 1 1 calc R . . O2 O 0.54090(19) 0.39022(16) 0.44471(14) 0.0494(5) Uani 1 1 d . . . H2B H 0.5175 0.4413 0.4138 0.074 Uiso 1 1 calc R . . C66 C 0.5231(3) 0.3148(3) 0.4072(2) 0.0559(9) Uani 1 1 d . . . H66A H 0.5558 0.2541 0.4407 0.084 Uiso 1 1 calc R . . H66B H 0.5528 0.3094 0.3507 0.084 Uiso 1 1 calc R . . H66C H 0.4486 0.3287 0.4042 0.084 Uiso 1 1 calc R . . C67 C 0.4110(4) 0.8127(4) 0.0795(3) 0.0924(15) Uani 1 1 d . . . H67A H 0.3940 0.8018 0.1389 0.111 Uiso 1 1 calc R . . H67B H 0.4797 0.8190 0.0774 0.111 Uiso 1 1 calc R . . Cl1 Cl 0.41866(11) 0.71261(10) 0.02761(8) 0.0936(4) Uani 1 1 d . . . Cl2 Cl 0.32053(10) 0.91946(9) 0.03915(9) 0.0857(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.02756(17) 0.02367(17) 0.03426(19) -0.00422(11) -0.00608(12) -0.00869(12) O1 0.0472(12) 0.0512(12) 0.0324(10) -0.0010(9) -0.0044(9) -0.0289(10) N1 0.0275(11) 0.0277(11) 0.0330(12) -0.0040(9) -0.0049(9) -0.0090(9) N2 0.0306(11) 0.0266(11) 0.0322(12) -0.0045(9) -0.0052(9) -0.0091(9) N3 0.0284(11) 0.0270(11) 0.0356(12) -0.0037(9) -0.0057(9) -0.0107(9) N4 0.0273(11) 0.0230(10) 0.0333(12) -0.0049(8) -0.0024(9) -0.0087(8) C1 0.0325(13) 0.0222(12) 0.0336(14) -0.0040(10) -0.0017(11) -0.0097(10) C2 0.0345(14) 0.0261(13) 0.0392(15) -0.0053(11) -0.0030(11) -0.0084(11) C3 0.0319(14) 0.0281(13) 0.0362(14) -0.0033(11) -0.0033(11) -0.0072(11) C4 0.0292(13) 0.0254(13) 0.0330(14) -0.0010(10) -0.0017(10) -0.0081(10) C5 0.0273(13) 0.0297(13) 0.0320(14) 0.0008(10) -0.0050(10) -0.0081(10) C6 0.0305(13) 0.0307(13) 0.0314(14) 0.0000(11) -0.0069(10) -0.0100(11) C7 0.0306(14) 0.0350(15) 0.0412(16) -0.0032(12) -0.0117(12) -0.0111(11) C8 0.0323(14) 0.0373(15) 0.0394(15) -0.0064(12) -0.0095(12) -0.0133(12) C9 0.0341(14) 0.0294(13) 0.0319(14) -0.0032(10) -0.0076(11) -0.0144(11) C10 0.0349(14) 0.0266(13) 0.0309(13) -0.0040(10) -0.0030(11) -0.0135(11) C11 0.0341(14) 0.0245(13) 0.0345(14) -0.0048(10) -0.0040(11) -0.0110(11) C12 0.0335(14) 0.0287(13) 0.0419(15) -0.0107(11) -0.0011(11) -0.0110(11) C13 0.0304(13) 0.0276(13) 0.0383(15) -0.0066(11) -0.0007(11) -0.0080(11) C14 0.0305(13) 0.0239(12) 0.0325(14) -0.0023(10) -0.0015(10) -0.0096(10) C15 0.0248(12) 0.0256(12) 0.0315(13) 0.0000(10) -0.0013(10) -0.0088(10) C16 0.0271(12) 0.0258(12) 0.0300(13) -0.0018(10) -0.0029(10) -0.0103(10) C17 0.0278(13) 0.0312(14) 0.0344(14) -0.0023(11) -0.0074(10) -0.0110(11) C18 0.0319(13) 0.0311(14) 0.0354(14) -0.0070(11) -0.0046(11) -0.0143(11) C19 0.0298(13) 0.0253(12) 0.0330(13) -0.0037(10) -0.0039(10) -0.0129(10) C20 0.0328(13) 0.0257(13) 0.0348(14) -0.0050(10) -0.0033(11) -0.0123(11) C21 0.0327(14) 0.0274(13) 0.0407(15) -0.0047(11) -0.0064(11) -0.0095(11) C22 0.0335(14) 0.0296(14) 0.0447(16) -0.0075(12) -0.0067(12) -0.0091(11) C23 0.0290(13) 0.0302(14) 0.0359(14) -0.0036(11) -0.0061(11) -0.0070(11) C24 0.0292(13) 0.0302(13) 0.0385(15) -0.0038(11) -0.0040(11) -0.0104(11) C25 0.0328(14) 0.0292(14) 0.0391(15) -0.0025(11) -0.0070(11) -0.0090(11) C26 0.0285(14) 0.0334(15) 0.0504(17) -0.0039(13) -0.0082(12) -0.0040(11) C27 0.0285(14) 0.0371(15) 0.0483(17) -0.0027(13) -0.0040(12) -0.0095(12) C28 0.0322(14) 0.0329(14) 0.0415(16) 0.0006(12) -0.0054(12) -0.0110(11) C29 0.0362(15) 0.0305(14) 0.0441(16) 0.0014(12) -0.0113(12) -0.0093(12) C30 0.061(2) 0.0389(17) 0.052(2) 0.0075(14) -0.0040(16) -0.0164(15) C31 0.068(2) 0.0370(17) 0.057(2) 0.0031(15) -0.0173(17) -0.0215(16) C32 0.0448(18) 0.0437(18) 0.072(2) 0.0165(16) -0.0187(16) -0.0126(15) C33 0.0322(16) 0.055(2) 0.069(2) 0.0049(17) -0.0021(15) -0.0165(14) C34 0.063(3) 0.097(4) 0.148(5) -0.043(3) 0.053(3) -0.038(3) C35 0.054(2) 0.078(3) 0.122(4) 0.027(3) -0.033(2) -0.038(2) C36 0.046(2) 0.073(3) 0.098(3) 0.021(2) -0.003(2) -0.0310(19) C37 0.0293(13) 0.0280(13) 0.0381(14) -0.0080(11) -0.0002(11) -0.0130(10) C38 0.0360(14) 0.0316(14) 0.0365(15) -0.0022(11) -0.0038(11) -0.0164(11) C39 0.0378(15) 0.0379(15) 0.0339(14) -0.0064(12) -0.0021(11) -0.0174(12) C40 0.0385(15) 0.0328(14) 0.0436(16) -0.0073(12) -0.0029(12) -0.0190(12) C41 0.0302(13) 0.0296(14) 0.0480(17) -0.0010(12) -0.0030(12) -0.0125(11) C42 0.0275(13) 0.0334(14) 0.0369(14) -0.0035(11) -0.0047(11) -0.0122(11) C43 0.0546(18) 0.0443(17) 0.0374(16) -0.0025(13) -0.0115(13) -0.0252(15) C44 0.073(2) 0.0512(19) 0.0447(19) 0.0048(15) -0.0239(17) -0.0267(18) C45 0.063(2) 0.070(2) 0.060(2) 0.0058(18) -0.0268(18) -0.034(2) C46 0.081(3) 0.059(2) 0.0376(18) -0.0085(15) -0.0053(17) -0.0285(19) C47 0.0410(16) 0.0304(15) 0.061(2) 0.0033(13) -0.0101(14) -0.0137(12) C48 0.059(2) 0.0475(19) 0.073(2) 0.0151(17) -0.0129(18) -0.0298(17) C49 0.060(2) 0.0320(17) 0.098(3) -0.0032(18) 0.000(2) -0.0055(16) C50 0.071(2) 0.0446(19) 0.083(3) 0.0219(18) -0.031(2) -0.0257(18) C51 0.0293(13) 0.0259(13) 0.0305(13) -0.0043(10) -0.0046(10) -0.0075(10) C52 0.0373(14) 0.0285(13) 0.0331(14) -0.0032(11) -0.0001(11) -0.0096(11) C53 0.0450(16) 0.0290(14) 0.0328(14) -0.0031(11) -0.0038(12) -0.0032(12) C54 0.0389(16) 0.0357(16) 0.0451(17) -0.0074(13) -0.0128(13) 0.0015(12) C55 0.0289(14) 0.0381(15) 0.0448(16) -0.0088(12) -0.0076(12) -0.0075(12) C56 0.0308(13) 0.0286(13) 0.0347(14) -0.0019(11) -0.0064(11) -0.0079(11) C57 0.062(2) 0.0319(16) 0.0441(18) 0.0061(13) -0.0032(15) -0.0011(14) C58 0.089(3) 0.051(2) 0.094(3) 0.021(2) 0.009(3) -0.021(2) C59 0.119(4) 0.036(2) 0.077(3) 0.0014(19) 0.025(3) -0.005(2) C60 0.151(5) 0.057(3) 0.058(3) 0.009(2) -0.018(3) -0.021(3) C61 0.0305(16) 0.0501(19) 0.084(3) -0.0049(18) -0.0138(16) -0.0130(14) C62 0.046(2) 0.066(3) 0.189(6) -0.036(3) -0.009(3) -0.027(2) C63 0.0333(18) 0.087(3) 0.102(3) -0.006(3) -0.021(2) -0.0141(19) C64 0.043(2) 0.084(3) 0.088(3) 0.012(2) 0.0024(19) -0.029(2) C65 0.0444(17) 0.059(2) 0.0467(18) -0.0064(15) 0.0033(14) -0.0295(16) O2 0.0591(14) 0.0504(13) 0.0411(12) 0.0007(10) -0.0112(10) -0.0223(11) C66 0.066(2) 0.066(2) 0.0468(19) -0.0085(17) 0.0022(16) -0.0362(19) C67 0.099(4) 0.110(4) 0.061(3) -0.001(3) -0.008(3) -0.029(3) Cl1 0.0906(8) 0.0907(9) 0.0807(8) -0.0151(6) 0.0073(6) -0.0087(7) Cl2 0.0799(8) 0.0840(8) 0.0958(9) -0.0188(6) 0.0035(6) -0.0301(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 Zn N3 2.050(2) . ? Zn N4 2.062(2) . ? Zn N2 2.062(2) . ? Zn N1 2.064(2) . ? Zn O1 2.158(2) . ? O1 C65 1.423(3) . ? N1 C1 1.365(3) . ? N1 C4 1.382(3) . ? N2 C6 1.376(3) . ? N2 C9 1.377(3) . ? N3 C14 1.372(3) . ? N3 C11 1.383(3) . ? N4 C19 1.369(3) . ? N4 C16 1.383(3) . ? C1 C20 1.413(4) . ? C1 C2 1.436(4) . ? C2 C3 1.351(4) . ? C3 C4 1.432(4) . ? C4 C5 1.398(4) . ? C5 C6 1.412(4) . ? C5 C23 1.502(3) . ? C6 C7 1.439(4) . ? C7 C8 1.338(4) . ? C8 C9 1.444(4) . ? C9 C10 1.413(4) . ? C10 C11 1.409(4) . ? C10 C37 1.498(3) . ? C11 C12 1.445(4) . ? C12 C13 1.357(4) . ? C13 C14 1.440(4) . ? C14 C15 1.410(4) . ? C15 C16 1.409(3) . ? C15 C51 1.494(3) . ? C16 C17 1.441(3) . ? C17 C18 1.347(4) . ? C18 C19 1.433(4) . ? C19 C20 1.405(4) . ? C20 C21 1.427(3) . ? C21 C22 1.202(4) . ? C22 C22 1.371(5) 2_656 ? C23 C24 1.389(4) . ? C23 C28 1.390(4) . ? C24 C25 1.398(4) . ? C25 C26 1.401(4) . ? C25 C29 1.537(4) . ? C26 C27 1.395(4) . ? C27 C28 1.391(4) . ? C27 C33 1.530(4) . ? C29 C32 1.525(4) . ? C29 C30 1.530(5) . ? C29 C31 1.537(4) . ? C33 C34 1.508(6) . ? C33 C36 1.531(5) . ? C33 C35 1.539(6) . ? C37 C38 1.393(4) . ? C37 C42 1.399(4) . ? C38 C39 1.397(4) . ? C39 C40 1.395(4) . ? C39 C43 1.532(4) . ? C40 C41 1.393(4) . ? C41 C42 1.397(4) . ? C41 C47 1.527(4) . ? C43 C44 1.536(4) . ? C43 C45 1.539(5) . ? C43 C46 1.540(5) . ? C47 C50 1.522(5) . ? C47 C48 1.532(4) . ? C47 C49 1.545(5) . ? C51 C56 1.386(4) . ? C51 C52 1.400(4) . ? C52 C53 1.386(4) . ? C53 C54 1.392(5) . ? C53 C57 1.537(4) . ? C54 C55 1.390(4) . ? C55 C56 1.400(4) . ? C55 C61 1.535(4) . ? C57 C60 1.500(6) . ? C57 C59 1.503(5) . ? C57 C58 1.576(6) . ? C61 C62 1.520(5) . ? C61 C63 1.539(5) . ? C61 C64 1.551(6) . ? O2 C66 1.422(4) . ? C67 Cl2 1.729(5) . ? C67 Cl1 1.742(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Zn N4 89.19(8) . . ? N3 Zn N2 89.95(8) . . ? N4 Zn N2 167.19(9) . . ? N3 Zn N1 165.54(9) . . ? N4 Zn N1 89.21(8) . . ? N2 Zn N1 88.44(8) . . ? N3 Zn O1 92.69(9) . . ? N4 Zn O1 93.26(8) . . ? N2 Zn O1 99.55(8) . . ? N1 Zn O1 101.75(9) . . ? C65 O1 Zn 122.86(18) . . ? C1 N1 C4 105.7(2) . . ? C1 N1 Zn 126.05(17) . . ? C4 N1 Zn 127.26(17) . . ? C6 N2 C9 106.6(2) . . ? C6 N2 Zn 127.10(17) . . ? C9 N2 Zn 125.87(17) . . ? C14 N3 C11 106.7(2) . . ? C14 N3 Zn 127.04(17) . . ? C11 N3 Zn 126.23(17) . . ? C19 N4 C16 106.0(2) . . ? C19 N4 Zn 126.14(17) . . ? C16 N4 Zn 126.35(16) . . ? N1 C1 C20 125.1(2) . . ? N1 C1 C2 110.6(2) . . ? C20 C1 C2 124.3(2) . . ? C3 C2 C1 106.6(2) . . ? C2 C3 C4 107.4(2) . . ? N1 C4 C5 125.5(2) . . ? N1 C4 C3 109.7(2) . . ? C5 C4 C3 124.7(2) . . ? C4 C5 C6 124.8(2) . . ? C4 C5 C23 117.3(2) . . ? C6 C5 C23 117.9(2) . . ? N2 C6 C5 125.7(2) . . ? N2 C6 C7 109.3(2) . . ? C5 C6 C7 125.0(2) . . ? C8 C7 C6 107.5(2) . . ? C7 C8 C9 107.5(2) . . ? N2 C9 C10 125.4(2) . . ? N2 C9 C8 109.1(2) . . ? C10 C9 C8 125.4(2) . . ? C11 C10 C9 125.2(2) . . ? C11 C10 C37 117.9(2) . . ? C9 C10 C37 116.9(2) . . ? N3 C11 C10 125.7(2) . . ? N3 C11 C12 109.2(2) . . ? C10 C11 C12 125.1(2) . . ? C13 C12 C11 107.1(2) . . ? C12 C13 C14 107.3(2) . . ? N3 C14 C15 125.7(2) . . ? N3 C14 C13 109.6(2) . . ? C15 C14 C13 124.7(2) . . ? C16 C15 C14 125.2(2) . . ? C16 C15 C51 116.6(2) . . ? C14 C15 C51 118.2(2) . . ? N4 C16 C15 124.8(2) . . ? N4 C16 C17 109.4(2) . . ? C15 C16 C17 125.8(2) . . ? C18 C17 C16 107.1(2) . . ? C17 C18 C19 107.3(2) . . ? N4 C19 C20 124.8(2) . . ? N4 C19 C18 110.1(2) . . ? C20 C19 C18 125.1(2) . . ? C19 C20 C1 126.2(2) . . ? C19 C20 C21 117.9(2) . . ? C1 C20 C21 115.8(2) . . ? C22 C21 C20 176.0(3) . . ? C21 C22 C22 179.2(4) . 2_656 ? C24 C23 C28 119.5(2) . . ? C24 C23 C5 120.3(2) . . ? C28 C23 C5 120.2(2) . . ? C23 C24 C25 121.6(3) . . ? C24 C25 C26 117.1(3) . . ? C24 C25 C29 120.3(2) . . ? C26 C25 C29 122.6(2) . . ? C27 C26 C25 122.8(3) . . ? C28 C27 C26 117.9(3) . . ? C28 C27 C33 122.0(3) . . ? C26 C27 C33 120.0(3) . . ? C23 C28 C27 121.2(3) . . ? C32 C29 C30 107.8(3) . . ? C32 C29 C25 112.4(2) . . ? C30 C29 C25 110.7(2) . . ? C32 C29 C31 108.1(3) . . ? C30 C29 C31 109.3(3) . . ? C25 C29 C31 108.5(2) . . ? C34 C33 C27 109.5(3) . . ? C34 C33 C36 110.1(4) . . ? C27 C33 C36 112.4(3) . . ? C34 C33 C35 109.9(4) . . ? C27 C33 C35 109.3(3) . . ? C36 C33 C35 105.5(3) . . ? C38 C37 C42 119.4(2) . . ? C38 C37 C10 121.0(2) . . ? C42 C37 C10 119.5(2) . . ? C37 C38 C39 121.3(3) . . ? C40 C39 C38 117.5(3) . . ? C40 C39 C43 120.5(2) . . ? C38 C39 C43 122.0(3) . . ? C41 C40 C39 123.0(2) . . ? C40 C41 C42 117.8(2) . . ? C40 C41 C47 119.5(2) . . ? C42 C41 C47 122.7(3) . . ? C41 C42 C37 120.9(3) . . ? C39 C43 C44 111.6(2) . . ? C39 C43 C45 109.6(3) . . ? C44 C43 C45 107.1(3) . . ? C39 C43 C46 109.1(3) . . ? C44 C43 C46 109.4(3) . . ? C45 C43 C46 109.9(3) . . ? C50 C47 C41 112.6(3) . . ? C50 C47 C48 108.3(3) . . ? C41 C47 C48 109.6(2) . . ? C50 C47 C49 109.5(3) . . ? C41 C47 C49 108.3(3) . . ? C48 C47 C49 108.5(3) . . ? C56 C51 C52 119.4(2) . . ? C56 C51 C15 121.5(2) . . ? C52 C51 C15 119.1(2) . . ? C53 C52 C51 120.7(3) . . ? C52 C53 C54 118.2(3) . . ? C52 C53 C57 121.6(3) . . ? C54 C53 C57 120.2(3) . . ? C55 C54 C53 122.9(3) . . ? C54 C55 C56 117.2(3) . . ? C54 C55 C61 123.1(3) . . ? C56 C55 C61 119.6(3) . . ? C51 C56 C55 121.4(3) . . ? C60 C57 C59 112.2(4) . . ? C60 C57 C53 110.0(3) . . ? C59 C57 C53 109.6(3) . . ? C60 C57 C58 106.1(4) . . ? C59 C57 C58 106.9(4) . . ? C53 C57 C58 112.0(3) . . ? C62 C61 C55 110.6(3) . . ? C62 C61 C63 108.1(3) . . ? C55 C61 C63 111.2(3) . . ? C62 C61 C64 111.2(4) . . ? C55 C61 C64 108.1(3) . . ? C63 C61 C64 107.6(3) . . ? Cl2 C67 Cl1 114.4(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.064 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.104 #===END