Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Tristram Chivers' _publ_contact_author_address ; Chemistry University of Calgary 2500 University Drive NW Calgary Alberta T2N 1N4 CANADA ; _publ_contact_author_email CHIVERS@UCALGARY.CA _publ_section_title ; Zinc complexes of anionic NPPN and N(S)PPN ligands and rearrangement to the isomeric NPNP and N(S)PNP ligands in mercury complexes ; loop_ _publ_author_name T.Chivers 'May Copsey' #===END data_complex8 _database_code_depnum_ccdc_archive 'CCDC 606734' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C44 H62 N2 P2 S Zn), 0.5(C6 H14)' _chemical_formula_sum 'C91 H131 N4 P4 S2 Zn2' _chemical_formula_weight 1599.74 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' S S 0.1246 0.1234 '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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.576(3) _cell_length_b 19.155(4) _cell_length_c 20.483(4) _cell_angle_alpha 112.34(3) _cell_angle_beta 99.04(3) _cell_angle_gamma 90.96(3) _cell_volume 4491(2) _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 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1714 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8452 _exptl_absorpt_correction_T_max 0.9660 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski and Minor 1997)' _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 'phi/omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14758 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0998 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 25.03 _reflns_number_total 14758 _reflns_number_gt 9159 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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 ; The complex crystallizes with two independent, chemically-equivalent molecules in the asymmetric unit and one ordered molecule of n-hexane, which lies on the inversion centre. Geometric restraints were applied to obtain reasonable C-C distances. The refinement was complicated by twinning of the data, stalling at R = 0.1260 and wR2 = 0.4161, with all atoms present and anisotropic. There were many signs of twinning, including an unusually large ratio of data to parameters and a significant number of high intensity bad reflections. Application of the twin determination program ROTAX (WinGX) showed that twinning occurred in a 180 degree rotation about the [1 -1 1] reciprocal lattice direction. WinGX was used to prepare an HKLF5 file for further refinement. 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^)+(0.0677P)^2^+1.0293P] 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 14759 _refine_ls_number_parameters 953 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1191 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1508 _refine_ls_wR_factor_gt 0.1228 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.032 _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 Zn1 Zn 0.40654(4) 0.19677(3) 0.22681(3) 0.03413(16) Uani 1 1 d . . . Zn2 Zn 0.01891(4) 0.68291(3) 0.27573(3) 0.02984(16) Uani 1 1 d . . . N1 N 0.5151(4) 0.1652(2) 0.2889(2) 0.0327(11) Uani 1 1 d . . . N2 N 0.5059(3) 0.2729(2) 0.2178(2) 0.0290(9) Uani 1 1 d . . . N3 N -0.1261(3) 0.6963(2) 0.2287(2) 0.0277(9) Uani 1 1 d . . . N4 N 0.0969(3) 0.76802(19) 0.2650(2) 0.0286(9) Uani 1 1 d . . . P1 P 0.64112(10) 0.18273(7) 0.28996(7) 0.0315(3) Uani 1 1 d . . . P2 P 0.63001(10) 0.28356(7) 0.25855(7) 0.0284(3) Uani 1 1 d . . . P3 P -0.13090(11) 0.74342(7) 0.17712(7) 0.0316(3) Uani 1 1 d . . . P4 P 0.02889(11) 0.81553(7) 0.22504(7) 0.0293(3) Uani 1 1 d . . . S1 S 0.74772(11) 0.19892(8) 0.37526(7) 0.0454(4) Uani 1 1 d . . . S2 S -0.25441(12) 0.79901(8) 0.16403(8) 0.0459(4) Uani 1 1 d . . . C1 C 0.4811(5) 0.1300(3) 0.3349(3) 0.0355(15) Uani 1 1 d . . . C2 C 0.4588(5) 0.1756(3) 0.4030(3) 0.0418(14) Uani 1 1 d . . . C3 C 0.4244(5) 0.1423(4) 0.4457(3) 0.0539(17) Uani 1 1 d . . . H3 H 0.4113 0.1735 0.4919 0.065 Uiso 1 1 calc R . . C4 C 0.4088(5) 0.0668(4) 0.4234(4) 0.0618(18) Uani 1 1 d . . . H4 H 0.3831 0.0451 0.4533 0.074 Uiso 1 1 calc R . . C5 C 0.4301(5) 0.0201(3) 0.3567(4) 0.0587(17) Uani 1 1 d . . . H5 H 0.4203 -0.0334 0.3417 0.070 Uiso 1 1 calc R . . C6 C 0.4658(4) 0.0511(3) 0.3117(3) 0.0414(13) Uani 1 1 d . . . C7 C 0.4899(5) -0.0012(3) 0.2398(4) 0.0520(16) Uani 1 1 d . . . H7 H 0.4928 0.0289 0.2095 0.062 Uiso 1 1 calc R . . C8 C 0.6009(7) -0.0303(4) 0.2511(4) 0.094(3) Uani 1 1 d . . . H8A H 0.6001 -0.0597 0.2811 0.141 Uiso 1 1 calc R . . H8B H 0.6556 0.0128 0.2749 0.141 Uiso 1 1 calc R . . H8C H 0.6183 -0.0625 0.2046 0.141 Uiso 1 1 calc R . . C9 C 0.4029(7) -0.0674(3) 0.1998(4) 0.084(3) Uani 1 1 d . . . H9A H 0.4193 -0.0972 0.1523 0.127 Uiso 1 1 calc R . . H9B H 0.3321 -0.0476 0.1946 0.127 Uiso 1 1 calc R . . H9C H 0.4018 -0.0997 0.2271 0.127 Uiso 1 1 calc R . . C10 C 0.4723(5) 0.2622(3) 0.4310(3) 0.0490(17) Uani 1 1 d . . . H10 H 0.5069 0.2763 0.3965 0.059 Uiso 1 1 calc R . . C11 C 0.5461(6) 0.2973(4) 0.5049(3) 0.079(2) Uani 1 1 d . . . H11A H 0.5144 0.2840 0.5398 0.118 Uiso 1 1 calc R . . H11B H 0.5536 0.3525 0.5204 0.118 Uiso 1 1 calc R . . H11C H 0.6174 0.2777 0.5016 0.118 Uiso 1 1 calc R . . C12 C 0.3613(7) 0.2942(4) 0.4331(5) 0.095(3) Uani 1 1 d . . . H12A H 0.3178 0.2738 0.3848 0.143 Uiso 1 1 calc R . . H12B H 0.3706 0.3495 0.4506 0.143 Uiso 1 1 calc R . . H12C H 0.3244 0.2796 0.4654 0.143 Uiso 1 1 calc R . . C13 C 0.6856(4) 0.1169(3) 0.2102(3) 0.0328(12) Uani 1 1 d . . . C14 C 0.6164(5) 0.0895(3) 0.1436(3) 0.0419(14) Uani 1 1 d . . . H14 H 0.5450 0.1048 0.1397 0.050 Uiso 1 1 calc R . . C15 C 0.6519(5) 0.0404(3) 0.0838(3) 0.0576(17) Uani 1 1 d . . . H15 H 0.6042 0.0217 0.0389 0.069 Uiso 1 1 calc R . . C16 C 0.7557(6) 0.0180(4) 0.0880(4) 0.071(2) Uani 1 1 d . . . H16 H 0.7798 -0.0151 0.0461 0.085 Uiso 1 1 calc R . . C17 C 0.8249(5) 0.0443(4) 0.1541(4) 0.0686(19) Uani 1 1 d . . . H17 H 0.8958 0.0280 0.1580 0.082 Uiso 1 1 calc R . . C18 C 0.7895(5) 0.0942(3) 0.2139(3) 0.0507(15) Uani 1 1 d . . . H18 H 0.8376 0.1135 0.2586 0.061 Uiso 1 1 calc R . . C19 C 0.6686(4) 0.3745(3) 0.3322(3) 0.0333(11) Uani 1 1 d . . . C20 C 0.6874(4) 0.4364(3) 0.3157(3) 0.0419(13) Uani 1 1 d . . . H20 H 0.6811 0.4304 0.2670 0.050 Uiso 1 1 calc R . . C21 C 0.7163(5) 0.5096(3) 0.3715(4) 0.0527(17) Uani 1 1 d . . . H21 H 0.7310 0.5523 0.3605 0.063 Uiso 1 1 calc R . . C22 C 0.7225(5) 0.5168(3) 0.4413(4) 0.0573(18) Uani 1 1 d . . . H22 H 0.7411 0.5652 0.4789 0.069 Uiso 1 1 calc R . . C23 C 0.7021(6) 0.4552(4) 0.4575(4) 0.0532(19) Uani 1 1 d . . . H23 H 0.7063 0.4613 0.5061 0.064 Uiso 1 1 calc R . . C24 C 0.6755(4) 0.3845(3) 0.4035(3) 0.0409(14) Uani 1 1 d . . . H24 H 0.6618 0.3421 0.4152 0.049 Uiso 1 1 calc R . . C25 C 0.7320(4) 0.2785(3) 0.2033(3) 0.0360(13) Uani 1 1 d D . . H25A H 0.7231 0.2280 0.1636 0.043 Uiso 1 1 calc R . . H25B H 0.7206 0.3169 0.1819 0.043 Uiso 1 1 calc R . . C26 C 0.8465(4) 0.2919(4) 0.2452(3) 0.0498(18) Uani 1 1 d D . . H26A H 0.8512 0.2653 0.2785 0.060 Uiso 1 1 calc R . . H26B H 0.8630 0.3467 0.2743 0.060 Uiso 1 1 calc R . . C27 C 0.9305(5) 0.2644(4) 0.1970(3) 0.0669(19) Uani 1 1 d D . . H27A H 1.0028 0.2734 0.2275 0.080 Uiso 1 1 calc R . . H27B H 0.9158 0.2091 0.1697 0.080 Uiso 1 1 calc R . . C28 C 0.9325(6) 0.3023(5) 0.1451(5) 0.090(3) Uani 1 1 d D . . H28A H 0.8646 0.2881 0.1105 0.135 Uiso 1 1 calc R . . H28B H 0.9932 0.2861 0.1196 0.135 Uiso 1 1 calc R . . H28C H 0.9411 0.3573 0.1713 0.135 Uiso 1 1 calc R . . C29 C 0.4654(4) 0.3249(3) 0.1858(3) 0.0309(12) Uani 1 1 d . . . C30 C 0.4143(5) 0.3881(3) 0.2254(3) 0.0375(15) Uani 1 1 d . . . C31 C 0.3743(5) 0.4365(3) 0.1924(4) 0.0537(18) Uani 1 1 d . . . H31 H 0.3408 0.4799 0.2189 0.064 Uiso 1 1 calc R . . C32 C 0.3821(6) 0.4231(4) 0.1238(4) 0.060(2) Uani 1 1 d . . . H32 H 0.3543 0.4571 0.1029 0.072 Uiso 1 1 calc R . . C33 C 0.4308(5) 0.3595(3) 0.0830(3) 0.0509(15) Uani 1 1 d . . . H33 H 0.4362 0.3509 0.0348 0.061 Uiso 1 1 calc R . . C34 C 0.4712(4) 0.3088(3) 0.1129(3) 0.0381(12) Uani 1 1 d . . . C35 C 0.5157(5) 0.2381(3) 0.0649(3) 0.0408(13) Uani 1 1 d . . . H35 H 0.5540 0.2144 0.0969 0.049 Uiso 1 1 calc R . . C36 C 0.5975(6) 0.2531(4) 0.0235(4) 0.066(2) Uani 1 1 d . . . H36A H 0.6295 0.2060 -0.0012 0.099 Uiso 1 1 calc R . . H36B H 0.6545 0.2911 0.0568 0.099 Uiso 1 1 calc R . . H36C H 0.5614 0.2719 -0.0119 0.099 Uiso 1 1 calc R . . C37 C 0.4243(5) 0.1809(3) 0.0144(4) 0.0639(19) Uani 1 1 d . . . H37A H 0.3819 0.2032 -0.0160 0.096 Uiso 1 1 calc R . . H37B H 0.3776 0.1671 0.0424 0.096 Uiso 1 1 calc R . . H37C H 0.4546 0.1355 -0.0158 0.096 Uiso 1 1 calc R . . C38 C 0.3966(5) 0.4036(3) 0.3013(3) 0.0486(15) Uani 1 1 d . . . H38 H 0.4445 0.3717 0.3200 0.058 Uiso 1 1 calc R . . C39 C 0.2801(6) 0.3798(4) 0.3011(5) 0.074(2) Uani 1 1 d . . . H39A H 0.2307 0.4055 0.2774 0.112 Uiso 1 1 calc R . . H39B H 0.2687 0.3938 0.3506 0.112 Uiso 1 1 calc R . . H39C H 0.2660 0.3249 0.2753 0.112 Uiso 1 1 calc R . . C40 C 0.4245(5) 0.4864(3) 0.3536(3) 0.0622(17) Uani 1 1 d . . . H40A H 0.4991 0.5022 0.3537 0.093 Uiso 1 1 calc R . . H40B H 0.4171 0.4912 0.4020 0.093 Uiso 1 1 calc R . . H40C H 0.3752 0.5188 0.3386 0.093 Uiso 1 1 calc R . . C41 C 0.2590(6) 0.1490(4) 0.1759(4) 0.0556(19) Uani 1 1 d . . . C42 C 0.1956(6) 0.1923(5) 0.1385(4) 0.083(2) Uani 1 1 d . . . H42A H 0.2356 0.1994 0.1038 0.125 Uiso 1 1 calc R . . H42B H 0.1839 0.2418 0.1738 0.125 Uiso 1 1 calc R . . H42C H 0.1257 0.1641 0.1134 0.125 Uiso 1 1 calc R . . C43 C 0.2792(8) 0.0727(4) 0.1198(5) 0.093(3) Uani 1 1 d . . . H43A H 0.2112 0.0487 0.0874 0.139 Uiso 1 1 calc R . . H43B H 0.3078 0.0398 0.1440 0.139 Uiso 1 1 calc R . . H43C H 0.3316 0.0809 0.0922 0.139 Uiso 1 1 calc R . . C44 C 0.1958(7) 0.1351(7) 0.2290(5) 0.115(4) Uani 1 1 d . . . H44A H 0.1872 0.1837 0.2669 0.172 Uiso 1 1 calc R . . H44B H 0.2355 0.1032 0.2504 0.172 Uiso 1 1 calc R . . H44C H 0.1244 0.1096 0.2035 0.172 Uiso 1 1 calc R . . C45 C -0.2237(4) 0.6744(3) 0.2475(3) 0.0324(12) Uani 1 1 d . . . C46 C -0.2854(4) 0.6060(3) 0.2020(3) 0.0378(13) Uani 1 1 d . . . C47 C -0.3773(5) 0.5850(3) 0.2228(4) 0.0518(16) Uani 1 1 d . . . H47 H -0.4191 0.5390 0.1926 0.062 Uiso 1 1 calc R . . C48 C -0.4089(5) 0.6295(3) 0.2864(4) 0.0502(16) Uani 1 1 d . . . H48 H -0.4724 0.6147 0.2993 0.060 Uiso 1 1 calc R . . C49 C -0.3480(4) 0.6947(3) 0.3305(3) 0.0458(14) Uani 1 1 d . . . H49 H -0.3689 0.7243 0.3748 0.055 Uiso 1 1 calc R . . C50 C -0.2548(4) 0.7199(3) 0.3124(3) 0.0337(12) Uani 1 1 d . . . C51 C -0.1922(4) 0.7923(3) 0.3639(3) 0.0404(13) Uani 1 1 d . . . H51 H -0.1295 0.8006 0.3424 0.048 Uiso 1 1 calc R . . C52 C -0.2604(5) 0.8598(3) 0.3738(4) 0.0575(17) Uani 1 1 d . . . H52A H -0.3194 0.8556 0.3985 0.086 Uiso 1 1 calc R . . H52B H -0.2905 0.8601 0.3268 0.086 Uiso 1 1 calc R . . H52C H -0.2150 0.9069 0.4024 0.086 Uiso 1 1 calc R . . C53 C -0.1472(5) 0.7894(4) 0.4358(3) 0.0675(18) Uani 1 1 d . . . H53A H -0.0983 0.8347 0.4647 0.101 Uiso 1 1 calc R . . H53B H -0.1076 0.7441 0.4284 0.101 Uiso 1 1 calc R . . H53C H -0.2067 0.7873 0.4609 0.101 Uiso 1 1 calc R . . C54 C -0.2553(6) 0.5545(4) 0.1306(4) 0.0521(19) Uani 1 1 d . . . H54 H -0.1798 0.5710 0.1298 0.063 Uiso 1 1 calc R . . C55 C -0.3304(7) 0.5627(4) 0.0678(3) 0.082(2) Uani 1 1 d . . . H55A H -0.3033 0.5358 0.0232 0.122 Uiso 1 1 calc R . . H55B H -0.3325 0.6164 0.0759 0.122 Uiso 1 1 calc R . . H55C H -0.4033 0.5410 0.0640 0.122 Uiso 1 1 calc R . . C56 C -0.2583(5) 0.4710(3) 0.1223(4) 0.0641(18) Uani 1 1 d . . . H56A H -0.2102 0.4667 0.1630 0.096 Uiso 1 1 calc R . . H56B H -0.2344 0.4401 0.0776 0.096 Uiso 1 1 calc R . . H56C H -0.3323 0.4530 0.1212 0.096 Uiso 1 1 calc R . . C57 C -0.0935(4) 0.6855(3) 0.0921(3) 0.0394(13) Uani 1 1 d . . . C58 C -0.1400(5) 0.6943(3) 0.0292(3) 0.0495(15) Uani 1 1 d . . . H58 H -0.1942 0.7285 0.0301 0.059 Uiso 1 1 calc R . . C59 C -0.1055(6) 0.6521(4) -0.0352(3) 0.073(2) Uani 1 1 d . . . H59 H -0.1379 0.6570 -0.0782 0.088 Uiso 1 1 calc R . . C60 C -0.0258(7) 0.6040(4) -0.0369(4) 0.070(2) Uani 1 1 d . . . H60 H -0.0020 0.5770 -0.0808 0.085 Uiso 1 1 calc R . . C61 C 0.0195(5) 0.5943(3) 0.0235(3) 0.0541(16) Uani 1 1 d . . . H61 H 0.0749 0.5608 0.0219 0.065 Uiso 1 1 calc R . . C62 C -0.0154(4) 0.6335(3) 0.0876(3) 0.0399(13) Uani 1 1 d . . . H62 H 0.0142 0.6249 0.1293 0.048 Uiso 1 1 calc R . . C63 C 0.0196(4) 0.9145(2) 0.2807(3) 0.0328(11) Uani 1 1 d . . . C64 C 0.1121(4) 0.9644(3) 0.3008(3) 0.0407(13) Uani 1 1 d . . . H64 H 0.1781 0.9462 0.2868 0.049 Uiso 1 1 calc R . . C65 C 0.1071(5) 1.0408(3) 0.3413(3) 0.0492(15) Uani 1 1 d . . . H65 H 0.1698 1.0749 0.3543 0.059 Uiso 1 1 calc R . . C66 C 0.0120(5) 1.0675(3) 0.3627(3) 0.0485(16) Uani 1 1 d . . . H66 H 0.0089 1.1199 0.3898 0.058 Uiso 1 1 calc R . . C67 C -0.0777(6) 1.0184(3) 0.3450(3) 0.0452(17) Uani 1 1 d . . . H67 H -0.1425 1.0367 0.3612 0.054 Uiso 1 1 calc R . . C68 C -0.0753(5) 0.9423(3) 0.3037(3) 0.0360(14) Uani 1 1 d . . . H68 H -0.1386 0.9089 0.2910 0.043 Uiso 1 1 calc R . . C69 C 0.0867(4) 0.8245(3) 0.1527(3) 0.0352(12) Uani 1 1 d D . . H69A H 0.1629 0.8454 0.1716 0.042 Uiso 1 1 calc R . . H69B H 0.0871 0.7732 0.1154 0.042 Uiso 1 1 calc R . . C70 C 0.0300(6) 0.8741(4) 0.1172(3) 0.053(2) Uani 1 1 d D . . H70A H 0.0379 0.9273 0.1519 0.063 Uiso 1 1 calc R . . H70B H -0.0480 0.8573 0.1022 0.063 Uiso 1 1 calc R . . C71 C 0.0788(8) 0.8689(4) 0.0517(4) 0.095(3) Uani 1 1 d D . . H71A H 0.1575 0.8830 0.0663 0.113 Uiso 1 1 calc R . . H71B H 0.0676 0.8161 0.0158 0.113 Uiso 1 1 calc R . . C72 C 0.0270(8) 0.9209(5) 0.0184(5) 0.117(3) Uani 1 1 d D . . H72A H -0.0506 0.9060 0.0029 0.176 Uiso 1 1 calc R . . H72B H 0.0597 0.9172 -0.0230 0.176 Uiso 1 1 calc R . . H72C H 0.0384 0.9732 0.0539 0.176 Uiso 1 1 calc R . . C73 C 0.2093(4) 0.7906(3) 0.2991(3) 0.0320(12) Uani 1 1 d . . . C74 C 0.2915(4) 0.7617(3) 0.2589(3) 0.0351(12) Uani 1 1 d . . . C75 C 0.3996(4) 0.7833(3) 0.2940(3) 0.0455(14) Uani 1 1 d . . . H75 H 0.4568 0.7651 0.2684 0.055 Uiso 1 1 calc R . . C76 C 0.4227(5) 0.8313(3) 0.3659(3) 0.0516(15) Uani 1 1 d . . . H76 H 0.4958 0.8463 0.3890 0.062 Uiso 1 1 calc R . . C77 C 0.3422(5) 0.8570(3) 0.4039(3) 0.0417(15) Uani 1 1 d . . . H77 H 0.3602 0.8885 0.4535 0.050 Uiso 1 1 calc R . . C78 C 0.2337(4) 0.8383(3) 0.3720(3) 0.0313(12) Uani 1 1 d . . . C79 C 0.1495(4) 0.8645(3) 0.4183(3) 0.0337(12) Uani 1 1 d . . . H79 H 0.0785 0.8585 0.3860 0.040 Uiso 1 1 calc R . . C80 C 0.1674(5) 0.9466(3) 0.4718(3) 0.0582(17) Uani 1 1 d . . . H80A H 0.2295 0.9520 0.5093 0.087 Uiso 1 1 calc R . . H80B H 0.1028 0.9609 0.4934 0.087 Uiso 1 1 calc R . . H80C H 0.1815 0.9796 0.4469 0.087 Uiso 1 1 calc R . . C81 C 0.1414(5) 0.8112(3) 0.4593(3) 0.0565(17) Uani 1 1 d . . . H81A H 0.1206 0.7591 0.4247 0.085 Uiso 1 1 calc R . . H81B H 0.0869 0.8277 0.4901 0.085 Uiso 1 1 calc R . . H81C H 0.2116 0.8132 0.4888 0.085 Uiso 1 1 calc R . . C82 C 0.2686(4) 0.7028(3) 0.1829(3) 0.0430(13) Uani 1 1 d . . . H82 H 0.1900 0.7015 0.1641 0.052 Uiso 1 1 calc R . . C83 C 0.2905(6) 0.6239(3) 0.1820(4) 0.068(2) Uani 1 1 d . . . H83A H 0.2617 0.5854 0.1344 0.102 Uiso 1 1 calc R . . H83B H 0.2552 0.6150 0.2179 0.102 Uiso 1 1 calc R . . H83C H 0.3686 0.6210 0.1933 0.102 Uiso 1 1 calc R . . C84 C 0.3317(7) 0.7195(4) 0.1313(4) 0.068(3) Uani 1 1 d . . . H84A H 0.3167 0.7695 0.1311 0.103 Uiso 1 1 calc R . . H84B H 0.3094 0.6808 0.0828 0.103 Uiso 1 1 calc R . . H84C H 0.4093 0.7189 0.1470 0.103 Uiso 1 1 calc R . . C85 C 0.0535(6) 0.5270(3) 0.2308(4) 0.0533(17) Uani 1 1 d . . . H85A H 0.1207 0.5305 0.2132 0.080 Uiso 1 1 calc R . . H85B H -0.0082 0.5273 0.1952 0.080 Uiso 1 1 calc R . . H85C H 0.0478 0.4798 0.2388 0.080 Uiso 1 1 calc R . . C86 C 0.0537(4) 0.5945(3) 0.3013(3) 0.0357(12) Uani 1 1 d . . . C87 C 0.1590(5) 0.6008(3) 0.3507(3) 0.0602(17) Uani 1 1 d . . . H87A H 0.1689 0.5525 0.3560 0.090 Uiso 1 1 calc R . . H87B H 0.1577 0.6409 0.3977 0.090 Uiso 1 1 calc R . . H87C H 0.2187 0.6132 0.3304 0.090 Uiso 1 1 calc R . . C88 C -0.0404(5) 0.5756(4) 0.3341(4) 0.0610(19) Uani 1 1 d . . . H88A H -0.1092 0.5721 0.3025 0.092 Uiso 1 1 calc R . . H88B H -0.0406 0.6156 0.3813 0.092 Uiso 1 1 calc R . . H88C H -0.0310 0.5271 0.3392 0.092 Uiso 1 1 calc R . . C90 C 0.9969(7) 0.5422(3) 0.5050(5) 0.122(4) Uani 1 1 d D . . H90A H 1.0677 0.5614 0.5003 0.147 Uiso 1 1 calc R . . H90B H 0.9426 0.5445 0.4654 0.147 Uiso 1 1 calc R . . C91 C 0.9679(8) 0.5958(5) 0.5765(4) 0.125(4) Uani 1 1 d D . . H91A H 1.0234 0.5963 0.6168 0.151 Uiso 1 1 calc R . . H91B H 0.8975 0.5775 0.5825 0.151 Uiso 1 1 calc R . . C92 C 0.9617(8) 0.6779(5) 0.5778(6) 0.160(5) Uani 1 1 d D . . H92A H 1.0124 0.6864 0.5492 0.241 Uiso 1 1 calc R . . H92B H 0.9808 0.7148 0.6273 0.241 Uiso 1 1 calc R . . H92C H 0.8881 0.6839 0.5575 0.241 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 Zn1 0.0300(3) 0.0364(3) 0.0395(4) 0.0189(3) 0.0056(3) 0.0020(2) Zn2 0.0304(3) 0.0304(3) 0.0317(3) 0.0149(2) 0.0065(3) 0.0039(2) N1 0.046(3) 0.028(2) 0.033(3) 0.018(2) 0.017(2) 0.011(2) N2 0.028(2) 0.031(2) 0.034(2) 0.0179(18) 0.0081(18) 0.0089(17) N3 0.028(2) 0.029(2) 0.029(2) 0.0146(17) 0.0034(18) 0.0014(17) N4 0.031(2) 0.026(2) 0.027(2) 0.0092(17) 0.0059(18) 0.0000(16) P1 0.0350(7) 0.0332(7) 0.0289(7) 0.0147(6) 0.0056(6) 0.0099(5) P2 0.0291(7) 0.0311(7) 0.0273(7) 0.0127(6) 0.0081(6) 0.0052(5) P3 0.0354(7) 0.0318(7) 0.0284(7) 0.0132(6) 0.0041(6) 0.0040(6) P4 0.0346(7) 0.0263(6) 0.0300(8) 0.0127(6) 0.0090(6) 0.0052(6) S1 0.0466(8) 0.0538(8) 0.0358(8) 0.0196(7) 0.0010(6) 0.0123(6) S2 0.0440(8) 0.0484(8) 0.0457(9) 0.0214(7) 0.0002(7) 0.0133(6) C1 0.031(3) 0.039(3) 0.038(4) 0.020(3) 0.000(3) -0.002(3) C2 0.046(4) 0.046(3) 0.038(4) 0.018(3) 0.012(3) 0.003(3) C3 0.063(4) 0.064(4) 0.044(4) 0.029(3) 0.017(3) -0.007(3) C4 0.068(4) 0.064(4) 0.063(5) 0.035(4) 0.013(4) -0.016(3) C5 0.069(4) 0.045(3) 0.070(5) 0.034(3) 0.006(4) -0.004(3) C6 0.044(3) 0.037(3) 0.049(4) 0.023(3) 0.006(3) 0.005(2) C7 0.066(4) 0.031(3) 0.064(4) 0.022(3) 0.018(3) 0.006(3) C8 0.123(7) 0.086(5) 0.109(7) 0.061(5) 0.057(6) 0.064(5) C9 0.134(7) 0.035(3) 0.073(5) 0.011(3) 0.017(5) -0.021(4) C10 0.065(4) 0.047(4) 0.041(4) 0.015(3) 0.032(3) 0.010(3) C11 0.116(6) 0.064(4) 0.048(4) 0.010(3) 0.024(4) -0.015(4) C12 0.120(7) 0.068(4) 0.127(7) 0.047(5) 0.076(6) 0.053(5) C13 0.037(3) 0.032(3) 0.034(3) 0.014(2) 0.017(2) 0.016(2) C14 0.050(4) 0.042(3) 0.034(3) 0.012(3) 0.018(3) 0.010(3) C15 0.058(4) 0.049(4) 0.050(4) 0.001(3) 0.012(3) -0.007(3) C16 0.089(6) 0.057(4) 0.061(5) 0.008(3) 0.035(4) 0.024(4) C17 0.057(4) 0.074(4) 0.072(5) 0.018(4) 0.028(4) 0.034(3) C18 0.053(4) 0.053(3) 0.046(4) 0.016(3) 0.015(3) 0.022(3) C19 0.032(3) 0.036(3) 0.032(3) 0.011(2) 0.010(2) 0.004(2) C20 0.042(3) 0.040(3) 0.043(3) 0.012(3) 0.015(3) 0.005(3) C21 0.040(3) 0.025(3) 0.083(5) 0.008(3) 0.015(3) -0.002(2) C22 0.045(4) 0.040(3) 0.064(5) -0.004(3) 0.008(3) -0.003(3) C23 0.053(4) 0.052(4) 0.045(4) 0.006(3) 0.014(3) -0.002(3) C24 0.040(3) 0.042(3) 0.035(3) 0.008(3) 0.008(3) 0.000(3) C25 0.038(3) 0.040(3) 0.031(3) 0.016(3) 0.005(2) 0.002(3) C26 0.030(4) 0.072(5) 0.043(4) 0.018(4) 0.008(3) 0.005(3) C27 0.043(4) 0.102(5) 0.061(4) 0.034(4) 0.018(3) 0.007(3) C28 0.059(5) 0.117(7) 0.114(7) 0.061(6) 0.031(5) 0.002(5) C29 0.031(3) 0.027(2) 0.034(3) 0.013(2) 0.001(2) -0.001(2) C30 0.033(3) 0.033(3) 0.047(4) 0.017(3) 0.004(3) 0.005(2) C31 0.057(4) 0.043(3) 0.064(5) 0.027(3) 0.003(4) 0.015(3) C32 0.063(4) 0.048(4) 0.074(5) 0.038(4) -0.011(4) 0.011(3) C33 0.060(4) 0.059(4) 0.042(4) 0.033(3) -0.002(3) 0.004(3) C34 0.036(3) 0.041(3) 0.040(3) 0.022(3) 0.000(2) -0.004(2) C35 0.054(4) 0.049(3) 0.028(3) 0.026(3) 0.004(3) 0.006(3) C36 0.084(5) 0.068(5) 0.055(5) 0.030(4) 0.021(4) -0.004(4) C37 0.065(4) 0.053(4) 0.053(4) 0.004(3) -0.005(3) -0.007(3) C38 0.048(4) 0.043(3) 0.058(4) 0.019(3) 0.019(3) 0.016(3) C39 0.070(5) 0.063(4) 0.100(6) 0.030(4) 0.043(5) 0.009(4) C40 0.059(4) 0.054(4) 0.061(4) 0.008(3) 0.011(3) 0.014(3) C41 0.050(4) 0.063(4) 0.053(5) 0.023(4) 0.006(4) 0.004(3) C42 0.054(4) 0.123(6) 0.068(5) 0.039(5) -0.005(4) 0.015(4) C43 0.100(7) 0.055(5) 0.093(7) 0.017(5) -0.034(5) -0.017(5) C44 0.059(6) 0.186(11) 0.107(8) 0.076(8) -0.006(5) -0.042(6) C45 0.029(3) 0.036(3) 0.035(3) 0.017(3) 0.003(2) 0.002(2) C46 0.038(3) 0.030(3) 0.044(3) 0.016(2) -0.002(3) -0.001(2) C47 0.046(4) 0.044(3) 0.066(5) 0.027(3) 0.001(3) -0.011(3) C48 0.034(3) 0.053(4) 0.073(5) 0.035(4) 0.010(3) 0.001(3) C49 0.041(3) 0.046(3) 0.061(4) 0.028(3) 0.019(3) 0.009(3) C50 0.027(3) 0.041(3) 0.037(3) 0.020(3) 0.003(2) 0.003(2) C51 0.028(3) 0.049(3) 0.040(3) 0.008(3) 0.017(2) 0.007(2) C52 0.051(4) 0.047(3) 0.076(5) 0.020(3) 0.025(3) 0.009(3) C53 0.057(4) 0.089(5) 0.047(4) 0.022(3) -0.006(3) 0.004(3) C54 0.056(4) 0.045(4) 0.048(4) 0.015(3) -0.001(3) -0.012(3) C55 0.117(7) 0.078(5) 0.041(4) 0.024(4) -0.012(4) -0.010(4) C56 0.070(4) 0.043(3) 0.065(4) 0.007(3) 0.010(4) -0.007(3) C57 0.047(3) 0.037(3) 0.032(3) 0.010(2) 0.011(3) -0.005(3) C58 0.059(4) 0.054(3) 0.035(3) 0.020(3) 0.002(3) -0.011(3) C59 0.100(6) 0.081(5) 0.025(4) 0.009(3) 0.005(4) -0.025(5) C60 0.099(6) 0.057(4) 0.041(4) -0.005(3) 0.031(4) -0.003(4) C61 0.073(4) 0.041(3) 0.040(4) 0.003(3) 0.019(3) 0.001(3) C62 0.053(3) 0.030(3) 0.037(3) 0.011(2) 0.014(3) 0.002(2) C63 0.046(3) 0.024(2) 0.031(3) 0.014(2) 0.008(2) 0.003(2) C64 0.045(3) 0.033(3) 0.043(3) 0.013(2) 0.011(3) 0.002(2) C65 0.061(4) 0.034(3) 0.048(4) 0.011(3) 0.012(3) -0.004(3) C66 0.070(4) 0.029(3) 0.043(4) 0.012(3) 0.007(3) 0.016(3) C67 0.058(4) 0.034(3) 0.040(4) 0.009(3) 0.013(3) 0.012(3) C68 0.037(3) 0.034(3) 0.037(3) 0.013(3) 0.009(3) 0.006(3) C69 0.050(3) 0.027(3) 0.033(3) 0.012(2) 0.018(3) 0.004(2) C70 0.087(6) 0.042(4) 0.030(4) 0.015(3) 0.013(4) -0.003(4) C71 0.181(10) 0.062(5) 0.059(5) 0.043(4) 0.023(6) 0.019(5) C72 0.154(9) 0.127(8) 0.084(7) 0.059(6) 0.010(6) -0.013(7) C73 0.032(3) 0.027(3) 0.041(3) 0.017(2) 0.006(2) 0.004(2) C74 0.032(3) 0.033(3) 0.047(3) 0.021(2) 0.017(3) 0.008(2) C75 0.032(3) 0.053(3) 0.072(4) 0.041(3) 0.022(3) 0.014(3) C76 0.031(3) 0.067(4) 0.066(5) 0.038(4) 0.002(3) -0.001(3) C77 0.036(3) 0.049(3) 0.041(4) 0.020(3) 0.002(3) 0.004(3) C78 0.032(3) 0.034(3) 0.033(3) 0.019(3) 0.002(2) 0.003(2) C79 0.029(3) 0.039(3) 0.036(3) 0.019(2) 0.006(2) -0.003(2) C80 0.074(4) 0.050(3) 0.043(4) 0.008(3) 0.014(3) 0.002(3) C81 0.066(4) 0.069(4) 0.052(4) 0.041(3) 0.018(3) 0.011(3) C82 0.046(3) 0.040(3) 0.052(4) 0.019(3) 0.029(3) 0.015(2) C83 0.077(5) 0.032(3) 0.098(6) 0.022(3) 0.029(4) 0.011(3) C84 0.090(6) 0.060(5) 0.061(5) 0.015(4) 0.052(4) -0.002(4) C85 0.057(4) 0.039(3) 0.064(5) 0.018(3) 0.013(4) 0.009(3) C86 0.033(3) 0.037(3) 0.039(3) 0.017(3) 0.006(3) 0.003(2) C87 0.063(4) 0.050(3) 0.069(4) 0.029(3) 0.002(3) 0.022(3) C88 0.064(5) 0.075(4) 0.079(5) 0.061(4) 0.029(4) 0.023(4) C90 0.071(5) 0.215(13) 0.110(8) 0.103(10) -0.004(5) 0.002(8) C91 0.124(8) 0.138(9) 0.093(7) 0.047(7) -0.044(6) -0.007(7) C92 0.094(8) 0.192(13) 0.167(12) 0.067(10) -0.048(7) -0.036(8) _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 Zn1 N1 1.979(5) . ? Zn1 N2 1.986(4) . ? Zn1 C41 1.995(7) . ? Zn2 N4 1.989(3) . ? Zn2 C86 1.990(5) . ? Zn2 N3 1.993(4) . ? N1 C1 1.457(7) . ? N1 P1 1.609(5) . ? N2 C29 1.445(6) . ? N2 P2 1.620(4) . ? N3 C45 1.445(6) . ? N3 P3 1.624(4) . ? N4 C73 1.453(6) . ? N4 P4 1.613(4) . ? P1 C13 1.821(5) . ? P1 S1 1.945(2) . ? P1 P2 2.2559(18) . ? P2 C19 1.813(5) . ? P2 C25 1.821(5) . ? P3 C57 1.814(5) . ? P3 S2 1.939(2) . ? P3 P4 2.273(2) . ? P4 C69 1.813(5) . ? P4 C63 1.821(5) . ? C1 C6 1.400(8) . ? C1 C2 1.411(8) . ? C2 C3 1.377(8) . ? C2 C10 1.531(8) . ? C3 C4 1.342(8) . ? C3 H3 0.9500 . ? C4 C5 1.390(9) . ? C4 H4 0.9500 . ? C5 C6 1.394(8) . ? C5 H5 0.9500 . ? C6 C7 1.513(8) . ? C7 C8 1.529(9) . ? C7 C9 1.536(8) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.535(10) . ? C10 C11 1.540(9) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.384(7) . ? C13 C14 1.401(7) . ? C14 C15 1.377(8) . ? C14 H14 0.9500 . ? C15 C16 1.382(9) . ? C15 H15 0.9500 . ? C16 C17 1.394(9) . ? C16 H16 0.9500 . ? C17 C18 1.382(8) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.378(7) . ? C19 C24 1.387(7) . ? C20 C21 1.427(8) . ? C20 H20 0.9500 . ? C21 C22 1.372(9) . ? C21 H21 0.9500 . ? C22 C23 1.373(9) . ? C22 H22 0.9500 . ? C23 C24 1.378(8) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.519(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.523(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.500(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.406(8) . ? C29 C34 1.421(7) . ? C30 C31 1.398(8) . ? C30 C38 1.521(9) . ? C31 C32 1.348(9) . ? C31 H31 0.9500 . ? C32 C33 1.404(9) . ? C32 H32 0.9500 . ? C33 C34 1.395(7) . ? C33 H33 0.9500 . ? C34 C35 1.515(7) . ? C35 C36 1.521(8) . ? C35 C37 1.522(8) . ? C35 H35 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.527(9) . ? C38 C40 1.536(7) . ? C38 H38 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.490(10) . ? C41 C43 1.532(11) . ? C41 C44 1.539(11) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C50 1.404(7) . ? C45 C46 1.415(7) . ? C46 C47 1.396(8) . ? C46 C54 1.531(8) . ? C47 C48 1.382(8) . ? C47 H47 0.9500 . ? C48 C49 1.363(8) . ? C48 H48 0.9500 . ? C49 C50 1.412(7) . ? C49 H49 0.9500 . ? C50 C51 1.499(7) . ? C51 C53 1.516(8) . ? C51 C52 1.529(7) . ? C51 H51 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.532(9) . ? C54 C56 1.543(8) . ? C54 H54 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C62 1.398(7) . ? C57 C58 1.402(8) . ? C58 C59 1.400(8) . ? C58 H58 0.9500 . ? C59 C60 1.369(10) . ? C59 H59 0.9500 . ? C60 C61 1.360(9) . ? C60 H60 0.9500 . ? C61 C62 1.387(7) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 C68 1.391(7) . ? C63 C64 1.396(7) . ? C64 C65 1.388(7) . ? C64 H64 0.9500 . ? C65 C66 1.379(8) . ? C65 H65 0.9500 . ? C66 C67 1.366(9) . ? C66 H66 0.9500 . ? C67 C68 1.384(8) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C70 1.524(5) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.531(6) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.509(6) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C78 1.402(7) . ? C73 C74 1.413(7) . ? C74 C75 1.409(7) . ? C74 C82 1.514(7) . ? C75 C76 1.388(8) . ? C75 H75 0.9500 . ? C76 C77 1.359(8) . ? C76 H76 0.9500 . ? C77 C78 1.394(7) . ? C77 H77 0.9500 . ? C78 C79 1.499(8) . ? C79 C80 1.525(7) . ? C79 C81 1.561(7) . ? C79 H79 1.0000 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 C83 1.535(7) . ? C82 C84 1.537(8) . ? C82 H82 1.0000 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 C86 1.530(8) . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 C87 1.506(8) . ? C86 C88 1.551(8) . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C90 C91 1.541(8) . ? C90 C90 1.555(9) 2_766 ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 C92 1.567(8) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N2 95.71(17) . . ? N1 Zn1 C41 129.4(3) . . ? N2 Zn1 C41 133.6(2) . . ? N4 Zn2 C86 138.44(19) . . ? N4 Zn2 N3 95.92(15) . . ? C86 Zn2 N3 124.53(18) . . ? C1 N1 P1 121.1(4) . . ? C1 N1 Zn1 120.4(4) . . ? P1 N1 Zn1 118.4(2) . . ? C29 N2 P2 120.9(3) . . ? C29 N2 Zn1 120.9(3) . . ? P2 N2 Zn1 117.4(2) . . ? C45 N3 P3 120.6(3) . . ? C45 N3 Zn2 121.0(3) . . ? P3 N3 Zn2 117.8(2) . . ? C73 N4 P4 121.7(3) . . ? C73 N4 Zn2 119.8(3) . . ? P4 N4 Zn2 118.1(2) . . ? N1 P1 C13 111.6(2) . . ? N1 P1 S1 120.42(18) . . ? C13 P1 S1 110.66(19) . . ? N1 P1 P2 99.39(16) . . ? C13 P1 P2 98.00(17) . . ? S1 P1 P2 114.04(8) . . ? N2 P2 C19 114.6(2) . . ? N2 P2 C25 115.3(2) . . ? C19 P2 C25 102.3(2) . . ? N2 P2 P1 102.65(14) . . ? C19 P2 P1 114.77(18) . . ? C25 P2 P1 107.48(19) . . ? N3 P3 C57 110.2(2) . . ? N3 P3 S2 120.97(16) . . ? C57 P3 S2 111.6(2) . . ? N3 P3 P4 99.67(14) . . ? C57 P3 P4 96.45(18) . . ? S2 P3 P4 114.77(8) . . ? N4 P4 C69 114.2(2) . . ? N4 P4 C63 115.3(2) . . ? C69 P4 C63 101.1(2) . . ? N4 P4 P3 102.55(14) . . ? C69 P4 P3 108.29(18) . . ? C63 P4 P3 115.69(18) . . ? C6 C1 C2 118.9(5) . . ? C6 C1 N1 121.1(5) . . ? C2 C1 N1 120.0(5) . . ? C3 C2 C1 119.9(6) . . ? C3 C2 C10 118.7(6) . . ? C1 C2 C10 121.4(5) . . ? C4 C3 C2 121.4(6) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 120.2(6) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 120.5(5) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 119.1(5) . . ? C5 C6 C7 119.2(5) . . ? C1 C6 C7 121.7(5) . . ? C6 C7 C8 109.1(6) . . ? C6 C7 C9 112.8(5) . . ? C8 C7 C9 110.8(6) . . ? C6 C7 H7 108.0 . . ? C8 C7 H7 108.0 . . ? C9 C7 H7 108.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 C12 110.0(5) . . ? C2 C10 C11 112.2(6) . . ? C12 C10 C11 111.1(6) . . ? C2 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? C11 C10 H10 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 118.6(5) . . ? C18 C13 P1 120.6(4) . . ? C14 C13 P1 120.8(4) . . ? C15 C14 C13 120.0(6) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 121.1(6) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C17 119.5(6) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C18 C17 C16 119.3(6) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C13 121.6(6) . . ? C17 C18 H18 119.2 . . ? C13 C18 H18 119.2 . . ? C20 C19 C24 119.1(5) . . ? C20 C19 P2 117.9(4) . . ? C24 C19 P2 122.9(4) . . ? C19 C20 C21 120.4(6) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C22 C21 C20 118.5(6) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? C21 C22 C23 121.1(6) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C22 C23 C24 120.2(7) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C19 120.7(6) . . ? C23 C24 H24 119.6 . . ? C19 C24 H24 119.6 . . ? C26 C25 P2 112.8(4) . . ? C26 C25 H25A 109.0 . . ? P2 C25 H25A 109.0 . . ? C26 C25 H25B 109.0 . . ? P2 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C25 C26 C27 112.8(5) . . ? C25 C26 H26A 109.0 . . ? C27 C26 H26A 109.0 . . ? C25 C26 H26B 109.0 . . ? C27 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? C28 C27 C26 113.8(6) . . ? C28 C27 H27A 108.8 . . ? C26 C27 H27A 108.8 . . ? C28 C27 H27B 108.8 . . ? C26 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C34 120.6(5) . . ? C30 C29 N2 120.0(5) . . ? C34 C29 N2 119.3(4) . . ? C31 C30 C29 118.5(6) . . ? C31 C30 C38 119.0(6) . . ? C29 C30 C38 122.5(5) . . ? C32 C31 C30 121.6(6) . . ? C32 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? C31 C32 C33 120.7(6) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C34 C33 C32 120.2(6) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C29 118.3(5) . . ? C33 C34 C35 118.1(5) . . ? C29 C34 C35 123.5(4) . . ? C34 C35 C36 114.2(5) . . ? C34 C35 C37 110.7(5) . . ? C36 C35 C37 110.8(5) . . ? C34 C35 H35 106.9 . . ? C36 C35 H35 106.9 . . ? C37 C35 H35 106.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C30 C38 C39 110.6(6) . . ? C30 C38 C40 114.2(5) . . ? C39 C38 C40 109.0(5) . . ? C30 C38 H38 107.6 . . ? C39 C38 H38 107.6 . . ? C40 C38 H38 107.6 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C43 108.7(7) . . ? C42 C41 C44 110.2(7) . . ? C43 C41 C44 109.4(8) . . ? C42 C41 Zn1 114.7(5) . . ? C43 C41 Zn1 104.2(5) . . ? C44 C41 Zn1 109.5(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C50 C45 C46 120.2(5) . . ? C50 C45 N3 119.8(4) . . ? C46 C45 N3 120.0(5) . . ? C47 C46 C45 118.7(5) . . ? C47 C46 C54 119.0(5) . . ? C45 C46 C54 122.3(5) . . ? C48 C47 C46 121.6(5) . . ? C48 C47 H47 119.2 . . ? C46 C47 H47 119.2 . . ? C49 C48 C47 119.3(5) . . ? C49 C48 H48 120.3 . . ? C47 C48 H48 120.3 . . ? C48 C49 C50 122.1(6) . . ? C48 C49 H49 118.9 . . ? C50 C49 H49 118.9 . . ? C45 C50 C49 118.1(5) . . ? C45 C50 C51 123.1(5) . . ? C49 C50 C51 118.8(5) . . ? C50 C51 C53 112.7(5) . . ? C50 C51 C52 111.2(5) . . ? C53 C51 C52 110.5(5) . . ? C50 C51 H51 107.4 . . ? C53 C51 H51 107.4 . . ? C52 C51 H51 107.4 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C46 C54 C55 110.4(6) . . ? C46 C54 C56 111.6(5) . . ? C55 C54 C56 110.4(5) . . ? C46 C54 H54 108.1 . . ? C55 C54 H54 108.1 . . ? C56 C54 H54 108.1 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C62 C57 C58 118.3(5) . . ? C62 C57 P3 121.6(4) . . ? C58 C57 P3 120.1(4) . . ? C59 C58 C57 119.1(6) . . ? C59 C58 H58 120.5 . . ? C57 C58 H58 120.5 . . ? C60 C59 C58 120.9(7) . . ? C60 C59 H59 119.5 . . ? C58 C59 H59 119.5 . . ? C61 C60 C59 120.7(6) . . ? C61 C60 H60 119.7 . . ? C59 C60 H60 119.7 . . ? C60 C61 C62 119.7(6) . . ? C60 C61 H61 120.2 . . ? C62 C61 H61 120.2 . . ? C61 C62 C57 121.2(6) . . ? C61 C62 H62 119.4 . . ? C57 C62 H62 119.4 . . ? C68 C63 C64 119.0(4) . . ? C68 C63 P4 122.9(4) . . ? C64 C63 P4 118.1(4) . . ? C65 C64 C63 119.7(5) . . ? C65 C64 H64 120.1 . . ? C63 C64 H64 120.1 . . ? C66 C65 C64 120.5(5) . . ? C66 C65 H65 119.8 . . ? C64 C65 H65 119.8 . . ? C67 C66 C65 119.9(5) . . ? C67 C66 H66 120.1 . . ? C65 C66 H66 120.1 . . ? C66 C67 C68 120.7(6) . . ? C66 C67 H67 119.7 . . ? C68 C67 H67 119.7 . . ? C67 C68 C63 120.2(5) . . ? C67 C68 H68 119.9 . . ? C63 C68 H68 119.9 . . ? C70 C69 P4 116.0(4) . . ? C70 C69 H69A 108.3 . . ? P4 C69 H69A 108.3 . . ? C70 C69 H69B 108.3 . . ? P4 C69 H69B 108.3 . . ? H69A C69 H69B 107.4 . . ? C69 C70 C71 110.3(5) . . ? C69 C70 H70A 109.6 . . ? C71 C70 H70A 109.6 . . ? C69 C70 H70B 109.6 . . ? C71 C70 H70B 109.6 . . ? H70A C70 H70B 108.1 . . ? C72 C71 C70 110.6(6) . . ? C72 C71 H71A 109.5 . . ? C70 C71 H71A 109.5 . . ? C72 C71 H71B 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 108.1 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C78 C73 C74 121.5(5) . . ? C78 C73 N4 119.2(5) . . ? C74 C73 N4 119.2(4) . . ? C75 C74 C73 117.8(5) . . ? C75 C74 C82 118.9(5) . . ? C73 C74 C82 122.9(4) . . ? C76 C75 C74 120.1(5) . . ? C76 C75 H75 119.9 . . ? C74 C75 H75 119.9 . . ? C77 C76 C75 120.9(5) . . ? C77 C76 H76 119.5 . . ? C75 C76 H76 119.5 . . ? C76 C77 C78 121.6(6) . . ? C76 C77 H77 119.2 . . ? C78 C77 H77 119.2 . . ? C77 C78 C73 118.0(5) . . ? C77 C78 C79 118.5(5) . . ? C73 C78 C79 123.2(5) . . ? C78 C79 C80 115.6(4) . . ? C78 C79 C81 108.4(4) . . ? C80 C79 C81 109.4(5) . . ? C78 C79 H79 107.7 . . ? C80 C79 H79 107.7 . . ? C81 C79 H79 107.7 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C79 C81 H81A 109.5 . . ? C79 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C79 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C74 C82 C83 110.5(5) . . ? C74 C82 C84 114.3(5) . . ? C83 C82 C84 109.4(5) . . ? C74 C82 H82 107.4 . . ? C83 C82 H82 107.4 . . ? C84 C82 H82 107.4 . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C82 C84 H84A 109.5 . . ? C82 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C82 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C86 C85 H85A 109.5 . . ? C86 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C86 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C87 C86 C85 108.4(5) . . ? C87 C86 C88 109.1(5) . . ? C85 C86 C88 106.1(5) . . ? C87 C86 Zn2 117.6(4) . . ? C85 C86 Zn2 106.6(4) . . ? C88 C86 Zn2 108.4(4) . . ? C86 C87 H87A 109.5 . . ? C86 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C86 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C86 C88 H88A 109.5 . . ? C86 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C86 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C91 C90 C90 115.9(9) . 2_766 ? C91 C90 H90A 108.3 . . ? C90 C90 H90A 108.3 2_766 . ? C91 C90 H90B 108.3 . . ? C90 C90 H90B 108.3 2_766 . ? H90A C90 H90B 107.4 . . ? C90 C91 C92 110.0(7) . . ? C90 C91 H91A 109.7 . . ? C92 C91 H91A 109.7 . . ? C90 C91 H91B 109.7 . . ? C92 C91 H91B 109.7 . . ? H91A C91 H91B 108.2 . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.96 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.96 _refine_diff_density_max 0.391 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.055 data_complex2 _database_code_depnum_ccdc_archive 'CCDC 606735' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C80 H106 Cl2 N4 P4 Zn2, 3(C6 H6)' _chemical_formula_sum 'C98 H124 Cl2 N4 P4 Zn2' _chemical_formula_weight 1683.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.185(2) _cell_length_b 13.705(3) _cell_length_c 15.157(3) _cell_angle_alpha 99.54(3) _cell_angle_beta 95.15(3) _cell_angle_gamma 107.22(3) _cell_volume 2358.2(10) _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 plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 894 _exptl_absorpt_coefficient_mu 0.678 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.9110 _exptl_absorpt_correction_T_max 0.9604 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski and Minor 1997)' _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 'phi/omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15939 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8308 _reflns_number_gt 6704 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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 ; The main residue is well-ordered and all non-hydrogen atoms were refined anisotropically. The structure contains two lattice molecules of benzene, one of which lies on an inversion centre and is well-ordered, C50-C52A. Geometric restraints were applied to obtain reasonable aromatic C-C distances. The second molecule of benzene is disordered and was modeled over two sites using geometric restraints. The thermal parameters were best refined using an anisotropic 75:25 mixture. 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^)+(0.0312P)^2^+0.9188P] 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 8308 _refine_ls_number_parameters 559 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0751 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.039 _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 P1 P 0.46544(4) 0.81228(4) 0.42834(4) 0.02733(13) Uani 1 1 d . . . P2 P 0.38279(4) 0.68946(4) 0.30249(4) 0.02672(13) Uani 1 1 d . . . Zn1 Zn 0.49272(2) 0.595638(18) 0.442870(16) 0.02742(8) Uani 1 1 d . . . Cl1 Cl 0.61599(5) 0.49816(4) 0.45507(4) 0.03742(14) Uani 1 1 d . . . N1 N 0.53976(13) 0.74740(13) 0.47920(11) 0.0272(4) Uani 1 1 d . . . N2 N 0.40714(14) 0.58362(12) 0.32106(11) 0.0274(4) Uani 1 1 d . . . C1 C 0.64979(17) 0.81157(15) 0.53117(14) 0.0288(5) Uani 1 1 d . . . C2 C 0.65572(18) 0.85313(16) 0.62401(15) 0.0329(5) Uani 1 1 d . . . C3 C 0.7625(2) 0.91378(18) 0.67353(16) 0.0412(6) Uani 1 1 d . . . H3 H 0.7664 0.9427 0.7356 0.049 Uiso 1 1 calc R . . C4 C 0.8630(2) 0.93321(18) 0.63491(17) 0.0432(6) Uani 1 1 d . . . H4 H 0.9354 0.9747 0.6701 0.052 Uiso 1 1 calc R . . C5 C 0.85737(19) 0.89190(18) 0.54490(16) 0.0389(5) Uani 1 1 d . . . H5 H 0.9270 0.9046 0.5187 0.047 Uiso 1 1 calc R . . C6 C 0.75241(17) 0.83192(16) 0.49082(15) 0.0318(5) Uani 1 1 d . . . C7 C 0.75331(19) 0.79248(18) 0.39113(15) 0.0377(5) Uani 1 1 d . . . H7 H 0.6713 0.7537 0.3626 0.045 Uiso 1 1 calc R . . C8 C 0.8239(2) 0.7169(2) 0.37770(18) 0.0499(7) Uani 1 1 d . . . H8A H 0.9052 0.7535 0.4040 0.075 Uiso 1 1 calc R . . H8B H 0.8193 0.6902 0.3129 0.075 Uiso 1 1 calc R . . H8C H 0.7924 0.6586 0.4076 0.075 Uiso 1 1 calc R . . C9 C 0.7995(2) 0.8832(2) 0.34310(18) 0.0536(7) Uani 1 1 d . . . H9A H 0.7564 0.9329 0.3550 0.080 Uiso 1 1 calc R . . H9B H 0.7894 0.8563 0.2778 0.080 Uiso 1 1 calc R . . H9C H 0.8822 0.9184 0.3657 0.080 Uiso 1 1 calc R . . C10 C 0.54774(19) 0.83420(17) 0.67016(15) 0.0370(5) Uani 1 1 d . . . H10 H 0.4837 0.7777 0.6284 0.044 Uiso 1 1 calc R . . C11 C 0.5643(3) 0.7976(2) 0.75862(18) 0.0609(8) Uani 1 1 d . . . H11A H 0.5889 0.7353 0.7474 0.091 Uiso 1 1 calc R . . H11B H 0.4908 0.7809 0.7832 0.091 Uiso 1 1 calc R . . H11C H 0.6238 0.8530 0.8021 0.091 Uiso 1 1 calc R . . C12 C 0.5099(2) 0.9315(2) 0.6861(2) 0.0583(7) Uani 1 1 d . . . H12A H 0.5695 0.9874 0.7292 0.087 Uiso 1 1 calc R . . H12B H 0.4363 0.9156 0.7107 0.087 Uiso 1 1 calc R . . H12C H 0.4995 0.9541 0.6288 0.087 Uiso 1 1 calc R . . C13 C 0.32755(17) 0.79546(16) 0.47561(14) 0.0295(5) Uani 1 1 d . . . C14 C 0.27603(19) 0.71318(18) 0.51631(16) 0.0389(6) Uani 1 1 d . . . H14 H 0.3117 0.6608 0.5204 0.047 Uiso 1 1 calc R . . C15 C 0.1734(2) 0.7066(2) 0.55094(18) 0.0491(7) Uani 1 1 d . . . H15 H 0.1390 0.6500 0.5788 0.059 Uiso 1 1 calc R . . C16 C 0.1212(2) 0.7824(2) 0.54490(18) 0.0506(7) Uani 1 1 d . . . H16 H 0.0504 0.7778 0.5683 0.061 Uiso 1 1 calc R . . C17 C 0.1713(2) 0.8645(2) 0.50517(18) 0.0480(6) Uani 1 1 d . . . H17 H 0.1349 0.9163 0.5008 0.058 Uiso 1 1 calc R . . C18 C 0.27476(19) 0.87186(17) 0.47143(15) 0.0365(5) Uani 1 1 d . . . H18 H 0.3099 0.9297 0.4452 0.044 Uiso 1 1 calc R . . C19 C 0.43908(18) 0.73473(16) 0.20424(14) 0.0297(5) Uani 1 1 d . . . C20 C 0.53185(19) 0.82492(18) 0.21338(16) 0.0384(5) Uani 1 1 d . . . H20 H 0.5698 0.8626 0.2720 0.046 Uiso 1 1 calc R . . C21 C 0.5701(2) 0.8610(2) 0.13740(17) 0.0493(7) Uani 1 1 d . . . H21 H 0.6351 0.9220 0.1443 0.059 Uiso 1 1 calc R . . C22 C 0.5138(2) 0.8084(2) 0.05246(17) 0.0507(7) Uani 1 1 d . . . H22 H 0.5394 0.8335 0.0006 0.061 Uiso 1 1 calc R . . C23 C 0.4199(2) 0.7193(2) 0.04244(16) 0.0451(6) Uani 1 1 d . . . H23 H 0.3806 0.6835 -0.0163 0.054 Uiso 1 1 calc R . . C24 C 0.38297(19) 0.68185(18) 0.11770(15) 0.0367(5) Uani 1 1 d . . . H24 H 0.3191 0.6198 0.1103 0.044 Uiso 1 1 calc R . . C25 C 0.22911(17) 0.67221(17) 0.27431(15) 0.0328(5) Uani 1 1 d . . . H25A H 0.1942 0.6068 0.2286 0.039 Uiso 1 1 calc R . . H25B H 0.1924 0.6624 0.3293 0.039 Uiso 1 1 calc R . . C26 C 0.19668(18) 0.75950(18) 0.23810(16) 0.0375(5) Uani 1 1 d . . . H26A H 0.2343 0.8265 0.2813 0.045 Uiso 1 1 calc R . . H26B H 0.2259 0.7659 0.1798 0.045 Uiso 1 1 calc R . . C27 C 0.0671(2) 0.7380(2) 0.22459(19) 0.0563(7) Uani 1 1 d . . . H27A H 0.0402 0.7421 0.2844 0.068 Uiso 1 1 calc R . . H27B H 0.0293 0.6660 0.1896 0.068 Uiso 1 1 calc R . . C28 C 0.0286(2) 0.8131(2) 0.1755(2) 0.0634(8) Uani 1 1 d . . . H28A H 0.0659 0.8846 0.2095 0.095 Uiso 1 1 calc R . . H28B H -0.0560 0.7963 0.1706 0.095 Uiso 1 1 calc R . . H28C H 0.0511 0.8068 0.1149 0.095 Uiso 1 1 calc R . . C29 C 0.36929(18) 0.49287(16) 0.24798(14) 0.0301(5) Uani 1 1 d . . . C30 C 0.44625(19) 0.47439(17) 0.18759(14) 0.0349(5) Uani 1 1 d . . . C31 C 0.4026(2) 0.39310(19) 0.11278(16) 0.0449(6) Uani 1 1 d . . . H31 H 0.4523 0.3822 0.0699 0.054 Uiso 1 1 calc R . . C32 C 0.2900(2) 0.3282(2) 0.09892(17) 0.0505(7) Uani 1 1 d . . . H32 H 0.2617 0.2748 0.0461 0.061 Uiso 1 1 calc R . . C33 C 0.2181(2) 0.34093(19) 0.16243(17) 0.0473(6) Uani 1 1 d . . . H33 H 0.1417 0.2932 0.1545 0.057 Uiso 1 1 calc R . . C34 C 0.25530(19) 0.42223(17) 0.23773(15) 0.0356(5) Uani 1 1 d . . . C35 C 0.17733(19) 0.42684(18) 0.31007(16) 0.0404(6) Uani 1 1 d . . . H35 H 0.2122 0.4951 0.3535 0.048 Uiso 1 1 calc R . . C36 C 0.1749(3) 0.3394(2) 0.36212(19) 0.0594(7) Uani 1 1 d . . . H36A H 0.1333 0.2717 0.3225 0.089 Uiso 1 1 calc R . . H36B H 0.1352 0.3486 0.4148 0.089 Uiso 1 1 calc R . . H36C H 0.2546 0.3420 0.3823 0.089 Uiso 1 1 calc R . . C37 C 0.0522(2) 0.4182(2) 0.2736(2) 0.0576(7) Uani 1 1 d . . . H37A H 0.0536 0.4703 0.2361 0.086 Uiso 1 1 calc R . . H37B H 0.0103 0.4305 0.3243 0.086 Uiso 1 1 calc R . . H37C H 0.0129 0.3482 0.2370 0.086 Uiso 1 1 calc R . . C38 C 0.5757(2) 0.53365(19) 0.20402(16) 0.0399(6) Uani 1 1 d . . . H38 H 0.5916 0.5903 0.2589 0.048 Uiso 1 1 calc R . . C39 C 0.6200(2) 0.5841(2) 0.12588(19) 0.0561(7) Uani 1 1 d . . . H39A H 0.6049 0.5301 0.0711 0.084 Uiso 1 1 calc R . . H39B H 0.7037 0.6202 0.1411 0.084 Uiso 1 1 calc R . . H39C H 0.5798 0.6343 0.1153 0.084 Uiso 1 1 calc R . . C40 C 0.6455(2) 0.4607(2) 0.22328(17) 0.0479(6) Uani 1 1 d . . . H40A H 0.6193 0.4289 0.2742 0.072 Uiso 1 1 calc R . . H40B H 0.7283 0.5008 0.2384 0.072 Uiso 1 1 calc R . . H40C H 0.6335 0.4059 0.1695 0.072 Uiso 1 1 calc R . . C41 C 0.1996(8) 0.8561(7) 0.8210(7) 0.103(3) Uani 0.75 1 d PD A 1 H41 H 0.2081 0.8147 0.7668 0.124 Uiso 0.75 1 calc PR A 1 C42 C 0.1226(13) 0.9134(13) 0.8232(12) 0.141(7) Uani 0.75 1 d PD A 1 H42 H 0.0772 0.9136 0.7690 0.169 Uiso 0.75 1 calc PR A 1 C43 C 0.1124(13) 0.9697(13) 0.9041(13) 0.154(6) Uani 0.75 1 d PD A 1 H43 H 0.0573 1.0063 0.9030 0.184 Uiso 0.75 1 calc PR A 1 C44 C 0.1753(13) 0.9778(13) 0.9871(11) 0.172(7) Uani 0.75 1 d PD A 1 H44 H 0.1648 1.0162 1.0422 0.207 Uiso 0.75 1 calc PR A 1 C45 C 0.2547(14) 0.9243(11) 0.9816(9) 0.113(4) Uani 0.75 1 d PD A 1 H45 H 0.3059 0.9298 1.0346 0.135 Uiso 0.75 1 calc PR A 1 C46 C 0.2625(9) 0.8641(7) 0.9034(10) 0.105(4) Uani 0.75 1 d PD A 1 H46 H 0.3149 0.8249 0.9057 0.126 Uiso 0.75 1 calc PR A 1 C41A C 0.141(3) 0.884(2) 0.825(2) 0.107(14) Uani 0.25 1 d PD B 2 H41A H 0.1224 0.8573 0.7620 0.128 Uiso 0.25 1 calc PR B 2 C42A C 0.091(3) 0.958(3) 0.8600(17) 0.086(8) Uani 0.25 1 d PD B 2 H42A H 0.0316 0.9727 0.8251 0.103 Uiso 0.25 1 calc PR B 2 C43A C 0.134(3) 1.010(2) 0.9489(15) 0.114(12) Uani 0.25 1 d PD B 2 H43A H 0.1104 1.0662 0.9760 0.136 Uiso 0.25 1 calc PR B 2 C44A C 0.214(2) 0.975(2) 0.9970(18) 0.085(8) Uani 0.25 1 d PD B 2 H44A H 0.2543 1.0173 1.0537 0.102 Uiso 0.25 1 calc PR B 2 C45A C 0.238(4) 0.882(3) 0.967(2) 0.112(16) Uani 0.25 1 d PD B 2 H45A H 0.2684 0.8473 1.0071 0.134 Uiso 0.25 1 calc PR B 2 C46A C 0.215(3) 0.844(2) 0.873(2) 0.128(18) Uani 0.25 1 d PD B 2 H46A H 0.2476 0.7947 0.8439 0.153 Uiso 0.25 1 calc PR B 2 C50 C 0.9984(5) 0.4089(3) 0.0267(3) 0.1000(13) Uani 1 1 d D . . H50 H 0.9973 0.3457 0.0452 0.120 Uiso 1 1 calc R . . C51 C 0.9068(3) 0.4462(4) 0.0347(3) 0.1024(14) Uani 1 1 d D . . H51 H 0.8415 0.4090 0.0590 0.123 Uiso 1 1 calc R . . C52 C 1.0911(4) 0.4630(4) -0.0078(3) 0.1052(14) Uani 1 1 d D . . H52 H 1.1552 0.4375 -0.0134 0.126 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 P1 0.0270(3) 0.0263(3) 0.0304(3) 0.0077(2) 0.0076(2) 0.0089(2) P2 0.0265(3) 0.0284(3) 0.0268(3) 0.0085(2) 0.0053(2) 0.0090(2) Zn1 0.02873(13) 0.02654(14) 0.02835(14) 0.00836(10) 0.00452(10) 0.00915(10) Cl1 0.0380(3) 0.0437(3) 0.0451(3) 0.0242(3) 0.0192(3) 0.0225(3) N1 0.0229(8) 0.0252(9) 0.0325(10) 0.0067(8) 0.0037(7) 0.0059(7) N2 0.0320(9) 0.0249(9) 0.0253(9) 0.0068(7) 0.0037(7) 0.0082(7) C1 0.0264(11) 0.0248(11) 0.0353(12) 0.0090(9) 0.0027(9) 0.0074(9) C2 0.0353(12) 0.0287(12) 0.0342(13) 0.0075(10) 0.0047(10) 0.0088(10) C3 0.0432(14) 0.0397(14) 0.0337(13) 0.0026(11) -0.0012(11) 0.0072(11) C4 0.0330(13) 0.0396(14) 0.0479(16) 0.0048(12) -0.0044(11) 0.0028(10) C5 0.0281(12) 0.0379(13) 0.0492(15) 0.0122(11) 0.0055(10) 0.0064(10) C6 0.0284(11) 0.0289(12) 0.0378(13) 0.0086(10) 0.0046(10) 0.0078(9) C7 0.0278(11) 0.0449(14) 0.0383(13) 0.0071(11) 0.0082(10) 0.0078(10) C8 0.0408(14) 0.0542(16) 0.0536(16) 0.0052(13) 0.0167(12) 0.0135(12) C9 0.0453(15) 0.0617(18) 0.0486(16) 0.0190(14) 0.0114(12) 0.0037(13) C10 0.0411(13) 0.0364(13) 0.0331(13) 0.0066(10) 0.0085(10) 0.0109(11) C11 0.0656(18) 0.071(2) 0.0523(17) 0.0298(15) 0.0183(14) 0.0186(15) C12 0.0620(17) 0.0523(17) 0.072(2) 0.0159(15) 0.0288(15) 0.0278(14) C13 0.0267(11) 0.0323(12) 0.0302(12) 0.0045(9) 0.0064(9) 0.0104(9) C14 0.0406(13) 0.0406(13) 0.0455(14) 0.0167(11) 0.0161(11) 0.0209(11) C15 0.0426(14) 0.0568(16) 0.0596(17) 0.0284(14) 0.0251(13) 0.0191(12) C16 0.0357(13) 0.0630(18) 0.0621(18) 0.0154(14) 0.0209(12) 0.0235(13) C17 0.0418(14) 0.0484(15) 0.0644(17) 0.0144(13) 0.0171(13) 0.0256(12) C18 0.0372(12) 0.0334(12) 0.0421(14) 0.0090(10) 0.0082(10) 0.0144(10) C19 0.0325(11) 0.0336(12) 0.0301(12) 0.0115(10) 0.0086(9) 0.0174(10) C20 0.0421(13) 0.0395(13) 0.0365(13) 0.0116(11) 0.0115(11) 0.0135(11) C21 0.0576(16) 0.0443(15) 0.0501(17) 0.0210(13) 0.0229(13) 0.0116(12) C22 0.0673(18) 0.0583(17) 0.0415(16) 0.0254(14) 0.0239(14) 0.0293(15) C23 0.0554(15) 0.0578(17) 0.0298(13) 0.0116(12) 0.0081(11) 0.0273(13) C24 0.0377(12) 0.0416(13) 0.0333(13) 0.0086(11) 0.0057(10) 0.0155(11) C25 0.0273(11) 0.0363(12) 0.0341(12) 0.0098(10) 0.0030(9) 0.0082(10) C26 0.0325(12) 0.0435(14) 0.0384(13) 0.0094(11) 0.0028(10) 0.0150(10) C27 0.0389(14) 0.078(2) 0.0634(18) 0.0267(16) 0.0077(13) 0.0281(14) C28 0.0517(16) 0.076(2) 0.068(2) 0.0118(16) -0.0052(14) 0.0350(15) C29 0.0390(12) 0.0268(11) 0.0259(11) 0.0090(9) 0.0017(9) 0.0113(10) C30 0.0452(13) 0.0348(13) 0.0293(12) 0.0096(10) 0.0077(10) 0.0171(10) C31 0.0596(16) 0.0489(15) 0.0319(13) 0.0067(12) 0.0077(12) 0.0263(13) C32 0.0661(18) 0.0423(15) 0.0367(15) -0.0061(12) -0.0080(13) 0.0196(13) C33 0.0470(14) 0.0371(14) 0.0483(16) 0.0025(12) -0.0080(12) 0.0066(11) C34 0.0410(13) 0.0301(12) 0.0346(13) 0.0087(10) 0.0004(10) 0.0100(10) C35 0.0394(13) 0.0338(13) 0.0420(14) 0.0086(11) 0.0047(11) 0.0025(10) C36 0.0680(18) 0.0463(16) 0.0591(18) 0.0211(14) 0.0135(14) 0.0041(14) C37 0.0376(14) 0.0580(18) 0.0696(19) 0.0144(15) 0.0106(13) 0.0024(12) C38 0.0432(13) 0.0431(14) 0.0366(13) 0.0065(11) 0.0124(11) 0.0172(11) C39 0.0576(17) 0.0634(18) 0.0634(18) 0.0282(15) 0.0276(14) 0.0294(14) C40 0.0519(15) 0.0574(17) 0.0390(14) 0.0097(12) 0.0073(12) 0.0239(13) C41 0.094(6) 0.079(5) 0.121(7) 0.042(5) -0.011(6) 0.001(4) C42 0.079(7) 0.147(16) 0.208(16) 0.114(12) -0.007(8) 0.017(7) C43 0.086(10) 0.192(17) 0.237(19) 0.126(16) 0.037(13) 0.076(12) C44 0.137(13) 0.260(14) 0.206(14) 0.158(12) 0.091(9) 0.112(11) C45 0.108(7) 0.125(12) 0.124(8) 0.075(7) 0.014(7) 0.040(8) C46 0.094(6) 0.082(7) 0.135(12) 0.045(7) -0.009(6) 0.019(6) C41A 0.10(3) 0.042(13) 0.15(3) 0.000(17) -0.05(2) -0.007(13) C42A 0.085(16) 0.093(16) 0.079(15) 0.020(13) -0.032(12) 0.038(11) C43A 0.13(2) 0.102(17) 0.077(16) 0.016(13) 0.021(14) -0.019(15) C44A 0.045(13) 0.103(19) 0.110(17) 0.022(15) 0.024(10) 0.022(11) C45A 0.18(4) 0.09(2) 0.13(3) 0.069(19) 0.09(2) 0.09(3) C46A 0.16(4) 0.080(17) 0.07(2) -0.006(14) 0.00(2) -0.05(2) C50 0.115(3) 0.099(3) 0.083(3) 0.015(2) -0.021(3) 0.041(3) C51 0.068(3) 0.146(4) 0.071(3) 0.026(3) -0.0076(19) 0.003(3) C52 0.091(3) 0.161(5) 0.077(3) 0.005(3) 0.000(2) 0.073(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 P1 N1 1.6684(18) . ? P1 C13 1.852(2) . ? P1 P2 2.2525(12) . ? P2 N2 1.6269(17) . ? P2 C25 1.818(2) . ? P2 C19 1.820(2) . ? Zn1 N1 1.9534(17) . ? Zn1 N2 1.9937(18) . ? Zn1 Cl1 2.3011(8) . ? Zn1 Cl1 2.4124(9) 2_666 ? Cl1 Zn1 2.4124(9) 2_666 ? N1 C1 1.440(3) . ? N2 C29 1.449(3) . ? C1 C2 1.415(3) . ? C1 C6 1.415(3) . ? C2 C3 1.387(3) . ? C2 C10 1.520(3) . ? C3 C4 1.379(3) . ? C3 H3 0.9500 . ? C4 C5 1.375(3) . ? C4 H4 0.9500 . ? C5 C6 1.396(3) . ? C5 H5 0.9500 . ? C6 C7 1.520(3) . ? C7 C8 1.531(3) . ? C7 C9 1.534(3) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.525(3) . ? C10 C12 1.526(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.388(3) . ? C13 C18 1.389(3) . ? C14 C15 1.383(3) . ? C14 H14 0.9500 . ? C15 C16 1.381(3) . ? C15 H15 0.9500 . ? C16 C17 1.372(4) . ? C16 H16 0.9500 . ? C17 C18 1.385(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.383(3) . ? C19 C24 1.394(3) . ? C20 C21 1.391(3) . ? C20 H20 0.9500 . ? C21 C22 1.374(4) . ? C21 H21 0.9500 . ? C22 C23 1.379(4) . ? C22 H22 0.9500 . ? C23 C24 1.385(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.532(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.506(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.520(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.414(3) . ? C29 C34 1.416(3) . ? C30 C31 1.390(3) . ? C30 C38 1.521(3) . ? C31 C32 1.372(4) . ? C31 H31 0.9500 . ? C32 C33 1.382(4) . ? C32 H32 0.9500 . ? C33 C34 1.392(3) . ? C33 H33 0.9500 . ? C34 C35 1.519(3) . ? C35 C36 1.535(3) . ? C35 C37 1.538(3) . ? C35 H35 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.529(3) . ? C38 C40 1.538(3) . ? C38 H38 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C46 1.377(13) . ? C41 C42 1.389(14) . ? C41 H41 0.9500 . ? C42 C43 1.373(15) . ? C42 H42 0.9500 . ? C43 C44 1.383(15) . ? C43 H43 0.9500 . ? C44 C45 1.376(13) . ? C44 H44 0.9500 . ? C45 C46 1.355(12) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C41A C42A 1.385(19) . ? C41A C46A 1.391(18) . ? C41A H41A 0.9500 . ? C42A C43A 1.389(18) . ? C42A H42A 0.9500 . ? C43A C44A 1.399(19) . ? C43A H43A 0.9500 . ? C44A C45A 1.406(18) . ? C44A H44A 0.9500 . ? C45A C46A 1.402(19) . ? C45A H45A 0.9500 . ? C46A H46A 0.9500 . ? C50 C52 1.356(5) . ? C50 C51 1.366(4) . ? C50 H50 0.9500 . ? C51 C52 1.366(4) 2_765 ? C51 H51 0.9500 . ? C52 C51 1.366(4) 2_765 ? C52 H52 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 N1 P1 C13 107.93(9) . . ? N1 P1 P2 98.27(7) . . ? C13 P1 P2 93.97(8) . . ? N2 P2 C25 112.87(10) . . ? N2 P2 C19 114.77(9) . . ? C25 P2 C19 101.19(10) . . ? N2 P2 P1 106.13(7) . . ? C25 P2 P1 112.11(8) . . ? C19 P2 P1 109.91(8) . . ? N1 Zn1 N2 97.21(8) . . ? N1 Zn1 Cl1 124.40(5) . . ? N2 Zn1 Cl1 118.14(6) . . ? N1 Zn1 Cl1 114.81(6) . 2_666 ? N2 Zn1 Cl1 116.55(5) . 2_666 ? Cl1 Zn1 Cl1 87.35(3) . 2_666 ? Zn1 Cl1 Zn1 92.65(3) . 2_666 ? C1 N1 P1 114.67(13) . . ? C1 N1 Zn1 124.62(13) . . ? P1 N1 Zn1 119.04(9) . . ? C29 N2 P2 117.81(13) . . ? C29 N2 Zn1 126.89(13) . . ? P2 N2 Zn1 115.26(9) . . ? C2 C1 C6 119.62(19) . . ? C2 C1 N1 119.63(18) . . ? C6 C1 N1 120.74(18) . . ? C3 C2 C1 119.0(2) . . ? C3 C2 C10 119.4(2) . . ? C1 C2 C10 121.54(19) . . ? C4 C3 C2 121.7(2) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 119.2(2) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 122.0(2) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 118.4(2) . . ? C5 C6 C7 118.56(19) . . ? C1 C6 C7 122.99(19) . . ? C6 C7 C8 111.61(19) . . ? C6 C7 C9 111.2(2) . . ? C8 C7 C9 110.34(19) . . ? C6 C7 H7 107.8 . . ? C8 C7 H7 107.8 . . ? C9 C7 H7 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 C11 112.4(2) . . ? C2 C10 C12 110.92(19) . . ? C11 C10 C12 110.4(2) . . ? C2 C10 H10 107.6 . . ? C11 C10 H10 107.6 . . ? C12 C10 H10 107.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 118.61(19) . . ? C14 C13 P1 124.17(16) . . ? C18 C13 P1 117.21(16) . . ? C15 C14 C13 120.8(2) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C16 C15 C14 119.8(2) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C17 C16 C15 120.1(2) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.2(2) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C13 120.5(2) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? C20 C19 C24 118.87(19) . . ? C20 C19 P2 121.39(17) . . ? C24 C19 P2 119.59(16) . . ? C19 C20 C21 120.5(2) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C22 C21 C20 120.1(2) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 120.0(2) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 120.2(2) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C19 120.3(2) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C26 C25 P2 117.42(15) . . ? C26 C25 H25A 107.9 . . ? P2 C25 H25A 107.9 . . ? C26 C25 H25B 107.9 . . ? P2 C25 H25B 107.9 . . ? H25A C25 H25B 107.2 . . ? C27 C26 C25 111.26(19) . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C26 C27 C28 113.5(2) . . ? C26 C27 H27A 108.9 . . ? C28 C27 H27A 108.9 . . ? C26 C27 H27B 108.9 . . ? C28 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C34 120.1(2) . . ? C30 C29 N2 120.09(19) . . ? C34 C29 N2 119.78(19) . . ? C31 C30 C29 118.1(2) . . ? C31 C30 C38 118.4(2) . . ? C29 C30 C38 123.3(2) . . ? C32 C31 C30 122.0(2) . . ? C32 C31 H31 119.0 . . ? C30 C31 H31 119.0 . . ? C31 C32 C33 119.5(2) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C32 C33 C34 121.4(2) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C33 C34 C29 118.4(2) . . ? C33 C34 C35 119.3(2) . . ? C29 C34 C35 122.1(2) . . ? C34 C35 C36 109.0(2) . . ? C34 C35 C37 114.3(2) . . ? C36 C35 C37 109.3(2) . . ? C34 C35 H35 108.0 . . ? C36 C35 H35 108.0 . . ? C37 C35 H35 108.0 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C30 C38 C39 114.2(2) . . ? C30 C38 C40 110.18(19) . . ? C39 C38 C40 108.47(19) . . ? C30 C38 H38 107.9 . . ? C39 C38 H38 107.9 . . ? C40 C38 H38 107.9 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C46 C41 C42 114.7(12) . . ? C46 C41 H41 122.7 . . ? C42 C41 H41 122.7 . . ? C43 C42 C41 119.8(14) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C42 C43 C44 125.7(12) . . ? C42 C43 H43 117.2 . . ? C44 C43 H43 117.2 . . ? C45 C44 C43 112.9(12) . . ? C45 C44 H44 123.6 . . ? C43 C44 H44 123.6 . . ? C46 C45 C44 122.5(12) . . ? C46 C45 H45 118.7 . . ? C44 C45 H45 118.7 . . ? C45 C46 C41 124.3(10) . . ? C45 C46 H46 117.9 . . ? C41 C46 H46 117.9 . . ? C42A C41A C46A 127(2) . . ? C42A C41A H41A 116.4 . . ? C46A C41A H41A 116.4 . . ? C41A C42A C43A 116(2) . . ? C41A C42A H42A 122.0 . . ? C43A C42A H42A 122.0 . . ? C42A C43A C44A 117(2) . . ? C42A C43A H43A 121.3 . . ? C44A C43A H43A 121.3 . . ? C43A C44A C45A 124(2) . . ? C43A C44A H44A 118.0 . . ? C45A C44A H44A 118.0 . . ? C46A C45A C44A 116(2) . . ? C46A C45A H45A 122.0 . . ? C44A C45A H45A 122.0 . . ? C41A C46A C45A 115(2) . . ? C41A C46A H46A 122.4 . . ? C45A C46A H46A 122.4 . . ? C52 C50 C51 119.3(4) . . ? C52 C50 H50 120.3 . . ? C51 C50 H50 120.3 . . ? C52 C51 C50 120.0(4) 2_765 . ? C52 C51 H51 120.0 2_765 . ? C50 C51 H51 120.0 . . ? C50 C52 C51 120.6(4) . 2_765 ? C50 C52 H52 119.7 . . ? C51 C52 H52 119.7 2_765 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.261 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.044 #===END data_complex3 _database_code_depnum_ccdc_archive 'CCDC 606736' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H62 N2 P2 Zn' _chemical_formula_sum 'C44 H62 N2 P2 Zn' _chemical_formula_weight 746.27 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.567(3) _cell_length_b 17.867(4) _cell_length_c 19.039(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.43(3) _cell_angle_gamma 90.00 _cell_volume 4262.1(17) _cell_formula_units_Z 4 _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 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.682 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8757 _exptl_absorpt_correction_T_max 0.9350 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski and Minor 1997)' _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 'phi/omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11961 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0722 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7140 _reflns_number_gt 5062 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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^)+(0.0401P)^2^+2.4944P] 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 7140 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1093 _refine_ls_wR_factor_gt 0.0947 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 P1 P 0.78219(6) 0.65957(4) 0.11093(4) 0.02396(19) Uani 1 1 d . . . P2 P 0.85203(6) 0.73832(4) 0.19260(4) 0.02189(19) Uani 1 1 d . . . Zn1 Zn 0.72248(3) 0.827359(18) 0.075867(19) 0.02698(12) Uani 1 1 d . . . N1 N 0.69051(18) 0.71876(13) 0.07632(13) 0.0248(6) Uani 1 1 d . . . N2 N 0.82440(19) 0.82191(12) 0.16257(12) 0.0230(6) Uani 1 1 d . . . C1 C 0.5919(2) 0.68386(15) 0.04962(17) 0.0289(7) Uani 1 1 d . . . C2 C 0.5878(3) 0.64548(17) -0.01533(18) 0.0348(8) Uani 1 1 d . . . C3 C 0.4931(3) 0.60734(19) -0.0376(2) 0.0444(9) Uani 1 1 d . . . H3 H 0.4893 0.5805 -0.0807 0.053 Uiso 1 1 calc R . . C4 C 0.4056(3) 0.6082(2) 0.0021(2) 0.0536(11) Uani 1 1 d . . . H4 H 0.3435 0.5804 -0.0131 0.064 Uiso 1 1 calc R . . C5 C 0.4080(3) 0.6488(2) 0.0630(2) 0.0477(10) Uani 1 1 d . . . H5 H 0.3461 0.6509 0.0886 0.057 Uiso 1 1 calc R . . C6 C 0.5000(3) 0.68742(17) 0.08842(19) 0.0353(8) Uani 1 1 d . . . C7 C 0.4965(3) 0.7354(2) 0.1540(2) 0.0456(9) Uani 1 1 d . . . H7 H 0.5720 0.7457 0.1720 0.055 Uiso 1 1 calc R . . C8 C 0.4441(4) 0.8104(2) 0.1351(3) 0.0899(17) Uani 1 1 d . . . H8A H 0.4834 0.8354 0.0993 0.135 Uiso 1 1 calc R . . H8B H 0.4451 0.8419 0.1773 0.135 Uiso 1 1 calc R . . H8C H 0.3701 0.8022 0.1166 0.135 Uiso 1 1 calc R . . C9 C 0.4405(4) 0.7004(3) 0.2141(2) 0.0765(14) Uani 1 1 d . . . H9A H 0.3661 0.6897 0.1981 0.115 Uiso 1 1 calc R . . H9B H 0.4428 0.7352 0.2539 0.115 Uiso 1 1 calc R . . H9C H 0.4767 0.6537 0.2288 0.115 Uiso 1 1 calc R . . C10 C 0.6807(3) 0.64532(18) -0.06215(17) 0.0373(8) Uani 1 1 d . . . H10 H 0.7363 0.6799 -0.0401 0.045 Uiso 1 1 calc R . . C11 C 0.7322(3) 0.5674(2) -0.0657(2) 0.0536(10) Uani 1 1 d . . . H11A H 0.6815 0.5327 -0.0901 0.080 Uiso 1 1 calc R . . H11B H 0.7511 0.5492 -0.0178 0.080 Uiso 1 1 calc R . . H11C H 0.7967 0.5708 -0.0913 0.080 Uiso 1 1 calc R . . C12 C 0.6497(3) 0.6748(2) -0.13629(19) 0.0526(10) Uani 1 1 d . . . H12A H 0.5964 0.6415 -0.1600 0.079 Uiso 1 1 calc R . . H12B H 0.7131 0.6766 -0.1632 0.079 Uiso 1 1 calc R . . H12C H 0.6197 0.7252 -0.1332 0.079 Uiso 1 1 calc R . . C13 C 0.9026(2) 0.66424(16) 0.05939(15) 0.0273(7) Uani 1 1 d . . . C14 C 0.9717(3) 0.60266(19) 0.06326(18) 0.0383(8) Uani 1 1 d . . . H14 H 0.9529 0.5589 0.0878 0.046 Uiso 1 1 calc R . . C15 C 1.0683(3) 0.6049(2) 0.0313(2) 0.0536(11) Uani 1 1 d . . . H15 H 1.1146 0.5629 0.0349 0.064 Uiso 1 1 calc R . . C16 C 1.0970(3) 0.6672(3) -0.0053(2) 0.0548(11) Uani 1 1 d . . . H16 H 1.1640 0.6693 -0.0252 0.066 Uiso 1 1 calc R . . C17 C 1.0269(3) 0.7267(2) -0.01256(19) 0.0462(9) Uani 1 1 d . . . H17 H 1.0443 0.7689 -0.0398 0.055 Uiso 1 1 calc R . . C18 C 0.9314(3) 0.72565(19) 0.01946(17) 0.0353(8) Uani 1 1 d . . . H18 H 0.8846 0.7674 0.0141 0.042 Uiso 1 1 calc R . . C19 C 0.8023(2) 0.71462(16) 0.27756(16) 0.0249(7) Uani 1 1 d . . . C20 C 0.7246(3) 0.65923(17) 0.28262(18) 0.0353(8) Uani 1 1 d . . . H20 H 0.6912 0.6374 0.2411 0.042 Uiso 1 1 calc R . . C21 C 0.6960(3) 0.6359(2) 0.3485(2) 0.0482(10) Uani 1 1 d . . . H21 H 0.6428 0.5985 0.3517 0.058 Uiso 1 1 calc R . . C22 C 0.7449(3) 0.66685(19) 0.40881(19) 0.0427(9) Uani 1 1 d . . . H22 H 0.7265 0.6502 0.4537 0.051 Uiso 1 1 calc R . . C23 C 0.8205(3) 0.72203(19) 0.40401(18) 0.0398(9) Uani 1 1 d . . . H23 H 0.8536 0.7437 0.4457 0.048 Uiso 1 1 calc R . . C24 C 0.8488(3) 0.74624(17) 0.33889(16) 0.0318(8) Uani 1 1 d . . . H24 H 0.9005 0.7848 0.3363 0.038 Uiso 1 1 calc R . . C25 C 0.9945(2) 0.72100(16) 0.20864(16) 0.0267(7) Uani 1 1 d . . . H25A H 1.0286 0.7283 0.1640 0.032 Uiso 1 1 calc R . . H25B H 1.0249 0.7586 0.2427 0.032 Uiso 1 1 calc R . . C26 C 1.0229(2) 0.64240(18) 0.23724(17) 0.0325(8) Uani 1 1 d . . . H26A H 1.0075 0.6396 0.2874 0.039 Uiso 1 1 calc R . . H26B H 0.9778 0.6049 0.2109 0.039 Uiso 1 1 calc R . . C27 C 1.1401(3) 0.6237(2) 0.2307(2) 0.0462(9) Uani 1 1 d . . . H27A H 1.1590 0.6368 0.1827 0.055 Uiso 1 1 calc R . . H27B H 1.1847 0.6546 0.2646 0.055 Uiso 1 1 calc R . . C28 C 1.1651(3) 0.5415(2) 0.2445(2) 0.0642(12) Uani 1 1 d . . . H28A H 1.1496 0.5288 0.2927 0.096 Uiso 1 1 calc R . . H28B H 1.2407 0.5323 0.2385 0.096 Uiso 1 1 calc R . . H28C H 1.1211 0.5106 0.2111 0.096 Uiso 1 1 calc R . . C29 C 0.8658(3) 0.88510(16) 0.20373(16) 0.0293(8) Uani 1 1 d . . . C30 C 0.9684(3) 0.91366(17) 0.19334(18) 0.0355(8) Uani 1 1 d . . . C31 C 1.0083(3) 0.97130(19) 0.2375(2) 0.0568(12) Uani 1 1 d . . . H31 H 1.0775 0.9907 0.2319 0.068 Uiso 1 1 calc R . . C32 C 0.9491(4) 1.0007(2) 0.2893(2) 0.0667(14) Uani 1 1 d . . . H32 H 0.9789 1.0381 0.3204 0.080 Uiso 1 1 calc R . . C33 C 0.8466(4) 0.9755(2) 0.2958(2) 0.0601(13) Uani 1 1 d . . . H33 H 0.8057 0.9972 0.3304 0.072 Uiso 1 1 calc R . . C34 C 0.8016(3) 0.91894(17) 0.25271(17) 0.0401(9) Uani 1 1 d . . . C35 C 1.0323(3) 0.8879(2) 0.13323(19) 0.0425(9) Uani 1 1 d . . . H35 H 1.0013 0.8392 0.1157 0.051 Uiso 1 1 calc R . . C36 C 1.1521(3) 0.8750(3) 0.1528(2) 0.0635(12) Uani 1 1 d . . . H36A H 1.1875 0.9233 0.1619 0.095 Uiso 1 1 calc R . . H36B H 1.1839 0.8498 0.1137 0.095 Uiso 1 1 calc R . . H36C H 1.1612 0.8437 0.1951 0.095 Uiso 1 1 calc R . . C37 C 1.0199(3) 0.9441(2) 0.0718(2) 0.0663(13) Uani 1 1 d . . . H37A H 0.9439 0.9543 0.0601 0.099 Uiso 1 1 calc R . . H37B H 1.0512 0.9230 0.0306 0.099 Uiso 1 1 calc R . . H37C H 1.0566 0.9908 0.0857 0.099 Uiso 1 1 calc R . . C38 C 0.6843(3) 0.8994(2) 0.2554(2) 0.0499(10) Uani 1 1 d . . . H38 H 0.6717 0.8495 0.2325 0.060 Uiso 1 1 calc R . . C39 C 0.6460(5) 0.8954(3) 0.3300(2) 0.101(2) Uani 1 1 d . . . H39A H 0.6934 0.8624 0.3592 0.151 Uiso 1 1 calc R . . H39B H 0.5731 0.8756 0.3277 0.151 Uiso 1 1 calc R . . H39C H 0.6472 0.9457 0.3507 0.151 Uiso 1 1 calc R . . C40 C 0.6188(4) 0.9577(3) 0.2121(2) 0.0729(13) Uani 1 1 d . . . H40A H 0.6329 1.0075 0.2323 0.109 Uiso 1 1 calc R . . H40B H 0.5427 0.9461 0.2128 0.109 Uiso 1 1 calc R . . H40C H 0.6389 0.9569 0.1634 0.109 Uiso 1 1 calc R . . C41 C 0.6866(3) 0.89976(17) -0.00221(18) 0.0367(8) Uani 1 1 d . . . C42 C 0.5714(3) 0.8857(2) -0.0336(2) 0.0621(12) Uani 1 1 d . . . H42A H 0.5210 0.9010 0.0005 0.093 Uiso 1 1 calc R . . H42B H 0.5620 0.8324 -0.0442 0.093 Uiso 1 1 calc R . . H42C H 0.5582 0.9149 -0.0770 0.093 Uiso 1 1 calc R . . C43 C 0.7624(3) 0.8825(2) -0.06046(18) 0.0478(10) Uani 1 1 d . . . H43A H 0.7453 0.9156 -0.1009 0.072 Uiso 1 1 calc R . . H43B H 0.7534 0.8303 -0.0754 0.072 Uiso 1 1 calc R . . H43C H 0.8364 0.8909 -0.0421 0.072 Uiso 1 1 calc R . . C44 C 0.6967(3) 0.98264(18) 0.0164(2) 0.0530(11) Uani 1 1 d . . . H44A H 0.6833 1.0127 -0.0264 0.079 Uiso 1 1 calc R . . H44B H 0.7688 0.9928 0.0375 0.079 Uiso 1 1 calc R . . H44C H 0.6444 0.9956 0.0501 0.079 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 P1 0.0243(4) 0.0212(4) 0.0260(4) -0.0003(3) -0.0006(3) 0.0006(3) P2 0.0222(4) 0.0208(4) 0.0224(4) 0.0010(3) 0.0006(3) 0.0000(3) Zn1 0.0282(2) 0.02255(19) 0.0294(2) 0.00273(15) -0.00259(16) 0.00168(15) N1 0.0201(14) 0.0226(13) 0.0307(15) -0.0014(11) -0.0037(12) -0.0005(10) N2 0.0248(14) 0.0206(12) 0.0234(14) 0.0005(10) 0.0004(11) -0.0015(11) C1 0.0238(18) 0.0216(16) 0.040(2) 0.0069(14) -0.0061(15) 0.0007(13) C2 0.036(2) 0.0258(16) 0.041(2) -0.0009(15) -0.0113(17) -0.0007(14) C3 0.042(2) 0.038(2) 0.050(2) -0.0029(17) -0.0172(19) -0.0048(17) C4 0.036(2) 0.046(2) 0.075(3) 0.007(2) -0.020(2) -0.0129(18) C5 0.029(2) 0.051(2) 0.063(3) 0.017(2) -0.0026(19) -0.0048(17) C6 0.0251(19) 0.0329(18) 0.047(2) 0.0071(16) -0.0022(16) 0.0015(14) C7 0.032(2) 0.049(2) 0.057(3) -0.0007(19) 0.0125(18) -0.0011(17) C8 0.117(5) 0.051(3) 0.103(4) -0.002(3) 0.018(4) 0.025(3) C9 0.083(4) 0.077(3) 0.074(3) -0.003(3) 0.035(3) -0.007(3) C10 0.042(2) 0.0361(18) 0.032(2) -0.0073(15) -0.0080(17) -0.0003(16) C11 0.063(3) 0.047(2) 0.050(2) -0.0104(19) -0.004(2) 0.011(2) C12 0.061(3) 0.056(2) 0.038(2) -0.0034(18) -0.0123(19) -0.007(2) C13 0.0275(18) 0.0324(17) 0.0214(17) -0.0054(13) -0.0013(14) 0.0021(14) C14 0.039(2) 0.040(2) 0.035(2) -0.0051(15) 0.0023(17) 0.0121(16) C15 0.043(2) 0.067(3) 0.051(3) -0.012(2) 0.007(2) 0.024(2) C16 0.039(2) 0.086(3) 0.042(2) -0.010(2) 0.0185(19) 0.005(2) C17 0.038(2) 0.067(3) 0.035(2) -0.0016(19) 0.0106(18) -0.005(2) C18 0.033(2) 0.0421(19) 0.0311(19) -0.0028(16) 0.0040(16) 0.0015(16) C19 0.0251(17) 0.0243(16) 0.0256(18) 0.0028(13) 0.0040(14) 0.0043(13) C20 0.042(2) 0.0326(18) 0.032(2) -0.0026(15) 0.0067(16) -0.0051(15) C21 0.058(3) 0.042(2) 0.047(2) 0.0032(18) 0.019(2) -0.0126(19) C22 0.062(3) 0.0368(19) 0.031(2) 0.0047(16) 0.0187(18) 0.0072(18) C23 0.052(2) 0.040(2) 0.027(2) -0.0012(16) 0.0013(17) 0.0090(17) C24 0.035(2) 0.0334(18) 0.0270(19) 0.0004(14) 0.0017(15) 0.0015(15) C25 0.0228(17) 0.0319(17) 0.0254(17) 0.0028(13) 0.0029(14) -0.0026(13) C26 0.0271(18) 0.0369(18) 0.0326(19) 0.0057(15) -0.0030(15) 0.0052(14) C27 0.030(2) 0.061(2) 0.047(2) 0.0046(19) -0.0002(17) 0.0150(18) C28 0.056(3) 0.071(3) 0.064(3) -0.004(2) -0.003(2) 0.038(2) C29 0.042(2) 0.0203(15) 0.0239(18) 0.0019(13) -0.0048(15) -0.0009(14) C30 0.043(2) 0.0231(16) 0.038(2) 0.0087(15) -0.0151(17) -0.0041(15) C31 0.067(3) 0.0274(19) 0.070(3) 0.007(2) -0.035(2) -0.0084(19) C32 0.112(4) 0.0229(19) 0.057(3) -0.0086(19) -0.043(3) 0.002(2) C33 0.111(4) 0.030(2) 0.035(2) -0.0048(17) -0.015(2) 0.020(2) C34 0.066(3) 0.0259(17) 0.0273(19) 0.0035(15) -0.0012(18) 0.0105(17) C35 0.034(2) 0.043(2) 0.049(2) 0.0127(18) -0.0078(18) -0.0174(16) C36 0.036(2) 0.079(3) 0.074(3) 0.024(2) -0.006(2) -0.017(2) C37 0.060(3) 0.078(3) 0.061(3) 0.036(2) 0.000(2) -0.012(2) C38 0.068(3) 0.040(2) 0.045(2) 0.0033(17) 0.026(2) 0.0168(19) C39 0.111(5) 0.133(5) 0.065(3) 0.030(3) 0.045(3) 0.053(4) C40 0.072(3) 0.073(3) 0.074(3) 0.011(3) 0.006(3) 0.021(2) C41 0.040(2) 0.0318(18) 0.037(2) 0.0072(15) -0.0092(17) 0.0019(15) C42 0.052(3) 0.063(3) 0.067(3) 0.018(2) -0.024(2) 0.003(2) C43 0.063(3) 0.045(2) 0.035(2) 0.0115(17) -0.0006(19) 0.0009(19) C44 0.076(3) 0.0309(19) 0.051(2) 0.0097(17) -0.002(2) 0.0076(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 N1 1.662(2) . ? P1 C13 1.868(3) . ? P1 P2 2.2264(11) . ? P2 N2 1.627(2) . ? P2 C25 1.819(3) . ? P2 C19 1.828(3) . ? Zn1 N1 1.982(2) . ? Zn1 C41 1.996(3) . ? Zn1 N2 2.012(2) . ? N1 C1 1.444(4) . ? N2 C29 1.448(4) . ? C1 C2 1.411(4) . ? C1 C6 1.420(4) . ? C2 C3 1.408(5) . ? C2 C10 1.523(5) . ? C3 C4 1.381(5) . ? C3 H3 0.9500 . ? C4 C5 1.367(5) . ? C4 H4 0.9500 . ? C5 C6 1.400(5) . ? C5 H5 0.9500 . ? C6 C7 1.517(5) . ? C7 C9 1.522(5) . ? C7 C8 1.525(5) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.529(5) . ? C10 C11 1.538(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.398(4) . ? C13 C14 1.400(4) . ? C14 C15 1.399(5) . ? C14 H14 0.9500 . ? C15 C16 1.376(5) . ? C15 H15 0.9500 . ? C16 C17 1.381(5) . ? C16 H16 0.9500 . ? C17 C18 1.389(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.385(4) . ? C19 C20 1.398(4) . ? C20 C21 1.395(5) . ? C20 H20 0.9500 . ? C21 C22 1.376(5) . ? C21 H21 0.9500 . ? C22 C23 1.377(5) . ? C22 H22 0.9500 . ? C23 C24 1.385(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.538(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.524(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.519(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.414(5) . ? C29 C34 1.415(5) . ? C30 C31 1.398(5) . ? C30 C35 1.520(5) . ? C31 C32 1.385(6) . ? C31 H31 0.9500 . ? C32 C33 1.378(6) . ? C32 H32 0.9500 . ? C33 C34 1.393(5) . ? C33 H33 0.9500 . ? C34 C38 1.520(5) . ? C35 C36 1.540(5) . ? C35 C37 1.541(5) . ? C35 H35 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C40 1.529(5) . ? C38 C39 1.536(5) . ? C38 H38 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C44 1.526(4) . ? C41 C42 1.543(5) . ? C41 C43 1.548(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 P1 C13 109.15(13) . . ? N1 P1 P2 95.66(9) . . ? C13 P1 P2 92.70(10) . . ? N2 P2 C25 113.30(13) . . ? N2 P2 C19 116.44(13) . . ? C25 P2 C19 102.20(14) . . ? N2 P2 P1 105.83(9) . . ? C25 P2 P1 109.84(11) . . ? C19 P2 P1 109.17(10) . . ? N1 Zn1 C41 127.13(12) . . ? N1 Zn1 N2 93.75(9) . . ? C41 Zn1 N2 137.34(11) . . ? C1 N1 P1 114.49(18) . . ? C1 N1 Zn1 126.15(18) . . ? P1 N1 Zn1 119.35(13) . . ? C29 N2 P2 117.87(19) . . ? C29 N2 Zn1 125.86(18) . . ? P2 N2 Zn1 115.96(12) . . ? C2 C1 C6 120.1(3) . . ? C2 C1 N1 119.3(3) . . ? C6 C1 N1 120.5(3) . . ? C3 C2 C1 118.1(3) . . ? C3 C2 C10 119.5(3) . . ? C1 C2 C10 122.5(3) . . ? C4 C3 C2 121.4(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 120.2(3) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 121.2(4) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 118.8(3) . . ? C5 C6 C7 119.2(3) . . ? C1 C6 C7 122.0(3) . . ? C6 C7 C9 115.5(3) . . ? C6 C7 C8 110.0(3) . . ? C9 C7 C8 108.7(3) . . ? C6 C7 H7 107.4 . . ? C9 C7 H7 107.4 . . ? C8 C7 H7 107.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 C12 112.8(3) . . ? C2 C10 C11 111.8(3) . . ? C12 C10 C11 110.5(3) . . ? C2 C10 H10 107.2 . . ? C12 C10 H10 107.2 . . ? C11 C10 H10 107.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 117.4(3) . . ? C18 C13 P1 125.1(2) . . ? C14 C13 P1 117.5(2) . . ? C15 C14 C13 120.6(3) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C16 C15 C14 120.9(3) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 118.9(4) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C16 C17 C18 120.8(4) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C13 121.2(3) . . ? C17 C18 H18 119.4 . . ? C13 C18 H18 119.4 . . ? C24 C19 C20 118.8(3) . . ? C24 C19 P2 120.0(2) . . ? C20 C19 P2 120.9(2) . . ? C21 C20 C19 120.2(3) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C22 C21 C20 120.0(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 119.9(3) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C22 C23 C24 120.6(3) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C19 120.4(3) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C26 C25 P2 114.4(2) . . ? C26 C25 H25A 108.7 . . ? P2 C25 H25A 108.7 . . ? C26 C25 H25B 108.7 . . ? P2 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? C27 C26 C25 111.8(3) . . ? C27 C26 H26A 109.3 . . ? C25 C26 H26A 109.3 . . ? C27 C26 H26B 109.3 . . ? C25 C26 H26B 109.3 . . ? H26A C26 H26B 107.9 . . ? C28 C27 C26 112.7(3) . . ? C28 C27 H27A 109.0 . . ? C26 C27 H27A 109.0 . . ? C28 C27 H27B 109.0 . . ? C26 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C34 120.7(3) . . ? C30 C29 N2 119.9(3) . . ? C34 C29 N2 119.3(3) . . ? C31 C30 C29 118.0(4) . . ? C31 C30 C35 119.4(3) . . ? C29 C30 C35 122.4(3) . . ? C32 C31 C30 121.4(4) . . ? C32 C31 H31 119.3 . . ? C30 C31 H31 119.3 . . ? C33 C32 C31 119.8(4) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 121.6(4) . . ? C32 C33 H33 119.2 . . ? C34 C33 H33 119.2 . . ? C33 C34 C29 118.1(4) . . ? C33 C34 C38 119.9(4) . . ? C29 C34 C38 121.9(3) . . ? C30 C35 C36 115.3(3) . . ? C30 C35 C37 110.2(3) . . ? C36 C35 C37 108.7(3) . . ? C30 C35 H35 107.4 . . ? C36 C35 H35 107.4 . . ? C37 C35 H35 107.4 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 C40 107.9(3) . . ? C34 C38 C39 114.5(4) . . ? C40 C38 C39 109.6(3) . . ? C34 C38 H38 108.2 . . ? C40 C38 H38 108.2 . . ? C39 C38 H38 108.2 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C44 C41 C42 107.8(3) . . ? C44 C41 C43 108.3(3) . . ? C42 C41 C43 107.5(3) . . ? C44 C41 Zn1 116.5(2) . . ? C42 C41 Zn1 109.5(2) . . ? C43 C41 Zn1 106.8(2) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.346 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.063 #===END data_complex4 _database_code_depnum_ccdc_archive 'CCDC 606737' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C80 H106 Hg N4 P4, C6 H14' _chemical_formula_sum 'C86 H120 Hg N4 P4' _chemical_formula_weight 1534.33 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' 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 C2/c _symmetry_space_group_name_Hall -C2yc 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 56.751(11) _cell_length_b 13.295(3) _cell_length_c 21.809(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.31(3) _cell_angle_gamma 90.00 _cell_volume 16076(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6432 _exptl_absorpt_coefficient_mu 2.039 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8221 _exptl_absorpt_correction_T_max 0.9413 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski and Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 446(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 'phi/omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52541 _diffrn_reflns_av_R_equivalents 0.0707 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -67 _diffrn_reflns_limit_h_max 67 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.03 _reflns_number_total 14181 _reflns_number_gt 10858 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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 ; The main residue is well-ordered and all non-hydrogen atoms were refined anisotropically, with the exception of carbon atoms C79-C81 from an n-butyl group. These were modeled over two sites using geometric restraints. The thermal parameters were refined best using a 75:25 isotropic mixture. The structure also contains a disordered lattice molecule of n-hexane which was modeled over two sites and the thermal parameters were optimally refined to an isotropic 70:30 mixture. 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^)+(0.0696P)^2^+74.2185P] 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 14181 _refine_ls_number_parameters 848 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1465 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 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 0.620350(4) 0.600412(18) 0.490101(11) 0.03272(10) Uani 1 1 d . . . N1 N 0.56946(9) 0.7151(4) 0.4546(2) 0.0350(12) Uani 1 1 d . . . N2 N 0.58791(9) 0.7856(4) 0.5669(2) 0.0379(13) Uani 1 1 d . . . N3 N 0.67012(9) 0.5101(4) 0.4662(2) 0.0336(12) Uani 1 1 d . . . N4 N 0.65474(10) 0.3676(4) 0.5317(3) 0.0393(13) Uani 1 1 d . . . P1 P 0.59587(3) 0.75061(13) 0.50627(8) 0.0314(4) Uani 1 1 d . . . P2 P 0.57399(3) 0.63474(14) 0.39588(8) 0.0394(4) Uani 1 1 d . . . P3 P 0.64508(3) 0.44843(12) 0.48093(8) 0.0311(4) Uani 1 1 d . . . P4 P 0.66379(3) 0.62319(13) 0.42705(10) 0.0457(5) Uani 1 1 d . B . C1 C 0.60991(12) 0.8536(5) 0.4707(3) 0.0342(14) Uani 1 1 d . . . C2 C 0.61608(14) 0.9433(6) 0.5031(3) 0.0471(18) Uani 1 1 d . . . H2 H 0.6118 0.9530 0.5416 0.057 Uiso 1 1 calc R . . C3 C 0.62854(15) 1.0183(5) 0.4791(4) 0.0514(19) Uani 1 1 d . . . H3 H 0.6325 1.0781 0.5011 0.062 Uiso 1 1 calc R . . C4 C 0.63505(15) 1.0035(6) 0.4222(3) 0.0524(19) Uani 1 1 d . . . H4 H 0.6434 1.0537 0.4059 0.063 Uiso 1 1 calc R . . C5 C 0.62932(14) 0.9152(5) 0.3894(3) 0.0470(18) Uani 1 1 d . . . H5 H 0.6337 0.9060 0.3511 0.056 Uiso 1 1 calc R . . C6 C 0.61725(13) 0.8414(5) 0.4133(3) 0.0421(17) Uani 1 1 d . . . H6 H 0.6138 0.7815 0.3912 0.050 Uiso 1 1 calc R . . C7 C 0.59623(13) 0.8356(5) 0.6232(3) 0.0388(16) Uani 1 1 d . . . C8 C 0.62066(13) 0.8284(5) 0.6585(3) 0.0390(16) Uani 1 1 d . . . C9 C 0.63867(13) 0.7620(5) 0.6359(3) 0.0437(17) Uani 1 1 d . . . H9 H 0.6348 0.7647 0.5899 0.052 Uiso 1 1 calc R . . C10 C 0.63531(15) 0.6524(6) 0.6546(4) 0.056(2) Uani 1 1 d . . . H10A H 0.6450 0.6091 0.6347 0.084 Uiso 1 1 calc R . . H10B H 0.6186 0.6339 0.6414 0.084 Uiso 1 1 calc R . . H10C H 0.6402 0.6456 0.6993 0.084 Uiso 1 1 calc R . . C11 C 0.66466(14) 0.7943(7) 0.6571(4) 0.063(2) Uani 1 1 d . . . H11A H 0.6661 0.8642 0.6474 0.094 Uiso 1 1 calc R . . H11B H 0.6746 0.7549 0.6359 0.094 Uiso 1 1 calc R . . H11C H 0.6697 0.7845 0.7016 0.094 Uiso 1 1 calc R . . C12 C 0.57930(15) 0.8944(6) 0.6479(4) 0.053(2) Uani 1 1 d . . . C13 C 0.58746(19) 0.9437(6) 0.7050(4) 0.062(2) Uani 1 1 d . . . H13 H 0.5766 0.9824 0.7213 0.074 Uiso 1 1 calc R . . C14 C 0.61116(19) 0.9373(6) 0.7383(4) 0.064(2) Uani 1 1 d . . . H14 H 0.6160 0.9713 0.7762 0.076 Uiso 1 1 calc R . . C15 C 0.62752(16) 0.8798(5) 0.7147(3) 0.053(2) Uani 1 1 d . . . H15 H 0.6434 0.8756 0.7369 0.063 Uiso 1 1 calc R . . C16 C 0.55393(15) 0.9078(7) 0.6126(4) 0.067(2) Uani 1 1 d . . . H16 H 0.5513 0.8634 0.5759 0.080 Uiso 1 1 calc R . . C17 C 0.53619(19) 0.8785(10) 0.6527(6) 0.106(4) Uani 1 1 d . . . H17A H 0.5397 0.8116 0.6686 0.159 Uiso 1 1 calc R . . H17B H 0.5201 0.8808 0.6277 0.159 Uiso 1 1 calc R . . H17C H 0.5376 0.9247 0.6872 0.159 Uiso 1 1 calc R . . C18 C 0.5504(2) 1.0175(8) 0.5893(6) 0.100(4) Uani 1 1 d . . . H18A H 0.5533 1.0623 0.6246 0.150 Uiso 1 1 calc R . . H18B H 0.5342 1.0263 0.5657 0.150 Uiso 1 1 calc R . . H18C H 0.5616 1.0321 0.5630 0.150 Uiso 1 1 calc R . . C19 C 0.54611(12) 0.7456(6) 0.4654(3) 0.0427(17) Uani 1 1 d . . . C20 C 0.53605(12) 0.6855(6) 0.5054(3) 0.0449(17) Uani 1 1 d . . . C21 C 0.51345(14) 0.7126(7) 0.5137(4) 0.060(2) Uani 1 1 d . . . H21 H 0.5059 0.6741 0.5395 0.072 Uiso 1 1 calc R . . C22 C 0.50192(15) 0.7971(8) 0.4837(5) 0.073(3) Uani 1 1 d . . . H22 H 0.4866 0.8139 0.4895 0.087 Uiso 1 1 calc R . . C23 C 0.51241(15) 0.8557(8) 0.4462(5) 0.070(2) Uani 1 1 d . . . H23 H 0.5044 0.9121 0.4268 0.084 Uiso 1 1 calc R . . C24 C 0.53501(13) 0.8314(6) 0.4367(4) 0.053(2) Uani 1 1 d . . . C25 C 0.54597(15) 0.9033(6) 0.3964(4) 0.060(2) Uani 1 1 d . . . H25 H 0.5603 0.8702 0.3875 0.072 Uiso 1 1 calc R . . C26 C 0.52896(17) 0.9261(8) 0.3322(4) 0.082(3) Uani 1 1 d . . . H26A H 0.5226 0.8642 0.3128 0.123 Uiso 1 1 calc R . . H26B H 0.5378 0.9602 0.3056 0.123 Uiso 1 1 calc R . . H26C H 0.5159 0.9680 0.3386 0.123 Uiso 1 1 calc R . . C27 C 0.55442(19) 1.0007(7) 0.4308(5) 0.089(3) Uani 1 1 d . . . H27A H 0.5407 1.0382 0.4372 0.134 Uiso 1 1 calc R . . H27B H 0.5632 1.0399 0.4062 0.134 Uiso 1 1 calc R . . H27C H 0.5647 0.9855 0.4706 0.134 Uiso 1 1 calc R . . C28 C 0.54816(12) 0.5960(6) 0.5419(3) 0.0488(18) Uani 1 1 d . . . H28 H 0.5633 0.5844 0.5284 0.059 Uiso 1 1 calc R . . C29 C 0.55443(15) 0.6154(7) 0.6118(4) 0.061(2) Uani 1 1 d . . . H29A H 0.5627 0.6786 0.6198 0.092 Uiso 1 1 calc R . . H29B H 0.5647 0.5625 0.6323 0.092 Uiso 1 1 calc R . . H29C H 0.5399 0.6172 0.6277 0.092 Uiso 1 1 calc R . . C30 C 0.53361(13) 0.4998(7) 0.5296(4) 0.058(2) Uani 1 1 d . . . H30A H 0.5428 0.4451 0.5516 0.087 Uiso 1 1 calc R . . H30B H 0.5300 0.4858 0.4854 0.087 Uiso 1 1 calc R . . H30C H 0.5189 0.5073 0.5441 0.087 Uiso 1 1 calc R . . C31 C 0.55053(13) 0.5385(6) 0.3853(4) 0.0512(19) Uani 1 1 d . . . C32 C 0.52590(15) 0.5611(8) 0.3631(4) 0.066(2) Uani 1 1 d . . . H32 H 0.5206 0.6275 0.3606 0.079 Uiso 1 1 calc R . . C33 C 0.50991(17) 0.4838(10) 0.3452(4) 0.084(3) Uani 1 1 d . . . H33 H 0.4936 0.4970 0.3312 0.101 Uiso 1 1 calc R . . C34 C 0.5186(2) 0.3832(9) 0.3482(5) 0.091(4) Uani 1 1 d . . . H34 H 0.5079 0.3305 0.3360 0.109 Uiso 1 1 calc R . . C35 C 0.54159(19) 0.3643(8) 0.3681(5) 0.078(3) Uani 1 1 d . . . H35 H 0.5470 0.2982 0.3710 0.093 Uiso 1 1 calc R . . C36 C 0.55743(15) 0.4407(7) 0.3843(4) 0.065(2) Uani 1 1 d . . . H36 H 0.5738 0.4256 0.3953 0.078 Uiso 1 1 calc R . . C37 C 0.56404(13) 0.7016(6) 0.3209(3) 0.0539(19) Uani 1 1 d . . . H37A H 0.5472 0.7196 0.3162 0.065 Uiso 1 1 calc R . . H37B H 0.5732 0.7635 0.3223 0.065 Uiso 1 1 calc R . . C38 C 0.56693(18) 0.6424(8) 0.2650(4) 0.076(3) Uani 1 1 d . . . H38A H 0.5573 0.5816 0.2627 0.092 Uiso 1 1 calc R . . H38B H 0.5837 0.6224 0.2703 0.092 Uiso 1 1 calc R . . C39 C 0.5594(2) 0.7005(10) 0.2030(4) 0.102(4) Uani 1 1 d . . . H39A H 0.5693 0.7602 0.2051 0.123 Uiso 1 1 calc R . . H39B H 0.5626 0.6588 0.1692 0.123 Uiso 1 1 calc R . . C40 C 0.5342(3) 0.7306(12) 0.1881(6) 0.139(6) Uani 1 1 d . . . H40A H 0.5243 0.6744 0.1936 0.208 Uiso 1 1 calc R . . H40B H 0.5300 0.7531 0.1453 0.208 Uiso 1 1 calc R . . H40C H 0.5317 0.7843 0.2155 0.208 Uiso 1 1 calc R . . C41 C 0.62873(11) 0.3916(5) 0.4069(3) 0.0357(15) Uani 1 1 d . . . C42 C 0.62038(12) 0.4493(5) 0.3528(3) 0.0394(16) Uani 1 1 d . . . H42 H 0.6237 0.5178 0.3533 0.047 Uiso 1 1 calc R . . C43 C 0.60734(13) 0.4060(6) 0.2991(3) 0.0469(18) Uani 1 1 d . . . H43 H 0.6024 0.4444 0.2630 0.056 Uiso 1 1 calc R . . C44 C 0.60155(14) 0.3034(6) 0.2988(3) 0.0523(19) Uani 1 1 d . . . H44 H 0.5926 0.2738 0.2626 0.063 Uiso 1 1 calc R . . C46 C 0.62285(13) 0.2891(5) 0.4056(3) 0.0430(17) Uani 1 1 d . . . H46 H 0.6282 0.2497 0.4410 0.052 Uiso 1 1 calc R . . C47 C 0.60922(13) 0.2464(6) 0.3522(3) 0.0468(18) Uani 1 1 d . . . H47 H 0.6051 0.1786 0.3521 0.056 Uiso 1 1 calc R . . C48 C 0.64832(12) 0.2846(5) 0.5638(3) 0.0377(15) Uani 1 1 d . . . C49 C 0.62442(13) 0.2628(5) 0.5695(3) 0.0415(16) Uani 1 1 d . . . C50 C 0.62017(16) 0.1799(6) 0.6048(3) 0.053(2) Uani 1 1 d . . . H50 H 0.6045 0.1667 0.6093 0.064 Uiso 1 1 calc R . . C51 C 0.63869(17) 0.1167(6) 0.6332(4) 0.057(2) Uani 1 1 d . . . H51 H 0.6356 0.0615 0.6565 0.068 Uiso 1 1 calc R . . C52 C 0.66165(16) 0.1369(6) 0.6262(4) 0.057(2) Uani 1 1 d . . . H52 H 0.6740 0.0938 0.6446 0.068 Uiso 1 1 calc R . . C53 C 0.66706(13) 0.2190(5) 0.5930(3) 0.0438(17) Uani 1 1 d . . . C54 C 0.69304(13) 0.2370(6) 0.5890(4) 0.056(2) Uani 1 1 d . . . H54 H 0.6937 0.2986 0.5648 0.067 Uiso 1 1 calc R . . C55 C 0.71021(18) 0.2485(7) 0.6524(5) 0.085(3) Uani 1 1 d . . . H55A H 0.7060 0.3076 0.6730 0.127 Uiso 1 1 calc R . . H55B H 0.7264 0.2549 0.6464 0.127 Uiso 1 1 calc R . . H55C H 0.7091 0.1904 0.6777 0.127 Uiso 1 1 calc R . . C56 C 0.70263(18) 0.1506(7) 0.5557(5) 0.083(3) Uani 1 1 d . . . H56A H 0.7032 0.0905 0.5804 0.124 Uiso 1 1 calc R . . H56B H 0.7186 0.1665 0.5503 0.124 Uiso 1 1 calc R . . H56C H 0.6922 0.1401 0.5154 0.124 Uiso 1 1 calc R . . C57 C 0.60308(13) 0.3324(5) 0.5428(4) 0.0454(18) Uani 1 1 d . . . H57 H 0.6068 0.3648 0.5056 0.054 Uiso 1 1 calc R . . C58 C 0.57903(15) 0.2787(7) 0.5213(4) 0.068(2) Uani 1 1 d . . . H58A H 0.5741 0.2498 0.5570 0.102 Uiso 1 1 calc R . . H58B H 0.5807 0.2264 0.4922 0.102 Uiso 1 1 calc R . . H58C H 0.5671 0.3260 0.5012 0.102 Uiso 1 1 calc R . . C59 C 0.60116(16) 0.4161(6) 0.5893(4) 0.064(2) Uani 1 1 d . . . H59A H 0.5968 0.3878 0.6258 0.096 Uiso 1 1 calc R . . H59B H 0.5890 0.4634 0.5700 0.096 Uiso 1 1 calc R . . H59C H 0.6164 0.4499 0.6012 0.096 Uiso 1 1 calc R . . C60 C 0.69424(11) 0.4694(5) 0.4854(3) 0.0384(16) Uani 1 1 d . . . C61 C 0.70857(12) 0.4989(5) 0.5428(3) 0.0435(17) Uani 1 1 d . . . C62 C 0.73177(14) 0.4604(6) 0.5593(4) 0.056(2) Uani 1 1 d . . . H62 H 0.7415 0.4780 0.5977 0.067 Uiso 1 1 calc R . . C63 C 0.74066(14) 0.3973(6) 0.5204(5) 0.061(2) Uani 1 1 d . . . H63 H 0.7564 0.3737 0.5326 0.073 Uiso 1 1 calc R . . C64 C 0.72689(14) 0.3682(6) 0.4641(4) 0.054(2) Uani 1 1 d . . . H64 H 0.7334 0.3259 0.4380 0.064 Uiso 1 1 calc R . . C65 C 0.70308(13) 0.4016(5) 0.4454(4) 0.0456(17) Uani 1 1 d . . . C66 C 0.68768(14) 0.3597(6) 0.3852(4) 0.0509(19) Uani 1 1 d . . . H66 H 0.6727 0.3988 0.3757 0.061 Uiso 1 1 calc R . . C67 C 0.69941(17) 0.3670(8) 0.3286(4) 0.077(3) Uani 1 1 d . . . H67A H 0.7127 0.3208 0.3336 0.115 Uiso 1 1 calc R . . H67B H 0.7051 0.4343 0.3252 0.115 Uiso 1 1 calc R . . H67C H 0.6878 0.3504 0.2911 0.115 Uiso 1 1 calc R . . C68 C 0.68094(16) 0.2500(6) 0.3943(5) 0.072(3) Uani 1 1 d . . . H68A H 0.6952 0.2092 0.4015 0.108 Uiso 1 1 calc R . . H68B H 0.6699 0.2269 0.3574 0.108 Uiso 1 1 calc R . . H68C H 0.6735 0.2452 0.4299 0.108 Uiso 1 1 calc R . . C69 C 0.69990(13) 0.5673(6) 0.5895(4) 0.0490(18) Uani 1 1 d . . . H69 H 0.6850 0.6001 0.5678 0.059 Uiso 1 1 calc R . . C70 C 0.69435(15) 0.5059(7) 0.6436(4) 0.063(2) Uani 1 1 d . . . H70A H 0.7089 0.4747 0.6662 0.095 Uiso 1 1 calc R . . H70B H 0.6827 0.4550 0.6274 0.095 Uiso 1 1 calc R . . H70C H 0.6880 0.5493 0.6713 0.095 Uiso 1 1 calc R . . C71 C 0.71827(15) 0.6490(7) 0.6148(4) 0.066(2) Uani 1 1 d . . . H71A H 0.7323 0.6189 0.6408 0.100 Uiso 1 1 calc R . . H71B H 0.7113 0.6961 0.6391 0.100 Uiso 1 1 calc R . . H71C H 0.7228 0.6834 0.5804 0.100 Uiso 1 1 calc R . . C72 C 0.68565(12) 0.7172(5) 0.4640(4) 0.0471(18) Uani 1 1 d . . . C73 C 0.70869(14) 0.7277(6) 0.4525(4) 0.060(2) Uani 1 1 d . . . H73 H 0.7149 0.6784 0.4300 0.072 Uiso 1 1 calc R . . C74 C 0.72263(14) 0.8123(7) 0.4745(5) 0.067(2) Uani 1 1 d . . . H74 H 0.7380 0.8190 0.4665 0.081 Uiso 1 1 calc R . . C75 C 0.71376(16) 0.8856(6) 0.5079(5) 0.066(2) Uani 1 1 d . . . H75 H 0.7231 0.9419 0.5221 0.079 Uiso 1 1 calc R . . C76 C 0.69083(15) 0.8753(6) 0.5202(4) 0.063(2) Uani 1 1 d . . . H76 H 0.6848 0.9237 0.5437 0.076 Uiso 1 1 calc R . . C77 C 0.67706(13) 0.7927(5) 0.4974(4) 0.0506(19) Uani 1 1 d . . . H77 H 0.6615 0.7873 0.5046 0.061 Uiso 1 1 calc R . . C78 C 0.67378(18) 0.6031(6) 0.3542(4) 0.068(2) Uani 1 1 d D . . H78A H 0.6903 0.5788 0.3653 0.082 Uiso 1 1 calc R A 1 H78B H 0.6641 0.5489 0.3321 0.082 Uiso 1 1 calc R A 1 C79 C 0.6733(2) 0.6907(11) 0.3066(7) 0.081(4) Uiso 0.75 1 d PD B 1 H79A H 0.6826 0.7474 0.3268 0.097 Uiso 0.75 1 calc PR B 1 H79B H 0.6800 0.6690 0.2716 0.097 Uiso 0.75 1 calc PR B 1 C80 C 0.6465(3) 0.7205(14) 0.2837(9) 0.122(6) Uiso 0.75 1 d PD B 1 H80A H 0.6449 0.7885 0.2671 0.146 Uiso 0.75 1 calc PR B 1 H80B H 0.6377 0.7152 0.3172 0.146 Uiso 0.75 1 calc PR B 1 C81 C 0.6375(3) 0.6416(15) 0.2312(8) 0.125(6) Uiso 0.75 1 d PD B 1 H81A H 0.6505 0.6237 0.2115 0.188 Uiso 0.75 1 calc PR B 1 H81B H 0.6245 0.6697 0.2005 0.188 Uiso 0.75 1 calc PR B 1 H81C H 0.6319 0.5827 0.2493 0.188 Uiso 0.75 1 calc PR B 1 C79A C 0.6646(7) 0.711(2) 0.3277(15) 0.079(12) Uiso 0.25 1 d PD B 2 H79C H 0.6510 0.7334 0.3447 0.095 Uiso 0.25 1 calc PR B 2 H79D H 0.6773 0.7609 0.3376 0.095 Uiso 0.25 1 calc PR B 2 C80A C 0.6568(7) 0.693(4) 0.2541(15) 0.105(15) Uiso 0.25 1 d PD B 2 H80C H 0.6610 0.6268 0.2410 0.126 Uiso 0.25 1 calc PR B 2 H80D H 0.6622 0.7452 0.2292 0.126 Uiso 0.25 1 calc PR B 2 C81A C 0.6281(5) 0.704(3) 0.2584(16) 0.071(10) Uiso 0.25 1 d PD B 2 H81D H 0.6260 0.6786 0.2981 0.106 Uiso 0.25 1 calc PR B 2 H81E H 0.6182 0.6660 0.2252 0.106 Uiso 0.25 1 calc PR B 2 H81F H 0.6235 0.7734 0.2545 0.106 Uiso 0.25 1 calc PR B 2 C93 C 0.7691(3) 0.5307(14) 0.2528(8) 0.090(5) Uiso 0.70 1 d PD C 1 H93A H 0.7724 0.4712 0.2790 0.108 Uiso 0.70 1 calc PR C 1 H93B H 0.7546 0.5172 0.2211 0.108 Uiso 0.70 1 calc PR C 1 C92 C 0.7882(3) 0.5434(15) 0.2223(10) 0.104(6) Uiso 0.70 1 d PD C 1 H92A H 0.8024 0.5633 0.2534 0.125 Uiso 0.70 1 calc PR C 1 H92B H 0.7842 0.5985 0.1928 0.125 Uiso 0.70 1 calc PR C 1 C90 C 0.8145(3) 0.4746(13) 0.1633(7) 0.150(6) Uiso 0.70 1 d PD C 1 H90A H 0.8112 0.5294 0.1341 0.226 Uiso 0.70 1 calc PR C 1 H90B H 0.8181 0.4153 0.1420 0.226 Uiso 0.70 1 calc PR C 1 H90C H 0.8281 0.4914 0.1962 0.226 Uiso 0.70 1 calc PR C 1 C91 C 0.7945(3) 0.4570(13) 0.1888(8) 0.094(5) Uiso 0.70 1 d PD C 1 H91A H 0.7978 0.4002 0.2173 0.113 Uiso 0.70 1 calc PR C 1 H91B H 0.7809 0.4394 0.1554 0.113 Uiso 0.70 1 calc PR C 1 C95 C 0.7430(3) 0.6138(15) 0.3245(9) 0.182(8) Uiso 0.70 1 d PD C 1 H95A H 0.7434 0.6747 0.3483 0.273 Uiso 0.70 1 calc PR C 1 H95B H 0.7443 0.5569 0.3521 0.273 Uiso 0.70 1 calc PR C 1 H95C H 0.7281 0.6102 0.2939 0.273 Uiso 0.70 1 calc PR C 1 C94 C 0.7638(4) 0.6131(15) 0.2917(10) 0.116(6) Uiso 0.70 1 d PD C 1 H94A H 0.7620 0.6727 0.2654 0.139 Uiso 0.70 1 calc PR C 1 H94B H 0.7783 0.6232 0.3240 0.139 Uiso 0.70 1 calc PR C 1 C90A C 0.8145(3) 0.4746(13) 0.1633(7) 0.150(6) Uiso 0.30 1 d PD D 2 H90D H 0.8214 0.5124 0.1340 0.226 Uiso 0.30 1 calc PR D 2 H90E H 0.8052 0.4198 0.1419 0.226 Uiso 0.30 1 calc PR D 2 H90F H 0.8271 0.4487 0.1959 0.226 Uiso 0.30 1 calc PR D 2 C91A C 0.7979(6) 0.544(3) 0.1926(16) 0.087(10) Uiso 0.30 1 d PD D 2 H91C H 0.8078 0.5996 0.2121 0.104 Uiso 0.30 1 calc PR D 2 H91D H 0.7861 0.5723 0.1579 0.104 Uiso 0.30 1 calc PR D 2 C92A C 0.7845(6) 0.509(3) 0.2378(15) 0.074(10) Uiso 0.30 1 d PD D 2 H92C H 0.7959 0.4877 0.2755 0.089 Uiso 0.30 1 calc PR D 2 H92D H 0.7752 0.4501 0.2208 0.089 Uiso 0.30 1 calc PR D 2 C93A C 0.7682(7) 0.584(3) 0.255(2) 0.101(14) Uiso 0.30 1 d PD D 2 H93C H 0.7553 0.5991 0.2193 0.121 Uiso 0.30 1 calc PR D 2 H93D H 0.7769 0.6452 0.2691 0.121 Uiso 0.30 1 calc PR D 2 C94A C 0.7579(8) 0.534(3) 0.3099(19) 0.126(15) Uiso 0.30 1 d PD D 2 H94C H 0.7485 0.4743 0.2958 0.151 Uiso 0.30 1 calc PR D 2 H94D H 0.7706 0.5172 0.3456 0.151 Uiso 0.30 1 calc PR D 2 C95A C 0.7430(3) 0.6138(15) 0.3245(9) 0.182(8) Uiso 0.30 1 d PD D 2 H95D H 0.7355 0.5931 0.3579 0.273 Uiso 0.30 1 calc PR D 2 H95E H 0.7308 0.6296 0.2880 0.273 Uiso 0.30 1 calc PR D 2 H95F H 0.7528 0.6722 0.3372 0.273 Uiso 0.30 1 calc PR D 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 0.03317(14) 0.02555(14) 0.03928(15) -0.00169(11) 0.00736(10) 0.00328(11) N1 0.033(3) 0.034(3) 0.037(3) -0.006(2) 0.006(2) 0.008(2) N2 0.035(3) 0.038(3) 0.040(3) -0.005(3) 0.008(2) 0.008(3) N3 0.027(3) 0.023(3) 0.052(3) 0.007(2) 0.012(2) 0.003(2) N4 0.041(3) 0.030(3) 0.046(3) 0.006(2) 0.006(3) 0.002(2) P1 0.0293(8) 0.0288(9) 0.0361(9) -0.0027(7) 0.0070(7) 0.0049(7) P2 0.0326(9) 0.0440(11) 0.0405(10) -0.0077(8) 0.0053(8) 0.0050(8) P3 0.0290(8) 0.0233(8) 0.0411(9) 0.0002(7) 0.0079(7) 0.0024(7) P4 0.0391(10) 0.0275(10) 0.0676(13) 0.0130(8) 0.0048(9) 0.0015(8) C1 0.037(3) 0.026(3) 0.040(4) 0.002(3) 0.008(3) 0.006(3) C2 0.071(5) 0.037(4) 0.036(4) -0.002(3) 0.018(4) 0.009(4) C3 0.073(5) 0.023(4) 0.060(5) 0.002(3) 0.018(4) 0.001(4) C4 0.073(5) 0.035(4) 0.049(4) 0.013(3) 0.014(4) 0.005(4) C5 0.063(5) 0.040(4) 0.044(4) 0.010(3) 0.025(4) 0.014(4) C6 0.051(4) 0.030(4) 0.043(4) 0.002(3) 0.004(3) 0.010(3) C7 0.056(4) 0.027(4) 0.036(4) -0.001(3) 0.015(3) -0.001(3) C8 0.060(4) 0.026(4) 0.032(3) 0.003(3) 0.013(3) -0.008(3) C9 0.055(4) 0.038(4) 0.034(4) 0.002(3) 0.001(3) -0.004(3) C10 0.072(5) 0.041(5) 0.052(5) 0.003(4) 0.008(4) 0.006(4) C11 0.053(5) 0.062(6) 0.064(5) -0.001(4) -0.007(4) -0.009(4) C12 0.077(6) 0.038(4) 0.051(4) -0.009(4) 0.029(4) -0.003(4) C13 0.102(7) 0.039(4) 0.055(5) -0.009(4) 0.039(5) 0.001(5) C14 0.113(8) 0.037(4) 0.042(4) -0.003(4) 0.019(5) -0.017(5) C15 0.082(6) 0.038(4) 0.036(4) 0.000(3) 0.008(4) -0.022(4) C16 0.056(5) 0.072(6) 0.076(6) -0.025(5) 0.021(4) 0.022(5) C17 0.071(7) 0.139(11) 0.116(9) -0.062(8) 0.038(6) -0.016(7) C18 0.092(8) 0.079(8) 0.125(9) -0.006(7) 0.014(7) 0.039(6) C19 0.034(4) 0.051(4) 0.043(4) -0.008(3) 0.008(3) 0.012(3) C20 0.031(4) 0.054(5) 0.052(4) -0.011(4) 0.014(3) 0.008(3) C21 0.049(5) 0.061(6) 0.074(6) 0.002(4) 0.025(4) 0.005(4) C22 0.040(4) 0.081(7) 0.099(7) -0.015(6) 0.018(5) 0.022(5) C23 0.052(5) 0.069(6) 0.091(7) 0.009(5) 0.020(5) 0.016(5) C24 0.037(4) 0.057(5) 0.063(5) -0.003(4) 0.007(4) 0.014(4) C25 0.057(5) 0.054(5) 0.071(5) 0.007(4) 0.016(4) 0.027(4) C26 0.074(6) 0.090(7) 0.079(7) 0.027(5) 0.011(5) 0.046(6) C27 0.092(7) 0.060(6) 0.121(9) -0.001(6) 0.036(7) 0.019(6) C28 0.032(4) 0.063(5) 0.053(4) -0.004(4) 0.014(3) 0.004(4) C29 0.049(5) 0.073(6) 0.065(5) 0.003(4) 0.020(4) -0.002(4) C30 0.041(4) 0.071(6) 0.064(5) 0.004(4) 0.017(4) 0.002(4) C31 0.036(4) 0.060(5) 0.057(5) -0.018(4) 0.009(3) -0.004(4) C32 0.050(5) 0.079(6) 0.069(6) -0.010(5) 0.016(4) -0.005(5) C33 0.054(5) 0.125(10) 0.073(6) -0.018(6) 0.010(5) -0.029(6) C34 0.118(10) 0.077(8) 0.081(7) -0.028(6) 0.031(7) -0.045(7) C35 0.066(6) 0.079(7) 0.092(7) -0.023(6) 0.025(6) -0.010(6) C36 0.053(5) 0.053(5) 0.096(7) -0.015(5) 0.034(5) -0.011(4) C37 0.043(4) 0.066(5) 0.049(4) -0.003(4) 0.001(3) 0.009(4) C38 0.082(7) 0.096(7) 0.052(5) -0.004(5) 0.016(5) 0.016(6) C39 0.125(10) 0.133(11) 0.053(6) 0.011(6) 0.028(6) 0.040(9) C40 0.166(15) 0.154(14) 0.083(9) 0.012(9) -0.004(9) 0.030(12) C41 0.036(3) 0.031(4) 0.042(4) -0.007(3) 0.014(3) -0.002(3) C42 0.044(4) 0.030(4) 0.046(4) -0.003(3) 0.012(3) 0.004(3) C43 0.053(4) 0.048(5) 0.038(4) -0.002(3) 0.007(3) 0.012(4) C44 0.058(5) 0.053(5) 0.044(4) -0.022(4) 0.007(4) 0.002(4) C46 0.053(4) 0.032(4) 0.047(4) -0.004(3) 0.019(3) 0.000(3) C47 0.061(5) 0.031(4) 0.048(4) -0.015(3) 0.011(4) -0.007(4) C48 0.054(4) 0.022(3) 0.038(4) 0.000(3) 0.012(3) -0.004(3) C49 0.062(5) 0.024(3) 0.042(4) -0.002(3) 0.019(3) -0.004(3) C50 0.078(6) 0.039(4) 0.048(4) -0.003(4) 0.025(4) -0.011(4) C51 0.091(7) 0.033(4) 0.049(4) 0.008(3) 0.020(4) -0.013(4) C52 0.076(6) 0.032(4) 0.057(5) 0.012(4) -0.001(4) -0.001(4) C53 0.057(4) 0.026(4) 0.047(4) 0.008(3) 0.007(3) 0.002(3) C54 0.048(4) 0.038(4) 0.077(6) 0.006(4) 0.004(4) 0.005(4) C55 0.080(7) 0.059(6) 0.098(8) 0.012(5) -0.019(6) 0.009(5) C56 0.079(7) 0.057(6) 0.122(9) 0.008(6) 0.042(6) 0.010(5) C57 0.049(4) 0.030(4) 0.064(5) 0.004(3) 0.026(4) -0.002(3) C58 0.057(5) 0.061(6) 0.090(7) 0.005(5) 0.021(5) -0.014(4) C59 0.072(6) 0.047(5) 0.082(6) -0.003(4) 0.036(5) 0.006(4) C60 0.033(3) 0.026(4) 0.058(4) 0.009(3) 0.015(3) 0.006(3) C61 0.042(4) 0.027(4) 0.059(5) 0.004(3) 0.004(3) 0.008(3) C62 0.047(4) 0.042(5) 0.072(5) 0.000(4) -0.002(4) 0.005(4) C63 0.040(4) 0.047(5) 0.093(7) 0.003(5) 0.009(4) 0.013(4) C64 0.046(4) 0.041(4) 0.079(6) 0.000(4) 0.024(4) 0.005(4) C65 0.042(4) 0.032(4) 0.065(5) 0.007(4) 0.015(3) -0.002(3) C66 0.051(4) 0.048(5) 0.058(5) -0.008(4) 0.020(4) 0.003(4) C67 0.063(6) 0.097(8) 0.077(6) -0.015(5) 0.029(5) -0.001(5) C68 0.063(5) 0.045(5) 0.107(7) -0.014(5) 0.018(5) 0.009(4) C69 0.038(4) 0.042(4) 0.061(5) -0.002(4) -0.005(3) 0.004(3) C70 0.059(5) 0.062(6) 0.062(5) -0.001(4) -0.001(4) 0.009(4) C71 0.058(5) 0.053(5) 0.079(6) -0.004(5) -0.006(5) 0.002(4) C72 0.035(4) 0.031(4) 0.075(5) 0.008(4) 0.011(4) 0.000(3) C73 0.049(5) 0.046(5) 0.088(6) 0.009(4) 0.018(4) 0.007(4) C74 0.039(4) 0.062(6) 0.100(7) 0.017(5) 0.011(4) -0.011(4) C75 0.059(5) 0.035(5) 0.098(7) 0.007(4) 0.006(5) -0.013(4) C76 0.057(5) 0.040(5) 0.090(7) 0.007(4) 0.006(5) -0.001(4) C77 0.043(4) 0.036(4) 0.070(5) 0.007(4) 0.006(4) -0.002(4) C78 0.085(6) 0.058(6) 0.060(5) 0.023(4) 0.011(5) -0.017(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 Hg1 P3 2.4922(16) . ? Hg1 P1 2.5001(16) . ? Hg1 P2 3.008(2) . ? Hg1 P4 3.083(2) . ? N1 C19 1.452(8) . ? N1 P2 1.728(5) . ? N1 P1 1.738(5) . ? N2 C7 1.387(8) . ? N2 P1 1.556(5) . ? N3 C60 1.448(8) . ? N3 P3 1.729(5) . ? N3 P4 1.729(5) . ? N4 C48 1.395(8) . ? N4 P3 1.557(6) . ? P1 C1 1.837(7) . ? P2 C31 1.825(8) . ? P2 C37 1.841(8) . ? P3 C41 1.844(7) . ? P4 C78 1.816(9) . ? P4 C72 1.823(7) . ? C1 C2 1.392(10) . ? C1 C6 1.410(9) . ? C2 C3 1.389(10) . ? C2 H2 0.9300 . ? C3 C4 1.382(10) . ? C3 H3 0.9300 . ? C4 C5 1.377(10) . ? C4 H4 0.9300 . ? C5 C6 1.362(10) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.430(10) . ? C7 C8 1.438(10) . ? C8 C15 1.384(9) . ? C8 C9 1.511(10) . ? C9 C11 1.511(10) . ? C9 C10 1.536(10) . ? C9 H9 0.9800 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.396(11) . ? C12 C16 1.491(12) . ? C13 C14 1.388(13) . ? C13 H13 0.9300 . ? C14 C15 1.385(12) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.518(13) . ? C16 C18 1.544(14) . ? C16 H16 0.9800 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C24 1.385(10) . ? C19 C20 1.393(10) . ? C20 C21 1.381(10) . ? C20 C28 1.513(10) . ? C21 C22 1.392(12) . ? C21 H21 0.9300 . ? C22 C23 1.356(13) . ? C22 H22 0.9300 . ? C23 C24 1.381(11) . ? C23 H23 0.9300 . ? C24 C25 1.519(12) . ? C25 C27 1.522(13) . ? C25 C26 1.551(12) . ? C25 H25 0.9800 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.511(11) . ? C28 C30 1.515(11) . ? C28 H28 0.9800 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C36 1.361(11) . ? C31 C32 1.411(11) . ? C32 C33 1.372(13) . ? C32 H32 0.9300 . ? C33 C34 1.422(16) . ? C33 H33 0.9300 . ? C34 C35 1.309(15) . ? C34 H34 0.9300 . ? C35 C36 1.352(13) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.490(11) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.536(13) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.452(16) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C46 1.401(9) . ? C41 C42 1.403(9) . ? C42 C43 1.371(10) . ? C42 H42 0.9300 . ? C43 C44 1.403(10) . ? C43 H43 0.9300 . ? C44 C47 1.380(11) . ? C44 H44 0.9300 . ? C46 C47 1.375(10) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 C53 1.418(9) . ? C48 C49 1.419(10) . ? C49 C50 1.395(10) . ? C49 C57 1.537(10) . ? C50 C51 1.384(11) . ? C50 H50 0.9300 . ? C51 C52 1.370(12) . ? C51 H51 0.9300 . ? C52 C53 1.380(10) . ? C52 H52 0.9300 . ? C53 C54 1.515(10) . ? C54 C55 1.519(12) . ? C54 C56 1.520(12) . ? C54 H54 0.9800 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C58 1.523(10) . ? C57 C59 1.525(10) . ? C57 H57 0.9800 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 C61 1.397(10) . ? C60 C65 1.418(10) . ? C61 C62 1.386(10) . ? C61 C69 1.523(10) . ? C62 C63 1.364(11) . ? C62 H62 0.9300 . ? C63 C64 1.364(12) . ? C63 H63 0.9300 . ? C64 C65 1.398(10) . ? C64 H64 0.9300 . ? C65 C66 1.518(11) . ? C66 C67 1.527(11) . ? C66 C68 1.531(11) . ? C66 H66 0.9800 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 C70 1.522(11) . ? C69 C71 1.525(11) . ? C69 H69 0.9800 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 C77 1.388(10) . ? C72 C73 1.390(10) . ? C73 C74 1.400(12) . ? C73 H73 0.9300 . ? C74 C75 1.374(13) . ? C74 H74 0.9300 . ? C75 C76 1.391(12) . ? C75 H75 0.9300 . ? C76 C77 1.378(11) . ? C76 H76 0.9300 . ? C77 H77 0.9300 . ? C78 C79 1.556(14) . ? C78 C79A 1.60(3) . ? C78 H78A 0.9700 . ? C78 H78B 0.9700 . ? C79 C80 1.546(19) . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 C81 1.56(2) . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C79A C80A 1.59(3) . ? C79A H79C 0.9700 . ? C79A H79D 0.9700 . ? C80A C81A 1.66(3) . ? C80A H80C 0.9700 . ? C80A H80D 0.9700 . ? C81A H81D 0.9600 . ? C81A H81E 0.9600 . ? C81A H81F 0.9600 . ? C93 C92 1.398(19) . ? C93 C94 1.46(2) . ? C93 H93A 0.9700 . ? C93 H93B 0.9700 . ? C92 C91 1.45(2) . ? C92 H92A 0.9700 . ? C92 H92B 0.9700 . ? C90 C91 1.384(17) . ? C90 H90A 0.9600 . ? C90 H90B 0.9600 . ? C90 H90C 0.9600 . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C95 C94 1.50(2) . ? C95 H95A 0.9600 . ? C95 H95B 0.9600 . ? C95 H95C 0.9600 . ? C94 H94A 0.9700 . ? C94 H94B 0.9700 . ? C91A C92A 1.44(3) . ? C91A H91C 0.9700 . ? C91A H91D 0.9700 . ? C92A C93A 1.46(3) . ? C92A H92C 0.9700 . ? C92A H92D 0.9700 . ? C93A C94A 1.59(3) . ? C93A H93C 0.9700 . ? C93A H93D 0.9700 . ? C94A H94C 0.9700 . ? C94A H94D 0.9700 . ? 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 P3 Hg1 P1 176.51(5) . . ? P3 Hg1 P2 119.58(5) . . ? P1 Hg1 P2 62.85(5) . . ? P3 Hg1 P4 61.73(5) . . ? P1 Hg1 P4 120.38(5) . . ? P2 Hg1 P4 110.27(5) . . ? C19 N1 P2 125.3(4) . . ? C19 N1 P1 120.6(4) . . ? P2 N1 P1 113.9(3) . . ? C7 N2 P1 142.1(5) . . ? C60 N3 P3 122.3(4) . . ? C60 N3 P4 123.5(4) . . ? P3 N3 P4 114.3(3) . . ? C48 N4 P3 144.3(5) . . ? N2 P1 N1 105.4(3) . . ? N2 P1 C1 111.5(3) . . ? N1 P1 C1 108.7(3) . . ? N2 P1 Hg1 129.0(2) . . ? N1 P1 Hg1 96.88(18) . . ? C1 P1 Hg1 103.4(2) . . ? N1 P2 C31 107.8(3) . . ? N1 P2 C37 107.1(3) . . ? C31 P2 C37 98.6(4) . . ? N1 P2 Hg1 80.46(18) . . ? C31 P2 Hg1 119.2(3) . . ? C37 P2 Hg1 137.6(3) . . ? N4 P3 N3 106.3(3) . . ? N4 P3 C41 112.1(3) . . ? N3 P3 C41 108.2(3) . . ? N4 P3 Hg1 128.4(2) . . ? N3 P3 Hg1 97.47(18) . . ? C41 P3 Hg1 102.5(2) . . ? N3 P4 C78 103.5(3) . . ? N3 P4 C72 109.2(3) . . ? C78 P4 C72 100.2(4) . . ? N3 P4 Hg1 78.24(17) . . ? C78 P4 Hg1 143.5(3) . . ? C72 P4 Hg1 113.8(3) . . ? C2 C1 C6 117.4(6) . . ? C2 C1 P1 120.6(5) . . ? C6 C1 P1 121.7(5) . . ? C3 C2 C1 121.1(6) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C4 C3 C2 119.4(7) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C5 C4 C3 120.6(7) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 119.9(7) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 121.6(7) . . ? C5 C6 H6 119.2 . . ? C1 C6 H6 119.2 . . ? N2 C7 C12 117.8(6) . . ? N2 C7 C8 123.3(6) . . ? C12 C7 C8 118.9(6) . . ? C15 C8 C7 119.9(7) . . ? C15 C8 C9 119.7(7) . . ? C7 C8 C9 120.4(6) . . ? C11 C9 C8 114.7(6) . . ? C11 C9 C10 110.9(6) . . ? C8 C9 C10 109.7(6) . . ? C11 C9 H9 107.1 . . ? C8 C9 H9 107.1 . . ? C10 C9 H9 107.1 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C7 118.1(8) . . ? C13 C12 C16 120.3(7) . . ? C7 C12 C16 121.5(7) . . ? C14 C13 C12 122.6(8) . . ? C14 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? C15 C14 C13 119.4(8) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C8 C15 C14 121.2(8) . . ? C8 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C12 C16 C17 111.0(8) . . ? C12 C16 C18 109.0(8) . . ? C17 C16 C18 112.2(8) . . ? C12 C16 H16 108.2 . . ? C17 C16 H16 108.2 . . ? C18 C16 H16 108.2 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 123.2(6) . . ? C24 C19 N1 120.0(6) . . ? C20 C19 N1 116.8(6) . . ? C21 C20 C19 116.7(7) . . ? C21 C20 C28 117.8(7) . . ? C19 C20 C28 125.5(6) . . ? C20 C21 C22 120.3(8) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C23 C22 C21 121.7(8) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C24 119.8(9) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C23 C24 C19 118.2(8) . . ? C23 C24 C25 116.6(7) . . ? C19 C24 C25 125.2(6) . . ? C24 C25 C27 112.0(8) . . ? C24 C25 C26 113.1(8) . . ? C27 C25 C26 110.4(8) . . ? C24 C25 H25 107.0 . . ? C27 C25 H25 107.0 . . ? C26 C25 H25 107.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C20 112.3(6) . . ? C29 C28 C30 109.0(6) . . ? C20 C28 C30 113.7(6) . . ? C29 C28 H28 107.2 . . ? C20 C28 H28 107.2 . . ? C30 C28 H28 107.2 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 117.7(8) . . ? C36 C31 P2 117.9(6) . . ? C32 C31 P2 122.5(7) . . ? C33 C32 C31 119.0(10) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C32 C33 C34 119.3(10) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C35 C34 C33 120.5(10) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 120.2(11) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 123.0(9) . . ? C35 C36 H36 118.5 . . ? C31 C36 H36 118.5 . . ? C38 C37 P2 113.9(6) . . ? C38 C37 H37A 108.8 . . ? P2 C37 H37A 108.8 . . ? C38 C37 H37B 108.8 . . ? P2 C37 H37B 108.8 . . ? H37A C37 H37B 107.7 . . ? C37 C38 C39 113.3(9) . . ? C37 C38 H38A 108.9 . . ? C39 C38 H38A 108.9 . . ? C37 C38 H38B 108.9 . . ? C39 C38 H38B 108.9 . . ? H38A C38 H38B 107.7 . . ? C40 C39 C38 114.4(10) . . ? C40 C39 H39A 108.7 . . ? C38 C39 H39A 108.7 . . ? C40 C39 H39B 108.7 . . ? C38 C39 H39B 108.7 . . ? H39A C39 H39B 107.6 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C46 C41 C42 118.5(6) . . ? C46 C41 P3 119.3(5) . . ? C42 C41 P3 122.0(5) . . ? C43 C42 C41 120.9(7) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C42 C43 C44 119.7(7) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C47 C44 C43 119.9(7) . . ? C47 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C47 C46 C41 120.5(7) . . ? C47 C46 H46 119.7 . . ? C41 C46 H46 119.7 . . ? C46 C47 C44 120.5(7) . . ? C46 C47 H47 119.8 . . ? C44 C47 H47 119.8 . . ? N4 C48 C53 117.5(6) . . ? N4 C48 C49 124.2(6) . . ? C53 C48 C49 118.3(6) . . ? C50 C49 C48 119.5(7) . . ? C50 C49 C57 118.1(7) . . ? C48 C49 C57 122.3(6) . . ? C51 C50 C49 121.5(8) . . ? C51 C50 H50 119.2 . . ? C49 C50 H50 119.3 . . ? C52 C51 C50 118.7(7) . . ? C52 C51 H51 120.6 . . ? C50 C51 H51 120.6 . . ? C51 C52 C53 122.5(8) . . ? C51 C52 H52 118.8 . . ? C53 C52 H52 118.8 . . ? C52 C53 C48 119.6(7) . . ? C52 C53 C54 118.9(7) . . ? C48 C53 C54 121.5(6) . . ? C53 C54 C55 114.0(8) . . ? C53 C54 C56 111.1(7) . . ? C55 C54 C56 106.6(7) . . ? C53 C54 H54 108.3 . . ? C55 C54 H54 108.3 . . ? C56 C54 H54 108.3 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 C59 111.1(6) . . ? C58 C57 C49 114.6(6) . . ? C59 C57 C49 110.4(7) . . ? C58 C57 H57 106.8 . . ? C59 C57 H57 106.8 . . ? C49 C57 H57 106.8 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C61 C60 C65 121.0(6) . . ? C61 C60 N3 119.2(6) . . ? C65 C60 N3 119.8(6) . . ? C62 C61 C60 117.9(7) . . ? C62 C61 C69 118.2(7) . . ? C60 C61 C69 123.9(6) . . ? C63 C62 C61 121.5(8) . . ? C63 C62 H62 119.2 . . ? C61 C62 H62 119.2 . . ? C62 C63 C64 121.2(7) . . ? C62 C63 H63 119.4 . . ? C64 C63 H63 119.4 . . ? C63 C64 C65 120.3(7) . . ? C63 C64 H64 119.8 . . ? C65 C64 H64 119.8 . . ? C64 C65 C60 118.0(7) . . ? C64 C65 C66 118.6(7) . . ? C60 C65 C66 123.4(6) . . ? C65 C66 C67 114.0(7) . . ? C65 C66 C68 110.5(7) . . ? C67 C66 C68 109.2(7) . . ? C65 C66 H66 107.6 . . ? C67 C66 H66 107.6 . . ? C68 C66 H66 107.6 . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C66 C68 H68A 109.5 . . ? C66 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C66 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C70 C69 C61 110.3(6) . . ? C70 C69 C71 109.9(7) . . ? C61 C69 C71 111.9(6) . . ? C70 C69 H69 108.2 . . ? C61 C69 H69 108.2 . . ? C71 C69 H69 108.2 . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C71 H71A 109.5 . . ? C69 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C69 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C77 C72 C73 118.1(7) . . ? C77 C72 P4 116.5(5) . . ? C73 C72 P4 124.5(6) . . ? C72 C73 C74 120.2(8) . . ? C72 C73 H73 119.9 . . ? C74 C73 H73 119.9 . . ? C75 C74 C73 120.5(8) . . ? C75 C74 H74 119.8 . . ? C73 C74 H74 119.8 . . ? C74 C75 C76 119.7(8) . . ? C74 C75 H75 120.1 . . ? C76 C75 H75 120.1 . . ? C77 C76 C75 119.4(8) . . ? C77 C76 H76 120.3 . . ? C75 C76 H76 120.3 . . ? C76 C77 C72 122.0(7) . . ? C76 C77 H77 119.0 . . ? C72 C77 H77 119.0 . . ? C79 C78 P4 120.5(8) . . ? C79A C78 P4 92.6(15) . . ? C79 C78 H78A 107.2 . . ? C79A C78 H78A 127.9 . . ? P4 C78 H78A 107.2 . . ? C79 C78 H78B 107.2 . . ? C79A C78 H78B 112.4 . . ? P4 C78 H78B 107.2 . . ? H78A C78 H78B 106.8 . . ? C80 C79 C78 106.5(11) . . ? C80 C79 H79A 110.4 . . ? C78 C79 H79A 110.4 . . ? C80 C79 H79B 110.4 . . ? C78 C79 H79B 110.4 . . ? H79A C79 H79B 108.6 . . ? C79 C80 C81 102.2(14) . . ? C79 C80 H80A 111.3 . . ? C81 C80 H80A 111.3 . . ? C79 C80 H80B 111.3 . . ? C81 C80 H80B 111.3 . . ? H80A C80 H80B 109.2 . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C80A C79A C78 103(2) . . ? C80A C79A H79C 111.2 . . ? C78 C79A H79C 111.1 . . ? C80A C79A H79D 111.1 . . ? C78 C79A H79D 111.1 . . ? H79C C79A H79D 109.1 . . ? C79A C80A C81A 90(2) . . ? C79A C80A H80C 113.7 . . ? C81A C80A H80C 113.7 . . ? C79A C80A H80D 113.7 . . ? C81A C80A H80D 113.7 . . ? H80C C80A H80D 111.0 . . ? C80A C81A H81D 109.5 . . ? C80A C81A H81E 109.5 . . ? H81D C81A H81E 109.5 . . ? C80A C81A H81F 109.5 . . ? H81D C81A H81F 109.5 . . ? H81E C81A H81F 109.5 . . ? C92 C93 C94 117.6(16) . . ? C92 C93 H93A 107.9 . . ? C94 C93 H93A 107.9 . . ? C92 C93 H93B 107.9 . . ? C94 C93 H93B 107.9 . . ? H93A C93 H93B 107.2 . . ? C93 C92 C91 116.4(18) . . ? C93 C92 H92A 108.2 . . ? C91 C92 H92A 108.2 . . ? C93 C92 H92B 108.2 . . ? C91 C92 H92B 108.2 . . ? H92A C92 H92B 107.3 . . ? C90 C91 C92 112.3(15) . . ? C90 C91 H91A 109.1 . . ? C92 C91 H91A 109.1 . . ? C90 C91 H91B 109.1 . . ? C92 C91 H91B 109.1 . . ? H91A C91 H91B 107.9 . . ? C94 C95 H95A 109.5 . . ? C94 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C94 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? C93 C94 C95 124.2(17) . . ? C93 C94 H94A 106.3 . . ? C95 C94 H94A 106.3 . . ? C93 C94 H94B 106.3 . . ? C95 C94 H94B 106.3 . . ? H94A C94 H94B 106.4 . . ? C92A C91A H91C 106.7 . . ? C92A C91A H91D 106.7 . . ? H91C C91A H91D 106.6 . . ? C91A C92A C93A 114(3) . . ? C91A C92A H92C 108.8 . . ? C93A C92A H92C 108.8 . . ? C91A C92A H92D 108.8 . . ? C93A C92A H92D 108.8 . . ? H92C C92A H92D 107.7 . . ? C92A C93A C94A 105(3) . . ? C92A C93A H93C 110.7 . . ? C94A C93A H93C 110.7 . . ? C92A C93A H93D 110.7 . . ? C94A C93A H93D 110.7 . . ? H93C C93A H93D 108.8 . . ? C93A C94A H94C 111.6 . . ? C93A C94A H94D 111.6 . . ? H94C C94A H94D 109.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.053 _refine_diff_density_min -0.839 _refine_diff_density_rms 0.136 #===END data_complex6 _database_code_depnum_ccdc_archive 'CCDC 606738' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H63 Li N2 O P2 S' _chemical_formula_sum 'C44 H63 Li N2 O P2 S' _chemical_formula_weight 736.90 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' Li Li -0.0003 0.0001 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.078(2) _cell_length_b 19.367(4) _cell_length_c 19.128(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.09(3) _cell_angle_gamma 90.00 _cell_volume 4390.7(15) _cell_formula_units_Z 4 _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 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.115 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 0.180 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.9718 _exptl_absorpt_correction_T_max 0.9893 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski and Minor 1997)' _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 'phi/omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14614 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7732 _reflns_number_gt 4960 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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^)+(0.0470P)^2^+1.6973P] 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 7732 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0964 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 P1 P 0.18185(5) 0.27315(3) 0.64698(4) 0.02982(17) Uani 1 1 d . . . P2 P 0.33467(5) 0.33327(3) 0.69948(4) 0.02800(17) Uani 1 1 d . . . N1 N 0.20429(16) 0.20032(10) 0.68654(11) 0.0331(5) Uani 1 1 d . . . N2 N 0.36697(15) 0.30069(10) 0.77741(10) 0.0287(5) Uani 1 1 d . . . Li1 Li 0.2977(4) 0.2092(2) 0.7822(2) 0.0405(11) Uani 1 1 d . . . O1 O 0.28175(16) 0.14822(10) 0.85690(10) 0.0521(5) Uani 1 1 d . . . S1 S 0.15607(6) 0.28128(4) 0.54354(4) 0.0466(2) Uani 1 1 d . . . C1 C 0.1765(2) 0.13533(12) 0.65160(13) 0.0354(6) Uani 1 1 d . . . C2 C 0.0641(2) 0.11756(14) 0.62020(15) 0.0443(7) Uani 1 1 d . . . C3 C 0.0426(3) 0.05221(15) 0.59048(16) 0.0554(8) Uani 1 1 d . . . H3 H -0.0326 0.0403 0.5690 0.067 Uiso 1 1 calc R . . C4 C 0.1263(3) 0.00449(16) 0.59113(17) 0.0618(9) Uani 1 1 d . . . H4 H 0.1093 -0.0398 0.5705 0.074 Uiso 1 1 calc R . . C5 C 0.2350(3) 0.02132(14) 0.62188(16) 0.0537(8) Uani 1 1 d . . . H5 H 0.2930 -0.0119 0.6224 0.064 Uiso 1 1 calc R . . C6 C 0.2627(2) 0.08600(13) 0.65245(14) 0.0394(7) Uani 1 1 d . . . C7 C -0.0350(2) 0.16611(17) 0.61995(18) 0.0605(9) Uani 1 1 d . . . H7 H -0.0031 0.2132 0.6322 0.073 Uiso 1 1 calc R . . C8 C -0.0994(4) 0.1454(2) 0.6779(3) 0.1179(18) Uani 1 1 d . . . H8A H -0.1221 0.0969 0.6717 0.177 Uiso 1 1 calc R . . H8B H -0.1667 0.1744 0.6746 0.177 Uiso 1 1 calc R . . H8C H -0.0508 0.1516 0.7248 0.177 Uiso 1 1 calc R . . C10 C 0.3854(2) 0.09925(14) 0.68474(14) 0.0441(7) Uani 1 1 d . . . H10 H 0.3921 0.1472 0.7045 0.053 Uiso 1 1 calc R . . C11 C 0.4271(3) 0.04858(17) 0.74595(17) 0.0676(10) Uani 1 1 d . . . H11A H 0.3792 0.0523 0.7817 0.101 Uiso 1 1 calc R . . H11B H 0.5052 0.0598 0.7679 0.101 Uiso 1 1 calc R . . H11C H 0.4236 0.0014 0.7273 0.101 Uiso 1 1 calc R . . C12 C 0.4619(3) 0.09329(16) 0.63017(17) 0.0585(9) Uani 1 1 d . . . H12A H 0.4639 0.0452 0.6146 0.088 Uiso 1 1 calc R . . H12B H 0.5383 0.1083 0.6518 0.088 Uiso 1 1 calc R . . H12C H 0.4326 0.1226 0.5890 0.088 Uiso 1 1 calc R . . C13 C 0.44411(19) 0.33311(12) 0.83513(13) 0.0298(6) Uani 1 1 d . . . C14 C 0.5595(2) 0.31539(13) 0.84835(14) 0.0361(6) Uani 1 1 d . . . C15 C 0.6303(2) 0.34509(15) 0.90705(16) 0.0460(7) Uani 1 1 d . . . H15 H 0.7082 0.3335 0.9164 0.055 Uiso 1 1 calc R . . C16 C 0.5911(3) 0.39020(15) 0.95127(16) 0.0499(8) Uani 1 1 d . . . H16 H 0.6414 0.4100 0.9905 0.060 Uiso 1 1 calc R . . C17 C 0.4783(2) 0.40691(14) 0.93875(14) 0.0433(7) Uani 1 1 d . . . H17 H 0.4513 0.4384 0.9697 0.052 Uiso 1 1 calc R . . C18 C 0.4030(2) 0.37867(12) 0.88177(13) 0.0327(6) Uani 1 1 d . . . C19 C 0.2780(2) 0.39362(13) 0.87483(15) 0.0389(6) Uani 1 1 d . . . H19 H 0.2397 0.3779 0.8264 0.047 Uiso 1 1 calc R . . C20 C 0.2303(3) 0.35053(19) 0.92950(17) 0.0668(10) Uani 1 1 d . . . H20A H 0.2439 0.3014 0.9221 0.100 Uiso 1 1 calc R . . H20B H 0.1489 0.3587 0.9236 0.100 Uiso 1 1 calc R . . H20C H 0.2674 0.3639 0.9777 0.100 Uiso 1 1 calc R . . C21 C 0.2514(3) 0.47002(16) 0.8809(2) 0.0756(11) Uani 1 1 d . . . H21A H 0.2770 0.4853 0.9302 0.113 Uiso 1 1 calc R . . H21B H 0.1698 0.4772 0.8670 0.113 Uiso 1 1 calc R . . H21C H 0.2902 0.4967 0.8493 0.113 Uiso 1 1 calc R . . C22 C 0.6062(2) 0.26212(16) 0.80445(16) 0.0514(8) Uani 1 1 d . . . H22 H 0.5550 0.2602 0.7567 0.062 Uiso 1 1 calc R . . C23 C 0.6048(3) 0.19110(18) 0.8388(2) 0.0872(12) Uani 1 1 d . . . H23A H 0.6516 0.1921 0.8867 0.131 Uiso 1 1 calc R . . H23B H 0.6347 0.1567 0.8098 0.131 Uiso 1 1 calc R . . H23C H 0.5272 0.1790 0.8421 0.131 Uiso 1 1 calc R . . C24 C 0.7254(3) 0.2794(3) 0.7923(2) 0.0985(15) Uani 1 1 d . . . H24A H 0.7263 0.3265 0.7737 0.148 Uiso 1 1 calc R . . H24B H 0.7466 0.2468 0.7580 0.148 Uiso 1 1 calc R . . H24C H 0.7793 0.2759 0.8376 0.148 Uiso 1 1 calc R . . C25 C 0.1887(3) 0.10045(18) 0.8442(2) 0.0767(11) Uani 1 1 d . . . H25A H 0.2152 0.0550 0.8646 0.092 Uiso 1 1 calc R . . H25B H 0.1638 0.0944 0.7922 0.092 Uiso 1 1 calc R . . C26 C 0.0928(4) 0.1220(3) 0.8743(3) 0.1174(18) Uani 1 1 d . . . H26A H 0.1141 0.1227 0.9263 0.176 Uiso 1 1 calc R . . H26B H 0.0304 0.0895 0.8598 0.176 Uiso 1 1 calc R . . H26C H 0.0691 0.1683 0.8569 0.176 Uiso 1 1 calc R . . C27 C 0.3483(3) 0.14894(18) 0.92777(16) 0.0627(9) Uani 1 1 d . . . H27A H 0.2978 0.1571 0.9620 0.075 Uiso 1 1 calc R . . H27B H 0.4021 0.1880 0.9319 0.075 Uiso 1 1 calc R . . C28 C 0.4136(3) 0.08311(19) 0.94813(19) 0.0808(11) Uani 1 1 d . . . H28A H 0.3608 0.0445 0.9468 0.121 Uiso 1 1 calc R . . H28B H 0.4585 0.0877 0.9963 0.121 Uiso 1 1 calc R . . H28C H 0.4637 0.0744 0.9145 0.121 Uiso 1 1 calc R . . C29 C 0.44519(19) 0.32801(13) 0.64654(13) 0.0323(6) Uani 1 1 d . . . C30 C 0.4535(2) 0.27247(14) 0.60211(14) 0.0400(7) Uani 1 1 d . . . H30 H 0.3961 0.2382 0.5949 0.048 Uiso 1 1 calc R . . C31 C 0.5445(3) 0.26634(16) 0.56817(17) 0.0563(8) Uani 1 1 d . . . H31 H 0.5487 0.2285 0.5372 0.068 Uiso 1 1 calc R . . C32 C 0.6292(3) 0.31539(18) 0.57958(18) 0.0615(9) Uani 1 1 d . . . H32 H 0.6924 0.3109 0.5570 0.074 Uiso 1 1 calc R . . C33 C 0.6221(2) 0.37073(17) 0.62352(19) 0.0601(9) Uani 1 1 d . . . H33 H 0.6803 0.4044 0.6311 0.072 Uiso 1 1 calc R . . C34 C 0.5307(2) 0.37766(15) 0.65685(16) 0.0453(7) Uani 1 1 d . . . H34 H 0.5260 0.4163 0.6868 0.054 Uiso 1 1 calc R . . C35 C 0.2975(2) 0.42471(12) 0.69645(14) 0.0343(6) Uani 1 1 d . . . H35A H 0.2295 0.4305 0.7177 0.041 Uiso 1 1 calc R . . H35B H 0.3597 0.4504 0.7267 0.041 Uiso 1 1 calc R . . C36 C 0.2744(2) 0.45754(13) 0.62216(15) 0.0429(7) Uani 1 1 d . . . H36A H 0.3471 0.4657 0.6068 0.051 Uiso 1 1 calc R . . H36B H 0.2299 0.4250 0.5880 0.051 Uiso 1 1 calc R . . C37 C 0.2109(3) 0.52521(14) 0.62025(18) 0.0557(8) Uani 1 1 d . . . H37A H 0.2562 0.5580 0.6538 0.067 Uiso 1 1 calc R . . H37B H 0.1390 0.5171 0.6365 0.067 Uiso 1 1 calc R . . C38 C 0.1860(3) 0.55730(18) 0.5466(2) 0.0861(12) Uani 1 1 d . . . H38A H 0.2570 0.5663 0.5306 0.129 Uiso 1 1 calc R . . H38B H 0.1452 0.6008 0.5483 0.129 Uiso 1 1 calc R . . H38C H 0.1396 0.5255 0.5133 0.129 Uiso 1 1 calc R . . C39 C 0.07707(19) 0.32428(13) 0.68214(15) 0.0364(7) Uani 1 1 d . . . C40 C 0.0606(2) 0.31491(16) 0.75109(17) 0.0494(8) Uani 1 1 d . . . H40 H 0.0999 0.2793 0.7799 0.059 Uiso 1 1 calc R . . C41 C -0.0143(2) 0.3581(2) 0.7785(2) 0.0690(11) Uani 1 1 d . . . H41 H -0.0255 0.3521 0.8259 0.083 Uiso 1 1 calc R . . C42 C -0.0718(3) 0.4094(2) 0.7358(3) 0.0738(12) Uani 1 1 d . . . H42 H -0.1212 0.4394 0.7545 0.089 Uiso 1 1 calc R . . C43 C -0.0583(3) 0.41717(17) 0.6678(3) 0.0691(10) Uani 1 1 d . . . H43 H -0.0999 0.4516 0.6386 0.083 Uiso 1 1 calc R . . C44 C 0.0155(2) 0.37548(14) 0.64044(19) 0.0515(8) Uani 1 1 d . . . H44 H 0.0245 0.3817 0.5926 0.062 Uiso 1 1 calc R . . C9 C -0.1121(3) 0.1713(2) 0.5479(2) 0.1139(18) Uani 1 1 d . . . H9A H -0.0679 0.1837 0.5119 0.171 Uiso 1 1 calc R . . H9B H -0.1694 0.2068 0.5495 0.171 Uiso 1 1 calc R . . H9C H -0.1492 0.1267 0.5356 0.171 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 P1 0.0273(3) 0.0279(4) 0.0326(4) -0.0035(3) 0.0018(3) -0.0004(3) P2 0.0263(3) 0.0261(3) 0.0312(4) -0.0028(3) 0.0047(3) -0.0010(3) N1 0.0366(11) 0.0247(11) 0.0361(13) -0.0046(10) 0.0024(10) -0.0026(9) N2 0.0273(10) 0.0280(11) 0.0296(12) -0.0041(9) 0.0025(9) -0.0020(9) Li1 0.048(2) 0.033(2) 0.037(3) 0.000(2) -0.001(2) -0.003(2) O1 0.0660(13) 0.0465(12) 0.0431(13) 0.0054(10) 0.0088(10) -0.0126(10) S1 0.0504(4) 0.0530(5) 0.0331(4) -0.0018(4) 0.0001(3) -0.0018(4) C1 0.0486(15) 0.0289(14) 0.0276(15) -0.0025(12) 0.0048(12) -0.0065(13) C2 0.0519(16) 0.0366(16) 0.0436(18) -0.0108(14) 0.0071(14) -0.0138(14) C3 0.074(2) 0.0443(18) 0.046(2) -0.0133(15) 0.0066(16) -0.0244(17) C4 0.101(3) 0.0311(17) 0.051(2) -0.0138(15) 0.0087(19) -0.0126(18) C5 0.084(2) 0.0312(16) 0.0441(19) -0.0080(14) 0.0088(17) 0.0060(16) C6 0.0610(17) 0.0281(14) 0.0277(15) -0.0026(12) 0.0052(13) 0.0019(13) C7 0.0424(16) 0.057(2) 0.079(3) -0.0283(18) 0.0054(17) -0.0171(15) C8 0.121(4) 0.102(3) 0.153(5) -0.049(3) 0.082(3) -0.020(3) C10 0.0601(18) 0.0320(15) 0.0380(17) -0.0033(13) 0.0039(14) 0.0136(14) C11 0.090(2) 0.057(2) 0.050(2) 0.0093(17) 0.0016(18) 0.0241(18) C12 0.069(2) 0.0460(18) 0.064(2) -0.0049(16) 0.0226(17) 0.0141(16) C13 0.0324(13) 0.0281(13) 0.0276(14) 0.0039(11) 0.0025(11) -0.0050(11) C14 0.0316(13) 0.0400(15) 0.0345(16) 0.0056(13) 0.0005(12) -0.0045(12) C15 0.0348(14) 0.0523(18) 0.0449(18) 0.0119(16) -0.0069(14) -0.0096(14) C16 0.0595(19) 0.0446(18) 0.0373(18) 0.0032(15) -0.0111(15) -0.0194(15) C17 0.0632(19) 0.0335(15) 0.0320(16) -0.0037(13) 0.0059(14) -0.0117(14) C18 0.0426(14) 0.0291(14) 0.0267(15) 0.0018(12) 0.0074(12) -0.0065(12) C19 0.0440(15) 0.0359(15) 0.0392(17) -0.0065(13) 0.0143(13) -0.0018(13) C20 0.0554(19) 0.100(3) 0.047(2) 0.0066(19) 0.0151(16) -0.0181(19) C21 0.068(2) 0.050(2) 0.111(3) -0.028(2) 0.024(2) 0.0074(17) C22 0.0334(14) 0.069(2) 0.0494(19) -0.0007(16) 0.0023(13) 0.0154(14) C23 0.105(3) 0.063(2) 0.090(3) -0.001(2) 0.011(2) 0.039(2) C24 0.0405(18) 0.163(4) 0.096(3) -0.015(3) 0.0220(19) 0.013(2) C25 0.088(3) 0.058(2) 0.087(3) 0.004(2) 0.024(2) -0.028(2) C26 0.100(3) 0.127(4) 0.138(4) -0.051(3) 0.053(3) -0.054(3) C27 0.084(2) 0.067(2) 0.038(2) -0.0022(17) 0.0130(17) 0.0028(19) C28 0.116(3) 0.072(3) 0.049(2) 0.0093(19) 0.003(2) 0.016(2) C29 0.0310(12) 0.0318(14) 0.0347(16) 0.0020(12) 0.0080(11) 0.0032(11) C30 0.0425(15) 0.0359(15) 0.0442(17) -0.0002(14) 0.0150(13) 0.0024(13) C31 0.064(2) 0.0518(19) 0.061(2) -0.0039(16) 0.0318(17) 0.0092(17) C32 0.0531(18) 0.065(2) 0.077(3) 0.0064(19) 0.0383(18) 0.0085(17) C33 0.0430(17) 0.062(2) 0.082(3) -0.0004(19) 0.0268(17) -0.0109(16) C34 0.0361(14) 0.0474(17) 0.0543(19) -0.0090(15) 0.0136(14) -0.0066(13) C35 0.0343(13) 0.0261(13) 0.0429(17) -0.0044(12) 0.0083(12) -0.0009(11) C36 0.0469(15) 0.0337(15) 0.0472(19) 0.0045(14) 0.0068(14) -0.0029(13) C37 0.0588(18) 0.0350(16) 0.071(2) 0.0091(16) 0.0057(16) 0.0015(14) C38 0.106(3) 0.058(2) 0.086(3) 0.030(2) -0.003(2) 0.012(2) C39 0.0241(12) 0.0310(14) 0.0532(19) -0.0131(13) 0.0049(12) -0.0042(11) C40 0.0282(13) 0.065(2) 0.056(2) -0.0128(17) 0.0098(14) -0.0044(14) C41 0.0377(16) 0.106(3) 0.066(2) -0.036(2) 0.0171(16) -0.0087(19) C42 0.0343(17) 0.075(3) 0.113(4) -0.037(3) 0.017(2) 0.0073(17) C43 0.0428(18) 0.049(2) 0.116(4) -0.007(2) 0.018(2) 0.0102(15) C44 0.0317(14) 0.0407(17) 0.081(2) 0.0018(16) 0.0090(15) 0.0066(13) C9 0.059(2) 0.132(4) 0.130(4) -0.053(3) -0.033(2) 0.027(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 P1 N1 1.599(2) . ? P1 C39 1.833(3) . ? P1 S1 1.9492(11) . ? P1 P2 2.2490(10) . ? P2 N2 1.596(2) . ? P2 C35 1.825(2) . ? P2 C29 1.827(2) . ? N1 C1 1.434(3) . ? N1 Li1 1.964(5) . ? N2 C13 1.444(3) . ? N2 Li1 1.969(5) . ? Li1 O1 1.892(5) . ? O1 C27 1.437(4) . ? O1 C25 1.440(4) . ? C1 C6 1.411(4) . ? C1 C2 1.417(4) . ? C2 C3 1.391(4) . ? C2 C7 1.521(4) . ? C3 C4 1.368(4) . ? C3 H3 0.9500 . ? C4 C5 1.370(4) . ? C4 H4 0.9500 . ? C5 C6 1.396(4) . ? C5 H5 0.9500 . ? C6 C10 1.514(4) . ? C7 C9 1.511(5) . ? C7 C8 1.526(5) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 C12 1.526(4) . ? C10 C11 1.537(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.410(3) . ? C13 C18 1.411(3) . ? C14 C15 1.398(4) . ? C14 C22 1.506(4) . ? C15 C16 1.363(4) . ? C15 H15 0.9500 . ? C16 C17 1.376(4) . ? C16 H16 0.9500 . ? C17 C18 1.390(4) . ? C17 H17 0.9500 . ? C18 C19 1.518(3) . ? C19 C21 1.523(4) . ? C19 C20 1.534(4) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.526(5) . ? C22 C24 1.539(4) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.450(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.510(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.386(3) . ? C29 C34 1.397(3) . ? C30 C31 1.385(4) . ? C30 H30 0.9500 . ? C31 C32 1.382(4) . ? C31 H31 0.9500 . ? C32 C33 1.375(4) . ? C32 H32 0.9500 . ? C33 C34 1.383(4) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.533(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.515(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.516(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.383(4) . ? C39 C44 1.394(4) . ? C40 C41 1.405(4) . ? C40 H40 0.9500 . ? C41 C42 1.385(5) . ? C41 H41 0.9500 . ? C42 C43 1.349(5) . ? C42 H42 0.9500 . ? C43 C44 1.378(4) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 P1 C39 111.65(12) . . ? N1 P1 S1 122.08(8) . . ? C39 P1 S1 110.00(10) . . ? N1 P1 P2 101.27(8) . . ? C39 P1 P2 96.99(8) . . ? S1 P1 P2 111.63(5) . . ? N2 P2 C35 115.32(11) . . ? N2 P2 C29 114.97(11) . . ? C35 P2 C29 103.76(11) . . ? N2 P2 P1 104.15(8) . . ? C35 P2 P1 108.21(9) . . ? C29 P2 P1 110.36(9) . . ? C1 N1 P1 123.39(17) . . ? C1 N1 Li1 123.5(2) . . ? P1 N1 Li1 112.23(17) . . ? C13 N2 P2 123.22(16) . . ? C13 N2 Li1 125.0(2) . . ? P2 N2 Li1 111.69(16) . . ? O1 Li1 N1 121.7(2) . . ? O1 Li1 N2 134.7(3) . . ? N1 Li1 N2 102.0(2) . . ? C27 O1 C25 116.2(2) . . ? C27 O1 Li1 125.9(2) . . ? C25 O1 Li1 117.6(2) . . ? C6 C1 C2 119.0(2) . . ? C6 C1 N1 118.9(2) . . ? C2 C1 N1 122.0(2) . . ? C3 C2 C1 118.8(3) . . ? C3 C2 C7 118.5(3) . . ? C1 C2 C7 122.7(2) . . ? C4 C3 C2 122.1(3) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C3 C4 C5 119.2(3) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C4 C5 C6 121.7(3) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 119.1(3) . . ? C5 C6 C10 117.4(2) . . ? C1 C6 C10 123.5(2) . . ? C9 C7 C2 113.0(3) . . ? C9 C7 C8 111.6(3) . . ? C2 C7 C8 110.2(3) . . ? C9 C7 H7 107.2 . . ? C2 C7 H7 107.2 . . ? C8 C7 H7 107.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C10 C12 112.5(2) . . ? C6 C10 C11 110.8(2) . . ? C12 C10 C11 108.7(2) . . ? C6 C10 H10 108.3 . . ? C12 C10 H10 108.3 . . ? C11 C10 H10 108.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 119.6(2) . . ? C14 C13 N2 120.1(2) . . ? C18 C13 N2 120.1(2) . . ? C15 C14 C13 118.3(3) . . ? C15 C14 C22 119.5(2) . . ? C13 C14 C22 122.0(2) . . ? C16 C15 C14 122.1(3) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C15 C16 C17 119.5(3) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C18 121.4(3) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C17 C18 C13 119.0(2) . . ? C17 C18 C19 118.9(2) . . ? C13 C18 C19 121.9(2) . . ? C18 C19 C21 113.6(2) . . ? C18 C19 C20 109.5(2) . . ? C21 C19 C20 111.4(3) . . ? C18 C19 H19 107.4 . . ? C21 C19 H19 107.4 . . ? C20 C19 H19 107.4 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C14 C22 C23 109.9(3) . . ? C14 C22 C24 113.4(3) . . ? C23 C22 C24 110.4(3) . . ? C14 C22 H22 107.6 . . ? C23 C22 H22 107.6 . . ? C24 C22 H22 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O1 C25 C26 113.9(3) . . ? O1 C25 H25A 108.8 . . ? C26 C25 H25A 108.8 . . ? O1 C25 H25B 108.8 . . ? C26 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O1 C27 C28 113.9(3) . . ? O1 C27 H27A 108.8 . . ? C28 C27 H27A 108.8 . . ? O1 C27 H27B 108.8 . . ? C28 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C34 118.8(2) . . ? C30 C29 P2 121.98(19) . . ? C34 C29 P2 118.8(2) . . ? C31 C30 C29 120.7(3) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C32 C31 C30 119.8(3) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C33 C32 C31 120.1(3) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120.4(3) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C33 C34 C29 120.1(3) . . ? C33 C34 H34 119.9 . . ? C29 C34 H34 119.9 . . ? C36 C35 P2 115.58(18) . . ? C36 C35 H35A 108.4 . . ? P2 C35 H35A 108.4 . . ? C36 C35 H35B 108.4 . . ? P2 C35 H35B 108.4 . . ? H35A C35 H35B 107.4 . . ? C37 C36 C35 112.5(2) . . ? C37 C36 H36A 109.1 . . ? C35 C36 H36A 109.1 . . ? C37 C36 H36B 109.1 . . ? C35 C36 H36B 109.1 . . ? H36A C36 H36B 107.8 . . ? C36 C37 C38 112.7(3) . . ? C36 C37 H37A 109.0 . . ? C38 C37 H37A 109.0 . . ? C36 C37 H37B 109.0 . . ? C38 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C44 118.7(3) . . ? C40 C39 P1 121.0(2) . . ? C44 C39 P1 120.3(2) . . ? C39 C40 C41 119.9(3) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C42 C41 C40 119.5(3) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C43 C42 C41 120.5(3) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C42 C43 C44 120.5(3) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C43 C44 C39 120.8(3) . . ? C43 C44 H44 119.6 . . ? C39 C44 H44 119.6 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.300 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.044 #===END data_complex9 _database_code_depnum_ccdc_archive 'CCDC 606739' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C80 H106 Hg N4 P4 S2' _chemical_formula_sum 'C80 H106 Hg N4 P4 S2' _chemical_formula_weight 1512.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 C2/c _symmetry_space_group_name_Hall -C2yc 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 48.827(10) _cell_length_b 17.090(3) _cell_length_c 24.266(5) _cell_angle_alpha 90.00 _cell_angle_beta 115.03(3) _cell_angle_gamma 90.00 _cell_volume 18347(8) _cell_formula_units_Z 8 _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 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6288 _exptl_absorpt_coefficient_mu 1.830 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8103 _exptl_absorpt_correction_T_max 0.8674 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski and Minor 1997)' _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 'phi/omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30879 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -57 _diffrn_reflns_limit_h_max 58 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 25.03 _reflns_number_total 16161 _reflns_number_gt 11981 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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 ; The complex contains a significant amount of disorder in the main residue The heavier atoms (Hg, S, P and N1 and N2) were refined with anisotropically. The phenyl ring located on P1, C1-C6, is disordered over two sites and the thermal parameters were refined best using a 60:40 isotropic mixture. The orientation of the phenyl ring and n-butyl group on P2 is disordered and the thermal parameters were refined best using a 50:50 isotropic mixture. The second position of the n-butyl C31-C34 group is further disordered over two positions and is modelled as a 20:20 isotropic mixture. The iso-propyl group C16-C18 is also disordered over two sites and was modelled using a 50:50 isotropic mixture. A second position for the ligand S2-P3-N3-P4, including all carbon atoms, was found with 60:40 disorder of the phenyl and n-butyl groups on P4. All carbon atoms on this ligand and N3 and N4 were refined isotropically. This structure also contains disordered molecules of solvent in the lattice, for which no reasonable model could be found. The data was treated with the program Squeeze (PLATON). 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^)+(0.0935P)^2^+27.5784P] 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 16161 _refine_ls_number_parameters 668 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1695 _refine_ls_wR_factor_gt 0.1607 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.117 _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 0.350916(5) 0.583157(14) 0.808753(10) 0.05411(11) Uani 1 1 d . . . N1 N 0.24214(11) 0.5666(3) 0.6830(2) 0.0579(12) Uani 1 1 d . . . N2 N 0.29218(10) 0.5348(3) 0.67823(18) 0.0456(10) Uani 1 1 d . . . P1 P 0.27464(3) 0.55031(8) 0.72623(6) 0.0445(3) Uani 1 1 d . A . P2 P 0.32921(3) 0.51800(9) 0.70827(6) 0.0500(3) Uani 1 1 d D C . S1 S 0.29821(3) 0.63069(8) 0.79011(6) 0.0481(3) Uani 1 1 d . A . C1 C 0.27652(17) 0.4559(3) 0.7595(3) 0.042(3) Uiso 0.60 1 d PG A 1 C2 C 0.25761(16) 0.3968(4) 0.7245(3) 0.054(2) Uiso 0.60 1 d PG A 1 H2 H 0.2422 0.4084 0.6854 0.064 Uiso 0.60 1 calc PR A 1 C3 C 0.26132(18) 0.3206(3) 0.7466(4) 0.071(3) Uiso 0.60 1 d PG A 1 H3 H 0.2484 0.2802 0.7227 0.085 Uiso 0.60 1 calc PR A 1 C4 C 0.2839(2) 0.3036(3) 0.8038(4) 0.074(4) Uiso 0.60 1 d PG A 1 H4 H 0.2865 0.2516 0.8189 0.089 Uiso 0.60 1 calc PR A 1 C5 C 0.30285(17) 0.3628(5) 0.8388(3) 0.082(4) Uiso 0.60 1 d PG A 1 H5 H 0.3183 0.3511 0.8778 0.098 Uiso 0.60 1 calc PR A 1 C6 C 0.29914(16) 0.4389(4) 0.8167(3) 0.054(3) Uiso 0.60 1 d PG A 1 H6 H 0.3121 0.4793 0.8406 0.064 Uiso 0.60 1 calc PR A 1 C1A C 0.2854(4) 0.4572(9) 0.7744(9) 0.050(4) Uiso 0.40 1 d P A 2 C2A C 0.2720(4) 0.3903(11) 0.7444(9) 0.073(5) Uiso 0.40 1 d P A 2 H2A H 0.2589 0.3938 0.7023 0.087 Uiso 0.40 1 calc PR A 2 C3A C 0.2768(4) 0.3115(10) 0.7745(9) 0.059(4) Uiso 0.40 1 d P A 2 H3A H 0.2675 0.2641 0.7552 0.071 Uiso 0.40 1 calc PR A 2 C4A C 0.2964(5) 0.3186(13) 0.8328(10) 0.082(5) Uiso 0.40 1 d P A 2 H4A H 0.3047 0.2707 0.8526 0.099 Uiso 0.40 1 calc PR A 2 C5A C 0.3061(4) 0.3823(11) 0.8676(9) 0.073(5) Uiso 0.40 1 d P A 2 H5A H 0.3159 0.3789 0.9107 0.088 Uiso 0.40 1 calc PR A 2 C6A C 0.3010(3) 0.4544(10) 0.8374(8) 0.051(3) Uiso 0.40 1 d P A 2 H6A H 0.3081 0.5013 0.8600 0.062 Uiso 0.40 1 calc PR A 2 C7 C 0.21519(12) 0.5888(3) 0.6831(3) 0.0482(13) Uani 1 1 d . B . C8 C 0.19186(13) 0.6062(4) 0.6259(3) 0.0586(15) Uani 1 1 d . . . C9 C 0.16430(14) 0.6260(4) 0.6221(3) 0.0699(17) Uani 1 1 d . B . H9 H 0.1484 0.6366 0.5833 0.084 Uiso 1 1 calc R . . C10 C 0.15874(16) 0.6312(5) 0.6729(4) 0.081(2) Uani 1 1 d . . . H10 H 0.1394 0.6468 0.6694 0.098 Uiso 1 1 calc R B . C11 C 0.18141(16) 0.6135(5) 0.7287(3) 0.0761(19) Uani 1 1 d . B . H11 H 0.1774 0.6163 0.7637 0.091 Uiso 1 1 calc R . . C12 C 0.20915(14) 0.5922(3) 0.7352(3) 0.0549(14) Uani 1 1 d . . . C13 C 0.23183(15) 0.5719(4) 0.7992(3) 0.0627(16) Uani 1 1 d . B . H13 H 0.2519 0.5664 0.7975 0.075 Uiso 1 1 calc R . . C14 C 0.23568(19) 0.6358(5) 0.8460(3) 0.089(2) Uani 1 1 d . . . H14A H 0.2382 0.6865 0.8300 0.134 Uiso 1 1 calc R B . H14B H 0.2535 0.6244 0.8837 0.134 Uiso 1 1 calc R . . H14C H 0.2177 0.6373 0.8544 0.134 Uiso 1 1 calc R . . C15 C 0.22492(18) 0.4914(5) 0.8203(3) 0.082(2) Uani 1 1 d . . . H15A H 0.2053 0.4938 0.8224 0.123 Uiso 1 1 calc R B . H15B H 0.2408 0.4788 0.8606 0.123 Uiso 1 1 calc R . . H15C H 0.2243 0.4509 0.7912 0.123 Uiso 1 1 calc R . . C16 C 0.1972(3) 0.6140(9) 0.5679(6) 0.049(3) Uiso 0.50 1 d P B 1 H16 H 0.2179 0.5944 0.5769 0.059 Uiso 0.50 1 calc PR B 1 C17 C 0.1942(4) 0.6994(10) 0.5433(8) 0.078(4) Uiso 0.50 1 d P B 1 H17A H 0.1978 0.6999 0.5066 0.117 Uiso 0.50 1 calc PR B 1 H17B H 0.2091 0.7328 0.5744 0.117 Uiso 0.50 1 calc PR B 1 H17C H 0.1739 0.7191 0.5336 0.117 Uiso 0.50 1 calc PR B 1 C18 C 0.1736(4) 0.5627(12) 0.5157(9) 0.097(5) Uiso 0.50 1 d P B 1 H18A H 0.1770 0.5682 0.4789 0.145 Uiso 0.50 1 calc PR B 1 H18B H 0.1531 0.5802 0.5072 0.145 Uiso 0.50 1 calc PR B 1 H18C H 0.1760 0.5077 0.5283 0.145 Uiso 0.50 1 calc PR B 1 C16A C 0.1950(4) 0.5864(9) 0.5675(7) 0.060(4) Uiso 0.50 1 d P B 2 H16A H 0.2164 0.5708 0.5789 0.072 Uiso 0.50 1 calc PR B 2 C17A C 0.1887(4) 0.6602(11) 0.5292(8) 0.086(5) Uiso 0.50 1 d P B 2 H17D H 0.1908 0.6489 0.4915 0.129 Uiso 0.50 1 calc PR B 2 H17E H 0.2031 0.7010 0.5520 0.129 Uiso 0.50 1 calc PR B 2 H17F H 0.1681 0.6783 0.5192 0.129 Uiso 0.50 1 calc PR B 2 C18A C 0.1753(4) 0.5216(10) 0.5319(7) 0.080(4) Uiso 0.50 1 d P B 2 H18D H 0.1785 0.5128 0.4951 0.119 Uiso 0.50 1 calc PR B 2 H18E H 0.1541 0.5353 0.5205 0.119 Uiso 0.50 1 calc PR B 2 H18F H 0.1803 0.4739 0.5566 0.119 Uiso 0.50 1 calc PR B 2 C19 C 0.27742(13) 0.5566(4) 0.6139(3) 0.0536(14) Uani 1 1 d . D . C20 C 0.27896(14) 0.6337(4) 0.5967(3) 0.0607(15) Uani 1 1 d . . . C21 C 0.26675(18) 0.6510(5) 0.5339(3) 0.084(2) Uani 1 1 d . D . H21 H 0.2678 0.7031 0.5213 0.100 Uiso 1 1 calc R . . C22 C 0.2535(2) 0.5948(6) 0.4911(4) 0.092(3) Uani 1 1 d . . . H22 H 0.2455 0.6073 0.4491 0.110 Uiso 1 1 calc R D . C23 C 0.25195(17) 0.5205(6) 0.5093(3) 0.084(2) Uani 1 1 d . D . H23 H 0.2422 0.4821 0.4790 0.101 Uiso 1 1 calc R . . C24 C 0.26401(14) 0.4972(4) 0.5708(3) 0.0611(15) Uani 1 1 d . . . C25 C 0.2624(2) 0.4136(5) 0.5871(4) 0.082(2) Uani 1 1 d . D . H25 H 0.2747 0.4070 0.6318 0.099 Uiso 1 1 calc R . . C26 C 0.2745(2) 0.3582(5) 0.5534(4) 0.101(3) Uani 1 1 d . . . H26A H 0.2738 0.3043 0.5666 0.151 Uiso 1 1 calc R D . H26B H 0.2954 0.3722 0.5624 0.151 Uiso 1 1 calc R . . H26C H 0.2620 0.3624 0.5095 0.151 Uiso 1 1 calc R . . C27 C 0.2306(2) 0.3897(7) 0.5721(5) 0.127(4) Uani 1 1 d . . . H27A H 0.2224 0.4225 0.5948 0.191 Uiso 1 1 calc R D . H27B H 0.2302 0.3347 0.5832 0.191 Uiso 1 1 calc R . . H27C H 0.2182 0.3962 0.5284 0.191 Uiso 1 1 calc R . . C28 C 0.29284(17) 0.6994(4) 0.6410(3) 0.0692(18) Uani 1 1 d . D . H28 H 0.3061 0.6750 0.6810 0.083 Uiso 1 1 calc R . . C29 C 0.2694(2) 0.7470(5) 0.6508(4) 0.096(3) Uani 1 1 d . . . H29A H 0.2565 0.7738 0.6129 0.144 Uiso 1 1 calc R D . H29B H 0.2794 0.7859 0.6828 0.144 Uiso 1 1 calc R . . H29C H 0.2570 0.7125 0.6631 0.144 Uiso 1 1 calc R . . C30 C 0.3129(2) 0.7532(5) 0.6234(4) 0.105(3) Uani 1 1 d . . . H30A H 0.3259 0.7215 0.6106 0.158 Uiso 1 1 calc R D . H30B H 0.3255 0.7853 0.6585 0.158 Uiso 1 1 calc R . . H30C H 0.3002 0.7873 0.5898 0.158 Uiso 1 1 calc R . . C31 C 0.34589(17) 0.5600(5) 0.6618(3) 0.049(3) Uiso 0.60 1 d PG C 1 C32 C 0.33660(16) 0.5409(5) 0.6009(3) 0.061(2) Uiso 0.60 1 d PGD C 1 H32 H 0.3193 0.5088 0.5809 0.073 Uiso 0.60 1 calc PR C 1 C33 C 0.3526(2) 0.5685(6) 0.5693(3) 0.124(8) Uiso 0.60 1 d PG C 1 H33 H 0.3463 0.5554 0.5277 0.149 Uiso 0.60 1 calc PR C 1 C34 C 0.3780(2) 0.6154(7) 0.5987(4) 0.112(5) Uiso 0.60 1 d PG C 1 H34 H 0.3889 0.6343 0.5771 0.135 Uiso 0.60 1 calc PR C 1 C35 C 0.38724(18) 0.6346(6) 0.6596(4) 0.102(4) Uiso 0.60 1 d PG C 1 H35 H 0.4045 0.6666 0.6796 0.122 Uiso 0.60 1 calc PR C 1 C36 C 0.37121(19) 0.6069(6) 0.6912(3) 0.089(4) Uiso 0.60 1 d PG C 1 H36 H 0.3776 0.6200 0.7328 0.106 Uiso 0.60 1 calc PR C 1 C37 C 0.3313(3) 0.4066(7) 0.7062(6) 0.066(3) Uiso 0.60 1 d P C 1 H37A H 0.3175 0.3833 0.7222 0.080 Uiso 0.60 1 calc PR C 1 H37B H 0.3248 0.3887 0.6638 0.080 Uiso 0.60 1 calc PR C 1 C38 C 0.3623(3) 0.3814(7) 0.7433(6) 0.073(3) Uiso 0.60 1 d P C 1 H38A H 0.3679 0.3953 0.7863 0.088 Uiso 0.60 1 calc PR C 1 H38B H 0.3762 0.4096 0.7300 0.088 Uiso 0.60 1 calc PR C 1 C39 C 0.3663(4) 0.2916(10) 0.7385(7) 0.097(4) Uiso 0.60 1 d P C 1 H39A H 0.3520 0.2636 0.7508 0.117 Uiso 0.60 1 calc PR C 1 H39B H 0.3611 0.2780 0.6955 0.117 Uiso 0.60 1 calc PR C 1 C40 C 0.3960(4) 0.2660(12) 0.7751(9) 0.135(6) Uiso 0.60 1 d P C 1 H40A H 0.3974 0.2095 0.7700 0.202 Uiso 0.60 1 calc PR C 1 H40B H 0.4010 0.2776 0.8178 0.202 Uiso 0.60 1 calc PR C 1 H40C H 0.4102 0.2932 0.7628 0.202 Uiso 0.60 1 calc PR C 1 C31A C 0.3427(5) 0.5445(17) 0.6503(10) 0.089(8) Uiso 0.20 1 d PD C 2 H31A H 0.3384 0.5012 0.6208 0.107 Uiso 0.20 1 calc PR C 2 H31B H 0.3318 0.5915 0.6280 0.107 Uiso 0.20 1 calc PR C 2 C32A C 0.3736(4) 0.5594(11) 0.6772(8) 0.072(4) Uiso 0.20 1 d PD C 2 H32A H 0.3847 0.5118 0.6980 0.087 Uiso 0.20 1 calc PR C 2 H32B H 0.3782 0.6015 0.7079 0.087 Uiso 0.20 1 calc PR C 2 C33A C 0.3835(5) 0.5848(14) 0.6270(11) 0.110(8) Uiso 0.20 1 d PD C 2 H33A H 0.3958 0.5436 0.6195 0.132 Uiso 0.20 1 calc PR C 2 H33B H 0.3953 0.6339 0.6382 0.132 Uiso 0.20 1 calc PR C 2 C34A C 0.3529(6) 0.597(2) 0.5701(11) 0.054(7) Uiso 0.20 1 d PD C 2 H34A H 0.3569 0.6121 0.5353 0.081 Uiso 0.20 1 calc PR C 2 H34B H 0.3412 0.6380 0.5785 0.081 Uiso 0.20 1 calc PR C 2 H34C H 0.3414 0.5479 0.5607 0.081 Uiso 0.20 1 calc PR C 2 C37A C 0.3403(3) 0.4205(7) 0.7142(6) 0.063(5) Uiso 0.40 1 d PG C 2 C38A C 0.3446(3) 0.3795(8) 0.7667(5) 0.091(6) Uiso 0.40 1 d PG C 2 H38C H 0.3418 0.4051 0.7987 0.110 Uiso 0.40 1 calc PR C 2 C39A C 0.3530(4) 0.3012(8) 0.7724(6) 0.122(8) Uiso 0.40 1 d PG C 2 H39C H 0.3560 0.2733 0.8084 0.147 Uiso 0.40 1 calc PR C 2 C40B C 0.3571(4) 0.2638(7) 0.7256(8) 0.098(7) Uiso 0.40 1 d PG C 2 H40D H 0.3629 0.2103 0.7295 0.118 Uiso 0.40 1 calc PR C 2 C41B C 0.3528(4) 0.3048(9) 0.6730(6) 0.116(8) Uiso 0.40 1 d PG C 2 H41B H 0.3556 0.2792 0.6410 0.139 Uiso 0.40 1 calc PR C 2 C42B C 0.3443(4) 0.3831(9) 0.6673(5) 0.106(7) Uiso 0.40 1 d PG C 2 H42B H 0.3414 0.4110 0.6314 0.127 Uiso 0.40 1 calc PR C 2 C31B C 0.3427(5) 0.5445(17) 0.6503(10) 0.089(8) Uiso 0.20 1 d P C 3 H31C H 0.3384 0.5012 0.6208 0.107 Uiso 0.20 1 calc PR C 3 H31D H 0.3318 0.5915 0.6280 0.107 Uiso 0.20 1 calc PR C 3 C32B C 0.3736(4) 0.5594(11) 0.6772(8) 0.072(4) Uiso 0.20 1 d P C 3 H32C H 0.3847 0.5118 0.6980 0.087 Uiso 0.20 1 calc PR C 3 H32D H 0.3782 0.6015 0.7079 0.087 Uiso 0.20 1 calc PR C 3 C33B C 0.3835(5) 0.5848(14) 0.6270(11) 0.110(8) Uiso 0.20 1 d P C 3 H33C H 0.4056 0.5774 0.6428 0.132 Uiso 0.20 1 calc PR C 3 H33D H 0.3739 0.5489 0.5919 0.132 Uiso 0.20 1 calc PR C 3 C34B C 0.3764(6) 0.6652(17) 0.6046(12) 0.051(6) Uiso 0.20 1 d P C 3 H34D H 0.3852 0.6759 0.5758 0.076 Uiso 0.20 1 calc PR C 3 H34E H 0.3849 0.7017 0.6389 0.076 Uiso 0.20 1 calc PR C 3 H34F H 0.3544 0.6719 0.5841 0.076 Uiso 0.20 1 calc PR C 3 S2 S 0.3699(3) 0.4925(12) 0.9044(6) 0.059(2) Uani 0.60 1 d P D 1 P3 P 0.4072(2) 0.5430(5) 0.9522(5) 0.0513(15) Uani 0.60 1 d P D 1 C41 C 0.43133(13) 0.5162(4) 0.9140(3) 0.0473(17) Uiso 0.60 1 d PG D 1 C42 C 0.42047(13) 0.4754(5) 0.8593(3) 0.076(3) Uiso 0.60 1 d PG D 1 H42 H 0.3997 0.4613 0.8397 0.091 Uiso 0.60 1 calc PR D 1 C43 C 0.43997(18) 0.4551(5) 0.8333(3) 0.085(4) Uiso 0.60 1 d PG D 1 H43 H 0.4326 0.4272 0.7960 0.102 Uiso 0.60 1 calc PR D 1 C44 C 0.47033(16) 0.4757(6) 0.8620(3) 0.082(3) Uiso 0.60 1 d PG D 1 H44 H 0.4837 0.4619 0.8442 0.099 Uiso 0.60 1 calc PR D 1 C45 C 0.48118(12) 0.5166(5) 0.9167(3) 0.076(3) Uiso 0.60 1 d PG D 1 H45 H 0.5019 0.5306 0.9362 0.091 Uiso 0.60 1 calc PR D 1 C46 C 0.46168(14) 0.5368(4) 0.9427(3) 0.056(2) Uiso 0.60 1 d PG D 1 H46 H 0.4691 0.5647 0.9800 0.067 Uiso 0.60 1 calc PR D 1 N3 N 0.4219(2) 0.5266(6) 1.0202(4) 0.056(2) Uiso 0.60 1 d P D 1 C47 C 0.4350(2) 0.4705(8) 1.0641(4) 0.049(2) Uiso 0.60 1 d P D 1 C48 C 0.4372(3) 0.3912(8) 1.0512(6) 0.064(3) Uiso 0.60 1 d P D 1 C49 C 0.4515(3) 0.3369(8) 1.1001(6) 0.074(3) Uiso 0.60 1 d P D 1 H49 H 0.4540 0.2839 1.0913 0.088 Uiso 0.60 1 calc PR D 1 C50 C 0.4617(3) 0.3609(9) 1.1595(7) 0.085(4) Uiso 0.60 1 d P D 1 H50 H 0.4704 0.3242 1.1917 0.101 Uiso 0.60 1 calc PR D 1 C51 C 0.4590(3) 0.4423(9) 1.1729(5) 0.065(3) Uiso 0.60 1 d P D 1 H51 H 0.4675 0.4610 1.2136 0.078 Uiso 0.60 1 calc PR D 1 C52 C 0.4439(3) 0.4915(8) 1.1252(5) 0.066(3) Uiso 0.60 1 d P D 1 C53 C 0.4390(3) 0.5729(8) 1.1413(6) 0.068(3) Uiso 0.60 1 d P D 1 H53 H 0.4353 0.6069 1.1054 0.081 Uiso 0.60 1 calc PR D 1 C54 C 0.4098(3) 0.5752(8) 1.1532(7) 0.086(4) Uiso 0.60 1 d P D 1 H54A H 0.4062 0.6289 1.1629 0.129 Uiso 0.60 1 calc PR D 1 H54B H 0.4124 0.5408 1.1873 0.129 Uiso 0.60 1 calc PR D 1 H54C H 0.3924 0.5575 1.1166 0.129 Uiso 0.60 1 calc PR D 1 C55 C 0.4634(3) 0.6104(10) 1.1960(7) 0.097(4) Uiso 0.60 1 d P D 1 H55A H 0.4573 0.6636 1.2007 0.146 Uiso 0.60 1 calc PR D 1 H55B H 0.4822 0.6123 1.1904 0.146 Uiso 0.60 1 calc PR D 1 H55C H 0.4667 0.5797 1.2323 0.146 Uiso 0.60 1 calc PR D 1 C56 C 0.4259(3) 0.3546(9) 0.9874(6) 0.066(3) Uiso 0.60 1 d P D 1 H56 H 0.4171 0.3985 0.9578 0.079 Uiso 0.60 1 calc PR D 1 C57 C 0.4007(3) 0.2989(10) 0.9761(7) 0.089(4) Uiso 0.60 1 d P D 1 H57A H 0.3852 0.3244 0.9853 0.133 Uiso 0.60 1 calc PR D 1 H57B H 0.4084 0.2529 1.0022 0.133 Uiso 0.60 1 calc PR D 1 H57C H 0.3919 0.2828 0.9333 0.133 Uiso 0.60 1 calc PR D 1 C58 C 0.4500(3) 0.3193(8) 0.9733(6) 0.077(3) Uiso 0.60 1 d P D 1 H58A H 0.4662 0.3577 0.9814 0.116 Uiso 0.60 1 calc PR D 1 H58B H 0.4415 0.3040 0.9304 0.116 Uiso 0.60 1 calc PR D 1 H58C H 0.4582 0.2731 0.9989 0.116 Uiso 0.60 1 calc PR D 1 N4 N 0.40330(19) 0.6440(6) 0.9430(4) 0.046(2) Uiso 0.60 1 d P D 1 C59 C 0.40567(15) 0.6932(4) 0.9932(3) 0.057(2) Uiso 0.60 1 d PG D 1 C60 C 0.38037(13) 0.7040(5) 1.0048(3) 0.062(3) Uiso 0.60 1 d PG D 1 C61 C 0.38219(15) 0.7510(5) 1.0529(4) 0.082(3) Uiso 0.60 1 d PG D 1 H61 H 0.3649 0.7584 1.0608 0.098 Uiso 0.60 1 calc PR D 1 C62 C 0.40931(18) 0.7873(5) 1.0895(3) 0.094(4) Uiso 0.60 1 d PG D 1 H62 H 0.4106 0.8195 1.1224 0.113 Uiso 0.60 1 calc PR D 1 C63 C 0.43462(14) 0.7766(5) 1.0780(3) 0.078(3) Uiso 0.60 1 d PG D 1 H63 H 0.4532 0.8014 1.1030 0.093 Uiso 0.60 1 calc PR D 1 C64 C 0.43280(13) 0.7295(5) 1.0298(3) 0.064(3) Uiso 0.60 1 d PG D 1 C65 C 0.4622(3) 0.7129(9) 1.0222(7) 0.077(3) Uiso 0.60 1 d P D 1 H65 H 0.4569 0.6820 0.9841 0.092 Uiso 0.60 1 calc PR D 1 C66 C 0.4834(3) 0.6670(9) 1.0733(6) 0.079(3) Uiso 0.60 1 d P D 1 H66A H 0.5018 0.6570 1.0675 0.119 Uiso 0.60 1 calc PR D 1 H66B H 0.4740 0.6172 1.0755 0.119 Uiso 0.60 1 calc PR D 1 H66C H 0.4886 0.6962 1.1112 0.119 Uiso 0.60 1 calc PR D 1 C67 C 0.4755(4) 0.7933(10) 1.0146(7) 0.096(4) Uiso 0.60 1 d P D 1 H67A H 0.4605 0.8211 0.9796 0.144 Uiso 0.60 1 calc PR D 1 H67B H 0.4938 0.7844 1.0082 0.144 Uiso 0.60 1 calc PR D 1 H67C H 0.4806 0.8248 1.0515 0.144 Uiso 0.60 1 calc PR D 1 C68 C 0.3504(3) 0.6642(8) 0.9694(6) 0.060(3) Uiso 0.60 1 d P D 1 H68 H 0.3505 0.6452 0.9305 0.071 Uiso 0.60 1 calc PR D 1 C69 C 0.3457(4) 0.5915(9) 1.0026(7) 0.084(4) Uiso 0.60 1 d P D 1 H69A H 0.3260 0.5680 0.9778 0.126 Uiso 0.60 1 calc PR D 1 H69B H 0.3464 0.6074 1.0420 0.126 Uiso 0.60 1 calc PR D 1 H69C H 0.3617 0.5533 1.0089 0.126 Uiso 0.60 1 calc PR D 1 C70 C 0.3251(3) 0.7241(8) 0.9526(6) 0.071(3) Uiso 0.60 1 d P D 1 H70A H 0.3056 0.6985 0.9293 0.106 Uiso 0.60 1 calc PR D 1 H70B H 0.3282 0.7656 0.9280 0.106 Uiso 0.60 1 calc PR D 1 H70C H 0.3252 0.7468 0.9898 0.106 Uiso 0.60 1 calc PR D 1 S2A S 0.3695(5) 0.505(2) 0.9046(11) 0.077(6) Uani 0.40 1 d P D 2 P3A P 0.4120(3) 0.5664(7) 0.9501(7) 0.051(2) Uani 0.40 1 d P D 2 C41A C 0.43441(19) 0.5466(6) 0.9117(4) 0.0473(17) Uiso 0.40 1 d PG D 2 C42A C 0.42351(15) 0.5100(6) 0.8553(4) 0.037(3) Uiso 0.40 1 d PG D 2 H42A H 0.4030 0.4940 0.8360 0.044 Uiso 0.40 1 calc PR D 2 C43A C 0.44265(19) 0.4969(6) 0.8271(3) 0.052(3) Uiso 0.40 1 d PG D 2 H43A H 0.4352 0.4719 0.7886 0.063 Uiso 0.40 1 calc PR D 2 C44A C 0.47269(18) 0.5203(7) 0.8553(4) 0.063(4) Uiso 0.40 1 d PG D 2 H44A H 0.4858 0.5114 0.8361 0.076 Uiso 0.40 1 calc PR D 2 C45A C 0.48360(16) 0.5569(7) 0.9118(4) 0.060(4) Uiso 0.40 1 d PG D 2 H45A H 0.5041 0.5730 0.9311 0.071 Uiso 0.40 1 calc PR D 2 C46A C 0.4645(2) 0.5701(6) 0.9399(4) 0.061(4) Uiso 0.40 1 d PG D 2 H46A H 0.4719 0.5951 0.9785 0.074 Uiso 0.40 1 calc PR D 2 N3A N 0.4270(3) 0.5618(8) 1.0202(6) 0.049(3) Uiso 0.40 1 d P D 2 C47A C 0.4393(3) 0.5117(9) 1.0693(6) 0.044(3) Uiso 0.40 1 d P D 2 C48A C 0.4429(4) 0.4258(11) 1.0616(7) 0.050(4) Uiso 0.40 1 d P D 2 C49A C 0.4572(3) 0.3791(10) 1.1124(7) 0.052(3) Uiso 0.40 1 d P D 2 H49A H 0.4612 0.3259 1.1072 0.062 Uiso 0.40 1 calc PR D 2 C50A C 0.4659(4) 0.4084(12) 1.1709(7) 0.056(4) Uiso 0.40 1 d P D 2 H50A H 0.4737 0.3747 1.2052 0.067 Uiso 0.40 1 calc PR D 2 C51A C 0.4627(4) 0.4946(11) 1.1784(8) 0.065(4) Uiso 0.40 1 d P D 2 H51A H 0.4709 0.5181 1.2176 0.078 Uiso 0.40 1 calc PR D 2 C52A C 0.4480(3) 0.5371(10) 1.1287(6) 0.048(3) Uiso 0.40 1 d P D 2 C53A C 0.4401(4) 0.6225(10) 1.1363(8) 0.063(4) Uiso 0.40 1 d P D 2 H53A H 0.4352 0.6509 1.0972 0.075 Uiso 0.40 1 calc PR D 2 C54A C 0.4136(4) 0.6279(12) 1.1514(9) 0.080(5) Uiso 0.40 1 d P D 2 H54D H 0.4088 0.6830 1.1542 0.120 Uiso 0.40 1 calc PR D 2 H54E H 0.4184 0.6020 1.1904 0.120 Uiso 0.40 1 calc PR D 2 H54F H 0.3962 0.6022 1.1195 0.120 Uiso 0.40 1 calc PR D 2 C55A C 0.4661(5) 0.6691(14) 1.1895(10) 0.096(6) Uiso 0.40 1 d P D 2 H55D H 0.4597 0.7234 1.1897 0.143 Uiso 0.40 1 calc PR D 2 H55E H 0.4845 0.6681 1.1830 0.143 Uiso 0.40 1 calc PR D 2 H55F H 0.4700 0.6444 1.2286 0.143 Uiso 0.40 1 calc PR D 2 C56A C 0.4333(4) 0.3858(12) 1.0000(9) 0.064(4) Uiso 0.40 1 d P D 2 H56A H 0.4249 0.4273 0.9681 0.076 Uiso 0.40 1 calc PR D 2 C57A C 0.4096(6) 0.3309(14) 0.9901(10) 0.085(6) Uiso 0.40 1 d P D 2 H57D H 0.3928 0.3574 0.9945 0.128 Uiso 0.40 1 calc PR D 2 H57E H 0.4172 0.2886 1.0199 0.128 Uiso 0.40 1 calc PR D 2 H57F H 0.4025 0.3092 0.9490 0.128 Uiso 0.40 1 calc PR D 2 C58A C 0.4596(5) 0.3489(13) 0.9926(10) 0.082(5) Uiso 0.40 1 d P D 2 H58D H 0.4751 0.3887 0.9987 0.123 Uiso 0.40 1 calc PR D 2 H58E H 0.4526 0.3269 0.9516 0.123 Uiso 0.40 1 calc PR D 2 H58F H 0.4682 0.3071 1.0227 0.123 Uiso 0.40 1 calc PR D 2 N4A N 0.4042(3) 0.6683(9) 0.9331(6) 0.048(4) Uiso 0.40 1 d P D 2 C59A C 0.4064(2) 0.7234(6) 0.9805(4) 0.057(2) Uiso 0.40 1 d PG D 2 C60A C 0.38172(18) 0.7358(6) 0.9939(5) 0.057(4) Uiso 0.40 1 d PG D 2 C61A C 0.38386(19) 0.7887(7) 1.0391(5) 0.066(4) Uiso 0.40 1 d PG D 2 H61A H 0.3670 0.7971 1.0483 0.079 Uiso 0.40 1 calc PR D 2 C62A C 0.4106(2) 0.8292(6) 1.0708(5) 0.069(4) Uiso 0.40 1 d PG D 2 H62A H 0.4121 0.8654 1.1016 0.083 Uiso 0.40 1 calc PR D 2 C63A C 0.43530(19) 0.8169(7) 1.0573(5) 0.074(5) Uiso 0.40 1 d PG D 2 H63A H 0.4536 0.8446 1.0790 0.089 Uiso 0.40 1 calc PR D 2 C64A C 0.43316(19) 0.7640(7) 1.0122(5) 0.058(4) Uiso 0.40 1 d PG D 2 C65A C 0.4601(4) 0.7455(11) 1.0042(8) 0.057(4) Uiso 0.40 1 d P D 2 H65A H 0.4543 0.7089 0.9689 0.069 Uiso 0.40 1 calc PR D 2 C66A C 0.4842(4) 0.7048(11) 1.0603(8) 0.066(4) Uiso 0.40 1 d P D 2 H66D H 0.5020 0.6933 1.0528 0.098 Uiso 0.40 1 calc PR D 2 H66E H 0.4760 0.6559 1.0680 0.098 Uiso 0.40 1 calc PR D 2 H66F H 0.4900 0.7393 1.0957 0.098 Uiso 0.40 1 calc PR D 2 C67A C 0.4714(5) 0.8275(14) 0.9857(10) 0.093(6) Uiso 0.40 1 d P D 2 H67D H 0.4896 0.8177 0.9790 0.139 Uiso 0.40 1 calc PR D 2 H67E H 0.4761 0.8656 1.0187 0.139 Uiso 0.40 1 calc PR D 2 H67F H 0.4554 0.8483 0.9484 0.139 Uiso 0.40 1 calc PR D 2 C68A C 0.3518(4) 0.6947(11) 0.9599(8) 0.057(4) Uiso 0.40 1 d P D 2 H68A H 0.3522 0.6696 0.9230 0.068 Uiso 0.40 1 calc PR D 2 C69A C 0.3469(4) 0.6273(13) 1.0005(9) 0.073(5) Uiso 0.40 1 d P D 2 H69D H 0.3274 0.6016 0.9775 0.109 Uiso 0.40 1 calc PR D 2 H69E H 0.3470 0.6503 1.0377 0.109 Uiso 0.40 1 calc PR D 2 H69F H 0.3632 0.5887 1.0114 0.109 Uiso 0.40 1 calc PR D 2 C70A C 0.3265(4) 0.7610(12) 0.9377(9) 0.076(5) Uiso 0.40 1 d P D 2 H70D H 0.3067 0.7370 0.9147 0.115 Uiso 0.40 1 calc PR D 2 H70E H 0.3308 0.7981 0.9115 0.115 Uiso 0.40 1 calc PR D 2 H70F H 0.3266 0.7887 0.9730 0.115 Uiso 0.40 1 calc PR D 2 P4 P 0.38851(11) 0.6800(3) 0.8703(3) 0.0517(11) Uani 0.60 1 d PD D 1 C71 C 0.4167(4) 0.7143(9) 0.8410(8) 0.084(5) Uiso 0.60 1 d PD D 1 H71A H 0.4309 0.7494 0.8726 0.101 Uiso 0.60 1 calc PR D 1 H71B H 0.4285 0.6675 0.8402 0.101 Uiso 0.60 1 calc PR D 1 C72 C 0.4093(4) 0.7508(11) 0.7878(8) 0.127(6) Uiso 0.60 1 d PD D 1 H72A H 0.4014 0.8032 0.7908 0.153 Uiso 0.60 1 calc PR D 1 H72B H 0.3925 0.7214 0.7563 0.153 Uiso 0.60 1 calc PR D 1 C73 C 0.4335(7) 0.762(2) 0.7654(13) 0.244(15) Uiso 0.60 1 d PD D 1 H73A H 0.4301 0.8111 0.7421 0.293 Uiso 0.60 1 calc PR D 1 H73B H 0.4330 0.7179 0.7382 0.293 Uiso 0.60 1 calc PR D 1 C74 C 0.4645(6) 0.7641(18) 0.8209(14) 0.223(8) Uiso 0.60 1 d PD D 1 H74A H 0.4806 0.7688 0.8070 0.334 Uiso 0.60 1 calc PR D 1 H74B H 0.4673 0.7158 0.8445 0.334 Uiso 0.60 1 calc PR D 1 H74C H 0.4652 0.8091 0.8465 0.334 Uiso 0.60 1 calc PR D 1 C75 C 0.37049(14) 0.7819(3) 0.8603(3) 0.066(2) Uiso 0.60 1 d PG D 1 C76 C 0.38440(16) 0.8452(4) 0.8977(3) 0.102(4) Uiso 0.60 1 d PG D 1 H76 H 0.4043 0.8401 0.9288 0.122 Uiso 0.60 1 calc PR D 1 C77 C 0.36916(19) 0.9160(4) 0.8895(4) 0.132(7) Uiso 0.60 1 d PG D 1 H77 H 0.3787 0.9593 0.9150 0.159 Uiso 0.60 1 calc PR D 1 C78 C 0.3400(2) 0.9235(4) 0.8440(5) 0.114(5) Uiso 0.60 1 d PG D 1 H78 H 0.3296 0.9719 0.8384 0.136 Uiso 0.60 1 calc PR D 1 C79 C 0.32609(15) 0.8602(5) 0.8066(4) 0.114(5) Uiso 0.60 1 d PG D 1 H79 H 0.3062 0.8653 0.7755 0.136 Uiso 0.60 1 calc PR D 1 C80 C 0.34133(13) 0.7894(4) 0.8148(4) 0.089(4) Uiso 0.60 1 d PG D 1 H80 H 0.3318 0.7461 0.7893 0.107 Uiso 0.60 1 calc PR D 1 P4A P 0.38878(18) 0.6950(3) 0.8600(4) 0.060(3) Uani 0.40 1 d PGD D 2 C71A C 0.42175(15) 0.7110(5) 0.8533(4) 0.063(7) Uiso 0.40 1 d PG D 2 C72A C 0.43129(13) 0.7884(5) 0.8594(4) 0.102(7) Uiso 0.40 1 d PG D 2 H72D H 0.4231 0.8257 0.8775 0.123 Uiso 0.40 1 calc PR D 2 C73A C 0.45278(18) 0.8114(6) 0.8392(6) 0.152(11) Uiso 0.40 1 d PG D 2 H73D H 0.4593 0.8643 0.8434 0.183 Uiso 0.40 1 calc PR D 2 C74A C 0.4647(2) 0.7569(8) 0.8128(6) 0.223(8) Uiso 0.40 1 d PG D 2 H74D H 0.4794 0.7726 0.7990 0.267 Uiso 0.40 1 calc PR D 2 C75A C 0.4552(2) 0.6795(7) 0.8067(5) 0.109(7) Uiso 0.40 1 d PG D 2 H75A H 0.4634 0.6422 0.7887 0.131 Uiso 0.40 1 calc PR D 2 C76A C 0.43369(19) 0.6565(5) 0.8270(5) 0.075(5) Uiso 0.40 1 d PG D 2 H76A H 0.4272 0.6036 0.8228 0.091 Uiso 0.40 1 calc PR D 2 C75B C 0.3683(4) 0.7735(9) 0.8723(8) 0.066(2) Uiso 0.40 1 d PD D 2 H75C H 0.3523 0.7551 0.8841 0.079 Uiso 0.40 1 calc PR D 2 H75D H 0.3817 0.8111 0.9029 0.079 Uiso 0.40 1 calc PR D 2 C76B C 0.3542(5) 0.8104(12) 0.8028(9) 0.102(4) Uiso 0.40 1 d PD D 2 H76C H 0.3708 0.8179 0.7902 0.122 Uiso 0.40 1 calc PR D 2 H76D H 0.3398 0.7721 0.7746 0.122 Uiso 0.40 1 calc PR D 2 C79B C 0.3395(6) 0.8802(16) 0.7975(12) 0.118(8) Uiso 0.40 1 d PD D 2 H79C H 0.3263 0.8898 0.7540 0.142 Uiso 0.40 1 calc PR D 2 H79D H 0.3546 0.9228 0.8118 0.142 Uiso 0.40 1 calc PR D 2 C80B C 0.3205(6) 0.8824(17) 0.8333(13) 0.124(8) Uiso 0.40 1 d PD D 2 H80C H 0.3100 0.9327 0.8267 0.186 Uiso 0.40 1 calc PR D 2 H80D H 0.3336 0.8759 0.8767 0.186 Uiso 0.40 1 calc PR D 2 H80E H 0.3057 0.8399 0.8197 0.186 Uiso 0.40 1 calc PR D 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 0.04879(15) 0.06730(17) 0.04729(15) 0.00327(10) 0.02135(11) 0.00231(10) N1 0.050(3) 0.078(3) 0.049(3) -0.007(2) 0.024(2) 0.003(2) N2 0.052(2) 0.052(3) 0.039(2) 0.0033(19) 0.025(2) 0.006(2) P1 0.0505(7) 0.0472(7) 0.0427(7) 0.0003(6) 0.0263(6) 0.0024(6) P2 0.0552(8) 0.0548(8) 0.0472(8) 0.0034(6) 0.0287(7) 0.0113(7) S1 0.0531(7) 0.0495(8) 0.0450(7) -0.0027(6) 0.0239(6) 0.0055(6) C7 0.047(3) 0.045(3) 0.055(3) -0.004(2) 0.024(3) -0.003(2) C8 0.051(3) 0.063(4) 0.063(4) -0.003(3) 0.024(3) -0.006(3) C9 0.054(4) 0.082(5) 0.069(4) 0.006(4) 0.022(3) 0.007(3) C10 0.060(4) 0.097(6) 0.096(6) -0.003(4) 0.041(4) 0.018(4) C11 0.074(4) 0.099(5) 0.077(5) 0.008(4) 0.053(4) 0.018(4) C12 0.056(3) 0.052(3) 0.064(4) 0.004(3) 0.032(3) 0.003(3) C13 0.062(4) 0.082(4) 0.057(4) 0.001(3) 0.038(3) -0.002(3) C14 0.101(6) 0.101(6) 0.076(5) -0.024(4) 0.047(4) -0.004(5) C15 0.097(5) 0.085(5) 0.074(5) 0.021(4) 0.045(4) 0.002(4) C19 0.054(3) 0.070(4) 0.043(3) -0.001(3) 0.026(3) 0.010(3) C20 0.072(4) 0.067(4) 0.048(3) 0.011(3) 0.031(3) 0.021(3) C21 0.106(6) 0.094(5) 0.059(4) 0.021(4) 0.044(4) 0.030(5) C22 0.113(7) 0.107(7) 0.054(4) 0.006(4) 0.034(4) 0.028(5) C23 0.084(5) 0.125(7) 0.042(4) -0.016(4) 0.026(3) 0.013(5) C24 0.066(4) 0.072(4) 0.052(3) -0.005(3) 0.031(3) 0.003(3) C25 0.096(6) 0.095(6) 0.066(4) -0.023(4) 0.043(4) -0.024(4) C26 0.144(8) 0.088(6) 0.081(5) -0.020(4) 0.057(5) -0.012(6) C27 0.134(9) 0.144(9) 0.121(8) -0.040(7) 0.070(7) -0.054(8) C28 0.101(5) 0.053(4) 0.058(4) 0.016(3) 0.037(4) 0.010(3) C29 0.152(8) 0.072(5) 0.077(5) 0.028(4) 0.060(5) 0.042(5) C30 0.150(8) 0.083(5) 0.086(6) 0.014(4) 0.053(6) -0.024(5) S2 0.048(4) 0.086(6) 0.047(5) 0.011(4) 0.025(3) 0.011(3) P3 0.040(3) 0.078(5) 0.0421(19) 0.001(3) 0.0236(18) 0.003(3) S2A 0.073(7) 0.091(10) 0.060(9) 0.040(7) 0.020(6) 0.027(5) P3A 0.039(4) 0.071(6) 0.047(3) 0.006(4) 0.021(3) -0.003(3) P4 0.040(2) 0.062(2) 0.056(2) -0.002(2) 0.0236(17) -0.0070(15) P4A 0.063(4) 0.051(4) 0.078(5) 0.003(3) 0.041(3) -0.001(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 Hg1 P4 2.453(6) . ? Hg1 P2 2.4742(16) . ? Hg1 S2A 2.50(3) . ? Hg1 S1 2.5501(14) . ? Hg1 P4A 2.583(8) . ? Hg1 S2 2.613(16) . ? N1 C7 1.371(7) . ? N1 P1 1.512(5) . ? N2 C19 1.463(7) . ? N2 P2 1.664(4) . ? N2 P1 1.733(4) . ? P1 C1 1.789(5) . ? P1 C1A 1.912(16) . ? P1 S1 2.026(2) . ? P2 C37A 1.739(11) . ? P2 C31 1.796(6) . ? P2 C31A 1.844(15) . ? P2 C37 1.908(12) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C2 H2 0.9500 . ? C3 C4 1.3900 . ? C3 H3 0.9500 . ? C4 C5 1.3900 . ? C4 H4 0.9500 . ? C5 C6 1.3900 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C1A C2A 1.36(2) . ? C1A C6A 1.39(3) . ? C2A C3A 1.50(3) . ? C2A H2A 0.9500 . ? C3A C4A 1.33(3) . ? C3A H3A 0.9500 . ? C4A C5A 1.34(3) . ? C4A H4A 0.9500 . ? C5A C6A 1.40(2) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C7 C8 1.405(8) . ? C7 C12 1.415(8) . ? C8 C9 1.352(9) . ? C8 C16A 1.525(17) . ? C8 C16 1.541(15) . ? C9 C10 1.372(10) . ? C9 H9 0.9500 . ? C10 C11 1.372(10) . ? C10 H10 0.9500 . ? C11 C12 1.346(9) . ? C11 H11 0.9500 . ? C12 C13 1.518(9) . ? C13 C14 1.530(9) . ? C13 C15 1.553(9) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.56(2) . ? C16 C18 1.57(2) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C16A C18A 1.48(2) . ? C16A C17A 1.52(2) . ? C16A H16A 1.0000 . ? C17A H17D 0.9800 . ? C17A H17E 0.9800 . ? C17A H17F 0.9800 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? C19 C20 1.393(9) . ? C19 C24 1.405(9) . ? C20 C21 1.412(9) . ? C20 C28 1.503(9) . ? C21 C22 1.361(12) . ? C21 H21 0.9500 . ? C22 C23 1.357(12) . ? C22 H22 0.9500 . ? C23 C24 1.411(9) . ? C23 H23 0.9500 . ? C24 C25 1.494(10) . ? C25 C27 1.493(12) . ? C25 C26 1.526(11) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.504(10) . ? C28 C30 1.530(10) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C32 H32 0.9500 . ? C33 C34 1.3900 . ? C33 H33 0.9500 . ? C34 C35 1.3900 . ? C34 H34 0.9500 . ? C35 C36 1.3900 . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.462(17) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.557(19) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.41(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C31A C32A 1.39(2) . ? C31A H31A 0.9900 . ? C31A H31B 0.9900 . ? C32A C33A 1.55(2) . ? C32A H32A 0.9900 . ? C32A H32B 0.9900 . ? C33A C34A 1.56(3) . ? C33A H33A 0.9900 . ? C33A H33B 0.9900 . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? C37A C38A 1.3900 . ? C37A C42B 1.3900 . ? C38A C39A 1.3900 . ? C38A H38C 0.9500 . ? C39A C40B 1.3900 . ? C39A H39C 0.9500 . ? C40B C41B 1.3900 . ? C40B H40D 0.9500 . ? C41B C42B 1.3900 . ? C41B H41B 0.9500 . ? C42B H42B 0.9500 . ? C34B H34D 0.9800 . ? C34B H34E 0.9800 . ? C34B H34F 0.9800 . ? S2 P3 1.904(17) . ? P3 N3 1.523(13) . ? P3 N4 1.741(12) . ? P3 C41 1.836(11) . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C42 H42 0.9500 . ? C43 C44 1.3900 . ? C43 H43 0.9500 . ? C44 C45 1.3900 . ? C44 H44 0.9500 . ? C45 C46 1.3900 . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? N3 C47 1.374(14) . ? C47 C52 1.405(15) . ? C47 C48 1.406(18) . ? C48 C49 1.434(17) . ? C48 C56 1.539(18) . ? C49 C50 1.375(19) . ? C49 H49 0.9500 . ? C50 C51 1.45(2) . ? C50 H50 0.9500 . ? C51 C52 1.366(17) . ? C51 H51 0.9500 . ? C52 C53 1.491(17) . ? C53 C55 1.501(19) . ? C53 C54 1.571(19) . ? C53 H53 1.0000 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.48(2) . ? C56 C58 1.486(18) . ? C56 H56 1.0000 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? N4 C59 1.445(10) . ? N4 P4 1.712(12) . ? C59 C60 1.3900 . ? C59 C64 1.3900 . ? C60 C61 1.3900 . ? C60 C68 1.510(13) . ? C61 C62 1.3900 . ? C61 H61 0.9500 . ? C62 C63 1.3900 . ? C62 H62 0.9500 . ? C63 C64 1.3900 . ? C63 H63 0.9500 . ? C64 C65 1.551(14) . ? C65 C66 1.46(2) . ? C65 C67 1.56(2) . ? C65 H65 1.0000 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C70 1.521(16) . ? C68 C69 1.55(2) . ? C68 H68 1.0000 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? S2A P3A 2.17(3) . ? P3A N3A 1.54(2) . ? P3A C41A 1.747(16) . ? P3A N4A 1.79(2) . ? C41A C42A 1.3900 . ? C41A C46A 1.3900 . ? C42A C43A 1.3900 . ? C42A H42A 0.9500 . ? C43A C44A 1.3900 . ? C43A H43A 0.9500 . ? C44A C45A 1.3900 . ? C44A H44A 0.9500 . ? C45A C46A 1.3900 . ? C45A H45A 0.9500 . ? C46A H46A 0.9500 . ? N3A C47A 1.382(19) . ? C47A C52A 1.39(2) . ? C47A C48A 1.50(2) . ? C48A C49A 1.38(2) . ? C48A C56A 1.53(3) . ? C49A C50A 1.39(2) . ? C49A H49A 0.9500 . ? C50A C51A 1.50(3) . ? C50A H50A 0.9500 . ? C51A C52A 1.33(2) . ? C51A H51A 0.9500 . ? C52A C53A 1.54(2) . ? C53A C54A 1.49(2) . ? C53A C55A 1.59(3) . ? C53A H53A 1.0000 . ? C54A H54D 0.9800 . ? C54A H54E 0.9800 . ? C54A H54F 0.9800 . ? C55A H55D 0.9800 . ? C55A H55E 0.9800 . ? C55A H55F 0.9800 . ? C56A C57A 1.43(3) . ? C56A C58A 1.51(3) . ? C56A H56A 1.0000 . ? C57A H57D 0.9800 . ? C57A H57E 0.9800 . ? C57A H57F 0.9800 . ? C58A H58D 0.9800 . ? C58A H58E 0.9800 . ? C58A H58F 0.9800 . ? N4A C59A 1.456(15) . ? N4A P4A 1.669(16) . ? C59A C60A 1.3900 . ? C59A C64A 1.3900 . ? C60A C61A 1.3900 . ? C60A C68A 1.512(18) . ? C61A C62A 1.3900 . ? C61A H61A 0.9500 . ? C62A C63A 1.3900 . ? C62A H62A 0.9500 . ? C63A C64A 1.3900 . ? C63A H63A 0.9500 . ? C64A C65A 1.442(17) . ? C65A C66A 1.54(2) . ? C65A C67A 1.64(3) . ? C65A H65A 1.0000 . ? C66A H66D 0.9800 . ? C66A H66E 0.9800 . ? C66A H66F 0.9800 . ? C67A H67D 0.9800 . ? C67A H67E 0.9800 . ? C67A H67F 0.9800 . ? C68A C70A 1.59(3) . ? C68A C69A 1.60(3) . ? C68A H68A 1.0000 . ? C69A H69D 0.9800 . ? C69A H69E 0.9800 . ? C69A H69F 0.9800 . ? C70A H70D 0.9800 . ? C70A H70E 0.9800 . ? C70A H70F 0.9800 . ? P4 C71 1.890(11) . ? P4 C75 1.921(10) . ? C71 C72 1.339(18) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.51(2) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.54(3) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C76 1.3900 . ? C75 C80 1.3900 . ? C76 C77 1.3900 . ? C76 H76 0.9500 . ? C77 C78 1.3900 . ? C77 H77 0.9500 . ? C78 C79 1.3900 . ? C78 H78 0.9500 . ? C79 C80 1.3900 . ? C79 H79 0.9500 . ? C80 H80 0.9500 . ? P4A C71A 1.7072 . ? P4A C75B 1.772(15) . ? C71A C76A 1.3898 . ? C71A C72A 1.3900 . ? C72A C73A 1.3901 . ? C72A H72D 0.9500 . ? C73A C74A 1.3899 . ? C73A H73D 0.9500 . ? C74A C75A 1.3899 . ? C74A H74D 0.9500 . ? C75A C76A 1.3904 . ? C75A H75A 0.9500 . ? C76A H76A 0.9500 . ? C75B C76B 1.65(2) . ? C75B H75C 0.9900 . ? C75B H75D 0.9900 . ? C76B C79B 1.37(3) . ? C76B H76C 0.9900 . ? C76B H76D 0.9900 . ? C79B C80B 1.52(3) . ? C79B H79C 0.9900 . ? C79B H79D 0.9900 . ? C80B H80C 0.9800 . ? C80B H80D 0.9800 . ? C80B H80E 0.9800 . ? 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 P4 Hg1 P2 143.30(17) . . ? P4 Hg1 S2A 85.0(7) . . ? P2 Hg1 S2A 120.7(8) . . ? P4 Hg1 S1 109.41(12) . . ? P2 Hg1 S1 89.37(5) . . ? S2A Hg1 S1 106.1(5) . . ? P2 Hg1 P4A 136.78(18) . . ? S2A Hg1 P4A 92.6(7) . . ? S1 Hg1 P4A 108.22(14) . . ? P4 Hg1 S2 88.0(4) . . ? P2 Hg1 S2 116.9(4) . . ? S1 Hg1 S2 107.4(2) . . ? P4A Hg1 S2 95.6(4) . . ? C7 N1 P1 140.9(4) . . ? C19 N2 P2 117.7(3) . . ? C19 N2 P1 121.2(3) . . ? P2 N2 P1 119.1(2) . . ? N1 P1 N2 103.5(2) . . ? N1 P1 C1 108.5(3) . . ? N2 P1 C1 102.7(3) . . ? N1 P1 C1A 120.8(6) . . ? N2 P1 C1A 101.5(5) . . ? N1 P1 S1 119.7(2) . . ? N2 P1 S1 109.58(17) . . ? C1 P1 S1 111.2(2) . . ? C1A P1 S1 100.2(6) . . ? N2 P2 C37A 116.3(5) . . ? N2 P2 C31 110.7(3) . . ? C37A P2 C31 103.2(6) . . ? N2 P2 C31A 107.2(7) . . ? C37A P2 C31A 95.7(10) . . ? N2 P2 C37 102.8(5) . . ? C31 P2 C37 109.9(5) . . ? C31A P2 C37 100.7(10) . . ? N2 P2 Hg1 106.68(16) . . ? C37A P2 Hg1 111.2(5) . . ? C31 P2 Hg1 108.6(3) . . ? C31A P2 Hg1 119.9(9) . . ? C37 P2 Hg1 118.0(4) . . ? P1 S1 Hg1 97.11(7) . . ? C2 C1 C6 120.0 . . ? C2 C1 P1 119.1(4) . . ? C6 C1 P1 120.4(4) . . ? C3 C2 C1 120.0 . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C2A C1A C6A 118.3(15) . . ? C2A C1A P1 115.2(15) . . ? C6A C1A P1 125.6(12) . . ? C1A C2A C3A 123.4(17) . . ? C1A C2A H2A 118.3 . . ? C3A C2A H2A 118.3 . . ? C4A C3A C2A 109.1(17) . . ? C4A C3A H3A 125.4 . . ? C2A C3A H3A 125.4 . . ? C3A C4A C5A 130(2) . . ? C3A C4A H4A 114.8 . . ? C5A C4A H4A 114.8 . . ? C4A C5A C6A 116.6(18) . . ? C4A C5A H5A 121.7 . . ? C6A C5A H5A 121.7 . . ? C1A C6A C5A 119.9(17) . . ? C1A C6A H6A 120.0 . . ? C5A C6A H6A 120.0 . . ? N1 C7 C8 115.7(5) . . ? N1 C7 C12 125.2(5) . . ? C8 C7 C12 119.0(5) . . ? C9 C8 C7 119.2(6) . . ? C9 C8 C16A 118.6(8) . . ? C7 C8 C16A 120.8(8) . . ? C9 C8 C16 117.6(7) . . ? C7 C8 C16 122.7(7) . . ? C8 C9 C10 121.6(6) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C11 C10 C9 119.3(6) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C12 C11 C10 121.8(6) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C7 119.1(6) . . ? C11 C12 C13 116.3(6) . . ? C7 C12 C13 124.5(5) . . ? C12 C13 C14 113.8(6) . . ? C12 C13 C15 111.9(6) . . ? C14 C13 C15 111.2(6) . . ? C12 C13 H13 106.4 . . ? C14 C13 H13 106.4 . . ? C15 C13 H13 106.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C8 C16 C17 114.0(11) . . ? C8 C16 C18 109.9(12) . . ? C17 C16 C18 107.2(13) . . ? C8 C16 H16 108.5 . . ? C17 C16 H16 108.5 . . ? C18 C16 H16 108.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C18A C16A C17A 110.5(14) . . ? C18A C16A C8 114.4(13) . . ? C17A C16A C8 108.1(12) . . ? C18A C16A H16A 107.9 . . ? C17A C16A H16A 107.9 . . ? C8 C16A H16A 107.9 . . ? C16A C17A H17D 109.5 . . ? C16A C17A H17E 109.5 . . ? H17D C17A H17E 109.5 . . ? C16A C17A H17F 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? C16A C18A H18D 109.5 . . ? C16A C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C16A C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? C20 C19 C24 121.8(5) . . ? C20 C19 N2 119.7(5) . . ? C24 C19 N2 118.3(6) . . ? C19 C20 C21 118.0(6) . . ? C19 C20 C28 123.8(5) . . ? C21 C20 C28 118.2(6) . . ? C22 C21 C20 121.6(8) . . ? C22 C21 H21 119.2 . . ? C20 C21 H21 119.2 . . ? C23 C22 C21 119.1(7) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C22 C23 C24 123.5(7) . . ? C22 C23 H23 118.2 . . ? C24 C23 H23 118.2 . . ? C19 C24 C23 116.0(7) . . ? C19 C24 C25 123.7(6) . . ? C23 C24 C25 120.3(7) . . ? C27 C25 C24 111.4(8) . . ? C27 C25 C26 107.4(7) . . ? C24 C25 C26 112.0(6) . . ? C27 C25 H25 108.7 . . ? C24 C25 H25 108.7 . . ? C26 C25 H25 108.7 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C20 C28 C29 112.0(7) . . ? C20 C28 C30 113.4(6) . . ? C29 C28 C30 109.8(6) . . ? C20 C28 H28 107.1 . . ? C29 C28 H28 107.1 . . ? C30 C28 H28 107.1 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C36 120.0 . . ? C32 C31 P2 122.9(5) . . ? C36 C31 P2 116.8(5) . . ? C31 C32 C33 120.0 . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? C38 C37 P2 109.3(10) . . ? C38 C37 H37A 109.8 . . ? P2 C37 H37A 109.8 . . ? C38 C37 H37B 109.8 . . ? P2 C37 H37B 109.8 . . ? H37A C37 H37B 108.3 . . ? C37 C38 C39 112.0(11) . . ? C37 C38 H38A 109.2 . . ? C39 C38 H38A 109.2 . . ? C37 C38 H38B 109.2 . . ? C39 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? C40 C39 C38 112.8(15) . . ? C40 C39 H39A 109.0 . . ? C38 C39 H39A 109.0 . . ? C40 C39 H39B 109.0 . . ? C38 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C32A C31A P2 110.7(14) . . ? C32A C31A H31A 109.5 . . ? P2 C31A H31A 109.5 . . ? C32A C31A H31B 109.5 . . ? P2 C31A H31B 109.5 . . ? H31A C31A H31B 108.1 . . ? C31A C32A C33A 108.6(15) . . ? C31A C32A H32A 110.0 . . ? C33A C32A H32A 110.0 . . ? C31A C32A H32B 110.0 . . ? C33A C32A H32B 110.0 . . ? H32A C32A H32B 108.4 . . ? C32A C33A C34A 103.5(17) . . ? C32A C33A H33A 111.1 . . ? C34A C33A H33A 111.1 . . ? C32A C33A H33B 111.1 . . ? C34A C33A H33B 111.1 . . ? H33A C33A H33B 109.0 . . ? C33A C34A H34A 109.5 . . ? C33A C34A H34B 109.5 . . ? H34A C34A H34B 109.5 . . ? C33A C34A H34C 109.5 . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? C38A C37A C42B 120.0 . . ? C38A C37A P2 118.6(8) . . ? C42B C37A P2 121.4(8) . . ? C39A C38A C37A 120.0 . . ? C39A C38A H38C 120.0 . . ? C37A C38A H38C 120.0 . . ? C38A C39A C40B 120.0 . . ? C38A C39A H39C 120.0 . . ? C40B C39A H39C 120.0 . . ? C41B C40B C39A 120.0 . . ? C41B C40B H40D 120.0 . . ? C39A C40B H40D 120.0 . . ? C40B C41B C42B 120.0 . . ? C40B C41B H41B 120.0 . . ? C42B C41B H41B 120.0 . . ? C41B C42B C37A 120.0 . . ? C41B C42B H42B 120.0 . . ? C37A C42B H42B 120.0 . . ? H34D C34B H34E 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? P3 S2 Hg1 99.2(7) . . ? N3 P3 N4 107.3(7) . . ? N3 P3 C41 113.2(7) . . ? N4 P3 C41 104.0(5) . . ? N3 P3 S2 117.8(7) . . ? N4 P3 S2 110.2(8) . . ? C41 P3 S2 103.5(6) . . ? C42 C41 C46 120.0 . . ? C42 C41 P3 122.6(5) . . ? C46 C41 P3 117.4(5) . . ? C43 C42 C41 120.0 . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C42 C43 C44 120.0 . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C46 120.0 . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C45 C46 C41 120.0 . . ? C45 C46 H46 120.0 . . ? C41 C46 H46 120.0 . . ? C47 N3 P3 145.1(10) . . ? N3 C47 C52 118.4(11) . . ? N3 C47 C48 123.7(10) . . ? C52 C47 C48 117.6(11) . . ? C47 C48 C49 119.7(11) . . ? C47 C48 C56 126.0(11) . . ? C49 C48 C56 114.3(12) . . ? C50 C49 C48 120.5(14) . . ? C50 C49 H49 119.7 . . ? C48 C49 H49 119.7 . . ? C49 C50 C51 119.7(13) . . ? C49 C50 H50 120.1 . . ? C51 C50 H50 120.1 . . ? C52 C51 C50 118.0(12) . . ? C52 C51 H51 121.0 . . ? C50 C51 H51 121.0 . . ? C51 C52 C47 123.5(12) . . ? C51 C52 C53 116.2(11) . . ? C47 C52 C53 120.2(11) . . ? C52 C53 C55 118.3(12) . . ? C52 C53 C54 109.3(10) . . ? C55 C53 C54 105.8(11) . . ? C52 C53 H53 107.7 . . ? C55 C53 H53 107.7 . . ? C54 C53 H53 107.7 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C57 C56 C58 111.9(12) . . ? C57 C56 C48 111.4(12) . . ? C58 C56 C48 114.3(11) . . ? C57 C56 H56 106.2 . . ? C58 C56 H56 106.2 . . ? C48 C56 H56 106.2 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C59 N4 P4 120.6(7) . . ? C59 N4 P3 120.3(8) . . ? P4 N4 P3 117.6(6) . . ? C60 C59 C64 120.0 . . ? C60 C59 N4 119.1(6) . . ? C64 C59 N4 120.9(6) . . ? C61 C60 C59 120.0 . . ? C61 C60 C68 116.1(6) . . ? C59 C60 C68 123.9(6) . . ? C60 C61 C62 120.0 . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C61 C62 C63 120.0 . . ? C61 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C64 C63 C62 120.0 . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C63 C64 C59 120.0 . . ? C63 C64 C65 118.2(7) . . ? C59 C64 C65 121.5(7) . . ? C66 C65 C64 110.8(11) . . ? C66 C65 C67 113.1(13) . . ? C64 C65 C67 107.8(11) . . ? C66 C65 H65 108.3 . . ? C64 C65 H65 108.3 . . ? C67 C65 H65 108.3 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C60 C68 C70 109.3(10) . . ? C60 C68 C69 112.8(11) . . ? C70 C68 C69 113.5(12) . . ? C60 C68 H68 107.0 . . ? C70 C68 H68 107.0 . . ? C69 C68 H68 107.0 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? P3A S2A Hg1 96.0(11) . . ? N3A P3A C41A 117.7(11) . . ? N3A P3A N4A 105.0(10) . . ? C41A P3A N4A 100.5(8) . . ? N3A P3A S2A 116.3(10) . . ? C41A P3A S2A 108.4(10) . . ? N4A P3A S2A 107.0(11) . . ? C42A C41A C46A 120.0 . . ? C42A C41A P3A 123.2(7) . . ? C46A C41A P3A 116.8(7) . . ? C41A C42A C43A 120.0 . . ? C41A C42A H42A 120.0 . . ? C43A C42A H42A 120.0 . . ? C42A C43A C44A 120.0 . . ? C42A C43A H43A 120.0 . . ? C44A C43A H43A 120.0 . . ? C43A C44A C45A 120.0 . . ? C43A C44A H44A 120.0 . . ? C45A C44A H44A 120.0 . . ? C46A C45A C44A 120.0 . . ? C46A C45A H45A 120.0 . . ? C44A C45A H45A 120.0 . . ? C45A C46A C41A 120.0 . . ? C45A C46A H46A 120.0 . . ? C41A C46A H46A 120.0 . . ? C47A N3A P3A 144.4(13) . . ? N3A C47A C52A 122.2(14) . . ? N3A C47A C48A 122.0(13) . . ? C52A C47A C48A 115.7(13) . . ? C49A C48A C47A 119.7(15) . . ? C49A C48A C56A 116.4(17) . . ? C47A C48A C56A 123.8(14) . . ? C48A C49A C50A 121.5(17) . . ? C48A C49A H49A 119.3 . . ? C50A C49A H49A 119.3 . . ? C49A C50A C51A 118.3(15) . . ? C49A C50A H50A 120.8 . . ? C51A C50A H50A 120.8 . . ? C52A C51A C50A 118.1(16) . . ? C52A C51A H51A 121.0 . . ? C50A C51A H51A 121.0 . . ? C51A C52A C47A 125.7(16) . . ? C51A C52A C53A 118.4(15) . . ? C47A C52A C53A 115.9(13) . . ? C54A C53A C52A 112.0(15) . . ? C54A C53A C55A 104.3(15) . . ? C52A C53A C55A 114.7(14) . . ? C54A C53A H53A 108.5 . . ? C52A C53A H53A 108.5 . . ? C55A C53A H53A 108.5 . . ? C53A C54A H54D 109.5 . . ? C53A C54A H54E 109.5 . . ? H54D C54A H54E 109.5 . . ? C53A C54A H54F 109.5 . . ? H54D C54A H54F 109.5 . . ? H54E C54A H54F 109.5 . . ? C53A C55A H55D 109.5 . . ? C53A C55A H55E 109.5 . . ? H55D C55A H55E 109.5 . . ? C53A C55A H55F 109.5 . . ? H55D C55A H55F 109.5 . . ? H55E C55A H55F 109.5 . . ? C57A C56A C58A 112.0(19) . . ? C57A C56A C48A 110.4(16) . . ? C58A C56A C48A 112.4(16) . . ? C57A C56A H56A 107.2 . . ? C58A C56A H56A 107.2 . . ? C48A C56A H56A 107.2 . . ? C56A C57A H57D 109.5 . . ? C56A C57A H57E 109.5 . . ? H57D C57A H57E 109.5 . . ? C56A C57A H57F 109.5 . . ? H57D C57A H57F 109.5 . . ? H57E C57A H57F 109.5 . . ? C56A C58A H58D 109.5 . . ? C56A C58A H58E 109.5 . . ? H58D C58A H58E 109.5 . . ? C56A C58A H58F 109.5 . . ? H58D C58A H58F 109.5 . . ? H58E C58A H58F 109.5 . . ? C59A N4A P4A 120.7(11) . . ? C59A N4A P3A 120.5(11) . . ? P4A N4A P3A 117.9(9) . . ? C60A C59A C64A 120.0 . . ? C60A C59A N4A 120.3(8) . . ? C64A C59A N4A 119.7(8) . . ? C59A C60A C61A 120.0 . . ? C59A C60A C68A 122.2(9) . . ? C61A C60A C68A 117.8(9) . . ? C62A C61A C60A 120.0 . . ? C62A C61A H61A 120.0 . . ? C60A C61A H61A 120.0 . . ? C61A C62A C63A 120.0 . . ? C61A C62A H62A 120.0 . . ? C63A C62A H62A 120.0 . . ? C64A C63A C62A 120.0 . . ? C64A C63A H63A 120.0 . . ? C62A C63A H63A 120.0 . . ? C63A C64A C59A 120.0 . . ? C63A C64A C65A 118.6(9) . . ? C59A C64A C65A 121.0(10) . . ? C64A C65A C66A 112.4(14) . . ? C64A C65A C67A 106.5(14) . . ? C66A C65A C67A 114.1(16) . . ? C64A C65A H65A 107.9 . . ? C66A C65A H65A 107.9 . . ? C67A C65A H65A 107.9 . . ? C65A C66A H66D 109.5 . . ? C65A C66A H66E 109.5 . . ? H66D C66A H66E 109.5 . . ? C65A C66A H66F 109.5 . . ? H66D C66A H66F 109.5 . . ? H66E C66A H66F 109.5 . . ? C65A C67A H67D 109.5 . . ? C65A C67A H67E 109.5 . . ? H67D C67A H67E 109.5 . . ? C65A C67A H67F 109.5 . . ? H67D C67A H67F 109.5 . . ? H67E C67A H67F 109.5 . . ? C60A C68A C70A 106.6(14) . . ? C60A C68A C69A 111.1(13) . . ? C70A C68A C69A 115.0(15) . . ? C60A C68A H68A 108.0 . . ? C70A C68A H68A 108.0 . . ? C69A C68A H68A 108.0 . . ? C68A C69A H69D 109.5 . . ? C68A C69A H69E 109.5 . . ? H69D C69A H69E 109.5 . . ? C68A C69A H69F 109.5 . . ? H69D C69A H69F 109.5 . . ? H69E C69A H69F 109.5 . . ? C68A C70A H70D 109.5 . . ? C68A C70A H70E 109.5 . . ? H70D C70A H70E 109.5 . . ? C68A C70A H70F 109.5 . . ? H70D C70A H70F 109.5 . . ? H70E C70A H70F 109.5 . . ? N4 P4 C71 116.2(7) . . ? N4 P4 C75 115.2(5) . . ? C71 P4 C75 92.2(6) . . ? N4 P4 Hg1 105.4(4) . . ? C71 P4 Hg1 117.2(6) . . ? C75 P4 Hg1 110.5(4) . . ? C72 C71 P4 124.4(13) . . ? C72 C71 H71A 106.2 . . ? P4 C71 H71A 106.2 . . ? C72 C71 H71B 106.2 . . ? P4 C71 H71B 106.2 . . ? H71A C71 H71B 106.4 . . ? C71 C72 C73 118.1(17) . . ? C71 C72 H72A 107.8 . . ? C73 C72 H72A 107.8 . . ? C71 C72 H72B 107.8 . . ? C73 C72 H72B 107.8 . . ? H72A C72 H72B 107.1 . . ? C72 C73 C74 108(2) . . ? C72 C73 H73A 110.0 . . ? C74 C73 H73A 110.0 . . ? C72 C73 H73B 110.0 . . ? C74 C73 H73B 110.0 . . ? H73A C73 H73B 108.4 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C76 C75 C80 120.0 . . ? C76 C75 P4 123.5(5) . . ? C80 C75 P4 116.4(5) . . ? C75 C76 C77 120.0 . . ? C75 C76 H76 120.0 . . ? C77 C76 H76 120.0 . . ? C78 C77 C76 120.0 . . ? C78 C77 H77 120.0 . . ? C76 C77 H77 120.0 . . ? C79 C78 C77 120.0 . . ? C79 C78 H78 120.0 . . ? C77 C78 H78 120.0 . . ? C78 C79 C80 120.0 . . ? C78 C79 H79 120.0 . . ? C80 C79 H79 120.0 . . ? C79 C80 C75 120.0 . . ? C79 C80 H80 120.0 . . ? C75 C80 H80 120.0 . . ? N4A P4A C71A 97.1(6) . . ? N4A P4A C75B 93.6(8) . . ? C71A P4A C75B 121.1(7) . . ? N4A P4A Hg1 102.7(6) . . ? C71A P4A Hg1 125.7(3) . . ? C75B P4A Hg1 107.5(8) . . ? C76A C71A C72A 120.0 . . ? C76A C71A P4A 122.2 . . ? C72A C71A P4A 115.4 . . ? C71A C72A C73A 120.0 . . ? C71A C72A H72D 120.0 . . ? C73A C72A H72D 120.0 . . ? C74A C73A C72A 120.0 . . ? C74A C73A H73D 120.0 . . ? C72A C73A H73D 120.0 . . ? C73A C74A C75A 120.0 . . ? C73A C74A H74D 120.0 . . ? C75A C74A H74D 120.0 . . ? C74A C75A C76A 120.0 . . ? C74A C75A H75A 120.0 . . ? C76A C75A H75A 120.0 . . ? C71A C76A C75A 120.0 . . ? C71A C76A H76A 120.0 . . ? C75A C76A H76A 120.0 . . ? C76B C75B P4A 98.0(11) . . ? C76B C75B H75C 112.2 . . ? P4A C75B H75C 112.2 . . ? C76B C75B H75D 112.2 . . ? P4A C75B H75D 112.2 . . ? H75C C75B H75D 109.8 . . ? C79B C76B C75B 113.9(18) . . ? C79B C76B H76C 108.8 . . ? C75B C76B H76C 108.8 . . ? C79B C76B H76D 108.8 . . ? C75B C76B H76D 108.8 . . ? H76C C76B H76D 107.7 . . ? C76B C79B C80B 113(2) . . ? C76B C79B H79C 109.0 . . ? C80B C79B H79C 109.0 . . ? C76B C79B H79D 109.0 . . ? C80B C79B H79D 109.0 . . ? H79C C79B H79D 107.8 . . ? C79B C80B H80C 109.5 . . ? C79B C80B H80D 109.5 . . ? H80C C80B H80D 109.5 . . ? C79B C80B H80E 109.5 . . ? H80C C80B H80E 109.5 . . ? H80D C80B H80E 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.790 _refine_diff_density_min -1.352 _refine_diff_density_rms 0.091