# Electronic Supplementary Material (ESI) for Catalysis Science & Technology # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Cat.Sci.Tech. _journal_coden_cambridge 1486 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Paul G. Hayes' _publ_contact_author_email p.hayes@uleth.ca loop_ _publ_author_name 'Craig A. Wheaton' 'Benjamin J. Ireland' 'Paul G. Hayes' data_L1 _database_code_depnum_ccdc_archive 'CCDC 833323' #TrackingRef '6184_web_deposit_cif_file_0_PaulG.Hayes_ #1310063407.Chem Eur J_AllCifs - Paul G Hayes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54.20 H48.40 Cl0.40 N2 O P2' _chemical_formula_weight 819.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5434(11) _cell_length_b 14.8956(15) _cell_length_c 15.1659(15) _cell_angle_alpha 62.3130(10) _cell_angle_beta 86.1340(10) _cell_angle_gamma 78.1150(10) _cell_volume 2258.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8967 _cell_measurement_theta_min 4.421 _cell_measurement_theta_max 54.126 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 865 _exptl_absorpt_coefficient_mu 0.161 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6810 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26448 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.0844 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7960 _reflns_number_gt 4429 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0551P)^2^+3.0800P] 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 7960 _refine_ls_number_parameters 563 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1432 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1827 _refine_ls_wR_factor_gt 0.1472 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0727(3) 0.6079(3) 0.5633(3) 0.0297(9) Uani 1 1 d . . . N1 N -0.1498(3) 0.8712(3) 0.2904(3) 0.0421(9) Uani 1 1 d . . . O1 O -0.0075(2) 0.62491(19) 0.62583(18) 0.0302(6) Uani 1 1 d . . . P1 P -0.08975(10) 0.81157(8) 0.39663(8) 0.0323(3) Uani 1 1 d . . . C2 C -0.1134(4) 0.6796(3) 0.4681(3) 0.0315(10) Uani 1 1 d . . . N2 N 0.2184(3) 0.6728(3) 0.7126(3) 0.0435(9) Uani 1 1 d . . . P2 P 0.14345(10) 0.61431(9) 0.80112(8) 0.0347(3) Uani 1 1 d . . . C3 C -0.1759(4) 0.6437(3) 0.4193(3) 0.0382(11) Uani 1 1 d . . . H3 H -0.2050 0.6894 0.3530 0.046 Uiso 1 1 calc R . . C4 C -0.1972(4) 0.5434(3) 0.4644(3) 0.0423(11) Uani 1 1 d . . . H4 H -0.2402 0.5222 0.4286 0.051 Uiso 1 1 calc R . . C5 C -0.1567(4) 0.4750(3) 0.5596(3) 0.0397(11) Uani 1 1 d . . . H5 H -0.1719 0.4068 0.5904 0.048 Uiso 1 1 calc R . . C6 C -0.0932(4) 0.5071(3) 0.6105(3) 0.0307(10) Uani 1 1 d . . . C7 C -0.0373(4) 0.4587(3) 0.7077(3) 0.0329(10) Uani 1 1 d . . . C8 C -0.0246(4) 0.3609(3) 0.7894(3) 0.0406(11) Uani 1 1 d . . . H8 H -0.0575 0.3084 0.7874 0.049 Uiso 1 1 calc R . . C9 C 0.0360(4) 0.3420(3) 0.8725(3) 0.0465(12) Uani 1 1 d . . . H9 H 0.0455 0.2755 0.9285 0.056 Uiso 1 1 calc R . . C10 C 0.0842(4) 0.4181(3) 0.8768(3) 0.0421(11) Uani 1 1 d . . . H10 H 0.1247 0.4022 0.9363 0.050 Uiso 1 1 calc R . . C11 C 0.0752(4) 0.5173(3) 0.7965(3) 0.0321(10) Uani 1 1 d . . . C12 C 0.0137(4) 0.5329(3) 0.7141(3) 0.0302(10) Uani 1 1 d . . . C13 C 0.0671(4) 0.8015(3) 0.3773(3) 0.0299(10) Uani 1 1 d . . . C14 C 0.1070(4) 0.8321(3) 0.2804(3) 0.0387(11) Uani 1 1 d . . . H14 H 0.0517 0.8619 0.2259 0.046 Uiso 1 1 calc R . . C15 C 0.2255(5) 0.8190(4) 0.2642(4) 0.0490(13) Uani 1 1 d . . . H15 H 0.2521 0.8404 0.1981 0.059 Uiso 1 1 calc R . . C16 C 0.3069(4) 0.7756(4) 0.3420(4) 0.0496(13) Uani 1 1 d . . . H16 H 0.3892 0.7651 0.3297 0.060 Uiso 1 1 calc R . . C17 C 0.2692(4) 0.7471(3) 0.4379(3) 0.0434(11) Uani 1 1 d . . . H17 H 0.3255 0.7189 0.4916 0.052 Uiso 1 1 calc R . . C18 C 0.1499(4) 0.7595(3) 0.4558(3) 0.0346(10) Uani 1 1 d . . . H18 H 0.1240 0.7392 0.5219 0.042 Uiso 1 1 calc R . . C19 C -0.1315(4) 0.8737(3) 0.4748(3) 0.0318(10) Uani 1 1 d . . . C20 C -0.1925(4) 0.8332(3) 0.5615(3) 0.0403(11) Uani 1 1 d . . . H20 H -0.2083 0.7655 0.5872 0.048 Uiso 1 1 calc R . . C21 C -0.2306(4) 0.8917(4) 0.6111(3) 0.0495(12) Uani 1 1 d . . . H21 H -0.2733 0.8642 0.6704 0.059 Uiso 1 1 calc R . . C22 C -0.2072(4) 0.9885(4) 0.5752(4) 0.0514(13) Uani 1 1 d . . . H22 H -0.2323 1.0277 0.6101 0.062 Uiso 1 1 calc R . . C23 C -0.1474(4) 1.0289(4) 0.4889(4) 0.0554(14) Uani 1 1 d . . . H23 H -0.1319 1.0967 0.4633 0.066 Uiso 1 1 calc R . . C24 C -0.1095(4) 0.9713(3) 0.4390(3) 0.0434(11) Uani 1 1 d . . . H24 H -0.0678 0.9997 0.3792 0.052 Uiso 1 1 calc R . . C25 C -0.2678(4) 0.9137(4) 0.2630(3) 0.0471(12) Uani 1 1 d . . . C26 C -0.2954(5) 0.9861(5) 0.1625(4) 0.0660(15) Uani 1 1 d . . . C27 C -0.4135(7) 1.0242(6) 0.1334(5) 0.100(2) Uani 1 1 d . . . H27 H -0.4337 1.0705 0.0653 0.120 Uiso 1 1 calc R . . C28 C -0.5041(6) 0.9972(6) 0.2004(7) 0.103(2) Uani 1 1 d . . . H28 H -0.5846 1.0245 0.1780 0.123 Uiso 1 1 calc R . . C29 C -0.4762(5) 0.9316(5) 0.2980(5) 0.0796(18) Uani 1 1 d . . . H29 H -0.5371 0.9144 0.3449 0.095 Uiso 1 1 calc R . . C30 C -0.3602(5) 0.8903(4) 0.3283(4) 0.0561(13) Uani 1 1 d . . . H30 H -0.3420 0.8438 0.3968 0.067 Uiso 1 1 calc R . . C31 C -0.1967(6) 1.0207(5) 0.0880(4) 0.0740(17) Uani 1 1 d . . . H31 H -0.1213 1.0005 0.1273 0.089 Uiso 1 1 calc R . . C32 C -0.1820(7) 0.9604(5) 0.0286(5) 0.118(3) Uani 1 1 d . . . H32A H -0.2562 0.9757 -0.0080 0.177 Uiso 1 1 calc R . . H32B H -0.1618 0.8861 0.0742 0.177 Uiso 1 1 calc R . . H32C H -0.1185 0.9804 -0.0186 0.177 Uiso 1 1 calc R . . C33 C -0.2155(7) 1.1352(5) 0.0196(5) 0.104(2) Uani 1 1 d . . . H33A H -0.1459 1.1511 -0.0213 0.157 Uiso 1 1 calc R . . H33B H -0.2272 1.1726 0.0593 0.157 Uiso 1 1 calc R . . H33C H -0.2856 1.1564 -0.0237 0.157 Uiso 1 1 calc R . . C34 C 0.0240(4) 0.7069(3) 0.8115(3) 0.0321(10) Uani 1 1 d . . . C35 C 0.0472(4) 0.8020(3) 0.7920(3) 0.0429(11) Uani 1 1 d . . . H35 H 0.1213 0.8193 0.7659 0.051 Uiso 1 1 calc R . . C36 C -0.0363(5) 0.8715(4) 0.8101(4) 0.0515(13) Uani 1 1 d . . . H36 H -0.0194 0.9362 0.7973 0.062 Uiso 1 1 calc R . . C37 C -0.1435(5) 0.8477(4) 0.8463(3) 0.0539(13) Uani 1 1 d . . . H37 H -0.2009 0.8956 0.8591 0.065 Uiso 1 1 calc R . . C38 C -0.1684(4) 0.7538(4) 0.8644(3) 0.0486(12) Uani 1 1 d . . . H38 H -0.2433 0.7377 0.8886 0.058 Uiso 1 1 calc R . . C39 C -0.0846(4) 0.6838(3) 0.8475(3) 0.0410(11) Uani 1 1 d . . . H39 H -0.1017 0.6191 0.8606 0.049 Uiso 1 1 calc R . . C40 C 0.2240(4) 0.5497(3) 0.9200(3) 0.0401(11) Uani 1 1 d . . . C41 C 0.3230(4) 0.4723(4) 0.9365(4) 0.0589(14) Uani 1 1 d . . . H41 H 0.3441 0.4496 0.8875 0.071 Uiso 1 1 calc R . . C42 C 0.3913(5) 0.4279(4) 1.0233(4) 0.0687(16) Uani 1 1 d . . . H42 H 0.4589 0.3750 1.0336 0.082 Uiso 1 1 calc R . . C43 C 0.3612(5) 0.4602(5) 1.0949(4) 0.0650(15) Uani 1 1 d . . . H43 H 0.4079 0.4299 1.1547 0.078 Uiso 1 1 calc R . . C44 C 0.2646(5) 0.5353(4) 1.0793(4) 0.0575(14) Uani 1 1 d . . . H44 H 0.2436 0.5572 1.1289 0.069 Uiso 1 1 calc R . . C45 C 0.1962(4) 0.5807(4) 0.9928(3) 0.0439(11) Uani 1 1 d . . . H45 H 0.1291 0.6339 0.9832 0.053 Uiso 1 1 calc R . . C46 C 0.3318(5) 0.6370(5) 0.6921(4) 0.0618(15) Uani 1 1 d . . . C47 C 0.4171(5) 0.7019(6) 0.6617(4) 0.0729(18) Uani 1 1 d . . . C48 C 0.5282(6) 0.6711(7) 0.6308(5) 0.087(2) Uani 1 1 d . . . H48 H 0.5845 0.7149 0.6094 0.105 Uiso 1 1 calc R . . C49 C 0.5545(7) 0.5773(11) 0.6318(7) 0.143(4) Uani 1 1 d . . . H49 H 0.6314 0.5556 0.6133 0.172 Uiso 1 1 calc R . . C50 C 0.4732(8) 0.5109(8) 0.6590(6) 0.128(3) Uani 1 1 d . . . H50 H 0.4937 0.4466 0.6573 0.154 Uiso 1 1 calc R . . C51 C 0.3626(6) 0.5422(6) 0.6883(5) 0.088(2) Uani 1 1 d . . . H51 H 0.3061 0.4988 0.7062 0.106 Uiso 1 1 calc R . . C52 C 0.3879(5) 0.8016(5) 0.6657(4) 0.0771(18) Uani 1 1 d . . . H52 H 0.3010 0.8284 0.6505 0.093 Uiso 1 1 calc R . . C53 C 0.4107(6) 0.7869(5) 0.7660(4) 0.0791(18) Uani 1 1 d . . . H53A H 0.3669 0.7358 0.8143 0.119 Uiso 1 1 calc R . . H53B H 0.3846 0.8528 0.7680 0.119 Uiso 1 1 calc R . . H53C H 0.4956 0.7622 0.7827 0.119 Uiso 1 1 calc R . . C54 C 0.4517(6) 0.8841(6) 0.5885(5) 0.127(3) Uani 1 1 d . . . H54A H 0.5367 0.8639 0.6055 0.191 Uiso 1 1 calc R . . H54B H 0.4202 0.9506 0.5882 0.191 Uiso 1 1 calc R . . H54C H 0.4390 0.8907 0.5223 0.191 Uiso 1 1 calc R . . C1S C 0.335(4) 0.258(3) 0.8412(14) 0.110(15) Uani 0.20 1 d PD . . H1S1 H 0.2588 0.3065 0.8322 0.132 Uiso 0.20 1 calc PR . . H1S2 H 0.3217 0.2036 0.8256 0.132 Uiso 0.20 1 calc PR . . Cl1 Cl 0.4280(19) 0.319(2) 0.7662(19) 0.290(13) Uani 0.20 1 d PD . . Cl2 Cl 0.3809(17) 0.2077(12) 0.9524(14) 0.209(8) Uani 0.20 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.035(2) 0.031(2) 0.028(2) -0.017(2) 0.0092(19) -0.0108(19) N1 0.052(3) 0.041(2) 0.033(2) -0.0184(18) -0.0001(18) -0.0060(19) O1 0.0433(17) 0.0246(15) 0.0273(15) -0.0132(13) 0.0064(13) -0.0150(13) P1 0.0446(7) 0.0291(6) 0.0258(6) -0.0142(5) 0.0052(5) -0.0105(5) C2 0.038(3) 0.032(2) 0.032(2) -0.020(2) 0.010(2) -0.011(2) N2 0.039(2) 0.053(2) 0.038(2) -0.0190(19) 0.0118(18) -0.0142(19) P2 0.0418(7) 0.0332(6) 0.0317(6) -0.0160(5) 0.0068(5) -0.0119(5) C3 0.045(3) 0.040(3) 0.037(3) -0.024(2) 0.004(2) -0.010(2) C4 0.049(3) 0.045(3) 0.051(3) -0.036(3) 0.009(2) -0.015(2) C5 0.050(3) 0.035(3) 0.048(3) -0.028(2) 0.013(2) -0.016(2) C6 0.038(2) 0.029(2) 0.035(2) -0.022(2) 0.015(2) -0.0122(19) C7 0.043(3) 0.025(2) 0.034(2) -0.017(2) 0.012(2) -0.0103(19) C8 0.062(3) 0.028(2) 0.040(3) -0.020(2) 0.013(2) -0.018(2) C9 0.075(4) 0.024(2) 0.035(3) -0.009(2) 0.011(2) -0.015(2) C10 0.055(3) 0.035(3) 0.032(2) -0.013(2) 0.006(2) -0.008(2) C11 0.040(3) 0.028(2) 0.029(2) -0.014(2) 0.0068(19) -0.0075(19) C12 0.039(3) 0.022(2) 0.029(2) -0.0119(19) 0.0087(19) -0.0052(19) C13 0.047(3) 0.019(2) 0.027(2) -0.0135(18) 0.007(2) -0.0105(19) C14 0.057(3) 0.031(2) 0.032(2) -0.016(2) 0.007(2) -0.013(2) C15 0.062(4) 0.053(3) 0.037(3) -0.023(2) 0.021(3) -0.023(3) C16 0.045(3) 0.058(3) 0.060(3) -0.038(3) 0.020(3) -0.020(3) C17 0.050(3) 0.044(3) 0.047(3) -0.027(2) 0.005(2) -0.017(2) C18 0.050(3) 0.029(2) 0.030(2) -0.016(2) 0.010(2) -0.017(2) C19 0.037(2) 0.030(2) 0.031(2) -0.017(2) 0.0006(19) -0.0048(19) C20 0.048(3) 0.039(3) 0.035(3) -0.019(2) 0.005(2) -0.006(2) C21 0.055(3) 0.059(3) 0.037(3) -0.027(3) 0.008(2) -0.005(3) C22 0.056(3) 0.053(3) 0.058(3) -0.041(3) -0.001(3) 0.001(3) C23 0.065(4) 0.047(3) 0.072(4) -0.041(3) 0.006(3) -0.014(3) C24 0.049(3) 0.039(3) 0.050(3) -0.027(2) 0.013(2) -0.015(2) C25 0.052(3) 0.054(3) 0.042(3) -0.029(3) -0.006(3) -0.007(3) C26 0.057(4) 0.085(4) 0.052(4) -0.031(3) -0.015(3) 0.001(3) C27 0.078(5) 0.137(7) 0.068(4) -0.040(5) -0.023(4) 0.004(5) C28 0.049(4) 0.143(7) 0.121(7) -0.071(6) -0.025(4) 0.004(4) C29 0.056(4) 0.114(5) 0.087(5) -0.060(4) 0.000(4) -0.019(4) C30 0.052(3) 0.067(4) 0.059(3) -0.036(3) 0.003(3) -0.014(3) C31 0.082(4) 0.077(4) 0.036(3) -0.011(3) -0.008(3) 0.005(3) C32 0.167(8) 0.075(5) 0.110(6) -0.050(5) 0.054(5) -0.017(5) C33 0.156(7) 0.092(5) 0.065(4) -0.034(4) 0.011(4) -0.030(5) C34 0.042(3) 0.030(2) 0.024(2) -0.0107(19) 0.0011(19) -0.011(2) C35 0.052(3) 0.037(3) 0.041(3) -0.018(2) 0.001(2) -0.011(2) C36 0.065(4) 0.040(3) 0.058(3) -0.030(3) -0.006(3) -0.004(3) C37 0.066(4) 0.053(3) 0.044(3) -0.030(3) -0.004(3) 0.008(3) C38 0.045(3) 0.057(3) 0.037(3) -0.019(2) 0.008(2) -0.004(2) C39 0.047(3) 0.041(3) 0.035(3) -0.017(2) 0.007(2) -0.012(2) C40 0.039(3) 0.044(3) 0.040(3) -0.021(2) 0.005(2) -0.010(2) C41 0.051(3) 0.073(4) 0.062(4) -0.042(3) -0.002(3) -0.003(3) C42 0.054(4) 0.068(4) 0.077(4) -0.032(3) -0.017(3) 0.005(3) C43 0.066(4) 0.076(4) 0.052(3) -0.027(3) -0.016(3) -0.012(3) C44 0.062(4) 0.068(4) 0.045(3) -0.029(3) -0.005(3) -0.011(3) C45 0.051(3) 0.046(3) 0.036(3) -0.019(2) 0.003(2) -0.012(2) C46 0.061(4) 0.086(4) 0.046(3) -0.039(3) 0.007(3) -0.011(3) C47 0.050(4) 0.123(6) 0.045(3) -0.037(4) 0.004(3) -0.024(4) C48 0.051(4) 0.157(7) 0.072(4) -0.069(5) 0.016(3) -0.021(4) C49 0.051(5) 0.275(14) 0.137(8) -0.134(9) 0.022(5) -0.011(7) C50 0.093(6) 0.194(10) 0.139(7) -0.131(7) 0.009(6) 0.018(6) C51 0.081(5) 0.119(6) 0.084(5) -0.070(4) 0.008(4) -0.001(4) C52 0.063(4) 0.077(4) 0.073(4) -0.013(4) 0.001(3) -0.028(3) C53 0.093(5) 0.065(4) 0.079(4) -0.031(3) -0.026(4) -0.012(3) C54 0.088(5) 0.166(8) 0.087(5) -0.001(5) -0.001(4) -0.081(5) C1S 0.19(4) 0.15(3) 0.034(16) -0.029(18) 0.000(19) -0.14(3) Cl1 0.24(2) 0.47(4) 0.36(3) -0.37(3) 0.10(2) -0.09(2) Cl2 0.26(2) 0.147(13) 0.226(18) -0.108(13) -0.048(15) 0.023(12) _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 C1 C2 1.378(5) . ? C1 O1 1.388(4) . ? C1 C6 1.396(5) . ? N1 C25 1.380(6) . ? N1 P1 1.560(4) . ? O1 C12 1.390(4) . ? P1 C13 1.801(4) . ? P1 C19 1.804(4) . ? P1 C2 1.821(4) . ? C2 C3 1.397(5) . ? N2 C46 1.380(6) . ? N2 P2 1.542(3) . ? P2 C34 1.794(4) . ? P2 C11 1.812(4) . ? P2 C40 1.813(5) . ? C3 C4 1.393(6) . ? C3 H3 0.9500 . ? C4 C5 1.367(6) . ? C4 H4 0.9500 . ? C5 C6 1.387(6) . ? C5 H5 0.9500 . ? C6 C7 1.434(6) . ? C7 C8 1.392(6) . ? C7 C12 1.399(5) . ? C8 C9 1.366(6) . ? C8 H8 0.9500 . ? C9 C10 1.389(6) . ? C9 H9 0.9500 . ? C10 C11 1.400(6) . ? C10 H10 0.9500 . ? C11 C12 1.378(6) . ? C13 C18 1.391(6) . ? C13 C14 1.398(5) . ? C14 C15 1.363(6) . ? C14 H14 0.9500 . ? C15 C16 1.371(7) . ? C15 H15 0.9500 . ? C16 C17 1.380(6) . ? C16 H16 0.9500 . ? C17 C18 1.378(6) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.369(5) . ? C19 C20 1.378(5) . ? C20 C21 1.388(6) . ? C20 H20 0.9500 . ? C21 C22 1.364(6) . ? C21 H21 0.9500 . ? C22 C23 1.367(7) . ? C22 H22 0.9500 . ? C23 C24 1.380(6) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.389(7) . ? C25 C26 1.409(7) . ? C26 C27 1.380(8) . ? C26 C31 1.539(8) . ? C27 C28 1.391(9) . ? C27 H27 0.9500 . ? C28 C29 1.356(9) . ? C28 H28 0.9500 . ? C29 C30 1.366(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C33 1.505(8) . ? C31 C32 1.523(8) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C39 1.378(6) . ? C34 C35 1.386(6) . ? C35 C36 1.376(6) . ? C35 H35 0.9500 . ? C36 C37 1.366(7) . ? C36 H36 0.9500 . ? C37 C38 1.383(7) . ? C37 H37 0.9500 . ? C38 C39 1.374(6) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.380(6) . ? C40 C41 1.387(6) . ? C41 C42 1.381(7) . ? C41 H41 0.9500 . ? C42 C43 1.378(7) . ? C42 H42 0.9500 . ? C43 C44 1.352(7) . ? C43 H43 0.9500 . ? C44 C45 1.378(6) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C51 1.411(8) . ? C46 C47 1.426(8) . ? C47 C48 1.397(8) . ? C47 C52 1.482(8) . ? C48 C49 1.360(12) . ? C48 H48 0.9500 . ? C49 C50 1.407(12) . ? C49 H49 0.9500 . ? C50 C51 1.384(9) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C53 1.467(8) . ? C52 C54 1.531(8) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C1S Cl2 1.57(2) . ? C1S Cl1 1.59(2) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? 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 C2 C1 O1 125.6(3) . . ? C2 C1 C6 123.8(4) . . ? O1 C1 C6 110.5(3) . . ? C25 N1 P1 129.1(3) . . ? C1 O1 C12 106.4(3) . . ? N1 P1 C13 105.63(19) . . ? N1 P1 C19 114.85(19) . . ? C13 P1 C19 108.89(18) . . ? N1 P1 C2 114.38(19) . . ? C13 P1 C2 106.14(18) . . ? C19 P1 C2 106.53(18) . . ? C1 C2 C3 115.1(4) . . ? C1 C2 P1 128.3(3) . . ? C3 C2 P1 116.5(3) . . ? C46 N2 P2 127.5(4) . . ? N2 P2 C34 108.30(19) . . ? N2 P2 C11 117.81(19) . . ? C34 P2 C11 105.77(19) . . ? N2 P2 C40 113.3(2) . . ? C34 P2 C40 105.37(19) . . ? C11 P2 C40 105.3(2) . . ? C4 C3 C2 122.4(4) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C5 C4 C3 120.8(4) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 118.8(4) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C5 C6 C1 119.2(4) . . ? C5 C6 C7 134.5(4) . . ? C1 C6 C7 106.3(3) . . ? C8 C7 C12 118.4(4) . . ? C8 C7 C6 135.0(4) . . ? C12 C7 C6 106.6(3) . . ? C9 C8 C7 118.6(4) . . ? C9 C8 H8 120.7 . . ? C7 C8 H8 120.7 . . ? C8 C9 C10 121.4(4) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C9 C10 C11 122.3(4) . . ? C9 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C12 C11 C10 114.4(4) . . ? C12 C11 P2 123.7(3) . . ? C10 C11 P2 121.9(3) . . ? C11 C12 O1 125.0(3) . . ? C11 C12 C7 124.8(4) . . ? O1 C12 C7 110.2(3) . . ? C18 C13 C14 119.0(4) . . ? C18 C13 P1 122.4(3) . . ? C14 C13 P1 118.6(3) . . ? C15 C14 C13 119.9(4) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 121.0(4) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C17 120.0(4) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 119.9(4) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C13 120.3(4) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? C24 C19 C20 119.3(4) . . ? C24 C19 P1 116.1(3) . . ? C20 C19 P1 124.2(3) . . ? C19 C20 C21 119.7(4) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 120.5(4) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 119.8(4) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C22 C23 C24 120.0(4) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C19 C24 C23 120.7(4) . . ? C19 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? N1 C25 C30 124.2(4) . . ? N1 C25 C26 117.5(4) . . ? C30 C25 C26 118.3(5) . . ? C27 C26 C25 117.7(6) . . ? C27 C26 C31 121.4(5) . . ? C25 C26 C31 120.8(5) . . ? C26 C27 C28 122.4(6) . . ? C26 C27 H27 118.8 . . ? C28 C27 H27 118.8 . . ? C29 C28 C27 119.3(6) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C28 C29 C30 119.6(6) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C29 C30 C25 122.5(5) . . ? C29 C30 H30 118.7 . . ? C25 C30 H30 118.7 . . ? C33 C31 C32 110.8(5) . . ? C33 C31 C26 114.9(5) . . ? C32 C31 C26 108.1(5) . . ? C33 C31 H31 107.6 . . ? C32 C31 H31 107.6 . . ? C26 C31 H31 107.6 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C39 C34 C35 119.1(4) . . ? C39 C34 P2 122.9(3) . . ? C35 C34 P2 117.7(3) . . ? C36 C35 C34 120.4(4) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C37 C36 C35 120.1(5) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 120.0(5) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C39 C38 C37 120.0(5) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C34 120.4(4) . . ? C38 C39 H39 119.8 . . ? C34 C39 H39 119.8 . . ? C45 C40 C41 117.9(4) . . ? C45 C40 P2 121.9(4) . . ? C41 C40 P2 119.9(3) . . ? C42 C41 C40 120.9(5) . . ? C42 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C43 C42 C41 120.0(5) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C44 C43 C42 119.4(5) . . ? C44 C43 H43 120.3 . . ? C42 C43 H43 120.3 . . ? C43 C44 C45 121.2(5) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? C44 C45 C40 120.6(5) . . ? C44 C45 H45 119.7 . . ? C40 C45 H45 119.7 . . ? N2 C46 C51 121.6(5) . . ? N2 C46 C47 119.9(5) . . ? C51 C46 C47 118.0(6) . . ? C48 C47 C46 120.6(7) . . ? C48 C47 C52 120.1(6) . . ? C46 C47 C52 119.3(5) . . ? C49 C48 C47 118.9(7) . . ? C49 C48 H48 120.6 . . ? C47 C48 H48 120.6 . . ? C48 C49 C50 123.1(7) . . ? C48 C49 H49 118.5 . . ? C50 C49 H49 118.5 . . ? C51 C50 C49 117.9(8) . . ? C51 C50 H50 121.0 . . ? C49 C50 H50 121.0 . . ? C50 C51 C46 121.5(7) . . ? C50 C51 H51 119.3 . . ? C46 C51 H51 119.3 . . ? C53 C52 C47 111.1(5) . . ? C53 C52 C54 110.3(6) . . ? C47 C52 C54 113.5(6) . . ? C53 C52 H52 107.2 . . ? C47 C52 H52 107.2 . . ? C54 C52 H52 107.2 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? Cl2 C1S Cl1 111(2) . . ? Cl2 C1S H1S1 109.3 . . ? Cl1 C1S H1S1 109.3 . . ? Cl2 C1S H1S2 109.3 . . ? Cl1 C1S H1S2 109.3 . . ? H1S1 C1S H1S2 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C1 O1 C12 179.5(4) . . . . ? C6 C1 O1 C12 0.2(4) . . . . ? C25 N1 P1 C13 -168.4(4) . . . . ? C25 N1 P1 C19 -48.4(4) . . . . ? C25 N1 P1 C2 75.2(4) . . . . ? O1 C1 C2 C3 179.3(3) . . . . ? C6 C1 C2 C3 -1.4(6) . . . . ? O1 C1 C2 P1 2.6(6) . . . . ? C6 C1 C2 P1 -178.1(3) . . . . ? N1 P1 C2 C1 -179.8(3) . . . . ? C13 P1 C2 C1 64.1(4) . . . . ? C19 P1 C2 C1 -51.8(4) . . . . ? N1 P1 C2 C3 3.5(4) . . . . ? C13 P1 C2 C3 -112.5(3) . . . . ? C19 P1 C2 C3 131.5(3) . . . . ? C46 N2 P2 C34 163.4(4) . . . . ? C46 N2 P2 C11 -76.7(5) . . . . ? C46 N2 P2 C40 46.9(5) . . . . ? C1 C2 C3 C4 1.0(6) . . . . ? P1 C2 C3 C4 178.1(3) . . . . ? C2 C3 C4 C5 -0.1(6) . . . . ? C3 C4 C5 C6 -0.5(6) . . . . ? C4 C5 C6 C1 0.2(6) . . . . ? C4 C5 C6 C7 -179.2(4) . . . . ? C2 C1 C6 C5 0.9(6) . . . . ? O1 C1 C6 C5 -179.8(3) . . . . ? C2 C1 C6 C7 -179.6(4) . . . . ? O1 C1 C6 C7 -0.2(4) . . . . ? C5 C6 C7 C8 -0.1(8) . . . . ? C1 C6 C7 C8 -179.5(4) . . . . ? C5 C6 C7 C12 179.6(4) . . . . ? C1 C6 C7 C12 0.2(4) . . . . ? C12 C7 C8 C9 0.6(6) . . . . ? C6 C7 C8 C9 -179.7(4) . . . . ? C7 C8 C9 C10 0.3(7) . . . . ? C8 C9 C10 C11 -1.0(7) . . . . ? C9 C10 C11 C12 0.7(6) . . . . ? C9 C10 C11 P2 -177.5(3) . . . . ? N2 P2 C11 C12 -46.8(4) . . . . ? C34 P2 C11 C12 74.4(4) . . . . ? C40 P2 C11 C12 -174.3(3) . . . . ? N2 P2 C11 C10 131.2(3) . . . . ? C34 P2 C11 C10 -107.6(4) . . . . ? C40 P2 C11 C10 3.7(4) . . . . ? C10 C11 C12 O1 179.6(3) . . . . ? P2 C11 C12 O1 -2.3(6) . . . . ? C10 C11 C12 C7 0.2(6) . . . . ? P2 C11 C12 C7 178.4(3) . . . . ? C1 O1 C12 C11 -179.5(4) . . . . ? C1 O1 C12 C7 -0.1(4) . . . . ? C8 C7 C12 C11 -0.9(6) . . . . ? C6 C7 C12 C11 179.4(4) . . . . ? C8 C7 C12 O1 179.7(3) . . . . ? C6 C7 C12 O1 -0.1(4) . . . . ? N1 P1 C13 C18 175.1(3) . . . . ? C19 P1 C13 C18 51.3(4) . . . . ? C2 P1 C13 C18 -63.1(3) . . . . ? N1 P1 C13 C14 -8.4(3) . . . . ? C19 P1 C13 C14 -132.2(3) . . . . ? C2 P1 C13 C14 113.4(3) . . . . ? C18 C13 C14 C15 0.9(6) . . . . ? P1 C13 C14 C15 -175.7(3) . . . . ? C13 C14 C15 C16 0.4(6) . . . . ? C14 C15 C16 C17 -1.9(7) . . . . ? C15 C16 C17 C18 2.0(7) . . . . ? C16 C17 C18 C13 -0.6(6) . . . . ? C14 C13 C18 C17 -0.8(6) . . . . ? P1 C13 C18 C17 175.6(3) . . . . ? N1 P1 C19 C24 -58.5(4) . . . . ? C13 P1 C19 C24 59.7(4) . . . . ? C2 P1 C19 C24 173.8(3) . . . . ? N1 P1 C19 C20 115.4(4) . . . . ? C13 P1 C19 C20 -126.5(4) . . . . ? C2 P1 C19 C20 -12.4(4) . . . . ? C24 C19 C20 C21 0.0(7) . . . . ? P1 C19 C20 C21 -173.6(3) . . . . ? C19 C20 C21 C22 -0.7(7) . . . . ? C20 C21 C22 C23 1.1(7) . . . . ? C21 C22 C23 C24 -0.8(8) . . . . ? C20 C19 C24 C23 0.2(7) . . . . ? P1 C19 C24 C23 174.4(4) . . . . ? C22 C23 C24 C19 0.2(8) . . . . ? P1 N1 C25 C30 -15.6(7) . . . . ? P1 N1 C25 C26 163.7(4) . . . . ? N1 C25 C26 C27 176.2(5) . . . . ? C30 C25 C26 C27 -4.4(8) . . . . ? N1 C25 C26 C31 -3.5(7) . . . . ? C30 C25 C26 C31 175.9(5) . . . . ? C25 C26 C27 C28 3.0(11) . . . . ? C31 C26 C27 C28 -177.2(7) . . . . ? C26 C27 C28 C29 0.3(12) . . . . ? C27 C28 C29 C30 -2.2(11) . . . . ? C28 C29 C30 C25 0.7(9) . . . . ? N1 C25 C30 C29 -178.0(5) . . . . ? C26 C25 C30 C29 2.7(8) . . . . ? C27 C26 C31 C33 44.2(9) . . . . ? C25 C26 C31 C33 -136.1(6) . . . . ? C27 C26 C31 C32 -80.2(8) . . . . ? C25 C26 C31 C32 99.6(6) . . . . ? N2 P2 C34 C39 149.5(3) . . . . ? C11 P2 C34 C39 22.4(4) . . . . ? C40 P2 C34 C39 -88.9(4) . . . . ? N2 P2 C34 C35 -37.3(4) . . . . ? C11 P2 C34 C35 -164.4(3) . . . . ? C40 P2 C34 C35 84.3(3) . . . . ? C39 C34 C35 C36 1.2(6) . . . . ? P2 C34 C35 C36 -172.2(3) . . . . ? C34 C35 C36 C37 -0.8(7) . . . . ? C35 C36 C37 C38 -0.3(7) . . . . ? C36 C37 C38 C39 1.0(7) . . . . ? C37 C38 C39 C34 -0.6(7) . . . . ? C35 C34 C39 C38 -0.5(6) . . . . ? P2 C34 C39 C38 172.6(3) . . . . ? N2 P2 C40 C45 112.6(4) . . . . ? C34 P2 C40 C45 -5.6(4) . . . . ? C11 P2 C40 C45 -117.2(4) . . . . ? N2 P2 C40 C41 -61.9(4) . . . . ? C34 P2 C40 C41 179.9(4) . . . . ? C11 P2 C40 C41 68.3(4) . . . . ? C45 C40 C41 C42 0.0(7) . . . . ? P2 C40 C41 C42 174.7(4) . . . . ? C40 C41 C42 C43 0.1(8) . . . . ? C41 C42 C43 C44 0.1(9) . . . . ? C42 C43 C44 C45 -0.5(8) . . . . ? C43 C44 C45 C40 0.6(8) . . . . ? C41 C40 C45 C44 -0.4(7) . . . . ? P2 C40 C45 C44 -175.0(4) . . . . ? P2 N2 C46 C51 52.0(7) . . . . ? P2 N2 C46 C47 -136.0(4) . . . . ? N2 C46 C47 C48 -173.3(5) . . . . ? C51 C46 C47 C48 -1.0(8) . . . . ? N2 C46 C47 C52 8.2(8) . . . . ? C51 C46 C47 C52 -179.5(5) . . . . ? C46 C47 C48 C49 -1.2(10) . . . . ? C52 C47 C48 C49 177.3(7) . . . . ? C47 C48 C49 C50 2.5(13) . . . . ? C48 C49 C50 C51 -1.6(14) . . . . ? C49 C50 C51 C46 -0.7(11) . . . . ? N2 C46 C51 C50 174.1(6) . . . . ? C47 C46 C51 C50 2.0(9) . . . . ? C48 C47 C52 C53 -94.9(7) . . . . ? C46 C47 C52 C53 83.5(7) . . . . ? C48 C47 C52 C54 30.1(8) . . . . ? C46 C47 C52 C54 -151.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.690 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.058 #===END data_L2 _database_code_depnum_ccdc_archive 'CCDC 833324' #TrackingRef '6184_web_deposit_cif_file_0_PaulG.Hayes_ #1310063407.Chem Eur J_AllCifs - Paul G Hayes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H40 N2 O P2' _chemical_formula_weight 746.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.0198(9) _cell_length_b 14.0045(7) _cell_length_c 16.7584(9) _cell_angle_alpha 90.00 _cell_angle_beta 109.6460(10) _cell_angle_gamma 90.00 _cell_volume 3982.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9867 _cell_measurement_theta_min 4.907 _cell_measurement_theta_max 54.844 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.150 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6705 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37535 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7010 _reflns_number_gt 5933 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0517P)^2^+1.5405P] 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 7010 _refine_ls_number_parameters 498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 0.12823(2) 0.56689(3) 0.41148(3) 0.02685(12) Uani 1 1 d . . . O1 O 0.27128(6) 0.40202(8) 0.47529(7) 0.0300(3) Uani 1 1 d . . . N1 N 0.05853(8) 0.63017(10) 0.41677(9) 0.0327(3) Uani 1 1 d . . . C1 C 0.24992(10) 0.45604(12) 0.53360(10) 0.0281(4) Uani 1 1 d . . . P2 P 0.35112(3) 0.22718(4) 0.38816(3) 0.03598(13) Uani 1 1 d . . . C2 C 0.18864(9) 0.52175(11) 0.51493(10) 0.0274(3) Uani 1 1 d . . . N2 N 0.42031(9) 0.16444(12) 0.37878(9) 0.0426(4) Uani 1 1 d . . . C3 C 0.17504(11) 0.56100(12) 0.58537(11) 0.0338(4) Uani 1 1 d . . . H3 H 0.1325 0.6044 0.5763 0.041 Uiso 1 1 calc R . . C4 C 0.22108(12) 0.53937(13) 0.66830(11) 0.0382(4) Uani 1 1 d . . . H4 H 0.2084 0.5664 0.7141 0.046 Uiso 1 1 calc R . . C5 C 0.28457(11) 0.47936(13) 0.68451(11) 0.0372(4) Uani 1 1 d . . . H5 H 0.3178 0.4671 0.7410 0.045 Uiso 1 1 calc R . . C6 C 0.29898(10) 0.43679(12) 0.61605(10) 0.0323(4) Uani 1 1 d . . . C7 C 0.35666(11) 0.37002(14) 0.60877(11) 0.0382(4) Uani 1 1 d . . . C8 C 0.42148(12) 0.32636(17) 0.66785(12) 0.0513(5) Uani 1 1 d . . . H8 H 0.4355 0.3403 0.7266 0.062 Uiso 1 1 calc R . . C9 C 0.46456(13) 0.26261(19) 0.63892(13) 0.0602(6) Uani 1 1 d . . . H9 H 0.5099 0.2335 0.6779 0.072 Uiso 1 1 calc R . . C10 C 0.44266(12) 0.24036(17) 0.55361(12) 0.0521(6) Uani 1 1 d . . . H10 H 0.4730 0.1949 0.5359 0.063 Uiso 1 1 calc R . . C11 C 0.37728(11) 0.28228(14) 0.49213(11) 0.0393(4) Uani 1 1 d . . . C12 C 0.33670(10) 0.34899(13) 0.52298(10) 0.0339(4) Uani 1 1 d . . . C13 C 0.08295(9) 0.46813(12) 0.34434(10) 0.0297(4) Uani 1 1 d . . . C14 C 0.11046(11) 0.43215(13) 0.28282(12) 0.0392(4) Uani 1 1 d . . . H14 H 0.1568 0.4578 0.2762 0.047 Uiso 1 1 calc R . . C15 C 0.07036(12) 0.35855(15) 0.23075(12) 0.0452(5) Uani 1 1 d . . . H15 H 0.0883 0.3356 0.1870 0.054 Uiso 1 1 calc R . . C16 C 0.00513(12) 0.31863(14) 0.24185(12) 0.0448(5) Uani 1 1 d . . . H16 H -0.0218 0.2677 0.2064 0.054 Uiso 1 1 calc R . . C17 C -0.02125(13) 0.35258(16) 0.30451(14) 0.0561(6) Uani 1 1 d . . . H17 H -0.0656 0.3238 0.3134 0.067 Uiso 1 1 calc R . . C18 C 0.01633(12) 0.42817(15) 0.35453(13) 0.0482(5) Uani 1 1 d . . . H18 H -0.0035 0.4530 0.3962 0.058 Uiso 1 1 calc R . . C19 C 0.19695(10) 0.62312(12) 0.36799(10) 0.0293(4) Uani 1 1 d . . . C20 C 0.27409(10) 0.64408(13) 0.41795(11) 0.0368(4) Uani 1 1 d . . . H20 H 0.2945 0.6198 0.4741 0.044 Uiso 1 1 calc R . . C21 C 0.32128(12) 0.70004(15) 0.38646(13) 0.0454(5) Uani 1 1 d . . . H21 H 0.3737 0.7145 0.4212 0.054 Uiso 1 1 calc R . . C22 C 0.29236(12) 0.73486(14) 0.30480(13) 0.0446(5) Uani 1 1 d . . . H22 H 0.3245 0.7740 0.2836 0.054 Uiso 1 1 calc R . . C23 C 0.21671(12) 0.71271(13) 0.25414(12) 0.0417(4) Uani 1 1 d . . . H23 H 0.1973 0.7351 0.1973 0.050 Uiso 1 1 calc R . . C24 C 0.16887(11) 0.65808(13) 0.28553(11) 0.0361(4) Uani 1 1 d . . . H24 H 0.1164 0.6443 0.2505 0.043 Uiso 1 1 calc R . . C25 C 0.05784(10) 0.71581(12) 0.45841(10) 0.0318(4) Uani 1 1 d . . . C26 C 0.12175(12) 0.77769(13) 0.48877(12) 0.0440(5) Uani 1 1 d . . . H26 H 0.1702 0.7620 0.4811 0.053 Uiso 1 1 calc R . . C27 C 0.11583(15) 0.86140(15) 0.52974(14) 0.0565(6) Uani 1 1 d . . . H27 H 0.1602 0.9024 0.5502 0.068 Uiso 1 1 calc R . . C28 C 0.04600(16) 0.88596(15) 0.54123(13) 0.0593(6) Uani 1 1 d . . . H28 H 0.0420 0.9432 0.5699 0.071 Uiso 1 1 calc R . . C29 C -0.01774(14) 0.82598(15) 0.51043(13) 0.0520(5) Uani 1 1 d . . . H29 H -0.0661 0.8432 0.5176 0.062 Uiso 1 1 calc R . . C30 C -0.01372(11) 0.74138(13) 0.46929(11) 0.0380(4) Uani 1 1 d . . . C31 C -0.08326(12) 0.67652(16) 0.43628(16) 0.0555(6) Uani 1 1 d . . . H31A H -0.1258 0.6990 0.4557 0.083 Uiso 1 1 calc R . . H31B H -0.0681 0.6116 0.4573 0.083 Uiso 1 1 calc R . . H31C H -0.1015 0.6764 0.3742 0.083 Uiso 1 1 calc R . . C32 C 0.27186(12) 0.14591(14) 0.38181(11) 0.0403(4) Uani 1 1 d . . . C33 C 0.19433(13) 0.17633(16) 0.35730(14) 0.0521(5) Uani 1 1 d . . . H33 H 0.1821 0.2416 0.3437 0.063 Uiso 1 1 calc R . . C34 C 0.13459(15) 0.11240(18) 0.35245(16) 0.0638(6) Uani 1 1 d . . . H34 H 0.0814 0.1334 0.3349 0.077 Uiso 1 1 calc R . . C35 C 0.15277(17) 0.01749(19) 0.37331(15) 0.0660(7) Uani 1 1 d . . . H35 H 0.1120 -0.0270 0.3697 0.079 Uiso 1 1 calc R . . C36 C 0.22990(17) -0.01215(17) 0.39927(15) 0.0649(7) Uani 1 1 d . . . H36 H 0.2422 -0.0770 0.4147 0.078 Uiso 1 1 calc R . . C37 C 0.28946(14) 0.05076(15) 0.40324(13) 0.0515(5) Uani 1 1 d . . . H37 H 0.3425 0.0293 0.4206 0.062 Uiso 1 1 calc R . . C38 C 0.31219(10) 0.31689(13) 0.30743(10) 0.0330(4) Uani 1 1 d . . . C39 C 0.27233(11) 0.28471(14) 0.22567(12) 0.0415(4) Uani 1 1 d . . . H39 H 0.2595 0.2189 0.2160 0.050 Uiso 1 1 calc R . . C40 C 0.25131(12) 0.34767(16) 0.15857(13) 0.0511(5) Uani 1 1 d . . . H40 H 0.2242 0.3253 0.1028 0.061 Uiso 1 1 calc R . . C41 C 0.26958(12) 0.44252(16) 0.17239(14) 0.0522(5) Uani 1 1 d . . . H41 H 0.2549 0.4858 0.1260 0.063 Uiso 1 1 calc R . . C42 C 0.30901(12) 0.47578(15) 0.25283(14) 0.0482(5) Uani 1 1 d . . . H42 H 0.3216 0.5417 0.2618 0.058 Uiso 1 1 calc R . . C43 C 0.33037(11) 0.41291(13) 0.32083(12) 0.0398(4) Uani 1 1 d . . . H43 H 0.3574 0.4357 0.3764 0.048 Uiso 1 1 calc R . . C44 C 0.49490(11) 0.19841(16) 0.38174(11) 0.0433(5) Uani 1 1 d . . . C45 C 0.51480(12) 0.29330(17) 0.37882(13) 0.0507(5) Uani 1 1 d . . . H45 H 0.4770 0.3410 0.3779 0.061 Uiso 1 1 calc R . . C46 C 0.58831(13) 0.3214(2) 0.37714(14) 0.0635(7) Uani 1 1 d . . . H46 H 0.5997 0.3872 0.3738 0.076 Uiso 1 1 calc R . . C47 C 0.64397(14) 0.2544(3) 0.38024(15) 0.0743(8) Uani 1 1 d . . . H47 H 0.6945 0.2728 0.3795 0.089 Uiso 1 1 calc R . . C48 C 0.62587(13) 0.1595(2) 0.38452(15) 0.0702(8) Uani 1 1 d . . . H48 H 0.6651 0.1130 0.3875 0.084 Uiso 1 1 calc R . . C49 C 0.55240(13) 0.12878(19) 0.38459(13) 0.0571(6) Uani 1 1 d . . . C50 C 0.53242(17) 0.0255(2) 0.38541(19) 0.0810(8) Uani 1 1 d . . . H50A H 0.5787 -0.0132 0.3889 0.122 Uiso 1 1 calc R . . H50B H 0.4892 0.0097 0.3333 0.122 Uiso 1 1 calc R . . H50C H 0.5162 0.0122 0.4345 0.122 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 0.0271(2) 0.0272(2) 0.0255(2) -0.00259(17) 0.00795(17) -0.00083(17) O1 0.0297(6) 0.0376(6) 0.0221(6) 0.0004(5) 0.0079(5) 0.0051(5) N1 0.0304(8) 0.0313(8) 0.0358(8) -0.0043(6) 0.0103(6) 0.0003(6) C1 0.0320(9) 0.0306(9) 0.0237(8) -0.0012(6) 0.0118(7) -0.0045(7) P2 0.0391(3) 0.0412(3) 0.0302(2) 0.00703(19) 0.0150(2) 0.0136(2) C2 0.0304(8) 0.0273(8) 0.0255(8) -0.0009(7) 0.0105(7) -0.0049(7) N2 0.0479(10) 0.0484(10) 0.0347(8) 0.0079(7) 0.0183(7) 0.0176(8) C3 0.0433(10) 0.0292(9) 0.0320(9) -0.0023(7) 0.0167(8) -0.0005(8) C4 0.0583(12) 0.0330(10) 0.0275(9) -0.0036(7) 0.0199(8) -0.0013(9) C5 0.0494(11) 0.0393(10) 0.0221(8) -0.0006(7) 0.0111(8) -0.0062(8) C6 0.0347(9) 0.0354(9) 0.0264(9) 0.0010(7) 0.0100(7) -0.0023(7) C7 0.0373(10) 0.0512(11) 0.0257(9) 0.0048(8) 0.0102(7) 0.0050(8) C8 0.0448(11) 0.0799(16) 0.0253(9) 0.0077(10) 0.0067(8) 0.0146(11) C9 0.0470(12) 0.0961(18) 0.0340(11) 0.0170(11) 0.0087(9) 0.0316(12) C10 0.0463(12) 0.0757(15) 0.0354(10) 0.0132(10) 0.0150(9) 0.0281(11) C11 0.0383(10) 0.0524(12) 0.0281(9) 0.0071(8) 0.0126(8) 0.0128(9) C12 0.0302(9) 0.0442(10) 0.0260(8) 0.0072(7) 0.0077(7) 0.0076(8) C13 0.0293(9) 0.0300(9) 0.0264(8) -0.0023(7) 0.0048(7) 0.0002(7) C14 0.0357(10) 0.0432(11) 0.0397(10) -0.0102(8) 0.0141(8) -0.0023(8) C15 0.0469(11) 0.0492(12) 0.0388(10) -0.0158(9) 0.0134(9) -0.0015(9) C16 0.0457(11) 0.0419(11) 0.0395(10) -0.0136(9) 0.0045(9) -0.0066(9) C17 0.0564(13) 0.0561(13) 0.0623(14) -0.0233(11) 0.0287(11) -0.0259(11) C18 0.0552(12) 0.0493(12) 0.0492(12) -0.0202(9) 0.0296(10) -0.0190(10) C19 0.0312(9) 0.0269(8) 0.0300(9) 0.0000(7) 0.0108(7) -0.0001(7) C20 0.0379(10) 0.0410(10) 0.0297(9) 0.0021(8) 0.0091(8) -0.0064(8) C21 0.0398(11) 0.0510(12) 0.0442(11) 0.0002(9) 0.0125(9) -0.0116(9) C22 0.0515(12) 0.0400(11) 0.0484(12) 0.0071(9) 0.0250(10) -0.0052(9) C23 0.0496(11) 0.0406(10) 0.0370(10) 0.0123(8) 0.0174(9) 0.0067(9) C24 0.0351(9) 0.0387(10) 0.0325(9) 0.0039(8) 0.0088(8) 0.0042(8) C25 0.0395(10) 0.0280(9) 0.0261(8) 0.0026(7) 0.0086(7) 0.0040(7) C26 0.0432(11) 0.0363(10) 0.0471(11) -0.0047(9) 0.0082(9) -0.0015(8) C27 0.0688(15) 0.0346(11) 0.0508(13) -0.0068(9) 0.0000(11) -0.0052(10) C28 0.0928(18) 0.0348(11) 0.0416(12) -0.0052(9) 0.0114(12) 0.0182(12) C29 0.0682(15) 0.0443(12) 0.0478(12) 0.0028(10) 0.0250(11) 0.0193(11) C30 0.0459(11) 0.0348(10) 0.0360(10) 0.0067(8) 0.0176(8) 0.0072(8) C31 0.0458(12) 0.0499(12) 0.0823(16) 0.0039(11) 0.0366(12) 0.0045(10) C32 0.0510(11) 0.0418(11) 0.0333(9) 0.0058(8) 0.0213(9) 0.0082(9) C33 0.0547(13) 0.0487(12) 0.0606(13) 0.0104(10) 0.0294(11) 0.0026(10) C34 0.0604(14) 0.0688(16) 0.0694(16) 0.0091(13) 0.0311(13) -0.0024(12) C35 0.0841(18) 0.0642(16) 0.0587(14) -0.0018(12) 0.0357(13) -0.0241(14) C36 0.094(2) 0.0466(13) 0.0622(15) 0.0058(11) 0.0378(14) 0.0018(13) C37 0.0675(14) 0.0442(12) 0.0488(12) 0.0097(9) 0.0275(11) 0.0083(10) C38 0.0306(9) 0.0401(10) 0.0309(9) 0.0065(7) 0.0137(7) 0.0099(7) C39 0.0433(11) 0.0429(11) 0.0369(10) 0.0050(8) 0.0116(8) 0.0027(9) C40 0.0480(12) 0.0638(14) 0.0338(10) 0.0105(10) 0.0035(9) -0.0002(10) C41 0.0470(12) 0.0583(14) 0.0502(12) 0.0248(10) 0.0150(10) 0.0091(10) C42 0.0508(12) 0.0413(11) 0.0586(13) 0.0105(10) 0.0265(10) 0.0058(9) C43 0.0405(10) 0.0438(11) 0.0392(10) 0.0020(8) 0.0189(8) 0.0047(8) C44 0.0339(10) 0.0737(15) 0.0219(9) 0.0006(9) 0.0088(7) 0.0183(10) C45 0.0386(11) 0.0678(15) 0.0433(11) -0.0023(10) 0.0105(9) 0.0032(10) C46 0.0428(12) 0.101(2) 0.0448(12) -0.0140(12) 0.0124(10) -0.0119(13) C47 0.0401(13) 0.134(3) 0.0502(14) -0.0334(16) 0.0168(11) -0.0072(15) C48 0.0374(12) 0.120(2) 0.0521(14) -0.0233(15) 0.0136(10) 0.0248(14) C49 0.0523(13) 0.0802(17) 0.0375(11) -0.0054(11) 0.0134(10) 0.0255(12) C50 0.0779(18) 0.087(2) 0.0833(19) 0.0039(16) 0.0336(15) 0.0397(16) _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 1.5638(14) . ? P1 C13 1.7965(16) . ? P1 C19 1.8143(17) . ? P1 C2 1.8223(16) . ? O1 C1 1.3886(19) . ? O1 C12 1.3951(19) . ? N1 C25 1.390(2) . ? C1 C2 1.390(2) . ? C1 C6 1.394(2) . ? P2 N2 1.5758(15) . ? P2 C32 1.801(2) . ? P2 C38 1.8063(17) . ? P2 C11 1.8169(19) . ? C2 C3 1.397(2) . ? N2 C44 1.411(3) . ? C3 C4 1.391(3) . ? C3 H3 0.9500 . ? C4 C5 1.371(3) . ? C4 H4 0.9500 . ? C5 C6 1.393(2) . ? C5 H5 0.9500 . ? C6 C7 1.433(3) . ? C7 C12 1.391(2) . ? C7 C8 1.393(3) . ? C8 C9 1.374(3) . ? C8 H8 0.9500 . ? C9 C10 1.385(3) . ? C9 H9 0.9500 . ? C10 C11 1.406(3) . ? C10 H10 0.9500 . ? C11 C12 1.389(2) . ? C13 C14 1.381(2) . ? C13 C18 1.386(3) . ? C14 C15 1.386(3) . ? C14 H14 0.9500 . ? C15 C16 1.370(3) . ? C15 H15 0.9500 . ? C16 C17 1.375(3) . ? C16 H16 0.9500 . ? C17 C18 1.378(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.391(2) . ? C19 C20 1.392(2) . ? C20 C21 1.385(3) . ? C20 H20 0.9500 . ? C21 C22 1.379(3) . ? C21 H21 0.9500 . ? C22 C23 1.377(3) . ? C22 H22 0.9500 . ? C23 C24 1.382(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.393(3) . ? C25 C30 1.408(2) . ? C26 C27 1.381(3) . ? C26 H26 0.9500 . ? C27 C28 1.379(3) . ? C27 H27 0.9500 . ? C28 C29 1.376(3) . ? C28 H28 0.9500 . ? C29 C30 1.385(3) . ? C29 H29 0.9500 . ? C30 C31 1.495(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.384(3) . ? C32 C37 1.389(3) . ? C33 C34 1.381(3) . ? C33 H33 0.9500 . ? C34 C35 1.385(4) . ? C34 H34 0.9500 . ? C35 C36 1.374(4) . ? C35 H35 0.9500 . ? C36 C37 1.373(3) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C43 1.384(3) . ? C38 C39 1.391(3) . ? C39 C40 1.378(3) . ? C39 H39 0.9500 . ? C40 C41 1.369(3) . ? C40 H40 0.9500 . ? C41 C42 1.377(3) . ? C41 H41 0.9500 . ? C42 C43 1.388(3) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.382(3) . ? C44 C49 1.412(3) . ? C45 C46 1.391(3) . ? C45 H45 0.9500 . ? C46 C47 1.362(4) . ? C46 H46 0.9500 . ? C47 C48 1.375(4) . ? C47 H47 0.9500 . ? C48 C49 1.393(4) . ? C48 H48 0.9500 . ? C49 C50 1.492(4) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 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 105.52(8) . . ? N1 P1 C19 116.52(8) . . ? C13 P1 C19 108.07(8) . . ? N1 P1 C2 112.14(8) . . ? C13 P1 C2 109.21(7) . . ? C19 P1 C2 105.23(7) . . ? C1 O1 C12 105.53(12) . . ? C25 N1 P1 131.34(12) . . ? O1 C1 C2 126.13(14) . . ? O1 C1 C6 111.02(14) . . ? C2 C1 C6 122.85(15) . . ? N2 P2 C32 106.26(9) . . ? N2 P2 C38 115.73(8) . . ? C32 P2 C38 107.14(8) . . ? N2 P2 C11 111.94(8) . . ? C32 P2 C11 105.66(9) . . ? C38 P2 C11 109.45(9) . . ? C1 C2 C3 114.97(15) . . ? C1 C2 P1 128.25(12) . . ? C3 C2 P1 116.69(13) . . ? C44 N2 P2 125.80(15) . . ? C4 C3 C2 122.92(17) . . ? C4 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? C5 C4 C3 120.59(16) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 118.26(16) . . ? C4 C5 H5 120.9 . . ? C6 C5 H5 120.9 . . ? C5 C6 C1 120.14(16) . . ? C5 C6 C7 133.69(16) . . ? C1 C6 C7 106.15(14) . . ? C12 C7 C8 120.35(17) . . ? C12 C7 C6 106.45(15) . . ? C8 C7 C6 133.19(17) . . ? C9 C8 C7 118.20(18) . . ? C9 C8 H8 120.9 . . ? C7 C8 H8 120.9 . . ? C8 C9 C10 120.79(18) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C9 C10 C11 122.70(19) . . ? C9 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? C12 C11 C10 115.11(17) . . ? C12 C11 P2 130.04(14) . . ? C10 C11 P2 114.11(14) . . ? C11 C12 C7 122.79(16) . . ? C11 C12 O1 126.44(15) . . ? C7 C12 O1 110.76(15) . . ? C14 C13 C18 119.20(16) . . ? C14 C13 P1 123.18(13) . . ? C18 C13 P1 117.61(13) . . ? C13 C14 C15 119.95(17) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.50(18) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 119.70(18) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C18 120.31(19) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 120.25(18) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? C24 C19 C20 118.66(16) . . ? C24 C19 P1 118.84(13) . . ? C20 C19 P1 121.90(13) . . ? C21 C20 C19 120.48(17) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C22 C21 C20 120.17(18) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 119.83(18) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.32(17) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C19 120.52(17) . . ? C23 C24 H24 119.7 . . ? C19 C24 H24 119.7 . . ? N1 C25 C26 125.04(16) . . ? N1 C25 C30 116.60(16) . . ? C26 C25 C30 118.36(16) . . ? C27 C26 C25 121.1(2) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C28 C27 C26 120.5(2) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C29 C28 C27 118.76(19) . . ? C29 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C28 C29 C30 122.2(2) . . ? C28 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C29 C30 C25 119.05(19) . . ? C29 C30 C31 121.76(18) . . ? C25 C30 C31 119.19(16) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C37 119.5(2) . . ? C33 C32 P2 121.62(15) . . ? C37 C32 P2 118.91(16) . . ? C34 C33 C32 120.5(2) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 119.6(2) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C36 C35 C34 119.9(2) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C37 C36 C35 120.8(2) . . ? C37 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C36 C37 C32 119.8(2) . . ? C36 C37 H37 120.1 . . ? C32 C37 H37 120.1 . . ? C43 C38 C39 119.35(17) . . ? C43 C38 P2 122.88(14) . . ? C39 C38 P2 117.02(14) . . ? C40 C39 C38 120.38(19) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C41 C40 C39 119.9(2) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C42 120.63(19) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C41 C42 C43 119.9(2) . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C38 C43 C42 119.85(19) . . ? C38 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C45 C44 N2 125.35(17) . . ? C45 C44 C49 118.0(2) . . ? N2 C44 C49 116.6(2) . . ? C44 C45 C46 122.2(2) . . ? C44 C45 H45 118.9 . . ? C46 C45 H45 118.9 . . ? C47 C46 C45 119.9(3) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C46 C47 C48 118.9(2) . . ? C46 C47 H47 120.6 . . ? C48 C47 H47 120.6 . . ? C47 C48 C49 122.7(2) . . ? C47 C48 H48 118.6 . . ? C49 C48 H48 118.6 . . ? C48 C49 C44 118.3(2) . . ? C48 C49 C50 122.2(2) . . ? C44 C49 C50 119.6(2) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 P1 N1 C25 -178.97(15) . . . . ? C19 P1 N1 C25 -59.09(18) . . . . ? C2 P1 N1 C25 62.24(17) . . . . ? C12 O1 C1 C2 178.36(16) . . . . ? C12 O1 C1 C6 -1.20(18) . . . . ? O1 C1 C2 C3 174.89(15) . . . . ? C6 C1 C2 C3 -5.6(2) . . . . ? O1 C1 C2 P1 -8.6(2) . . . . ? C6 C1 C2 P1 170.88(13) . . . . ? N1 P1 C2 C1 172.73(14) . . . . ? C13 P1 C2 C1 56.14(16) . . . . ? C19 P1 C2 C1 -59.66(16) . . . . ? N1 P1 C2 C3 -10.85(15) . . . . ? C13 P1 C2 C3 -127.44(13) . . . . ? C19 P1 C2 C3 116.76(13) . . . . ? C32 P2 N2 C44 -178.66(14) . . . . ? C38 P2 N2 C44 62.57(17) . . . . ? C11 P2 N2 C44 -63.78(16) . . . . ? C1 C2 C3 C4 2.5(2) . . . . ? P1 C2 C3 C4 -174.39(14) . . . . ? C2 C3 C4 C5 2.0(3) . . . . ? C3 C4 C5 C6 -3.5(3) . . . . ? C4 C5 C6 C1 0.5(3) . . . . ? C4 C5 C6 C7 -177.96(19) . . . . ? O1 C1 C6 C5 -176.13(15) . . . . ? C2 C1 C6 C5 4.3(3) . . . . ? O1 C1 C6 C7 2.69(19) . . . . ? C2 C1 C6 C7 -176.89(16) . . . . ? C5 C6 C7 C12 175.51(19) . . . . ? C1 C6 C7 C12 -3.1(2) . . . . ? C5 C6 C7 C8 -3.1(4) . . . . ? C1 C6 C7 C8 178.3(2) . . . . ? C12 C7 C8 C9 0.0(3) . . . . ? C6 C7 C8 C9 178.5(2) . . . . ? C7 C8 C9 C10 -1.9(4) . . . . ? C8 C9 C10 C11 1.4(4) . . . . ? C9 C10 C11 C12 0.9(3) . . . . ? C9 C10 C11 P2 -170.2(2) . . . . ? N2 P2 C11 C12 173.17(18) . . . . ? C32 P2 C11 C12 -71.6(2) . . . . ? C38 P2 C11 C12 43.5(2) . . . . ? N2 P2 C11 C10 -17.30(19) . . . . ? C32 P2 C11 C10 97.95(17) . . . . ? C38 P2 C11 C10 -146.99(15) . . . . ? C10 C11 C12 C7 -2.8(3) . . . . ? P2 C11 C12 C7 166.62(16) . . . . ? C10 C11 C12 O1 178.47(18) . . . . ? P2 C11 C12 O1 -12.1(3) . . . . ? C8 C7 C12 C11 2.4(3) . . . . ? C6 C7 C12 C11 -176.42(17) . . . . ? C8 C7 C12 O1 -178.69(18) . . . . ? C6 C7 C12 O1 2.5(2) . . . . ? C1 O1 C12 C11 177.99(18) . . . . ? C1 O1 C12 C7 -0.84(19) . . . . ? N1 P1 C13 C14 138.02(15) . . . . ? C19 P1 C13 C14 12.71(17) . . . . ? C2 P1 C13 C14 -101.25(16) . . . . ? N1 P1 C13 C18 -40.68(17) . . . . ? C19 P1 C13 C18 -165.99(15) . . . . ? C2 P1 C13 C18 80.05(16) . . . . ? C18 C13 C14 C15 1.6(3) . . . . ? P1 C13 C14 C15 -177.06(15) . . . . ? C13 C14 C15 C16 -2.4(3) . . . . ? C14 C15 C16 C17 0.7(3) . . . . ? C15 C16 C17 C18 1.8(3) . . . . ? C16 C17 C18 C13 -2.6(4) . . . . ? C14 C13 C18 C17 0.9(3) . . . . ? P1 C13 C18 C17 179.62(18) . . . . ? N1 P1 C19 C24 -60.21(16) . . . . ? C13 P1 C19 C24 58.29(15) . . . . ? C2 P1 C19 C24 174.87(13) . . . . ? N1 P1 C19 C20 110.75(15) . . . . ? C13 P1 C19 C20 -130.74(15) . . . . ? C2 P1 C19 C20 -14.17(17) . . . . ? C24 C19 C20 C21 1.1(3) . . . . ? P1 C19 C20 C21 -169.86(15) . . . . ? C19 C20 C21 C22 -0.6(3) . . . . ? C20 C21 C22 C23 -0.9(3) . . . . ? C21 C22 C23 C24 1.9(3) . . . . ? C22 C23 C24 C19 -1.3(3) . . . . ? C20 C19 C24 C23 -0.2(3) . . . . ? P1 C19 C24 C23 171.10(14) . . . . ? P1 N1 C25 C26 17.3(3) . . . . ? P1 N1 C25 C30 -163.50(14) . . . . ? N1 C25 C26 C27 -179.81(18) . . . . ? C30 C25 C26 C27 1.0(3) . . . . ? C25 C26 C27 C28 -0.3(3) . . . . ? C26 C27 C28 C29 -0.6(3) . . . . ? C27 C28 C29 C30 0.8(3) . . . . ? C28 C29 C30 C25 -0.1(3) . . . . ? C28 C29 C30 C31 179.8(2) . . . . ? N1 C25 C30 C29 179.95(16) . . . . ? C26 C25 C30 C29 -0.8(3) . . . . ? N1 C25 C30 C31 0.0(2) . . . . ? C26 C25 C30 C31 179.30(18) . . . . ? N2 P2 C32 C33 -156.32(16) . . . . ? C38 P2 C32 C33 -32.04(18) . . . . ? C11 P2 C32 C33 84.60(17) . . . . ? N2 P2 C32 C37 24.59(17) . . . . ? C38 P2 C32 C37 148.87(15) . . . . ? C11 P2 C32 C37 -94.49(16) . . . . ? C37 C32 C33 C34 -1.3(3) . . . . ? P2 C32 C33 C34 179.60(17) . . . . ? C32 C33 C34 C35 0.8(3) . . . . ? C33 C34 C35 C36 0.5(4) . . . . ? C34 C35 C36 C37 -1.4(4) . . . . ? C35 C36 C37 C32 0.8(3) . . . . ? C33 C32 C37 C36 0.5(3) . . . . ? P2 C32 C37 C36 179.63(16) . . . . ? N2 P2 C38 C43 -102.99(16) . . . . ? C32 P2 C38 C43 138.72(15) . . . . ? C11 P2 C38 C43 24.61(17) . . . . ? N2 P2 C38 C39 67.08(16) . . . . ? C32 P2 C38 C39 -51.20(16) . . . . ? C11 P2 C38 C39 -165.32(14) . . . . ? C43 C38 C39 C40 0.2(3) . . . . ? P2 C38 C39 C40 -170.26(15) . . . . ? C38 C39 C40 C41 -0.1(3) . . . . ? C39 C40 C41 C42 0.1(3) . . . . ? C40 C41 C42 C43 -0.2(3) . . . . ? C39 C38 C43 C42 -0.2(3) . . . . ? P2 C38 C43 C42 169.61(14) . . . . ? C41 C42 C43 C38 0.3(3) . . . . ? P2 N2 C44 C45 -11.7(3) . . . . ? P2 N2 C44 C49 170.87(14) . . . . ? N2 C44 C45 C46 -176.22(18) . . . . ? C49 C44 C45 C46 1.1(3) . . . . ? C44 C45 C46 C47 -1.4(3) . . . . ? C45 C46 C47 C48 0.4(3) . . . . ? C46 C47 C48 C49 1.0(4) . . . . ? C47 C48 C49 C44 -1.2(3) . . . . ? C47 C48 C49 C50 177.2(2) . . . . ? C45 C44 C49 C48 0.2(3) . . . . ? N2 C44 C49 C48 177.76(17) . . . . ? C45 C44 C49 C50 -178.3(2) . . . . ? N2 C44 C49 C50 -0.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.533 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.038 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.000 70 6 ' ' 2 0.594 0.111 0.613 8 0 ' ' 3 0.594 0.389 0.113 8 0 ' ' 4 0.500 0.500 0.500 70 7 ' ' 5 0.406 0.611 0.887 8 0 ' ' 6 0.406 0.889 0.387 8 0 ' ' _platon_squeeze_details ; ; #===END data_L3 _database_code_depnum_ccdc_archive 'CCDC 833325' #TrackingRef '6184_web_deposit_cif_file_0_PaulG.Hayes_ #1310063407.Chem Eur J_AllCifs - Paul G Hayes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H39 N2 O P2' _chemical_formula_weight 757.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.373(11) _cell_length_b 13.769(17) _cell_length_c 17.95(2) _cell_angle_alpha 104.285(15) _cell_angle_beta 90.990(14) _cell_angle_gamma 92.535(15) _cell_volume 2242(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4068 _cell_measurement_theta_min 4.661 _cell_measurement_theta_max 45.127 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.123 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 794 _exptl_absorpt_coefficient_mu 0.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9651 _exptl_absorpt_correction_T_max 0.9898 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26495 _diffrn_reflns_av_R_equivalents 0.1176 _diffrn_reflns_av_sigmaI/netI 0.1608 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7900 _reflns_number_gt 3097 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0918P)^2^+0.0000P] 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 7900 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1780 _refine_ls_R_factor_gt 0.0794 _refine_ls_wR_factor_ref 0.2141 _refine_ls_wR_factor_gt 0.1825 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.915 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.76025(13) 0.03208(11) 0.30615(8) 0.0495(4) Uani 1 1 d . . . O1 O 0.5947(3) -0.1969(3) 0.23598(17) 0.0511(9) Uani 1 1 d . . . N1 N 0.7758(4) 0.1493(3) 0.3415(2) 0.0541(11) Uani 1 1 d . . . C1 C 0.5189(5) -0.1094(4) 0.2525(3) 0.0467(13) Uani 1 1 d . . . P2 P 0.71161(14) -0.41825(13) 0.17588(9) 0.0757(6) Uani 1 1 d . . . C2 C 0.5754(5) -0.0115(4) 0.2807(3) 0.0477(13) Uani 1 1 d . . . N2 N 0.8250(4) -0.3630(4) 0.1356(3) 0.0861(16) Uani 1 1 d . . . C3 C 0.4765(5) 0.0624(4) 0.2898(3) 0.0590(15) Uani 1 1 d . . . H3 H 0.5088 0.1304 0.3097 0.071 Uiso 1 1 calc R . . C4 C 0.3309(5) 0.0405(5) 0.2709(3) 0.0665(16) Uani 1 1 d . . . H4 H 0.2683 0.0940 0.2758 0.080 Uiso 1 1 calc R . . C5 C 0.2780(5) -0.0554(5) 0.2457(3) 0.0597(15) Uani 1 1 d . . . H5 H 0.1787 -0.0697 0.2345 0.072 Uiso 1 1 calc R . . C6 C 0.3726(5) -0.1327(5) 0.2365(3) 0.0547(14) Uani 1 1 d . . . C7 C 0.3578(5) -0.2394(5) 0.2082(3) 0.0547(14) Uani 1 1 d . . . C8 C 0.2439(5) -0.3087(5) 0.1827(3) 0.0719(18) Uani 1 1 d . . . H8 H 0.1491 -0.2869 0.1827 0.086 Uiso 1 1 calc R . . C9 C 0.2693(6) -0.4082(5) 0.1577(3) 0.087(2) Uani 1 1 d . . . H9 H 0.1910 -0.4551 0.1406 0.104 Uiso 1 1 calc R . . C10 C 0.4092(6) -0.4434(5) 0.1564(3) 0.0800(19) Uani 1 1 d . . . H10 H 0.4225 -0.5133 0.1385 0.096 Uiso 1 1 calc R . . C11 C 0.5294(5) -0.3769(4) 0.1813(3) 0.0613(15) Uani 1 1 d . . . C12 C 0.4955(5) -0.2765(4) 0.2081(3) 0.0543(14) Uani 1 1 d . . . C13 C 0.8335(3) -0.0463(2) 0.36378(17) 0.0456(12) Uani 1 1 d G . . C14 C 0.7506(3) -0.1054(3) 0.4007(2) 0.0723(17) Uani 1 1 d G . . H14 H 0.6495 -0.1093 0.3941 0.087 Uiso 1 1 calc R . . C15 C 0.8155(4) -0.1586(3) 0.4473(2) 0.088(2) Uani 1 1 d G . . H15 H 0.7588 -0.1990 0.4725 0.105 Uiso 1 1 calc R . . C16 C 0.9633(5) -0.1528(2) 0.45696(19) 0.0763(19) Uani 1 1 d G . . H16 H 1.0077 -0.1892 0.4888 0.092 Uiso 1 1 calc R . . C17 C 1.0463(3) -0.0937(3) 0.4201(2) 0.0650(16) Uani 1 1 d G . . H17 H 1.1473 -0.0898 0.4267 0.078 Uiso 1 1 calc R . . C18 C 0.9814(3) -0.0405(2) 0.37347(18) 0.0493(13) Uani 1 1 d G . . H18 H 1.0380 -0.0001 0.3482 0.059 Uiso 1 1 calc R . . C19 C 0.8619(3) 0.0067(3) 0.21872(16) 0.0482(13) Uani 1 1 d G . . C20 C 0.9263(4) 0.0862(2) 0.1947(2) 0.0601(15) Uani 1 1 d G . . H20 H 0.9145 0.1533 0.2230 0.072 Uiso 1 1 calc R . . C21 C 1.0081(3) 0.0675(3) 0.1293(2) 0.0782(19) Uani 1 1 d G . . H21 H 1.0522 0.1219 0.1129 0.094 Uiso 1 1 calc R . . C22 C 1.0254(3) -0.0306(3) 0.08790(16) 0.0661(16) Uani 1 1 d G . . H22 H 1.0813 -0.0433 0.0432 0.079 Uiso 1 1 calc R . . C23 C 0.9610(3) -0.1101(2) 0.11192(18) 0.0605(15) Uani 1 1 d G . . H23 H 0.9728 -0.1771 0.0836 0.073 Uiso 1 1 calc R . . C24 C 0.8792(3) -0.0914(2) 0.1773(2) 0.0590(15) Uani 1 1 d G . . H24 H 0.8351 -0.1457 0.1937 0.071 Uiso 1 1 calc R . . C25 C 0.7277(3) 0.2036(3) 0.41421(17) 0.0544(14) Uani 1 1 d G . . C26 C 0.7586(3) 0.3065(3) 0.4337(2) 0.0546(14) Uani 1 1 d G . . H26 H 0.8068 0.3373 0.3987 0.066 Uiso 1 1 calc R . . C27 C 0.7189(4) 0.3646(2) 0.5045(2) 0.0718(17) Uani 1 1 d G . . H27 H 0.7400 0.4350 0.5178 0.086 Uiso 1 1 calc R . . C28 C 0.6484(4) 0.3196(4) 0.55576(17) 0.083(2) Uani 1 1 d G . . H28 H 0.6214 0.3593 0.6041 0.100 Uiso 1 1 calc R . . C29 C 0.6176(3) 0.2166(4) 0.5362(2) 0.0795(19) Uani 1 1 d G . . H29 H 0.5694 0.1859 0.5713 0.095 Uiso 1 1 calc R . . C30 C 0.6572(4) 0.1586(2) 0.4655(2) 0.0669(16) Uani 1 1 d G . . H30 H 0.6361 0.0882 0.4521 0.080 Uiso 1 1 calc R . . C31 C 0.7753(4) -0.4055(3) 0.27492(19) 0.0767(18) Uani 1 1 d G . . C32 C 0.9213(4) -0.4007(3) 0.2913(3) 0.094(2) Uani 1 1 d G . . H32 H 0.9872 -0.3938 0.2531 0.112 Uiso 1 1 calc R . . C33 C 0.9709(3) -0.4062(3) 0.3635(3) 0.095(2) Uani 1 1 d G . . H33 H 1.0707 -0.4029 0.3746 0.114 Uiso 1 1 calc R . . C34 C 0.8744(5) -0.4163(3) 0.4193(2) 0.088(2) Uani 1 1 d G . . H34 H 0.9083 -0.4200 0.4687 0.106 Uiso 1 1 calc R . . C35 C 0.7284(5) -0.4210(3) 0.4030(2) 0.0755(17) Uani 1 1 d G . . H35 H 0.6625 -0.4280 0.4412 0.091 Uiso 1 1 calc R . . C36 C 0.6789(3) -0.4156(3) 0.3308(2) 0.0703(17) Uani 1 1 d G . . H36 H 0.5791 -0.4189 0.3196 0.084 Uiso 1 1 calc R . . C37 C 0.6904(3) -0.5541(3) 0.1344(3) 0.0766(19) Uani 1 1 d G . . C38 C 0.6818(3) -0.5885(3) 0.0548(2) 0.0778(19) Uani 1 1 d G . . H38 H 0.6799 -0.5420 0.0235 0.093 Uiso 1 1 calc R . . C39 C 0.6759(3) -0.6910(4) 0.0209(2) 0.094(2) Uani 1 1 d G . . H39 H 0.6701 -0.7145 -0.0336 0.113 Uiso 1 1 calc R . . C40 C 0.6787(3) -0.7590(3) 0.0666(3) 0.093(2) Uani 1 1 d G . . H40 H 0.6747 -0.8290 0.0434 0.111 Uiso 1 1 calc R . . C41 C 0.6873(4) -0.7246(4) 0.1462(3) 0.094(2) Uani 1 1 d G . . H41 H 0.6891 -0.7710 0.1774 0.113 Uiso 1 1 calc R . . C42 C 0.6931(4) -0.6221(4) 0.18009(19) 0.089(2) Uani 1 1 d G . . H42 H 0.6990 -0.5985 0.2345 0.107 Uiso 1 1 calc R . . C43 C 0.8169(4) -0.3540(3) 0.0592(2) 0.085(2) Uani 1 1 d G . . C44 C 0.6995(3) -0.3170(3) 0.0288(2) 0.083(2) Uani 1 1 d G . . H44 H 0.6157 -0.3038 0.0579 0.100 Uiso 1 1 calc R . . C45 C 0.7048(4) -0.2994(3) -0.0441(3) 0.088(2) Uani 1 1 d G . . H45 H 0.6246 -0.2741 -0.0648 0.105 Uiso 1 1 calc R . . C46 C 0.8275(5) -0.3187(3) -0.0866(2) 0.096(2) Uani 1 1 d G . . H46 H 0.8311 -0.3066 -0.1364 0.115 Uiso 1 1 calc R . . C47 C 0.9448(4) -0.3556(3) -0.0562(3) 0.106(3) Uani 1 1 d G . . H47 H 1.0287 -0.3688 -0.0853 0.127 Uiso 1 1 calc R . . C48 C 0.9395(3) -0.3733(3) 0.0167(3) 0.099(2) Uani 1 1 d G . . H48 H 1.0198 -0.3986 0.0374 0.119 Uiso 1 1 calc R . . C1S C 0.5836(9) -1.0278(6) -0.0615(4) 0.099(2) Uani 1 1 d . . . H1S H 0.6412 -1.0486 -0.1051 0.119 Uiso 1 1 calc R . . C2S C 0.6233(7) -1.0453(5) 0.0069(6) 0.100(2) Uani 1 1 d . . . H2S H 0.7108 -1.0757 0.0119 0.120 Uiso 1 1 calc R . . C3S C 0.5384(10) -1.0195(6) 0.0677(4) 0.096(2) Uani 1 1 d . . . H3S H 0.5641 -1.0343 0.1149 0.116 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 0.0299(7) 0.0726(10) 0.0559(9) 0.0344(8) 0.0046(6) 0.0038(7) O1 0.0284(18) 0.085(3) 0.038(2) 0.0126(18) 0.0014(15) -0.0002(19) N1 0.042(2) 0.052(3) 0.081(3) 0.039(2) 0.010(2) 0.005(2) C1 0.026(3) 0.082(4) 0.038(3) 0.027(3) 0.003(2) 0.007(3) P2 0.0292(8) 0.1022(13) 0.0689(11) -0.0295(9) 0.0038(7) 0.0014(8) C2 0.025(3) 0.073(4) 0.053(3) 0.029(3) 0.004(2) 0.001(3) N2 0.029(3) 0.110(4) 0.094(4) -0.020(3) 0.006(3) -0.013(3) C3 0.033(3) 0.097(4) 0.056(4) 0.035(3) 0.000(3) 0.009(3) C4 0.029(3) 0.112(5) 0.069(4) 0.039(4) 0.003(3) 0.013(3) C5 0.030(3) 0.104(5) 0.046(3) 0.020(3) 0.004(3) 0.000(3) C6 0.027(3) 0.100(5) 0.034(3) 0.011(3) 0.001(2) 0.000(3) C7 0.022(3) 0.100(5) 0.034(3) 0.002(3) 0.001(2) -0.001(3) C8 0.027(3) 0.112(5) 0.054(4) -0.022(3) 0.002(3) 0.000(3) C9 0.028(3) 0.123(6) 0.076(4) -0.033(4) -0.001(3) -0.011(3) C10 0.042(4) 0.100(5) 0.070(4) -0.028(3) -0.004(3) -0.006(3) C11 0.036(3) 0.091(4) 0.040(3) -0.015(3) 0.002(2) -0.008(3) C12 0.027(3) 0.092(4) 0.031(3) -0.005(3) -0.001(2) -0.016(3) C13 0.038(3) 0.056(3) 0.044(3) 0.016(2) -0.003(2) -0.005(2) C14 0.062(4) 0.095(4) 0.071(4) 0.048(4) -0.027(3) -0.030(3) C15 0.104(5) 0.081(4) 0.093(5) 0.058(4) -0.045(4) -0.035(4) C16 0.108(5) 0.047(4) 0.072(4) 0.017(3) -0.047(4) 0.007(3) C17 0.054(4) 0.073(4) 0.060(4) 0.002(3) -0.017(3) 0.010(3) C18 0.042(3) 0.063(3) 0.044(3) 0.016(3) -0.010(2) -0.001(3) C19 0.030(3) 0.063(3) 0.059(3) 0.027(3) 0.007(2) 0.011(3) C20 0.046(3) 0.075(4) 0.072(4) 0.041(3) 0.012(3) 0.009(3) C21 0.054(4) 0.115(6) 0.083(5) 0.060(4) 0.007(3) -0.015(4) C22 0.036(3) 0.113(5) 0.058(4) 0.041(4) 0.007(3) -0.005(3) C23 0.034(3) 0.091(4) 0.056(4) 0.017(3) 0.008(3) 0.005(3) C24 0.026(3) 0.092(4) 0.074(4) 0.046(3) 0.005(3) 0.006(3) C25 0.030(3) 0.089(4) 0.056(4) 0.039(3) 0.006(3) 0.015(3) C26 0.049(3) 0.055(4) 0.067(4) 0.028(3) 0.011(3) 0.009(3) C27 0.050(4) 0.096(5) 0.072(4) 0.021(4) 0.004(3) 0.019(3) C28 0.042(4) 0.151(7) 0.059(4) 0.030(5) 0.007(3) 0.017(4) C29 0.040(3) 0.143(6) 0.067(5) 0.049(4) 0.006(3) -0.003(4) C30 0.039(3) 0.103(5) 0.068(4) 0.040(4) 0.004(3) -0.011(3) C31 0.038(3) 0.100(5) 0.068(4) -0.027(3) -0.002(3) 0.016(3) C32 0.042(4) 0.114(5) 0.096(5) -0.027(4) 0.000(4) 0.009(3) C33 0.043(4) 0.103(5) 0.112(6) -0.023(5) -0.027(4) 0.013(3) C34 0.085(5) 0.066(4) 0.095(5) -0.017(4) -0.036(4) 0.014(4) C35 0.066(4) 0.072(4) 0.078(5) -0.003(3) -0.010(4) 0.010(3) C36 0.045(3) 0.092(4) 0.058(4) -0.011(3) -0.009(3) 0.011(3) C37 0.023(3) 0.115(5) 0.066(4) -0.026(4) 0.003(3) 0.002(3) C38 0.038(3) 0.097(5) 0.065(4) -0.042(3) 0.010(3) -0.012(3) C39 0.032(3) 0.137(7) 0.076(5) -0.042(5) 0.016(3) -0.025(4) C40 0.034(3) 0.101(5) 0.109(6) -0.038(5) 0.004(4) -0.007(3) C41 0.047(4) 0.112(6) 0.100(6) -0.019(4) -0.003(4) 0.017(4) C42 0.052(4) 0.114(6) 0.073(5) -0.031(4) -0.006(3) 0.020(4) C43 0.052(4) 0.123(5) 0.047(4) -0.038(4) 0.008(3) -0.007(4) C44 0.039(4) 0.115(5) 0.077(5) -0.015(4) 0.021(3) 0.004(3) C45 0.041(4) 0.126(6) 0.069(4) -0.023(4) 0.015(3) -0.019(3) C46 0.057(4) 0.114(5) 0.078(5) -0.043(4) 0.016(4) -0.031(4) C47 0.042(4) 0.146(6) 0.078(5) -0.066(5) 0.015(4) -0.020(4) C48 0.032(3) 0.144(6) 0.077(5) -0.054(4) 0.002(3) -0.008(3) C1S 0.060(5) 0.163(7) 0.066(5) 0.017(5) 0.012(4) -0.027(5) C2S 0.041(4) 0.125(6) 0.135(8) 0.036(6) -0.019(5) 0.004(4) C3S 0.086(6) 0.147(7) 0.075(6) 0.072(5) -0.027(5) -0.034(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 P1 N1 1.582(4) . ? P1 C13 1.816(3) . ? P1 C19 1.817(3) . ? P1 C2 1.821(5) . ? O1 C12 1.393(5) . ? O1 C1 1.396(6) . ? N1 C25 1.425(5) . ? C1 C2 1.394(7) . ? C1 C6 1.403(6) . ? P2 N2 1.569(5) . ? P2 C11 1.820(6) . ? P2 C31 1.830(4) . ? P2 C37 1.835(4) . ? C2 C3 1.389(6) . ? N2 C43 1.407(6) . ? C3 C4 1.402(7) . ? C3 H3 0.9500 . ? C4 C5 1.355(7) . ? C4 H4 0.9500 . ? C5 C6 1.396(7) . ? C5 H5 0.9500 . ? C6 C7 1.431(7) . ? C7 C8 1.392(7) . ? C7 C12 1.409(6) . ? C8 C9 1.366(7) . ? C8 H8 0.9500 . ? C9 C10 1.417(7) . ? C9 H9 0.9500 . ? C10 C11 1.413(7) . ? C10 H10 0.9500 . ? C11 C12 1.400(7) . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C14 H14 0.9500 . ? C15 C16 1.3900 . ? C15 H15 0.9500 . ? C16 C17 1.3900 . ? C16 H16 0.9500 . ? C17 C18 1.3900 . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C20 H20 0.9500 . ? C21 C22 1.3900 . ? C21 H21 0.9500 . ? C22 C23 1.3900 . ? C22 H22 0.9500 . ? C23 C24 1.3900 . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C26 H26 0.9500 . ? C27 C28 1.3900 . ? C27 H27 0.9500 . ? C28 C29 1.3900 . ? C28 H28 0.9500 . ? C29 C30 1.3900 . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? 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 1.3900 . ? C37 C42 1.3900 . ? C38 C39 1.3900 . ? C38 H38 0.9500 . ? C39 C40 1.3900 . ? C39 H39 0.9500 . ? C40 C41 1.3900 . ? C40 H40 0.9500 . ? C41 C42 1.3900 . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C44 C45 1.3900 . ? C44 H44 0.9500 . ? C45 C46 1.3900 . ? C45 H45 0.9500 . ? C46 C47 1.3900 . ? C46 H46 0.9500 . ? C47 C48 1.3900 . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C1S C3S 1.357(9) 2_635 ? C1S C2S 1.358(9) . ? C1S H1S 0.9500 . ? C2S C3S 1.346(9) . ? C2S H2S 0.9500 . ? C3S C1S 1.357(9) 2_635 ? C3S H3S 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 116.5(2) . . ? N1 P1 C19 106.46(19) . . ? C13 P1 C19 105.18(18) . . ? N1 P1 C2 112.2(2) . . ? C13 P1 C2 107.8(2) . . ? C19 P1 C2 108.2(2) . . ? C12 O1 C1 106.9(4) . . ? C25 N1 P1 127.1(3) . . ? C2 C1 O1 126.8(4) . . ? C2 C1 C6 122.9(5) . . ? O1 C1 C6 110.3(5) . . ? N2 P2 C11 118.5(3) . . ? N2 P2 C31 107.7(2) . . ? C11 P2 C31 106.6(2) . . ? N2 P2 C37 114.3(2) . . ? C11 P2 C37 104.0(2) . . ? C31 P2 C37 104.8(2) . . ? C3 C2 C1 115.1(5) . . ? C3 C2 P1 116.0(4) . . ? C1 C2 P1 128.9(4) . . ? C43 N2 P2 126.3(3) . . ? C2 C3 C4 122.6(5) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C5 C4 C3 121.2(5) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 118.5(5) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? C5 C6 C1 119.6(5) . . ? C5 C6 C7 134.1(5) . . ? C1 C6 C7 106.1(5) . . ? C8 C7 C12 117.6(5) . . ? C8 C7 C6 135.1(5) . . ? C12 C7 C6 107.3(4) . . ? C9 C8 C7 119.5(5) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 121.9(5) . . ? C8 C9 H9 119.1 . . ? C10 C9 H9 119.1 . . ? C11 C10 C9 121.4(6) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C12 C11 C10 113.8(5) . . ? C12 C11 P2 123.4(4) . . ? C10 C11 P2 122.7(5) . . ? O1 C12 C11 124.8(4) . . ? O1 C12 C7 109.3(5) . . ? C11 C12 C7 125.8(5) . . ? C14 C13 C18 120.0 . . ? C14 C13 P1 123.9(2) . . ? C18 C13 P1 116.0(2) . . ? C15 C14 C13 120.0 . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 120.0 . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C20 C19 C24 120.0 . . ? C20 C19 P1 119.5(2) . . ? C24 C19 P1 120.5(2) . . ? C21 C20 C19 120.0 . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 120.0 . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C26 C25 C30 120.0 . . ? C26 C25 N1 116.3(3) . . ? C30 C25 N1 123.6(3) . . ? C25 C26 C27 120.0 . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C28 C27 C26 120.0 . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 120.0 . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 P2 119.5(3) . . ? C36 C31 P2 119.8(3) . . ? 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 C42 120.0 . . ? C38 C37 P2 118.2(3) . . ? C42 C37 P2 121.6(3) . . ? C39 C38 C37 120.0 . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 120.0 . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C41 C40 C39 120.0 . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C42 C41 C40 120.0 . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C37 120.0 . . ? C41 C42 H42 120.0 . . ? C37 C42 H42 120.0 . . ? C44 C43 C48 120.0 . . ? C44 C43 N2 122.9(3) . . ? C48 C43 N2 116.7(3) . . ? C43 C44 C45 120.0 . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C46 120.0 . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C47 C46 C45 120.0 . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 120.0 . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C47 C48 C43 120.0 . . ? C47 C48 H48 120.0 . . ? C43 C48 H48 120.0 . . ? C3S C1S C2S 119.9(6) 2_635 . ? C3S C1S H1S 120.0 2_635 . ? C2S C1S H1S 120.0 . . ? C3S C2S C1S 119.9(6) . . ? C3S C2S H2S 120.1 . . ? C1S C2S H2S 120.1 . . ? C2S C3S C1S 120.1(6) . 2_635 ? C2S C3S H3S 119.9 . . ? C1S C3S H3S 119.9 2_635 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 P1 N1 C25 -55.9(4) . . . . ? C19 P1 N1 C25 -172.8(3) . . . . ? C2 P1 N1 C25 69.0(4) . . . . ? C12 O1 C1 C2 -179.1(4) . . . . ? C12 O1 C1 C6 0.9(5) . . . . ? O1 C1 C2 C3 178.1(4) . . . . ? C6 C1 C2 C3 -1.8(7) . . . . ? O1 C1 C2 P1 -1.4(7) . . . . ? C6 C1 C2 P1 178.7(4) . . . . ? N1 P1 C2 C3 4.6(4) . . . . ? C13 P1 C2 C3 134.2(4) . . . . ? C19 P1 C2 C3 -112.6(4) . . . . ? N1 P1 C2 C1 -176.0(4) . . . . ? C13 P1 C2 C1 -46.4(5) . . . . ? C19 P1 C2 C1 66.9(5) . . . . ? C11 P2 N2 C43 -58.5(5) . . . . ? C31 P2 N2 C43 -179.4(4) . . . . ? C37 P2 N2 C43 64.6(5) . . . . ? C1 C2 C3 C4 -1.0(7) . . . . ? P1 C2 C3 C4 178.5(4) . . . . ? C2 C3 C4 C5 3.0(8) . . . . ? C3 C4 C5 C6 -2.0(8) . . . . ? C4 C5 C6 C1 -0.8(7) . . . . ? C4 C5 C6 C7 -176.3(5) . . . . ? C2 C1 C6 C5 2.8(7) . . . . ? O1 C1 C6 C5 -177.1(4) . . . . ? C2 C1 C6 C7 179.4(4) . . . . ? O1 C1 C6 C7 -0.5(5) . . . . ? C5 C6 C7 C8 -4.1(10) . . . . ? C1 C6 C7 C8 -180.0(6) . . . . ? C5 C6 C7 C12 175.8(5) . . . . ? C1 C6 C7 C12 -0.1(5) . . . . ? C12 C7 C8 C9 -1.1(8) . . . . ? C6 C7 C8 C9 178.8(6) . . . . ? C7 C8 C9 C10 -0.4(9) . . . . ? C8 C9 C10 C11 0.2(9) . . . . ? C9 C10 C11 C12 1.5(8) . . . . ? C9 C10 C11 P2 -176.7(4) . . . . ? N2 P2 C11 C12 -50.2(5) . . . . ? C31 P2 C11 C12 71.3(5) . . . . ? C37 P2 C11 C12 -178.3(4) . . . . ? N2 P2 C11 C10 127.8(5) . . . . ? C31 P2 C11 C10 -110.6(5) . . . . ? C37 P2 C11 C10 -0.3(5) . . . . ? C1 O1 C12 C11 176.6(4) . . . . ? C1 O1 C12 C7 -0.9(5) . . . . ? C10 C11 C12 O1 179.7(4) . . . . ? P2 C11 C12 O1 -2.1(7) . . . . ? C10 C11 C12 C7 -3.2(8) . . . . ? P2 C11 C12 C7 175.0(4) . . . . ? C8 C7 C12 O1 -179.5(4) . . . . ? C6 C7 C12 O1 0.6(5) . . . . ? C8 C7 C12 C11 3.1(7) . . . . ? C6 C7 C12 C11 -176.8(5) . . . . ? N1 P1 C13 C14 108.9(2) . . . . ? C19 P1 C13 C14 -133.6(2) . . . . ? C2 P1 C13 C14 -18.3(3) . . . . ? N1 P1 C13 C18 -67.6(2) . . . . ? C19 P1 C13 C18 50.0(2) . . . . ? C2 P1 C13 C18 165.3(2) . . . . ? C18 C13 C14 C15 0.0 . . . . ? P1 C13 C14 C15 -176.3(3) . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C17 0.0 . . . . ? C15 C16 C17 C18 0.0 . . . . ? C16 C17 C18 C13 0.0 . . . . ? C14 C13 C18 C17 0.0 . . . . ? P1 C13 C18 C17 176.6(2) . . . . ? N1 P1 C19 C20 -3.3(2) . . . . ? C13 P1 C19 C20 -127.5(2) . . . . ? C2 P1 C19 C20 117.5(2) . . . . ? N1 P1 C19 C24 174.6(2) . . . . ? C13 P1 C19 C24 50.4(2) . . . . ? C2 P1 C19 C24 -64.6(3) . . . . ? C24 C19 C20 C21 0.0 . . . . ? P1 C19 C20 C21 177.9(2) . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C19 0.0 . . . . ? C20 C19 C24 C23 0.0 . . . . ? P1 C19 C24 C23 -177.9(2) . . . . ? P1 N1 C25 C26 177.8(2) . . . . ? P1 N1 C25 C30 -0.4(5) . . . . ? C30 C25 C26 C27 0.0 . . . . ? N1 C25 C26 C27 -178.2(3) . . . . ? C25 C26 C27 C28 0.0 . . . . ? C26 C27 C28 C29 0.0 . . . . ? C27 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C25 0.0 . . . . ? C26 C25 C30 C29 0.0 . . . . ? N1 C25 C30 C29 178.1(3) . . . . ? N2 P2 C31 C32 -31.7(3) . . . . ? C11 P2 C31 C32 -159.8(3) . . . . ? C37 P2 C31 C32 90.4(2) . . . . ? N2 P2 C31 C36 157.9(2) . . . . ? C11 P2 C31 C36 29.8(3) . . . . ? C37 P2 C31 C36 -80.0(2) . . . . ? C36 C31 C32 C33 0.0 . . . . ? P2 C31 C32 C33 -170.4(3) . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C31 0.0 . . . . ? C32 C31 C36 C35 0.0 . . . . ? P2 C31 C36 C35 170.3(3) . . . . ? N2 P2 C37 C38 -44.7(3) . . . . ? C11 P2 C37 C38 85.9(2) . . . . ? C31 P2 C37 C38 -162.4(2) . . . . ? N2 P2 C37 C42 130.7(3) . . . . ? C11 P2 C37 C42 -98.7(2) . . . . ? C31 P2 C37 C42 13.0(2) . . . . ? C42 C37 C38 C39 0.0 . . . . ? P2 C37 C38 C39 175.4(2) . . . . ? C37 C38 C39 C40 0.0 . . . . ? C38 C39 C40 C41 0.0 . . . . ? C39 C40 C41 C42 0.0 . . . . ? C40 C41 C42 C37 0.0 . . . . ? C38 C37 C42 C41 0.0 . . . . ? P2 C37 C42 C41 -175.3(2) . . . . ? P2 N2 C43 C44 53.1(5) . . . . ? P2 N2 C43 C48 -134.0(3) . . . . ? C48 C43 C44 C45 0.0 . . . . ? N2 C43 C44 C45 172.7(4) . . . . ? C43 C44 C45 C46 0.0 . . . . ? C44 C45 C46 C47 0.0 . . . . ? C45 C46 C47 C48 0.0 . . . . ? C46 C47 C48 C43 0.0 . . . . ? C44 C43 C48 C47 0.0 . . . . ? N2 C43 C48 C47 -173.1(4) . . . . ? C3S C1S C2S C3S 2.8(12) 2_635 . . . ? C1S C2S C3S C1S -2.8(12) . . . 2_635 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.236 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.053 #===END data_4b _database_code_depnum_ccdc_archive 'CCDC 833326' #TrackingRef '6184_web_deposit_cif_file_0_PaulG.Hayes_ #1310063407.Chem Eur J_AllCifs - Paul G Hayes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C85 H77 B N2 O P2 Zn' _chemical_formula_weight 1280.61 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' B B 0.0013 0.0007 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.3702(7) _cell_length_b 15.2542(7) _cell_length_c 17.2588(8) _cell_angle_alpha 81.4510(10) _cell_angle_beta 66.4690(10) _cell_angle_gamma 76.8670(10) _cell_volume 3370.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9822 _cell_measurement_theta_min 4.544 _cell_measurement_theta_max 57.083 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 0.462 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7684 _exptl_absorpt_correction_T_max 0.9157 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32672 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.03 _reflns_number_total 11879 _reflns_number_gt 10320 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0422P)^2^+1.3532P] 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 11879 _refine_ls_number_parameters 834 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0825 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 Zn1 Zn 0.793915(14) 0.920861(12) 0.177082(11) 0.02283(6) Uani 1 1 d . . . P1 P 0.90451(3) 0.90103(3) 0.30944(3) 0.02262(10) Uani 1 1 d . . . O1 O 0.74626(9) 0.78369(7) 0.33533(7) 0.0250(2) Uani 1 1 d . . . N1 N 0.82318(10) 0.96106(9) 0.27199(8) 0.0231(3) Uani 1 1 d . . . C1 C 0.78103(12) 0.77555(11) 0.40018(10) 0.0242(3) Uani 1 1 d . . . B1 B 0.23260(15) 0.42131(13) 0.18496(13) 0.0281(4) Uani 1 1 d . . . C1S C 0.2035(3) 0.6962(3) 0.52489(19) 0.0956(12) Uani 1 1 d . . . H1S H 0.1967 0.6815 0.5821 0.115 Uiso 1 1 calc R . . P2 P 0.64589(3) 0.78401(3) 0.21108(3) 0.02179(10) Uani 1 1 d . . . N2 N 0.65065(10) 0.88681(9) 0.21761(8) 0.0224(3) Uani 1 1 d . . . C2 C 0.85346(13) 0.82288(11) 0.39856(10) 0.0253(4) Uani 1 1 d . . . C2S C 0.2773(2) 0.7453(2) 0.4704(2) 0.0799(9) Uani 1 1 d . . . H2S H 0.3211 0.7657 0.4902 0.096 Uiso 1 1 calc R . . C3 C 0.88428(14) 0.80173(12) 0.46728(11) 0.0295(4) Uani 1 1 d . . . H3 H 0.9349 0.8308 0.4697 0.035 Uiso 1 1 calc R . . C3S C 0.2863(2) 0.76363(18) 0.3899(2) 0.0693(7) Uani 1 1 d . . . H3S H 0.3372 0.7969 0.3525 0.083 Uiso 1 1 calc R . . C4 C 0.84244(15) 0.73876(13) 0.53277(11) 0.0344(4) Uani 1 1 d . . . H4 H 0.8655 0.7260 0.5784 0.041 Uiso 1 1 calc R . . C4S C 0.2252(2) 0.73608(17) 0.36123(17) 0.0659(7) Uani 1 1 d . . . H4S H 0.2334 0.7499 0.3036 0.079 Uiso 1 1 calc R . . C5 C 0.76847(14) 0.69467(12) 0.53277(11) 0.0320(4) Uani 1 1 d . . . H5 H 0.7400 0.6527 0.5780 0.038 Uiso 1 1 calc R . . C5S C 0.1524(2) 0.68924(17) 0.4118(2) 0.0698(8) Uani 1 1 d . . . H5S H 0.1099 0.6703 0.3897 0.084 Uiso 1 1 calc R . . C6 C 0.73660(13) 0.71322(11) 0.46475(10) 0.0256(4) Uani 1 1 d . . . C6S C 0.1390(2) 0.66887(19) 0.4934(2) 0.0845(10) Uani 1 1 d . . . H6S H 0.0866 0.6364 0.5294 0.101 Uiso 1 1 calc R . . C7 C 0.66707(13) 0.68111(11) 0.43790(10) 0.0256(4) Uani 1 1 d . . . C8 C 0.59987(14) 0.61961(12) 0.46970(11) 0.0337(4) Uani 1 1 d . . . H8 H 0.5913 0.5867 0.5226 0.040 Uiso 1 1 calc R . . C9 C 0.54616(15) 0.60773(13) 0.42239(12) 0.0380(4) Uani 1 1 d . . . H9 H 0.4995 0.5666 0.4439 0.046 Uiso 1 1 calc R . . C10 C 0.55804(14) 0.65399(12) 0.34414(11) 0.0321(4) Uani 1 1 d . . . H10 H 0.5197 0.6437 0.3136 0.039 Uiso 1 1 calc R . . C11 C 0.62536(13) 0.71510(11) 0.30989(10) 0.0250(3) Uani 1 1 d . . . C12 C 0.67703(12) 0.72604(11) 0.35949(10) 0.0243(3) Uani 1 1 d . . . C13 C 0.97112(13) 0.96383(11) 0.34482(11) 0.0276(4) Uani 1 1 d . . . C14 C 1.07855(14) 0.94151(13) 0.31789(12) 0.0357(4) Uani 1 1 d . . . H14 H 1.1156 0.8940 0.2811 0.043 Uiso 1 1 calc R . . C15 C 1.13118(16) 0.98819(15) 0.34446(13) 0.0445(5) Uani 1 1 d . . . H15 H 1.2042 0.9721 0.3267 0.053 Uiso 1 1 calc R . . C16 C 1.07815(18) 1.05761(15) 0.39642(13) 0.0453(5) Uani 1 1 d . . . H16 H 1.1148 1.0907 0.4132 0.054 Uiso 1 1 calc R . . C17 C 0.97203(18) 1.07986(14) 0.42451(13) 0.0448(5) Uani 1 1 d . . . H17 H 0.9360 1.1279 0.4608 0.054 Uiso 1 1 calc R . . C18 C 0.91748(16) 1.03228(13) 0.39997(12) 0.0365(4) Uani 1 1 d . . . H18 H 0.8442 1.0464 0.4207 0.044 Uiso 1 1 calc R . . C19 C 1.00024(12) 0.83502(11) 0.22583(10) 0.0248(3) Uani 1 1 d . . . C20 C 1.02709(13) 0.74155(12) 0.23600(11) 0.0303(4) Uani 1 1 d . . . H20 H 0.9927 0.7103 0.2880 0.036 Uiso 1 1 calc R . . C21 C 1.10411(15) 0.69442(13) 0.16996(13) 0.0376(4) Uani 1 1 d . . . H21 H 1.1227 0.6307 0.1768 0.045 Uiso 1 1 calc R . . C22 C 1.15401(14) 0.73944(14) 0.09422(12) 0.0380(4) Uani 1 1 d . . . H22 H 1.2059 0.7066 0.0488 0.046 Uiso 1 1 calc R . . C23 C 1.12844(14) 0.83250(13) 0.08443(12) 0.0368(4) Uani 1 1 d . . . H23 H 1.1638 0.8635 0.0326 0.044 Uiso 1 1 calc R . . C24 C 1.05197(13) 0.88022(12) 0.14960(11) 0.0313(4) Uani 1 1 d . . . H24 H 1.0345 0.9440 0.1426 0.038 Uiso 1 1 calc R . . C25 C 0.74793(12) 1.03630(11) 0.31511(10) 0.0233(3) Uani 1 1 d . . . C26 C 0.76341(13) 1.12536(11) 0.28828(11) 0.0274(4) Uani 1 1 d . . . C27 C 0.68357(15) 1.19466(12) 0.32878(12) 0.0359(4) Uani 1 1 d . . . H27 H 0.6920 1.2554 0.3116 0.043 Uiso 1 1 calc R . . C28 C 0.59279(15) 1.17789(13) 0.39300(12) 0.0379(4) Uani 1 1 d . . . H28 H 0.5399 1.2267 0.4190 0.045 Uiso 1 1 calc R . . C29 C 0.57904(14) 1.09022(13) 0.41926(11) 0.0353(4) Uani 1 1 d . . . H29 H 0.5170 1.0781 0.4636 0.042 Uiso 1 1 calc R . . C30 C 0.65643(13) 1.02020(12) 0.38037(11) 0.0293(4) Uani 1 1 d . . . H30 H 0.6471 0.9598 0.3985 0.035 Uiso 1 1 calc R . . C31 C 0.86164(14) 1.14739(12) 0.21824(12) 0.0360(4) Uani 1 1 d . . . H31 H 0.9159 1.0915 0.2097 0.043 Uiso 1 1 calc R . . C32 C 0.84622(18) 1.17520(16) 0.13533(13) 0.0498(5) Uani 1 1 d . . . H32A H 0.8222 1.1273 0.1205 0.075 Uiso 1 1 calc R . . H32B H 0.9119 1.1853 0.0905 0.075 Uiso 1 1 calc R . . H32C H 0.7947 1.2310 0.1416 0.075 Uiso 1 1 calc R . . C33 C 0.9018(2) 1.22119(18) 0.24005(15) 0.0580(6) Uani 1 1 d . . . H33A H 0.8551 1.2791 0.2399 0.087 Uiso 1 1 calc R . . H33B H 0.9710 1.2254 0.1979 0.087 Uiso 1 1 calc R . . H33C H 0.9049 1.2064 0.2963 0.087 Uiso 1 1 calc R . . C34 C 0.76823(12) 0.73323(11) 0.13599(10) 0.0239(3) Uani 1 1 d . . . C35 C 0.78705(13) 0.75588(12) 0.05069(11) 0.0298(4) Uani 1 1 d . . . H35 H 0.7367 0.7976 0.0347 0.036 Uiso 1 1 calc R . . C36 C 0.87789(14) 0.71830(13) -0.01068(12) 0.0357(4) Uani 1 1 d . . . H36 H 0.8898 0.7334 -0.0689 0.043 Uiso 1 1 calc R . . C37 C 0.95181(14) 0.65849(13) 0.01256(12) 0.0382(4) Uani 1 1 d . . . H37 H 1.0150 0.6331 -0.0297 0.046 Uiso 1 1 calc R . . C38 C 0.93403(15) 0.63561(13) 0.09699(13) 0.0396(5) Uani 1 1 d . . . H38 H 0.9851 0.5946 0.1126 0.048 Uiso 1 1 calc R . . C39 C 0.84220(14) 0.67209(12) 0.15907(12) 0.0324(4) Uani 1 1 d . . . H39 H 0.8297 0.6555 0.2171 0.039 Uiso 1 1 calc R . . C40 C 0.54948(12) 0.76846(11) 0.17466(10) 0.0250(4) Uani 1 1 d . . . C41 C 0.46659(13) 0.83606(12) 0.17313(11) 0.0304(4) Uani 1 1 d . . . H41 H 0.4578 0.8936 0.1927 0.036 Uiso 1 1 calc R . . C42 C 0.39679(14) 0.81856(14) 0.14276(12) 0.0376(4) Uani 1 1 d . . . H42 H 0.3401 0.8644 0.1417 0.045 Uiso 1 1 calc R . . C43 C 0.40898(15) 0.73533(14) 0.11418(12) 0.0394(5) Uani 1 1 d . . . H43 H 0.3606 0.7241 0.0939 0.047 Uiso 1 1 calc R . . C44 C 0.49140(15) 0.66831(13) 0.11506(12) 0.0369(4) Uani 1 1 d . . . H44 H 0.4996 0.6110 0.0954 0.044 Uiso 1 1 calc R . . C45 C 0.56185(14) 0.68463(12) 0.14452(11) 0.0309(4) Uani 1 1 d . . . H45 H 0.6190 0.6387 0.1443 0.037 Uiso 1 1 calc R . . C46 C 0.55756(12) 0.94836(11) 0.26156(10) 0.0237(3) Uani 1 1 d . . . C47 C 0.53710(13) 1.03491(11) 0.22381(11) 0.0272(4) Uani 1 1 d . . . C48 C 0.44370(14) 1.09083(13) 0.26637(13) 0.0372(4) Uani 1 1 d . . . H48 H 0.4280 1.1492 0.2414 0.045 Uiso 1 1 calc R . . C49 C 0.37339(14) 1.06443(13) 0.34326(13) 0.0410(5) Uani 1 1 d . . . H49 H 0.3103 1.1041 0.3702 0.049 Uiso 1 1 calc R . . C50 C 0.39486(14) 0.98051(13) 0.38078(12) 0.0355(4) Uani 1 1 d . . . H50 H 0.3471 0.9619 0.4340 0.043 Uiso 1 1 calc R . . C51 C 0.48692(13) 0.92323(12) 0.34030(11) 0.0299(4) Uani 1 1 d . . . H51 H 0.5022 0.8656 0.3667 0.036 Uiso 1 1 calc R . . C52 C 0.61196(13) 1.06622(11) 0.13856(11) 0.0311(4) Uani 1 1 d . . . H52 H 0.6831 1.0443 0.1384 0.037 Uiso 1 1 calc R . . C53 C 0.60712(16) 1.02381(13) 0.06564(12) 0.0421(5) Uani 1 1 d . . . H53A H 0.6254 0.9580 0.0726 0.063 Uiso 1 1 calc R . . H53B H 0.6559 1.0456 0.0117 0.063 Uiso 1 1 calc R . . H53C H 0.5370 1.0407 0.0659 0.063 Uiso 1 1 calc R . . C54 C 0.59809(15) 1.16880(12) 0.12242(13) 0.0407(5) Uani 1 1 d . . . H54A H 0.5318 1.1923 0.1164 0.061 Uiso 1 1 calc R . . H54B H 0.6543 1.1843 0.0704 0.061 Uiso 1 1 calc R . . H54C H 0.5993 1.1955 0.1702 0.061 Uiso 1 1 calc R . . C55 C 0.31271(13) 0.42921(12) 0.22906(11) 0.0294(4) Uani 1 1 d . . . C56 C 0.31831(15) 0.51173(13) 0.25229(12) 0.0379(4) Uani 1 1 d . . . H56 H 0.2728 0.5645 0.2435 0.046 Uiso 1 1 calc R . . C57 C 0.38723(16) 0.51969(15) 0.28747(13) 0.0427(5) Uani 1 1 d . . . H57 H 0.3869 0.5768 0.3033 0.051 Uiso 1 1 calc R . . C58 C 0.45627(16) 0.44539(15) 0.29961(12) 0.0432(5) Uani 1 1 d . . . H58 H 0.5047 0.4508 0.3225 0.052 Uiso 1 1 calc R . . C59 C 0.45348(16) 0.36331(15) 0.27783(12) 0.0436(5) Uani 1 1 d . . . H59 H 0.5003 0.3112 0.2859 0.052 Uiso 1 1 calc R . . C60 C 0.38271(15) 0.35567(13) 0.24394(11) 0.0362(4) Uani 1 1 d . . . H60 H 0.3821 0.2978 0.2303 0.043 Uiso 1 1 calc R . . C61 C 0.11160(14) 0.45592(11) 0.24821(12) 0.0325(4) Uani 1 1 d . . . C62 C 0.08199(16) 0.49458(13) 0.32509(13) 0.0429(5) Uani 1 1 d . . . H62 H 0.1342 0.5004 0.3435 0.051 Uiso 1 1 calc R . . C63 C -0.02060(18) 0.52488(14) 0.37562(15) 0.0562(6) Uani 1 1 d . . . H63 H -0.0367 0.5517 0.4268 0.067 Uiso 1 1 calc R . . C64 C -0.09843(17) 0.51648(14) 0.35248(16) 0.0583(7) Uani 1 1 d . . . H64 H -0.1684 0.5384 0.3866 0.070 Uiso 1 1 calc R . . C65 C -0.07407(16) 0.47574(16) 0.27871(16) 0.0543(6) Uani 1 1 d . . . H65 H -0.1274 0.4678 0.2625 0.065 Uiso 1 1 calc R . . C66 C 0.02877(15) 0.44642(14) 0.22836(13) 0.0435(5) Uani 1 1 d . . . H66 H 0.0439 0.4185 0.1779 0.052 Uiso 1 1 calc R . . C67 C 0.24824(13) 0.31556(11) 0.16468(11) 0.0284(4) Uani 1 1 d . . . C68 C 0.18270(16) 0.25617(12) 0.21314(12) 0.0369(4) Uani 1 1 d . . . H68 H 0.1240 0.2770 0.2614 0.044 Uiso 1 1 calc R . . C69 C 0.20073(19) 0.16709(14) 0.19286(14) 0.0480(5) Uani 1 1 d . . . H69 H 0.1531 0.1291 0.2263 0.058 Uiso 1 1 calc R . . C70 C 0.28644(19) 0.13343(13) 0.12515(14) 0.0469(5) Uani 1 1 d . . . H70 H 0.2990 0.0724 0.1121 0.056 Uiso 1 1 calc R . . C71 C 0.35375(16) 0.18982(13) 0.07660(13) 0.0387(5) Uani 1 1 d . . . H71 H 0.4138 0.1677 0.0298 0.046 Uiso 1 1 calc R . . C72 C 0.33394(14) 0.27865(12) 0.09602(12) 0.0334(4) Uani 1 1 d . . . H72 H 0.3809 0.3165 0.0609 0.040 Uiso 1 1 calc R . . C73 C 0.26254(13) 0.48022(11) 0.09172(11) 0.0281(4) Uani 1 1 d . . . C74 C 0.34662(14) 0.52439(12) 0.05633(12) 0.0345(4) Uani 1 1 d . . . H74 H 0.3857 0.5255 0.0893 0.041 Uiso 1 1 calc R . . C75 C 0.37644(15) 0.56694(13) -0.02474(13) 0.0413(5) Uani 1 1 d . . . H75 H 0.4344 0.5961 -0.0456 0.050 Uiso 1 1 calc R . . C76 C 0.32205(16) 0.56674(13) -0.07475(12) 0.0435(5) Uani 1 1 d . . . H76 H 0.3418 0.5954 -0.1302 0.052 Uiso 1 1 calc R . . C77 C 0.23758(16) 0.52359(14) -0.04227(12) 0.0430(5) Uani 1 1 d . . . H77 H 0.1987 0.5230 -0.0755 0.052 Uiso 1 1 calc R . . C78 C 0.20998(15) 0.48163(13) 0.03817(12) 0.0365(4) Uani 1 1 d . . . H78 H 0.1523 0.4521 0.0584 0.044 Uiso 1 1 calc R . . C79 C 0.88297(14) 0.93154(13) 0.05683(11) 0.0346(4) Uani 1 1 d . . . H79A H 0.9186 0.9824 0.0464 0.052 Uiso 1 1 calc R . . H79B H 0.8408 0.9418 0.0225 0.052 Uiso 1 1 calc R . . H79C H 0.9341 0.8758 0.0416 0.052 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 0.02204(10) 0.02373(11) 0.02171(10) -0.00207(7) -0.00696(8) -0.00440(8) P1 0.0231(2) 0.0232(2) 0.0224(2) -0.00351(17) -0.00917(17) -0.00369(17) O1 0.0289(6) 0.0282(6) 0.0220(6) 0.0031(5) -0.0128(5) -0.0104(5) N1 0.0236(7) 0.0228(7) 0.0226(7) -0.0045(5) -0.0084(6) -0.0025(6) C1 0.0269(9) 0.0264(8) 0.0196(8) -0.0031(7) -0.0105(7) -0.0011(7) B1 0.0269(10) 0.0250(10) 0.0307(10) -0.0029(8) -0.0100(8) -0.0024(8) C1S 0.108(3) 0.105(3) 0.0467(16) -0.0037(16) -0.0262(18) 0.026(2) P2 0.0218(2) 0.0223(2) 0.0227(2) 0.00056(16) -0.01031(17) -0.00463(16) N2 0.0206(7) 0.0228(7) 0.0237(7) -0.0006(5) -0.0085(6) -0.0042(5) C2 0.0281(9) 0.0257(8) 0.0221(8) -0.0048(7) -0.0095(7) -0.0026(7) C2S 0.0645(18) 0.088(2) 0.104(3) -0.0367(19) -0.0454(19) -0.0009(16) C3 0.0328(9) 0.0325(9) 0.0265(9) -0.0054(7) -0.0143(8) -0.0044(8) C3S 0.0512(15) 0.0571(16) 0.085(2) -0.0033(14) -0.0091(14) -0.0136(12) C4 0.0418(11) 0.0407(11) 0.0245(9) -0.0028(8) -0.0183(8) -0.0037(8) C4S 0.0752(18) 0.0537(15) 0.0580(16) -0.0034(12) -0.0236(14) 0.0053(14) C5 0.0374(10) 0.0342(10) 0.0204(9) 0.0014(7) -0.0094(8) -0.0039(8) C5S 0.0662(17) 0.0486(15) 0.109(2) -0.0127(16) -0.0489(18) -0.0037(13) C6 0.0270(9) 0.0255(8) 0.0211(8) -0.0024(7) -0.0073(7) -0.0016(7) C6S 0.0597(17) 0.0518(16) 0.111(3) 0.0213(17) -0.0071(18) -0.0147(13) C7 0.0266(9) 0.0254(8) 0.0218(8) -0.0002(7) -0.0072(7) -0.0033(7) C8 0.0393(10) 0.0333(10) 0.0261(9) 0.0074(8) -0.0104(8) -0.0116(8) C9 0.0415(11) 0.0386(11) 0.0374(10) 0.0105(8) -0.0147(9) -0.0229(9) C10 0.0350(10) 0.0328(10) 0.0334(10) 0.0031(8) -0.0160(8) -0.0133(8) C11 0.0249(8) 0.0251(8) 0.0243(8) 0.0011(7) -0.0094(7) -0.0051(7) C12 0.0241(8) 0.0226(8) 0.0246(8) -0.0002(7) -0.0074(7) -0.0055(7) C13 0.0339(9) 0.0262(9) 0.0280(9) 0.0008(7) -0.0162(8) -0.0088(7) C14 0.0357(10) 0.0375(10) 0.0388(11) -0.0042(8) -0.0157(9) -0.0122(8) C15 0.0411(11) 0.0581(13) 0.0429(12) -0.0030(10) -0.0184(10) -0.0215(10) C16 0.0596(14) 0.0535(13) 0.0377(11) 0.0013(10) -0.0246(10) -0.0307(11) C17 0.0707(15) 0.0365(11) 0.0372(11) -0.0077(9) -0.0289(11) -0.0100(10) C18 0.0446(11) 0.0362(10) 0.0352(10) -0.0068(8) -0.0223(9) -0.0038(9) C19 0.0226(8) 0.0280(9) 0.0263(9) -0.0055(7) -0.0118(7) -0.0026(7) C20 0.0304(9) 0.0278(9) 0.0333(10) -0.0043(7) -0.0131(8) -0.0033(7) C21 0.0359(10) 0.0298(10) 0.0466(12) -0.0109(8) -0.0168(9) 0.0024(8) C22 0.0266(9) 0.0464(12) 0.0379(11) -0.0171(9) -0.0105(8) 0.0049(8) C23 0.0293(10) 0.0464(11) 0.0286(10) -0.0035(8) -0.0074(8) -0.0013(8) C24 0.0283(9) 0.0299(9) 0.0315(10) -0.0019(7) -0.0098(8) -0.0005(7) C25 0.0242(8) 0.0263(8) 0.0219(8) -0.0047(7) -0.0115(7) -0.0021(7) C26 0.0279(9) 0.0266(9) 0.0288(9) -0.0012(7) -0.0126(7) -0.0040(7) C27 0.0407(11) 0.0255(9) 0.0408(11) -0.0034(8) -0.0172(9) -0.0009(8) C28 0.0345(10) 0.0378(11) 0.0360(10) -0.0126(8) -0.0128(9) 0.0091(8) C29 0.0290(9) 0.0431(11) 0.0271(9) -0.0059(8) -0.0047(8) -0.0024(8) C30 0.0300(9) 0.0304(9) 0.0257(9) 0.0003(7) -0.0090(7) -0.0065(7) C31 0.0318(10) 0.0283(9) 0.0416(11) 0.0031(8) -0.0088(8) -0.0060(8) C32 0.0528(13) 0.0649(14) 0.0328(11) -0.0027(10) -0.0081(10) -0.0287(11) C33 0.0646(15) 0.0746(17) 0.0469(13) 0.0074(12) -0.0219(12) -0.0424(13) C34 0.0228(8) 0.0229(8) 0.0271(9) -0.0024(7) -0.0100(7) -0.0051(7) C35 0.0286(9) 0.0320(9) 0.0302(9) -0.0006(7) -0.0138(8) -0.0041(7) C36 0.0349(10) 0.0424(11) 0.0267(9) -0.0021(8) -0.0080(8) -0.0079(8) C37 0.0282(10) 0.0412(11) 0.0387(11) -0.0115(9) -0.0053(8) -0.0017(8) C38 0.0332(10) 0.0393(11) 0.0446(12) -0.0052(9) -0.0186(9) 0.0054(8) C39 0.0323(10) 0.0328(10) 0.0319(10) -0.0019(8) -0.0153(8) 0.0000(8) C40 0.0233(8) 0.0303(9) 0.0236(8) 0.0016(7) -0.0098(7) -0.0095(7) C41 0.0294(9) 0.0338(10) 0.0302(9) -0.0014(7) -0.0137(8) -0.0062(8) C42 0.0276(10) 0.0501(12) 0.0372(10) 0.0013(9) -0.0170(8) -0.0053(8) C43 0.0357(10) 0.0560(13) 0.0367(11) -0.0006(9) -0.0187(9) -0.0202(9) C44 0.0406(11) 0.0414(11) 0.0356(10) -0.0039(8) -0.0152(9) -0.0185(9) C45 0.0308(9) 0.0319(9) 0.0324(10) -0.0007(8) -0.0132(8) -0.0093(8) C46 0.0213(8) 0.0268(8) 0.0254(8) -0.0059(7) -0.0101(7) -0.0039(7) C47 0.0250(9) 0.0267(9) 0.0310(9) -0.0036(7) -0.0118(7) -0.0034(7) C48 0.0297(10) 0.0292(10) 0.0469(12) -0.0049(8) -0.0113(9) 0.0009(8) C49 0.0243(9) 0.0409(11) 0.0487(12) -0.0140(9) -0.0047(9) 0.0019(8) C50 0.0278(9) 0.0448(11) 0.0299(10) -0.0084(8) -0.0033(8) -0.0093(8) C51 0.0291(9) 0.0322(9) 0.0286(9) -0.0030(7) -0.0104(8) -0.0066(7) C52 0.0263(9) 0.0259(9) 0.0363(10) 0.0026(7) -0.0108(8) -0.0006(7) C53 0.0492(12) 0.0367(11) 0.0343(11) 0.0013(8) -0.0150(9) -0.0003(9) C54 0.0350(10) 0.0294(10) 0.0499(12) 0.0053(9) -0.0127(9) -0.0023(8) C55 0.0278(9) 0.0314(9) 0.0249(9) -0.0014(7) -0.0064(7) -0.0045(7) C56 0.0384(11) 0.0344(10) 0.0431(11) -0.0041(8) -0.0178(9) -0.0054(8) C57 0.0438(12) 0.0483(12) 0.0404(11) -0.0055(9) -0.0157(9) -0.0159(10) C58 0.0376(11) 0.0670(14) 0.0282(10) -0.0028(9) -0.0138(9) -0.0136(10) C59 0.0410(11) 0.0544(13) 0.0325(10) -0.0026(9) -0.0186(9) 0.0055(10) C60 0.0416(11) 0.0362(10) 0.0284(10) -0.0034(8) -0.0138(8) -0.0007(8) C61 0.0311(10) 0.0237(9) 0.0355(10) 0.0025(7) -0.0084(8) -0.0019(7) C62 0.0426(11) 0.0332(10) 0.0428(12) -0.0079(9) -0.0030(9) -0.0089(9) C63 0.0530(14) 0.0384(12) 0.0531(14) -0.0137(10) 0.0086(11) -0.0090(10) C64 0.0353(12) 0.0360(12) 0.0694(16) 0.0022(11) 0.0082(11) 0.0033(9) C65 0.0308(11) 0.0545(14) 0.0630(15) 0.0176(12) -0.0123(11) -0.0038(10) C66 0.0333(11) 0.0483(12) 0.0407(11) 0.0051(9) -0.0105(9) -0.0038(9) C67 0.0321(9) 0.0262(9) 0.0301(9) -0.0001(7) -0.0172(8) -0.0020(7) C68 0.0435(11) 0.0321(10) 0.0339(10) 0.0027(8) -0.0148(9) -0.0071(8) C69 0.0683(15) 0.0320(11) 0.0511(13) 0.0104(9) -0.0295(12) -0.0191(10) C70 0.0735(15) 0.0252(10) 0.0512(13) -0.0044(9) -0.0374(12) -0.0002(10) C71 0.0463(11) 0.0344(10) 0.0391(11) -0.0085(9) -0.0257(9) 0.0071(9) C72 0.0347(10) 0.0318(10) 0.0356(10) -0.0039(8) -0.0176(8) -0.0008(8) C73 0.0268(9) 0.0213(8) 0.0312(9) -0.0059(7) -0.0078(7) 0.0022(7) C74 0.0330(10) 0.0303(9) 0.0376(10) -0.0034(8) -0.0111(8) -0.0042(8) C75 0.0357(11) 0.0350(10) 0.0414(11) 0.0001(9) -0.0034(9) -0.0065(8) C76 0.0473(12) 0.0365(11) 0.0290(10) 0.0012(8) -0.0040(9) 0.0046(9) C77 0.0430(12) 0.0496(12) 0.0336(11) -0.0031(9) -0.0170(9) 0.0016(10) C78 0.0343(10) 0.0389(11) 0.0348(10) -0.0018(8) -0.0118(8) -0.0067(8) C79 0.0306(10) 0.0459(11) 0.0260(9) -0.0034(8) -0.0053(8) -0.0141(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 C79 1.9609(17) . ? Zn1 N1 2.0499(13) . ? Zn1 N2 2.0556(13) . ? P1 N1 1.6009(14) . ? P1 C19 1.7905(17) . ? P1 C13 1.8067(17) . ? P1 C2 1.8101(17) . ? O1 C1 1.3766(19) . ? O1 C12 1.3763(19) . ? N1 C25 1.445(2) . ? C1 C2 1.385(2) . ? C1 C6 1.395(2) . ? B1 C55 1.646(3) . ? B1 C67 1.648(3) . ? B1 C61 1.653(3) . ? B1 C73 1.666(3) . ? C1S C2S 1.387(5) . ? C1S C6S 1.405(5) . ? C1S H1S 0.9500 . ? P2 N2 1.6074(13) . ? P2 C34 1.7974(17) . ? P2 C40 1.8054(16) . ? P2 C11 1.8184(16) . ? N2 C46 1.441(2) . ? C2 C3 1.395(2) . ? C2S C3S 1.335(4) . ? C2S H2S 0.9500 . ? C3 C4 1.400(3) . ? C3 H3 0.9500 . ? C3S C4S 1.330(4) . ? C3S H3S 0.9500 . ? C4 C5 1.381(3) . ? C4 H4 0.9500 . ? C4S C5S 1.338(4) . ? C4S H4S 0.9500 . ? C5 C6 1.393(2) . ? C5 H5 0.9500 . ? C5S C6S 1.340(4) . ? C5S H5S 0.9500 . ? C6 C7 1.453(2) . ? C6S H6S 0.9500 . ? C7 C12 1.391(2) . ? C7 C8 1.396(2) . ? C8 C9 1.381(3) . ? C8 H8 0.9500 . ? C9 C10 1.392(3) . ? C9 H9 0.9500 . ? C10 C11 1.394(2) . ? C10 H10 0.9500 . ? C11 C12 1.385(2) . ? C13 C18 1.391(3) . ? C13 C14 1.397(3) . ? C14 C15 1.381(3) . ? C14 H14 0.9500 . ? C15 C16 1.370(3) . ? C15 H15 0.9500 . ? C16 C17 1.378(3) . ? C16 H16 0.9500 . ? C17 C18 1.391(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.393(2) . ? C19 C20 1.394(2) . ? C20 C21 1.384(3) . ? C20 H20 0.9500 . ? C21 C22 1.380(3) . ? C21 H21 0.9500 . ? C22 C23 1.386(3) . ? C22 H22 0.9500 . ? C23 C24 1.377(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.393(2) . ? C25 C26 1.406(2) . ? C26 C27 1.397(2) . ? C26 C31 1.516(2) . ? C27 C28 1.381(3) . ? C27 H27 0.9500 . ? C28 C29 1.379(3) . ? C28 H28 0.9500 . ? C29 C30 1.380(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.519(3) . ? C31 C33 1.528(3) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.390(2) . ? C34 C39 1.391(2) . ? C35 C36 1.375(3) . ? C35 H35 0.9500 . ? C36 C37 1.383(3) . ? C36 H36 0.9500 . ? C37 C38 1.379(3) . ? C37 H37 0.9500 . ? C38 C39 1.383(3) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.393(2) . ? C40 C45 1.399(2) . ? C41 C42 1.391(2) . ? C41 H41 0.9500 . ? C42 C43 1.379(3) . ? C42 H42 0.9500 . ? C43 C44 1.381(3) . ? C43 H43 0.9500 . ? C44 C45 1.382(2) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C51 1.395(2) . ? C46 C47 1.405(2) . ? C47 C48 1.395(2) . ? C47 C52 1.520(2) . ? C48 C49 1.378(3) . ? C48 H48 0.9500 . ? C49 C50 1.374(3) . ? C49 H49 0.9500 . ? C50 C51 1.386(3) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C54 1.529(2) . ? C52 C53 1.530(3) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C60 1.394(3) . ? C55 C56 1.405(3) . ? C56 C57 1.386(3) . ? C56 H56 0.9500 . ? C57 C58 1.377(3) . ? C57 H57 0.9500 . ? C58 C59 1.373(3) . ? C58 H58 0.9500 . ? C59 C60 1.392(3) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C62 1.399(3) . ? C61 C66 1.405(3) . ? C62 C63 1.390(3) . ? C62 H62 0.9500 . ? C63 C64 1.365(4) . ? C63 H63 0.9500 . ? C64 C65 1.382(4) . ? C64 H64 0.9500 . ? C65 C66 1.389(3) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C68 1.393(3) . ? C67 C72 1.398(3) . ? C68 C69 1.395(3) . ? C68 H68 0.9500 . ? C69 C70 1.374(3) . ? C69 H69 0.9500 . ? C70 C71 1.376(3) . ? C70 H70 0.9500 . ? C71 C72 1.383(3) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.395(3) . ? C73 C78 1.403(3) . ? C74 C75 1.393(3) . ? C74 H74 0.9500 . ? C75 C76 1.377(3) . ? C75 H75 0.9500 . ? C76 C77 1.390(3) . ? C76 H76 0.9500 . ? C77 C78 1.381(3) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 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 C79 Zn1 N1 123.67(7) . . ? C79 Zn1 N2 122.37(7) . . ? N1 Zn1 N2 113.30(5) . . ? N1 P1 C19 106.73(7) . . ? N1 P1 C13 115.21(7) . . ? C19 P1 C13 107.29(8) . . ? N1 P1 C2 115.98(7) . . ? C19 P1 C2 106.87(8) . . ? C13 P1 C2 104.23(8) . . ? C1 O1 C12 105.56(12) . . ? C25 N1 P1 122.03(11) . . ? C25 N1 Zn1 113.73(10) . . ? P1 N1 Zn1 122.69(7) . . ? O1 C1 C2 122.78(14) . . ? O1 C1 C6 111.84(14) . . ? C2 C1 C6 125.36(15) . . ? C55 B1 C67 109.36(14) . . ? C55 B1 C61 110.76(14) . . ? C67 B1 C61 109.48(14) . . ? C55 B1 C73 109.40(14) . . ? C67 B1 C73 106.22(14) . . ? C61 B1 C73 111.51(14) . . ? C2S C1S C6S 118.4(3) . . ? C2S C1S H1S 120.8 . . ? C6S C1S H1S 120.8 . . ? N2 P2 C34 108.09(7) . . ? N2 P2 C40 115.84(7) . . ? C34 P2 C40 106.00(8) . . ? N2 P2 C11 113.91(7) . . ? C34 P2 C11 106.47(8) . . ? C40 P2 C11 105.88(7) . . ? C46 N2 P2 119.97(11) . . ? C46 N2 Zn1 121.72(10) . . ? P2 N2 Zn1 117.73(7) . . ? C1 C2 C3 114.71(15) . . ? C1 C2 P1 119.96(12) . . ? C3 C2 P1 125.27(13) . . ? C3S C2S C1S 119.5(3) . . ? C3S C2S H2S 120.3 . . ? C1S C2S H2S 120.3 . . ? C2 C3 C4 121.59(16) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C4S C3S C2S 121.1(3) . . ? C4S C3S H3S 119.5 . . ? C2S C3S H3S 119.5 . . ? C5 C4 C3 121.73(16) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C3S C4S C5S 121.4(3) . . ? C3S C4S H4S 119.3 . . ? C5S C4S H4S 119.3 . . ? C4 C5 C6 118.36(16) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? C6S C5S C4S 120.6(3) . . ? C6S C5S H5S 119.7 . . ? C4S C5S H5S 119.7 . . ? C5 C6 C1 118.21(16) . . ? C5 C6 C7 136.52(16) . . ? C1 C6 C7 105.21(14) . . ? C5S C6S C1S 119.1(3) . . ? C5S C6S H6S 120.5 . . ? C1S C6S H6S 120.5 . . ? C12 C7 C8 117.84(16) . . ? C12 C7 C6 105.54(14) . . ? C8 C7 C6 136.62(16) . . ? C9 C8 C7 118.39(16) . . ? C9 C8 H8 120.8 . . ? C7 C8 H8 120.8 . . ? C8 C9 C10 122.17(17) . . ? C8 C9 H9 118.9 . . ? C10 C9 H9 118.9 . . ? C9 C10 C11 121.06(17) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C12 C11 C10 115.17(15) . . ? C12 C11 P2 118.20(12) . . ? C10 C11 P2 126.55(13) . . ? O1 C12 C11 122.79(14) . . ? O1 C12 C7 111.84(14) . . ? C11 C12 C7 125.36(15) . . ? C18 C13 C14 119.36(16) . . ? C18 C13 P1 121.40(14) . . ? C14 C13 P1 119.21(13) . . ? C15 C14 C13 120.30(18) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 120.0(2) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.52(18) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C18 120.30(19) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C13 C18 C17 119.46(19) . . ? C13 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C24 C19 C20 119.68(16) . . ? C24 C19 P1 117.98(13) . . ? C20 C19 P1 122.28(13) . . ? C21 C20 C19 119.68(17) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C22 C21 C20 120.35(17) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 120.03(17) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.22(18) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C19 120.03(17) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C30 C25 C26 119.97(15) . . ? C30 C25 N1 119.27(15) . . ? C26 C25 N1 120.64(14) . . ? C27 C26 C25 117.24(16) . . ? C27 C26 C31 120.20(16) . . ? C25 C26 C31 122.56(15) . . ? C28 C27 C26 122.28(17) . . ? C28 C27 H27 118.9 . . ? C26 C27 H27 118.9 . . ? C27 C28 C29 119.88(17) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C30 C29 C28 119.25(17) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C29 C30 C25 121.38(17) . . ? C29 C30 H30 119.3 . . ? C25 C30 H30 119.3 . . ? C26 C31 C32 111.16(16) . . ? C26 C31 C33 112.66(17) . . ? C32 C31 C33 109.33(17) . . ? C26 C31 H31 107.8 . . ? C32 C31 H31 107.8 . . ? C33 C31 H31 107.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C39 119.49(16) . . ? C35 C34 P2 117.03(12) . . ? C39 C34 P2 123.46(13) . . ? C36 C35 C34 120.52(16) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C37 119.80(17) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C38 C37 C36 120.17(17) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C39 120.36(17) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C38 C39 C34 119.63(17) . . ? C38 C39 H39 120.2 . . ? C34 C39 H39 120.2 . . ? C41 C40 C45 119.43(15) . . ? C41 C40 P2 123.26(13) . . ? C45 C40 P2 117.28(13) . . ? C40 C41 C42 119.39(17) . . ? C40 C41 H41 120.3 . . ? C42 C41 H41 120.3 . . ? C43 C42 C41 120.70(18) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C42 C43 C44 120.12(17) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C45 C44 C43 119.99(18) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C40 120.36(17) . . ? C44 C45 H45 119.8 . . ? C40 C45 H45 119.8 . . ? C51 C46 C47 119.46(15) . . ? C51 C46 N2 121.23(15) . . ? C47 C46 N2 119.31(14) . . ? C48 C47 C46 117.55(16) . . ? C48 C47 C52 120.76(15) . . ? C46 C47 C52 121.67(15) . . ? C49 C48 C47 122.43(18) . . ? C49 C48 H48 118.8 . . ? C47 C48 H48 118.8 . . ? C50 C49 C48 119.76(17) . . ? C50 C49 H49 120.1 . . ? C48 C49 H49 120.1 . . ? C49 C50 C51 119.36(17) . . ? C49 C50 H50 120.3 . . ? C51 C50 H50 120.3 . . ? C50 C51 C46 121.40(17) . . ? C50 C51 H51 119.3 . . ? C46 C51 H51 119.3 . . ? C47 C52 C54 113.83(15) . . ? C47 C52 C53 111.57(15) . . ? C54 C52 C53 110.04(15) . . ? C47 C52 H52 107.0 . . ? C54 C52 H52 107.0 . . ? C53 C52 H52 107.0 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C60 C55 C56 114.45(17) . . ? C60 C55 B1 123.11(16) . . ? C56 C55 B1 122.40(16) . . ? C57 C56 C55 122.99(18) . . ? C57 C56 H56 118.5 . . ? C55 C56 H56 118.5 . . ? C58 C57 C56 120.51(19) . . ? C58 C57 H57 119.7 . . ? C56 C57 H57 119.7 . . ? C59 C58 C57 118.44(19) . . ? C59 C58 H58 120.8 . . ? C57 C58 H58 120.8 . . ? C58 C59 C60 120.64(19) . . ? C58 C59 H59 119.7 . . ? C60 C59 H59 119.7 . . ? C55 C60 C59 122.94(18) . . ? C55 C60 H60 118.5 . . ? C59 C60 H60 118.5 . . ? C62 C61 C66 114.34(18) . . ? C62 C61 B1 124.47(17) . . ? C66 C61 B1 121.18(17) . . ? C63 C62 C61 122.8(2) . . ? C63 C62 H62 118.6 . . ? C61 C62 H62 118.6 . . ? C64 C63 C62 120.7(2) . . ? C64 C63 H63 119.7 . . ? C62 C63 H63 119.7 . . ? C63 C64 C65 119.1(2) . . ? C63 C64 H64 120.4 . . ? C65 C64 H64 120.4 . . ? C64 C65 C66 119.7(2) . . ? C64 C65 H65 120.2 . . ? C66 C65 H65 120.2 . . ? C65 C66 C61 123.3(2) . . ? C65 C66 H66 118.3 . . ? C61 C66 H66 118.3 . . ? C68 C67 C72 115.14(16) . . ? C68 C67 B1 124.76(16) . . ? C72 C67 B1 120.07(16) . . ? C67 C68 C69 121.95(19) . . ? C67 C68 H68 119.0 . . ? C69 C68 H68 119.0 . . ? C70 C69 C68 120.9(2) . . ? C70 C69 H69 119.5 . . ? C68 C69 H69 119.5 . . ? C69 C70 C71 118.70(18) . . ? C69 C70 H70 120.7 . . ? C71 C70 H70 120.7 . . ? C70 C71 C72 119.95(19) . . ? C70 C71 H71 120.0 . . ? C72 C71 H71 120.0 . . ? C71 C72 C67 123.31(18) . . ? C71 C72 H72 118.3 . . ? C67 C72 H72 118.3 . . ? C74 C73 C78 114.11(17) . . ? C74 C73 B1 123.93(16) . . ? C78 C73 B1 121.67(16) . . ? C75 C74 C73 123.60(18) . . ? C75 C74 H74 118.2 . . ? C73 C74 H74 118.2 . . ? C76 C75 C74 120.08(19) . . ? C76 C75 H75 120.0 . . ? C74 C75 H75 120.0 . . ? C75 C76 C77 118.47(18) . . ? C75 C76 H76 120.8 . . ? C77 C76 H76 120.8 . . ? C78 C77 C76 120.24(19) . . ? C78 C77 H77 119.9 . . ? C76 C77 H77 119.9 . . ? C77 C78 C73 123.50(18) . . ? C77 C78 H78 118.2 . . ? C73 C78 H78 118.2 . . ? Zn1 C79 H79A 109.5 . . ? Zn1 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? Zn1 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C19 P1 N1 C25 -166.44(12) . . . . ? C13 P1 N1 C25 -47.47(15) . . . . ? C2 P1 N1 C25 74.65(14) . . . . ? C19 P1 N1 Zn1 28.61(11) . . . . ? C13 P1 N1 Zn1 147.59(9) . . . . ? C2 P1 N1 Zn1 -90.30(10) . . . . ? C79 Zn1 N1 C25 113.93(12) . . . . ? N2 Zn1 N1 C25 -56.93(12) . . . . ? C79 Zn1 N1 P1 -79.99(11) . . . . ? N2 Zn1 N1 P1 109.15(9) . . . . ? C12 O1 C1 C2 179.23(15) . . . . ? C12 O1 C1 C6 0.74(17) . . . . ? C34 P2 N2 C46 168.92(12) . . . . ? C40 P2 N2 C46 50.20(14) . . . . ? C11 P2 N2 C46 -72.98(13) . . . . ? C34 P2 N2 Zn1 -19.69(10) . . . . ? C40 P2 N2 Zn1 -138.41(8) . . . . ? C11 P2 N2 Zn1 98.42(9) . . . . ? C79 Zn1 N2 C46 -115.98(13) . . . . ? N1 Zn1 N2 C46 55.01(13) . . . . ? C79 Zn1 N2 P2 72.78(11) . . . . ? N1 Zn1 N2 P2 -116.22(8) . . . . ? O1 C1 C2 C3 -176.09(14) . . . . ? C6 C1 C2 C3 2.2(2) . . . . ? O1 C1 C2 P1 1.3(2) . . . . ? C6 C1 C2 P1 179.53(13) . . . . ? N1 P1 C2 C1 39.83(16) . . . . ? C19 P1 C2 C1 -79.01(15) . . . . ? C13 P1 C2 C1 167.59(13) . . . . ? N1 P1 C2 C3 -143.13(14) . . . . ? C19 P1 C2 C3 98.03(15) . . . . ? C13 P1 C2 C3 -15.37(17) . . . . ? C6S C1S C2S C3S -1.2(5) . . . . ? C1 C2 C3 C4 -1.3(2) . . . . ? P1 C2 C3 C4 -178.46(14) . . . . ? C1S C2S C3S C4S 0.4(4) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? C2S C3S C4S C5S 0.1(4) . . . . ? C3 C4 C5 C6 0.9(3) . . . . ? C3S C4S C5S C6S 0.1(4) . . . . ? C4 C5 C6 C1 -0.1(2) . . . . ? C4 C5 C6 C7 176.85(18) . . . . ? O1 C1 C6 C5 176.89(14) . . . . ? C2 C1 C6 C5 -1.5(3) . . . . ? O1 C1 C6 C7 -0.93(18) . . . . ? C2 C1 C6 C7 -179.37(16) . . . . ? C4S C5S C6S C1S -0.9(4) . . . . ? C2S C1S C6S C5S 1.5(4) . . . . ? C5 C6 C7 C12 -176.48(19) . . . . ? C1 C6 C7 C12 0.74(18) . . . . ? C5 C6 C7 C8 2.2(4) . . . . ? C1 C6 C7 C8 179.5(2) . . . . ? C12 C7 C8 C9 -0.9(3) . . . . ? C6 C7 C8 C9 -179.50(19) . . . . ? C7 C8 C9 C10 0.9(3) . . . . ? C8 C9 C10 C11 -0.1(3) . . . . ? C9 C10 C11 C12 -0.6(3) . . . . ? C9 C10 C11 P2 -177.35(15) . . . . ? N2 P2 C11 C12 -40.62(15) . . . . ? C34 P2 C11 C12 78.42(14) . . . . ? C40 P2 C11 C12 -169.06(13) . . . . ? N2 P2 C11 C10 136.06(15) . . . . ? C34 P2 C11 C10 -104.91(16) . . . . ? C40 P2 C11 C10 7.61(18) . . . . ? C1 O1 C12 C11 -179.76(15) . . . . ? C1 O1 C12 C7 -0.23(17) . . . . ? C10 C11 C12 O1 -179.98(15) . . . . ? P2 C11 C12 O1 -2.9(2) . . . . ? C10 C11 C12 C7 0.6(3) . . . . ? P2 C11 C12 C7 177.61(13) . . . . ? C8 C7 C12 O1 -179.33(15) . . . . ? C6 C7 C12 O1 -0.32(18) . . . . ? C8 C7 C12 C11 0.2(3) . . . . ? C6 C7 C12 C11 179.19(16) . . . . ? N1 P1 C13 C18 50.99(17) . . . . ? C19 P1 C13 C18 169.66(14) . . . . ? C2 P1 C13 C18 -77.24(16) . . . . ? N1 P1 C13 C14 -130.70(14) . . . . ? C19 P1 C13 C14 -12.03(16) . . . . ? C2 P1 C13 C14 101.07(15) . . . . ? C18 C13 C14 C15 -1.3(3) . . . . ? P1 C13 C14 C15 -179.63(15) . . . . ? C13 C14 C15 C16 -1.0(3) . . . . ? C14 C15 C16 C17 1.8(3) . . . . ? C15 C16 C17 C18 -0.4(3) . . . . ? C14 C13 C18 C17 2.7(3) . . . . ? P1 C13 C18 C17 -178.98(14) . . . . ? C16 C17 C18 C13 -1.9(3) . . . . ? N1 P1 C19 C24 55.72(15) . . . . ? C13 P1 C19 C24 -68.29(15) . . . . ? C2 P1 C19 C24 -179.60(13) . . . . ? N1 P1 C19 C20 -127.07(14) . . . . ? C13 P1 C19 C20 108.92(14) . . . . ? C2 P1 C19 C20 -2.38(16) . . . . ? C24 C19 C20 C21 -0.7(3) . . . . ? P1 C19 C20 C21 -177.87(14) . . . . ? C19 C20 C21 C22 -0.2(3) . . . . ? C20 C21 C22 C23 1.2(3) . . . . ? C21 C22 C23 C24 -1.2(3) . . . . ? C22 C23 C24 C19 0.2(3) . . . . ? C20 C19 C24 C23 0.7(3) . . . . ? P1 C19 C24 C23 177.99(14) . . . . ? P1 N1 C25 C30 -82.61(18) . . . . ? Zn1 N1 C25 C30 83.58(16) . . . . ? P1 N1 C25 C26 101.44(16) . . . . ? Zn1 N1 C25 C26 -92.37(15) . . . . ? C30 C25 C26 C27 -0.9(2) . . . . ? N1 C25 C26 C27 175.05(15) . . . . ? C30 C25 C26 C31 179.37(16) . . . . ? N1 C25 C26 C31 -4.7(2) . . . . ? C25 C26 C27 C28 0.4(3) . . . . ? C31 C26 C27 C28 -179.86(18) . . . . ? C26 C27 C28 C29 0.3(3) . . . . ? C27 C28 C29 C30 -0.4(3) . . . . ? C28 C29 C30 C25 -0.1(3) . . . . ? C26 C25 C30 C29 0.8(3) . . . . ? N1 C25 C30 C29 -175.21(15) . . . . ? C27 C26 C31 C32 -78.6(2) . . . . ? C25 C26 C31 C32 101.1(2) . . . . ? C27 C26 C31 C33 44.5(2) . . . . ? C25 C26 C31 C33 -135.78(19) . . . . ? N2 P2 C34 C35 -76.37(14) . . . . ? C40 P2 C34 C35 48.43(15) . . . . ? C11 P2 C34 C35 160.87(13) . . . . ? N2 P2 C34 C39 105.09(15) . . . . ? C40 P2 C34 C39 -130.10(15) . . . . ? C11 P2 C34 C39 -17.67(16) . . . . ? C39 C34 C35 C36 0.0(3) . . . . ? P2 C34 C35 C36 -178.55(14) . . . . ? C34 C35 C36 C37 -0.9(3) . . . . ? C35 C36 C37 C38 0.8(3) . . . . ? C36 C37 C38 C39 0.1(3) . . . . ? C37 C38 C39 C34 -1.0(3) . . . . ? C35 C34 C39 C38 0.9(3) . . . . ? P2 C34 C39 C38 179.42(14) . . . . ? N2 P2 C40 C41 -16.48(17) . . . . ? C34 P2 C40 C41 -136.34(14) . . . . ? C11 P2 C40 C41 110.82(15) . . . . ? N2 P2 C40 C45 161.66(12) . . . . ? C34 P2 C40 C45 41.79(15) . . . . ? C11 P2 C40 C45 -71.05(15) . . . . ? C45 C40 C41 C42 0.9(3) . . . . ? P2 C40 C41 C42 178.99(13) . . . . ? C40 C41 C42 C43 -0.1(3) . . . . ? C41 C42 C43 C44 -0.3(3) . . . . ? C42 C43 C44 C45 -0.1(3) . . . . ? C43 C44 C45 C40 0.9(3) . . . . ? C41 C40 C45 C44 -1.3(3) . . . . ? P2 C40 C45 C44 -179.50(14) . . . . ? P2 N2 C46 C51 45.51(19) . . . . ? Zn1 N2 C46 C51 -125.53(14) . . . . ? P2 N2 C46 C47 -133.73(14) . . . . ? Zn1 N2 C46 C47 55.24(18) . . . . ? C51 C46 C47 C48 -2.4(2) . . . . ? N2 C46 C47 C48 176.80(15) . . . . ? C51 C46 C47 C52 179.30(15) . . . . ? N2 C46 C47 C52 -1.5(2) . . . . ? C46 C47 C48 C49 1.0(3) . . . . ? C52 C47 C48 C49 179.25(18) . . . . ? C47 C48 C49 C50 0.5(3) . . . . ? C48 C49 C50 C51 -0.5(3) . . . . ? C49 C50 C51 C46 -1.1(3) . . . . ? C47 C46 C51 C50 2.6(3) . . . . ? N2 C46 C51 C50 -176.67(15) . . . . ? C48 C47 C52 C54 22.6(2) . . . . ? C46 C47 C52 C54 -159.20(16) . . . . ? C48 C47 C52 C53 -102.67(19) . . . . ? C46 C47 C52 C53 75.5(2) . . . . ? C67 B1 C55 C60 1.1(2) . . . . ? C61 B1 C55 C60 121.86(18) . . . . ? C73 B1 C55 C60 -114.84(18) . . . . ? C67 B1 C55 C56 178.94(16) . . . . ? C61 B1 C55 C56 -60.3(2) . . . . ? C73 B1 C55 C56 63.0(2) . . . . ? C60 C55 C56 C57 -0.3(3) . . . . ? B1 C55 C56 C57 -178.30(17) . . . . ? C55 C56 C57 C58 1.5(3) . . . . ? C56 C57 C58 C59 -1.4(3) . . . . ? C57 C58 C59 C60 0.3(3) . . . . ? C56 C55 C60 C59 -0.9(3) . . . . ? B1 C55 C60 C59 177.08(17) . . . . ? C58 C59 C60 C55 1.0(3) . . . . ? C55 B1 C61 C62 5.6(2) . . . . ? C67 B1 C61 C62 126.28(18) . . . . ? C73 B1 C61 C62 -116.47(19) . . . . ? C55 B1 C61 C66 -173.04(16) . . . . ? C67 B1 C61 C66 -52.4(2) . . . . ? C73 B1 C61 C66 64.9(2) . . . . ? C66 C61 C62 C63 -2.9(3) . . . . ? B1 C61 C62 C63 178.40(18) . . . . ? C61 C62 C63 C64 1.2(3) . . . . ? C62 C63 C64 C65 1.3(3) . . . . ? C63 C64 C65 C66 -1.8(3) . . . . ? C64 C65 C66 C61 -0.1(3) . . . . ? C62 C61 C66 C65 2.3(3) . . . . ? B1 C61 C66 C65 -178.92(18) . . . . ? C55 B1 C67 C68 102.19(19) . . . . ? C61 B1 C67 C68 -19.3(2) . . . . ? C73 B1 C67 C68 -139.85(17) . . . . ? C55 B1 C67 C72 -75.79(19) . . . . ? C61 B1 C67 C72 162.69(15) . . . . ? C73 B1 C67 C72 42.2(2) . . . . ? C72 C67 C68 C69 -1.4(3) . . . . ? B1 C67 C68 C69 -179.51(18) . . . . ? C67 C68 C69 C70 2.1(3) . . . . ? C68 C69 C70 C71 -1.0(3) . . . . ? C69 C70 C71 C72 -0.5(3) . . . . ? C70 C71 C72 C67 1.1(3) . . . . ? C68 C67 C72 C71 -0.1(3) . . . . ? B1 C67 C72 C71 178.06(16) . . . . ? C55 B1 C73 C74 3.3(2) . . . . ? C67 B1 C73 C74 -114.66(17) . . . . ? C61 B1 C73 C74 126.13(17) . . . . ? C55 B1 C73 C78 176.73(15) . . . . ? C67 B1 C73 C78 58.8(2) . . . . ? C61 B1 C73 C78 -60.4(2) . . . . ? C78 C73 C74 C75 0.4(3) . . . . ? B1 C73 C74 C75 174.26(16) . . . . ? C73 C74 C75 C76 -0.1(3) . . . . ? C74 C75 C76 C77 0.1(3) . . . . ? C75 C76 C77 C78 -0.4(3) . . . . ? C76 C77 C78 C73 0.7(3) . . . . ? C74 C73 C78 C77 -0.6(3) . . . . ? B1 C73 C78 C77 -174.68(17) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.337 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.039 #===END data_5b _database_code_depnum_ccdc_archive 'CCDC 833327' #TrackingRef '6184_web_deposit_cif_file_0_PaulG.Hayes_ #1310063407.Chem Eur J_AllCifs - Paul G Hayes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76.18 H63.47 B N2 O P2 Zn' _chemical_formula_weight 1160.98 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' B B 0.0013 0.0007 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9214(8) _cell_length_b 17.1175(13) _cell_length_c 18.4747(14) _cell_angle_alpha 86.7540(10) _cell_angle_beta 78.7250(10) _cell_angle_gamma 80.8590(10) _cell_volume 3036.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4611 _cell_measurement_theta_min 4.403 _cell_measurement_theta_max 43.128 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1215 _exptl_absorpt_coefficient_mu 0.505 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6780 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36687 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_sigmaI/netI 0.0717 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10686 _reflns_number_gt 6972 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0341P)^2^+0.9448P] 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 10686 _refine_ls_number_parameters 784 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.0987 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.008 _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 0.73217(3) 0.803774(19) 0.636425(19) 0.03316(11) Uani 1 1 d . . . P1 P 0.58355(8) 0.64220(4) 0.67542(4) 0.03168(19) Uani 1 1 d . . . O1 O 0.51121(18) 0.77038(10) 0.79108(10) 0.0307(5) Uani 1 1 d . A . N1 N 0.7117(2) 0.69047(13) 0.66535(12) 0.0311(6) Uani 1 1 d . A . C1 C 0.4559(3) 0.70201(16) 0.81208(15) 0.0292(7) Uani 1 1 d . . . B1 B 0.9162(3) 0.70740(19) 0.15074(18) 0.0305(8) Uani 1 1 d . . . P2 P 0.62714(8) 0.92494(4) 0.77480(4) 0.03090(19) Uani 1 1 d . . . N2 N 0.6234(2) 0.89801(12) 0.69365(12) 0.0300(6) Uani 1 1 d . A . C2 C 0.4822(3) 0.63663(16) 0.76767(16) 0.0313(7) Uani 1 1 d . A . C3 C 0.4167(3) 0.57258(17) 0.79883(17) 0.0386(8) Uani 1 1 d . . . H3 H 0.4310 0.5254 0.7718 0.046 Uiso 1 1 calc R A . C4 C 0.3309(3) 0.57635(19) 0.86847(17) 0.0418(8) Uani 1 1 d . A . H4 H 0.2884 0.5316 0.8875 0.050 Uiso 1 1 calc R . . C5 C 0.3061(3) 0.64313(18) 0.91046(17) 0.0395(8) Uani 1 1 d . . . H5 H 0.2478 0.6446 0.9579 0.047 Uiso 1 1 calc R A . C6 C 0.3688(3) 0.70837(17) 0.88156(15) 0.0317(7) Uani 1 1 d . A . C7 C 0.3676(3) 0.78865(16) 0.90436(15) 0.0308(7) Uani 1 1 d . . . C8 C 0.3046(3) 0.83485(19) 0.96479(16) 0.0404(8) Uani 1 1 d . A . H8 H 0.2422 0.8146 1.0045 0.048 Uiso 1 1 calc R . . C9 C 0.3346(3) 0.9108(2) 0.96584(18) 0.0474(9) Uani 1 1 d . . . H9 H 0.2913 0.9429 1.0068 0.057 Uiso 1 1 calc R A . C10 C 0.4265(3) 0.94186(18) 0.90877(17) 0.0413(8) Uani 1 1 d . A . H10 H 0.4455 0.9941 0.9119 0.050 Uiso 1 1 calc R . . C11 C 0.4914(3) 0.89732(17) 0.84698(16) 0.0324(7) Uani 1 1 d . A . C12 C 0.4567(3) 0.82186(16) 0.84775(15) 0.0300(7) Uani 1 1 d . A . C13 C 0.6192(3) 1.02962(16) 0.78042(16) 0.0331(7) Uani 1 1 d . A . C14 C 0.7387(3) 1.06270(18) 0.77963(18) 0.0461(9) Uani 1 1 d . . . H14 H 0.8231 1.0294 0.7841 0.055 Uiso 1 1 calc R A . C15 C 0.7356(4) 1.14338(19) 0.7725(2) 0.0574(10) Uani 1 1 d . A . H15 H 0.8174 1.1657 0.7723 0.069 Uiso 1 1 calc R . . C16 C 0.6123(4) 1.1922(2) 0.7655(2) 0.0594(10) Uani 1 1 d . . . H16 H 0.6108 1.2478 0.7592 0.071 Uiso 1 1 calc R A . C17 C 0.4926(3) 1.16037(18) 0.76773(19) 0.0488(9) Uani 1 1 d . A . H17 H 0.4082 1.1941 0.7642 0.059 Uiso 1 1 calc R . . C18 C 0.4952(3) 1.07939(17) 0.77511(17) 0.0394(8) Uani 1 1 d . . . H18 H 0.4125 1.0575 0.7766 0.047 Uiso 1 1 calc R A . C19 C 0.7864(3) 0.87513(16) 0.79727(16) 0.0319(7) Uani 1 1 d . A . C20 C 0.9086(3) 0.86977(17) 0.74459(17) 0.0381(8) Uani 1 1 d . . . H20 H 0.9071 0.8927 0.6967 0.046 Uiso 1 1 calc R A . C21 C 1.0325(3) 0.83100(18) 0.7619(2) 0.0478(9) Uani 1 1 d . A . H21 H 1.1158 0.8279 0.7260 0.057 Uiso 1 1 calc R . . C22 C 1.0350(3) 0.79708(19) 0.8311(2) 0.0512(9) Uani 1 1 d . . . H22 H 1.1199 0.7700 0.8424 0.061 Uiso 1 1 calc R A . C23 C 0.9162(4) 0.8021(2) 0.8834(2) 0.0526(9) Uani 1 1 d . A . H23 H 0.9186 0.7784 0.9310 0.063 Uiso 1 1 calc R . . C24 C 0.7922(3) 0.84168(18) 0.86724(17) 0.0421(8) Uani 1 1 d . . . H24 H 0.7103 0.8460 0.9042 0.051 Uiso 1 1 calc R A . C25 C 0.5152(3) 0.93894(16) 0.65644(16) 0.0346(7) Uani 1 1 d . . . C26 C 0.5352(4) 1.00568(18) 0.61198(18) 0.0482(9) Uani 1 1 d . A . C27 C 0.4239(4) 1.0419(2) 0.5787(2) 0.0639(11) Uani 1 1 d . . . H27 H 0.4337 1.0888 0.5494 0.077 Uiso 1 1 calc R A . C28 C 0.3025(4) 1.0114(2) 0.5875(2) 0.0615(11) Uani 1 1 d . A . H28 H 0.2290 1.0375 0.5648 0.074 Uiso 1 1 calc R . . C29 C 0.2859(4) 0.9439(2) 0.62863(19) 0.0504(9) Uani 1 1 d . . . H29 H 0.2025 0.9218 0.6332 0.060 Uiso 1 1 calc R A . C30 C 0.3909(3) 0.90784(18) 0.66365(17) 0.0408(8) Uani 1 1 d . A . H30 H 0.3788 0.8612 0.6931 0.049 Uiso 1 1 calc R . . C31 C 0.6679(4) 1.0399(2) 0.5990(2) 0.0645(11) Uani 1 1 d . . . H31A H 0.6593 1.0828 0.6333 0.097 Uiso 1 1 calc R A . H31B H 0.6868 1.0609 0.5481 0.097 Uiso 1 1 calc R . . H31C H 0.7445 0.9986 0.6069 0.097 Uiso 1 1 calc R . . C32 C 0.4674(3) 0.69171(16) 0.61807(16) 0.0327(7) Uani 1 1 d . A . C33 C 0.3243(3) 0.69650(16) 0.63937(17) 0.0383(8) Uani 1 1 d . . . H33 H 0.2857 0.6756 0.6862 0.046 Uiso 1 1 calc R A . C34 C 0.2376(3) 0.73164(17) 0.59259(19) 0.0444(8) Uani 1 1 d . A . H34 H 0.1397 0.7348 0.6075 0.053 Uiso 1 1 calc R . . C35 C 0.2922(4) 0.76198(18) 0.52476(19) 0.0455(9) Uani 1 1 d . . . H35 H 0.2319 0.7869 0.4933 0.055 Uiso 1 1 calc R A . C36 C 0.4344(4) 0.75635(17) 0.50208(18) 0.0444(8) Uani 1 1 d . A . H36 H 0.4721 0.7762 0.4546 0.053 Uiso 1 1 calc R . . C37 C 0.5219(3) 0.72176(17) 0.54856(17) 0.0408(8) Uani 1 1 d . . . H37 H 0.6197 0.7184 0.5331 0.049 Uiso 1 1 calc R A . C38 C 0.6355(3) 0.54105(16) 0.64788(16) 0.0299(7) Uani 1 1 d . A . C39 C 0.6160(3) 0.51590(17) 0.58078(16) 0.0359(7) Uani 1 1 d . . . H39 H 0.5668 0.5512 0.5501 0.043 Uiso 1 1 calc R A . C40 C 0.6688(3) 0.43915(18) 0.55895(18) 0.0427(8) Uani 1 1 d . A . H40 H 0.6561 0.4221 0.5130 0.051 Uiso 1 1 calc R . . C41 C 0.7395(3) 0.38761(18) 0.6035(2) 0.0470(9) Uani 1 1 d . . . H41 H 0.7758 0.3351 0.5883 0.056 Uiso 1 1 calc R A . C42 C 0.7574(3) 0.41221(18) 0.6700(2) 0.0465(9) Uani 1 1 d . A . H42 H 0.8054 0.3764 0.7009 0.056 Uiso 1 1 calc R . . C43 C 0.7064(3) 0.48830(17) 0.69224(17) 0.0374(8) Uani 1 1 d . . . H43 H 0.7198 0.5048 0.7382 0.045 Uiso 1 1 calc R A . C44 C 0.8374(3) 0.64893(16) 0.68830(18) 0.0353(7) Uani 1 1 d . . . C45 C 0.9421(3) 0.60705(17) 0.63744(19) 0.0401(8) Uani 1 1 d . A . C46 C 1.0589(3) 0.56782(19) 0.6635(2) 0.0550(10) Uani 1 1 d . . . H46 H 1.1315 0.5383 0.6300 0.066 Uiso 1 1 calc R A . C47 C 1.0718(4) 0.5707(2) 0.7354(3) 0.0598(11) Uani 1 1 d . A . H47 H 1.1518 0.5425 0.7513 0.072 Uiso 1 1 calc R . . C48 C 0.9697(4) 0.6142(2) 0.7851(2) 0.0548(10) Uani 1 1 d . . . H48 H 0.9800 0.6174 0.8349 0.066 Uiso 1 1 calc R A . C49 C 0.8516(3) 0.65341(17) 0.76162(19) 0.0435(8) Uani 1 1 d . A . H49 H 0.7804 0.6834 0.7955 0.052 Uiso 1 1 calc R . . C50 C 0.9339(3) 0.6025(2) 0.55784(19) 0.0568(10) Uani 1 1 d . . . H50A H 0.8952 0.5549 0.5506 0.085 Uiso 1 1 calc R A . H50B H 1.0272 0.6001 0.5275 0.085 Uiso 1 1 calc R . . H50C H 0.8738 0.6495 0.5433 0.085 Uiso 1 1 calc R . . C51 C 0.8313(3) 0.67239(16) 0.22758(16) 0.0333(7) Uani 1 1 d . . . C52 C 0.7045(3) 0.64369(16) 0.23503(17) 0.0375(8) Uani 1 1 d . . . H52 H 0.6655 0.6420 0.1922 0.045 Uiso 1 1 calc R . . C53 C 0.6332(3) 0.61762(17) 0.30207(19) 0.0451(9) Uani 1 1 d . . . H53 H 0.5469 0.5994 0.3042 0.054 Uiso 1 1 calc R . . C54 C 0.6861(4) 0.6179(2) 0.3647(2) 0.0550(10) Uani 1 1 d . . . H54 H 0.6372 0.6003 0.4106 0.066 Uiso 1 1 calc R . . C55 C 0.8115(4) 0.6442(2) 0.36044(19) 0.0605(10) Uani 1 1 d . . . H55 H 0.8502 0.6444 0.4036 0.073 Uiso 1 1 calc R . . C56 C 0.8815(3) 0.6706(2) 0.29333(18) 0.0523(9) Uani 1 1 d . . . H56 H 0.9680 0.6883 0.2920 0.063 Uiso 1 1 calc R . . C57 C 0.9105(3) 0.80335(17) 0.15336(17) 0.0346(7) Uani 1 1 d . . . C58 C 0.8765(3) 0.84826(19) 0.21672(19) 0.0466(9) Uani 1 1 d . . . H58 H 0.8498 0.8227 0.2631 0.056 Uiso 1 1 calc R . . C59 C 0.8804(4) 0.9292(2) 0.2145(3) 0.0678(12) Uani 1 1 d . . . H59 H 0.8573 0.9574 0.2592 0.081 Uiso 1 1 calc R . . C60 C 0.9166(4) 0.9690(2) 0.1492(3) 0.0759(14) Uani 1 1 d . . . H60 H 0.9187 1.0244 0.1478 0.091 Uiso 1 1 calc R . . C61 C 0.9498(4) 0.9269(2) 0.0862(3) 0.0756(13) Uani 1 1 d . . . H61 H 0.9750 0.9533 0.0400 0.091 Uiso 1 1 calc R . . C62 C 0.9472(3) 0.84662(19) 0.0883(2) 0.0522(9) Uani 1 1 d . . . H62 H 0.9717 0.8194 0.0431 0.063 Uiso 1 1 calc R . . C63 C 0.8449(3) 0.68805(17) 0.08173(15) 0.0323(7) Uani 1 1 d . . . C64 C 0.8861(3) 0.62052(18) 0.03948(17) 0.0423(8) Uani 1 1 d . . . H64 H 0.9673 0.5858 0.0469 0.051 Uiso 1 1 calc R . . C65 C 0.8144(4) 0.6015(2) -0.01282(19) 0.0540(9) Uani 1 1 d . . . H65 H 0.8466 0.5544 -0.0399 0.065 Uiso 1 1 calc R . . C66 C 0.6970(4) 0.6505(2) -0.02564(19) 0.0526(9) Uani 1 1 d . . . H66 H 0.6467 0.6375 -0.0609 0.063 Uiso 1 1 calc R . . C67 C 0.6542(3) 0.7185(2) 0.01368(18) 0.0459(9) Uani 1 1 d . . . H67 H 0.5744 0.7536 0.0048 0.055 Uiso 1 1 calc R . . C68 C 0.7258(3) 0.73664(19) 0.06607(17) 0.0405(8) Uani 1 1 d . . . H68 H 0.6930 0.7840 0.0926 0.049 Uiso 1 1 calc R . . C69 C 1.0801(3) 0.66504(16) 0.13905(15) 0.0302(7) Uani 1 1 d . . . C70 C 1.1919(3) 0.70657(18) 0.12327(16) 0.0394(8) Uani 1 1 d . . . H70 H 1.1736 0.7628 0.1217 0.047 Uiso 1 1 calc R . . C71 C 1.3295(3) 0.6701(2) 0.10961(18) 0.0497(9) Uani 1 1 d . . . H71 H 1.4022 0.7014 0.0992 0.060 Uiso 1 1 calc R . . C72 C 1.3609(3) 0.5892(2) 0.11106(17) 0.0485(9) Uani 1 1 d . . . H72 H 1.4547 0.5640 0.0998 0.058 Uiso 1 1 calc R . . C73 C 1.2539(3) 0.54509(19) 0.12915(17) 0.0450(8) Uani 1 1 d . . . H73 H 1.2737 0.4890 0.1318 0.054 Uiso 1 1 calc R . . C74 C 1.1168(3) 0.58264(17) 0.14357(16) 0.0366(7) Uani 1 1 d . . . H74 H 1.0448 0.5510 0.1571 0.044 Uiso 1 1 calc R . . C75 C 0.8652(5) 0.8234(3) 0.5459(3) 0.0381(18) Uani 0.76 1 d P A 1 H75A H 0.9508 0.7854 0.5440 0.057 Uiso 0.76 1 calc PR A 1 H75B H 0.8867 0.8773 0.5457 0.057 Uiso 0.76 1 calc PR A 1 H75C H 0.8244 0.8172 0.5027 0.057 Uiso 0.76 1 calc PR A 1 C75B C 0.8704(12) 0.8347(7) 0.5456(5) 0.056(7) Uani 0.24 1 d PGU A 2 C76B C 0.9387(11) 0.8997(6) 0.5449(5) 0.059(4) Uani 0.24 1 d PGU A 2 H76B H 0.9291 0.9282 0.5887 0.070 Uiso 0.24 1 calc PR A 2 C77B C 1.0209(9) 0.9231(5) 0.4799(6) 0.065(4) Uani 0.24 1 d PGU A 2 H77B H 1.0675 0.9676 0.4794 0.078 Uiso 0.24 1 calc PR A 2 C78B C 1.0349(9) 0.8815(6) 0.4158(5) 0.061(4) Uani 0.24 1 d PGU A 2 H78B H 1.0911 0.8975 0.3714 0.073 Uiso 0.24 1 calc PR A 2 C79B C 0.9666(10) 0.8165(6) 0.4165(5) 0.056(4) Uani 0.24 1 d PGU A 2 H79B H 0.9762 0.7880 0.3727 0.068 Uiso 0.24 1 calc PR A 2 C80B C 0.8844(10) 0.7931(5) 0.4815(6) 0.060(4) Uani 0.24 1 d PGU A 2 H80B H 0.8377 0.7486 0.4820 0.072 Uiso 0.24 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0341(2) 0.0298(2) 0.0334(2) 0.00005(15) -0.00498(16) -0.00041(15) P1 0.0323(4) 0.0296(4) 0.0317(5) -0.0015(3) -0.0046(4) -0.0017(3) O1 0.0316(11) 0.0299(11) 0.0288(12) -0.0038(9) -0.0005(9) -0.0046(9) N1 0.0308(13) 0.0290(13) 0.0330(15) -0.0015(11) -0.0058(11) -0.0032(11) C1 0.0251(16) 0.0304(16) 0.0326(18) 0.0030(14) -0.0087(14) -0.0035(13) B1 0.0301(19) 0.0328(19) 0.028(2) -0.0016(15) -0.0066(15) -0.0006(15) P2 0.0289(4) 0.0294(4) 0.0332(5) -0.0028(3) -0.0071(4) 0.0014(3) N2 0.0337(14) 0.0281(13) 0.0287(14) -0.0006(11) -0.0099(11) -0.0011(11) C2 0.0286(16) 0.0331(17) 0.0316(18) 0.0023(14) -0.0058(13) -0.0040(13) C3 0.0376(18) 0.0353(18) 0.043(2) 0.0006(15) -0.0081(16) -0.0055(14) C4 0.0327(18) 0.045(2) 0.046(2) 0.0121(17) -0.0040(16) -0.0098(15) C5 0.0309(17) 0.049(2) 0.0337(19) 0.0084(16) -0.0012(14) -0.0013(15) C6 0.0236(15) 0.0419(18) 0.0276(18) 0.0070(14) -0.0073(13) 0.0011(13) C7 0.0250(16) 0.0373(17) 0.0281(18) 0.0019(14) -0.0077(13) 0.0033(13) C8 0.0351(18) 0.052(2) 0.0291(19) -0.0005(15) -0.0004(14) 0.0027(15) C9 0.048(2) 0.052(2) 0.035(2) -0.0114(16) 0.0025(17) 0.0058(17) C10 0.0409(19) 0.0375(18) 0.044(2) -0.0085(16) -0.0088(16) 0.0017(15) C11 0.0294(16) 0.0361(17) 0.0312(18) -0.0044(14) -0.0085(14) 0.0015(13) C12 0.0251(16) 0.0366(17) 0.0267(17) -0.0043(14) -0.0070(13) 0.0034(13) C13 0.0312(17) 0.0304(16) 0.0378(19) -0.0068(14) -0.0093(14) 0.0003(13) C14 0.0399(19) 0.0406(19) 0.060(2) -0.0138(17) -0.0149(17) -0.0020(15) C15 0.045(2) 0.041(2) 0.092(3) -0.0184(19) -0.015(2) -0.0132(17) C16 0.053(2) 0.0331(19) 0.092(3) -0.0131(19) -0.012(2) -0.0042(17) C17 0.043(2) 0.0298(18) 0.071(3) -0.0079(17) -0.0102(18) 0.0036(15) C18 0.0335(18) 0.0355(18) 0.049(2) -0.0078(15) -0.0082(15) -0.0007(14) C19 0.0297(17) 0.0335(16) 0.0329(19) -0.0046(14) -0.0088(14) -0.0015(13) C20 0.0347(18) 0.0381(18) 0.039(2) -0.0007(15) -0.0070(15) 0.0013(14) C21 0.0300(18) 0.044(2) 0.066(3) -0.0058(18) -0.0047(17) 0.0001(15) C22 0.036(2) 0.043(2) 0.076(3) -0.0004(19) -0.022(2) 0.0015(16) C23 0.050(2) 0.061(2) 0.050(2) 0.0055(18) -0.0271(19) 0.0004(18) C24 0.0329(18) 0.057(2) 0.036(2) -0.0023(16) -0.0078(15) -0.0031(15) C25 0.0445(19) 0.0296(17) 0.0293(18) -0.0046(14) -0.0125(15) 0.0031(14) C26 0.067(2) 0.0360(19) 0.045(2) 0.0031(16) -0.0191(18) -0.0080(17) C27 0.092(3) 0.044(2) 0.061(3) 0.0131(19) -0.039(2) 0.000(2) C28 0.077(3) 0.050(2) 0.063(3) 0.000(2) -0.041(2) 0.007(2) C29 0.051(2) 0.047(2) 0.056(2) -0.0056(18) -0.0237(19) 0.0010(17) C30 0.043(2) 0.0342(18) 0.045(2) -0.0048(15) -0.0137(16) 0.0030(15) C31 0.087(3) 0.058(2) 0.056(3) 0.0171(19) -0.022(2) -0.029(2) C32 0.0364(18) 0.0274(16) 0.0335(19) -0.0020(13) -0.0074(14) -0.0011(13) C33 0.0382(19) 0.0349(17) 0.040(2) -0.0015(15) -0.0069(16) 0.0001(14) C34 0.0366(19) 0.0382(18) 0.062(3) -0.0055(17) -0.0208(18) -0.0017(15) C35 0.054(2) 0.0344(18) 0.052(2) -0.0004(16) -0.0276(19) 0.0020(16) C36 0.062(2) 0.0366(18) 0.035(2) 0.0059(15) -0.0165(18) -0.0040(16) C37 0.0408(19) 0.0366(18) 0.045(2) -0.0014(16) -0.0086(16) -0.0045(15) C38 0.0292(16) 0.0271(15) 0.0322(18) -0.0004(13) -0.0046(14) -0.0025(13) C39 0.0351(18) 0.0370(18) 0.036(2) 0.0003(15) -0.0084(15) -0.0042(14) C40 0.0427(19) 0.045(2) 0.041(2) -0.0146(16) -0.0048(16) -0.0065(16) C41 0.041(2) 0.0317(18) 0.067(3) -0.0137(18) -0.0089(18) 0.0004(15) C42 0.041(2) 0.0336(18) 0.064(3) 0.0044(17) -0.0184(18) 0.0029(15) C43 0.0379(18) 0.0338(17) 0.041(2) -0.0011(15) -0.0120(15) -0.0004(14) C44 0.0322(17) 0.0263(16) 0.049(2) -0.0028(14) -0.0104(15) -0.0043(13) C45 0.0326(18) 0.0282(17) 0.058(2) -0.0047(15) -0.0054(16) -0.0046(14) C46 0.033(2) 0.037(2) 0.092(3) 0.006(2) -0.006(2) -0.0061(15) C47 0.037(2) 0.050(2) 0.096(3) 0.021(2) -0.027(2) -0.0102(17) C48 0.059(2) 0.049(2) 0.068(3) 0.020(2) -0.034(2) -0.0209(19) C49 0.047(2) 0.0361(18) 0.051(2) 0.0025(16) -0.0178(17) -0.0089(15) C50 0.050(2) 0.057(2) 0.056(3) -0.0140(19) 0.0066(18) -0.0018(18) C51 0.0359(18) 0.0276(16) 0.0336(19) -0.0006(13) -0.0057(14) 0.0027(13) C52 0.0448(19) 0.0295(16) 0.036(2) -0.0029(14) -0.0045(16) -0.0029(14) C53 0.047(2) 0.0360(18) 0.047(2) -0.0011(16) 0.0067(18) -0.0084(15) C54 0.059(2) 0.054(2) 0.040(2) 0.0083(18) 0.0110(19) 0.0011(19) C55 0.061(3) 0.087(3) 0.028(2) 0.0106(19) -0.0083(18) 0.001(2) C56 0.043(2) 0.076(3) 0.036(2) 0.0087(18) -0.0096(17) -0.0062(18) C57 0.0285(17) 0.0385(18) 0.037(2) -0.0025(15) -0.0112(14) 0.0001(13) C58 0.0318(18) 0.052(2) 0.056(2) -0.0127(18) -0.0084(16) -0.0029(15) C59 0.047(2) 0.052(3) 0.106(4) -0.036(2) -0.020(2) 0.0051(19) C60 0.059(3) 0.033(2) 0.145(5) -0.004(3) -0.044(3) -0.0010(19) C61 0.081(3) 0.045(2) 0.105(4) 0.032(2) -0.032(3) -0.018(2) C62 0.067(2) 0.042(2) 0.049(2) 0.0088(17) -0.0123(19) -0.0125(18) C63 0.0287(17) 0.0396(18) 0.0271(18) 0.0030(14) -0.0041(13) -0.0037(14) C64 0.0421(19) 0.048(2) 0.039(2) -0.0033(16) -0.0180(16) 0.0001(16) C65 0.061(2) 0.053(2) 0.053(2) -0.0146(18) -0.027(2) -0.0002(18) C66 0.049(2) 0.072(3) 0.044(2) -0.0023(19) -0.0199(18) -0.0164(19) C67 0.0320(18) 0.065(2) 0.040(2) 0.0110(18) -0.0105(16) -0.0043(17) C68 0.0337(18) 0.050(2) 0.035(2) 0.0000(15) -0.0038(15) 0.0001(15) C69 0.0316(16) 0.0351(17) 0.0246(17) 0.0000(13) -0.0087(13) -0.0034(13) C70 0.0398(19) 0.0433(19) 0.0354(19) 0.0023(15) -0.0063(15) -0.0092(15) C71 0.0329(19) 0.066(2) 0.049(2) 0.0063(18) -0.0047(16) -0.0107(17) C72 0.037(2) 0.066(2) 0.039(2) -0.0027(18) -0.0118(16) 0.0089(18) C73 0.052(2) 0.045(2) 0.039(2) -0.0068(16) -0.0224(17) 0.0088(17) C74 0.0405(19) 0.0373(18) 0.0352(19) -0.0013(14) -0.0177(15) -0.0026(14) C75 0.043(4) 0.035(3) 0.034(4) -0.002(3) -0.003(3) -0.005(3) C75B 0.076(17) 0.016(10) 0.056(11) 0.011(9) 0.028(13) -0.003(9) C76B 0.040(8) 0.074(9) 0.061(8) -0.001(7) 0.000(7) -0.017(7) C77B 0.053(9) 0.082(10) 0.067(9) 0.015(7) -0.009(8) -0.038(8) C78B 0.040(8) 0.095(11) 0.047(7) 0.023(7) -0.014(7) -0.011(7) C79B 0.054(9) 0.072(9) 0.041(8) -0.006(7) -0.017(6) 0.010(6) C80B 0.036(8) 0.051(8) 0.081(11) -0.013(7) 0.011(7) 0.005(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 C75 1.967(4) . ? Zn1 N1 2.013(2) . ? Zn1 N2 2.020(2) . ? Zn1 C75B 2.051(7) . ? P1 N1 1.599(2) . ? P1 C32 1.799(3) . ? P1 C38 1.799(3) . ? P1 C2 1.807(3) . ? O1 C1 1.375(3) . ? O1 C12 1.377(3) . ? N1 C44 1.460(3) . ? C1 C2 1.386(4) . ? C1 C6 1.400(4) . ? B1 C51 1.637(4) . ? B1 C57 1.638(4) . ? B1 C63 1.646(4) . ? B1 C69 1.650(4) . ? P2 N2 1.602(2) . ? P2 C19 1.785(3) . ? P2 C13 1.789(3) . ? P2 C11 1.801(3) . ? N2 C25 1.453(3) . ? C2 C3 1.402(4) . ? C3 C4 1.395(4) . ? C3 H3 0.9500 . ? C4 C5 1.380(4) . ? C4 H4 0.9500 . ? C5 C6 1.394(4) . ? C5 H5 0.9500 . ? C6 C7 1.458(4) . ? C7 C12 1.389(4) . ? C7 C8 1.390(4) . ? C8 C9 1.382(4) . ? C8 H8 0.9500 . ? C9 C10 1.393(4) . ? C9 H9 0.9500 . ? C10 C11 1.398(4) . ? C10 H10 0.9500 . ? C11 C12 1.387(4) . ? C13 C14 1.390(4) . ? C13 C18 1.398(4) . ? C14 C15 1.376(4) . ? C14 H14 0.9500 . ? C15 C16 1.391(4) . ? C15 H15 0.9500 . ? C16 C17 1.375(4) . ? C16 H16 0.9500 . ? C17 C18 1.382(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.392(4) . ? C19 C20 1.392(4) . ? C20 C21 1.387(4) . ? C20 H20 0.9500 . ? C21 C22 1.376(4) . ? C21 H21 0.9500 . ? C22 C23 1.365(4) . ? C22 H22 0.9500 . ? C23 C24 1.385(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.386(4) . ? C25 C30 1.399(4) . ? C26 C27 1.409(4) . ? C26 C31 1.496(5) . ? C27 C28 1.365(5) . ? C27 H27 0.9500 . ? C28 C29 1.360(5) . ? C28 H28 0.9500 . ? C29 C30 1.379(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.388(4) . ? C32 C37 1.396(4) . ? C33 C34 1.384(4) . ? C33 H33 0.9500 . ? C34 C35 1.373(4) . ? C34 H34 0.9500 . ? C35 C36 1.381(4) . ? C35 H35 0.9500 . ? C36 C37 1.383(4) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C43 1.386(4) . ? C38 C39 1.393(4) . ? C39 C40 1.386(4) . ? C39 H39 0.9500 . ? C40 C41 1.376(4) . ? C40 H40 0.9500 . ? C41 C42 1.374(4) . ? C41 H41 0.9500 . ? C42 C43 1.375(4) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.391(4) . ? C44 C49 1.397(4) . ? C45 C46 1.400(4) . ? C45 C50 1.496(4) . ? C46 C47 1.363(5) . ? C46 H46 0.9500 . ? C47 C48 1.378(5) . ? C47 H47 0.9500 . ? C48 C49 1.388(4) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C56 1.398(4) . ? C51 C52 1.401(4) . ? C52 C53 1.389(4) . ? C52 H52 0.9500 . ? C53 C54 1.362(4) . ? C53 H53 0.9500 . ? C54 C55 1.376(5) . ? C54 H54 0.9500 . ? C55 C56 1.387(4) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C58 1.393(4) . ? C57 C62 1.393(4) . ? C58 C59 1.391(5) . ? C58 H58 0.9500 . ? C59 C60 1.365(5) . ? C59 H59 0.9500 . ? C60 C61 1.362(6) . ? C60 H60 0.9500 . ? C61 C62 1.376(5) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 C64 1.393(4) . ? C63 C68 1.402(4) . ? C64 C65 1.387(4) . ? C64 H64 0.9500 . ? C65 C66 1.375(4) . ? C65 H65 0.9500 . ? C66 C67 1.372(4) . ? C66 H66 0.9500 . ? C67 C68 1.382(4) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C70 1.386(4) . ? C69 C74 1.402(4) . ? C70 C71 1.389(4) . ? C70 H70 0.9500 . ? C71 C72 1.370(4) . ? C71 H71 0.9500 . ? C72 C73 1.377(4) . ? C72 H72 0.9500 . ? C73 C74 1.390(4) . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C75B C76B 1.3900 . ? C75B C80B 1.3900 . ? C76B C77B 1.3900 . ? C76B H76B 0.9500 . ? C77B C78B 1.3900 . ? C77B H77B 0.9500 . ? C78B C79B 1.3900 . ? C78B H78B 0.9500 . ? C79B C80B 1.3900 . ? C79B H79B 0.9500 . ? C80B H80B 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 C75 Zn1 N1 117.57(18) . . ? C75 Zn1 N2 118.22(18) . . ? N1 Zn1 N2 124.20(9) . . ? C75 Zn1 C75B 5.4(4) . . ? N1 Zn1 C75B 122.7(3) . . ? N2 Zn1 C75B 113.1(3) . . ? N1 P1 C32 106.73(13) . . ? N1 P1 C38 112.77(12) . . ? C32 P1 C38 108.91(13) . . ? N1 P1 C2 116.38(13) . . ? C32 P1 C2 106.71(13) . . ? C38 P1 C2 105.05(13) . . ? C1 O1 C12 105.6(2) . . ? C44 N1 P1 116.08(18) . . ? C44 N1 Zn1 110.64(16) . . ? P1 N1 Zn1 132.94(13) . . ? O1 C1 C2 122.9(2) . . ? O1 C1 C6 111.6(2) . . ? C2 C1 C6 125.5(3) . . ? C51 B1 C57 111.3(2) . . ? C51 B1 C63 108.9(2) . . ? C57 B1 C63 108.6(2) . . ? C51 B1 C69 108.7(2) . . ? C57 B1 C69 108.7(2) . . ? C63 B1 C69 110.6(2) . . ? N2 P2 C19 106.32(13) . . ? N2 P2 C13 112.92(13) . . ? C19 P2 C13 109.88(13) . . ? N2 P2 C11 115.44(13) . . ? C19 P2 C11 105.90(13) . . ? C13 P2 C11 106.13(13) . . ? C25 N2 P2 118.20(18) . . ? C25 N2 Zn1 111.36(16) . . ? P2 N2 Zn1 129.89(13) . . ? C1 C2 C3 114.4(3) . . ? C1 C2 P1 119.5(2) . . ? C3 C2 P1 125.9(2) . . ? C4 C3 C2 121.7(3) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 122.0(3) . . ? C5 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? C4 C5 C6 118.3(3) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? C5 C6 C1 118.1(3) . . ? C5 C6 C7 136.5(3) . . ? C1 C6 C7 105.4(2) . . ? C12 C7 C8 118.0(3) . . ? C12 C7 C6 105.2(2) . . ? C8 C7 C6 136.8(3) . . ? C9 C8 C7 118.6(3) . . ? C9 C8 H8 120.7 . . ? C7 C8 H8 120.7 . . ? C8 C9 C10 122.0(3) . . ? C8 C9 H9 119.0 . . ? C10 C9 H9 119.0 . . ? C9 C10 C11 121.1(3) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C12 C11 C10 115.0(3) . . ? C12 C11 P2 118.8(2) . . ? C10 C11 P2 125.8(2) . . ? O1 C12 C11 122.4(2) . . ? O1 C12 C7 112.2(2) . . ? C11 C12 C7 125.4(3) . . ? C14 C13 C18 119.2(3) . . ? C14 C13 P2 120.9(2) . . ? C18 C13 P2 119.3(2) . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.8(3) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 120.3(3) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 120.0(3) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 120.1(3) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? C24 C19 C20 118.6(3) . . ? C24 C19 P2 121.3(2) . . ? C20 C19 P2 120.1(2) . . ? C21 C20 C19 120.2(3) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C22 C21 C20 120.1(3) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 120.4(3) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 120.0(3) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 120.6(3) . . ? C23 C24 H24 119.7 . . ? C19 C24 H24 119.7 . . ? C26 C25 C30 119.9(3) . . ? C26 C25 N2 121.3(3) . . ? C30 C25 N2 118.7(3) . . ? C25 C26 C27 117.3(3) . . ? C25 C26 C31 122.8(3) . . ? C27 C26 C31 119.9(3) . . ? C28 C27 C26 121.8(3) . . ? C28 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? C29 C28 C27 120.5(3) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C28 C29 C30 119.5(3) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? C29 C30 C25 120.9(3) . . ? C29 C30 H30 119.6 . . ? C25 C30 H30 119.6 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C37 118.9(3) . . ? C33 C32 P1 121.5(2) . . ? C37 C32 P1 119.5(2) . . ? C34 C33 C32 120.2(3) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C35 C34 C33 120.4(3) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 120.1(3) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C37 119.9(3) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C36 C37 C32 120.4(3) . . ? C36 C37 H37 119.8 . . ? C32 C37 H37 119.8 . . ? C43 C38 C39 119.2(3) . . ? C43 C38 P1 118.8(2) . . ? C39 C38 P1 121.9(2) . . ? C40 C39 C38 119.8(3) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C41 C40 C39 120.3(3) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C42 C41 C40 119.9(3) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C41 C42 C43 120.5(3) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C42 C43 C38 120.3(3) . . ? C42 C43 H43 119.8 . . ? C38 C43 H43 119.8 . . ? C45 C44 C49 120.8(3) . . ? C45 C44 N1 120.3(3) . . ? C49 C44 N1 118.9(3) . . ? C44 C45 C46 117.3(3) . . ? C44 C45 C50 122.9(3) . . ? C46 C45 C50 119.8(3) . . ? C47 C46 C45 122.0(3) . . ? C47 C46 H46 119.0 . . ? C45 C46 H46 119.0 . . ? C46 C47 C48 120.5(3) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C47 C48 C49 119.2(4) . . ? C47 C48 H48 120.4 . . ? C49 C48 H48 120.4 . . ? C48 C49 C44 120.2(3) . . ? C48 C49 H49 119.9 . . ? C44 C49 H49 119.9 . . ? C45 C50 H50A 109.5 . . ? C45 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C45 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C56 C51 C52 114.0(3) . . ? C56 C51 B1 120.9(3) . . ? C52 C51 B1 125.1(3) . . ? C53 C52 C51 123.1(3) . . ? C53 C52 H52 118.5 . . ? C51 C52 H52 118.5 . . ? C54 C53 C52 120.5(3) . . ? C54 C53 H53 119.7 . . ? C52 C53 H53 119.7 . . ? C53 C54 C55 118.9(3) . . ? C53 C54 H54 120.6 . . ? C55 C54 H54 120.6 . . ? C54 C55 C56 120.2(3) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C55 C56 C51 123.3(3) . . ? C55 C56 H56 118.4 . . ? C51 C56 H56 118.4 . . ? C58 C57 C62 114.2(3) . . ? C58 C57 B1 125.9(3) . . ? C62 C57 B1 119.8(3) . . ? C59 C58 C57 122.3(4) . . ? C59 C58 H58 118.8 . . ? C57 C58 H58 118.8 . . ? C60 C59 C58 121.2(4) . . ? C60 C59 H59 119.4 . . ? C58 C59 H59 119.4 . . ? C61 C60 C59 117.9(4) . . ? C61 C60 H60 121.1 . . ? C59 C60 H60 121.1 . . ? C60 C61 C62 121.1(4) . . ? C60 C61 H61 119.5 . . ? C62 C61 H61 119.5 . . ? C61 C62 C57 123.3(4) . . ? C61 C62 H62 118.4 . . ? C57 C62 H62 118.4 . . ? C64 C63 C68 114.4(3) . . ? C64 C63 B1 124.6(2) . . ? C68 C63 B1 120.7(3) . . ? C65 C64 C63 123.2(3) . . ? C65 C64 H64 118.4 . . ? C63 C64 H64 118.4 . . ? C66 C65 C64 120.3(3) . . ? C66 C65 H65 119.9 . . ? C64 C65 H65 119.9 . . ? C67 C66 C65 118.5(3) . . ? C67 C66 H66 120.7 . . ? C65 C66 H66 120.7 . . ? C66 C67 C68 120.8(3) . . ? C66 C67 H67 119.6 . . ? C68 C67 H67 119.6 . . ? C67 C68 C63 122.8(3) . . ? C67 C68 H68 118.6 . . ? C63 C68 H68 118.6 . . ? C70 C69 C74 114.5(3) . . ? C70 C69 B1 123.8(3) . . ? C74 C69 B1 121.7(3) . . ? C69 C70 C71 123.2(3) . . ? C69 C70 H70 118.4 . . ? C71 C70 H70 118.4 . . ? C72 C71 C70 120.4(3) . . ? C72 C71 H71 119.8 . . ? C70 C71 H71 119.8 . . ? C71 C72 C73 118.7(3) . . ? C71 C72 H72 120.6 . . ? C73 C72 H72 120.6 . . ? C72 C73 C74 120.1(3) . . ? C72 C73 H73 120.0 . . ? C74 C73 H73 120.0 . . ? C73 C74 C69 122.9(3) . . ? C73 C74 H74 118.5 . . ? C69 C74 H74 118.5 . . ? Zn1 C75 H75A 109.5 . . ? Zn1 C75 H75B 109.5 . . ? Zn1 C75 H75C 109.5 . . ? C76B C75B C80B 120.0 . . ? C76B C75B Zn1 122.0(6) . . ? C80B C75B Zn1 117.7(6) . . ? C75B C76B C77B 120.0 . . ? C75B C76B H76B 120.0 . . ? C77B C76B H76B 120.0 . . ? C78B C77B C76B 120.0 . . ? C78B C77B H77B 120.0 . . ? C76B C77B H77B 120.0 . . ? C77B C78B C79B 120.0 . . ? C77B C78B H78B 120.0 . . ? C79B C78B H78B 120.0 . . ? C80B C79B C78B 120.0 . . ? C80B C79B H79B 120.0 . . ? C78B C79B H79B 120.0 . . ? C79B C80B C75B 120.0 . . ? C79B C80B H80B 120.0 . . ? C75B C80B H80B 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C32 P1 N1 C44 -162.1(2) . . . . ? C38 P1 N1 C44 -42.6(2) . . . . ? C2 P1 N1 C44 78.9(2) . . . . ? C32 P1 N1 Zn1 25.4(2) . . . . ? C38 P1 N1 Zn1 144.92(17) . . . . ? C2 P1 N1 Zn1 -93.6(2) . . . . ? C75 Zn1 N1 C44 68.8(3) . . . . ? N2 Zn1 N1 C44 -111.99(19) . . . . ? C75B Zn1 N1 C44 66.8(5) . . . . ? C75 Zn1 N1 P1 -118.4(2) . . . . ? N2 Zn1 N1 P1 60.8(2) . . . . ? C75B Zn1 N1 P1 -120.4(5) . . . . ? C12 O1 C1 C2 177.5(3) . . . . ? C12 O1 C1 C6 -0.9(3) . . . . ? C19 P2 N2 C25 -170.6(2) . . . . ? C13 P2 N2 C25 -50.0(2) . . . . ? C11 P2 N2 C25 72.3(2) . . . . ? C19 P2 N2 Zn1 18.7(2) . . . . ? C13 P2 N2 Zn1 139.24(16) . . . . ? C11 P2 N2 Zn1 -98.40(18) . . . . ? C75 Zn1 N2 C25 74.0(3) . . . . ? N1 Zn1 N2 C25 -105.14(19) . . . . ? C75B Zn1 N2 C25 76.0(4) . . . . ? C75 Zn1 N2 P2 -114.7(2) . . . . ? N1 Zn1 N2 P2 66.1(2) . . . . ? C75B Zn1 N2 P2 -112.8(4) . . . . ? O1 C1 C2 C3 179.8(2) . . . . ? C6 C1 C2 C3 -2.0(4) . . . . ? O1 C1 C2 P1 -4.4(4) . . . . ? C6 C1 C2 P1 173.7(2) . . . . ? N1 P1 C2 C1 38.3(3) . . . . ? C32 P1 C2 C1 -80.7(2) . . . . ? C38 P1 C2 C1 163.8(2) . . . . ? N1 P1 C2 C3 -146.6(2) . . . . ? C32 P1 C2 C3 94.5(3) . . . . ? C38 P1 C2 C3 -21.1(3) . . . . ? C1 C2 C3 C4 0.8(4) . . . . ? P1 C2 C3 C4 -174.6(2) . . . . ? C2 C3 C4 C5 -0.1(5) . . . . ? C3 C4 C5 C6 0.3(4) . . . . ? C4 C5 C6 C1 -1.3(4) . . . . ? C4 C5 C6 C7 177.3(3) . . . . ? O1 C1 C6 C5 -179.4(2) . . . . ? C2 C1 C6 C5 2.3(4) . . . . ? O1 C1 C6 C7 1.7(3) . . . . ? C2 C1 C6 C7 -176.7(3) . . . . ? C5 C6 C7 C12 179.6(3) . . . . ? C1 C6 C7 C12 -1.7(3) . . . . ? C5 C6 C7 C8 0.6(6) . . . . ? C1 C6 C7 C8 179.2(3) . . . . ? C12 C7 C8 C9 -0.6(4) . . . . ? C6 C7 C8 C9 178.4(3) . . . . ? C7 C8 C9 C10 -0.6(5) . . . . ? C8 C9 C10 C11 0.9(5) . . . . ? C9 C10 C11 C12 0.1(4) . . . . ? C9 C10 C11 P2 -172.1(2) . . . . ? N2 P2 C11 C12 42.8(3) . . . . ? C19 P2 C11 C12 -74.5(2) . . . . ? C13 P2 C11 C12 168.7(2) . . . . ? N2 P2 C11 C10 -145.3(2) . . . . ? C19 P2 C11 C10 97.4(3) . . . . ? C13 P2 C11 C10 -19.3(3) . . . . ? C1 O1 C12 C11 178.7(2) . . . . ? C1 O1 C12 C7 -0.2(3) . . . . ? C10 C11 C12 O1 179.9(2) . . . . ? P2 C11 C12 O1 -7.3(4) . . . . ? C10 C11 C12 C7 -1.3(4) . . . . ? P2 C11 C12 C7 171.4(2) . . . . ? C8 C7 C12 O1 -179.5(2) . . . . ? C6 C7 C12 O1 1.2(3) . . . . ? C8 C7 C12 C11 1.6(4) . . . . ? C6 C7 C12 C11 -177.6(3) . . . . ? N2 P2 C13 C14 -100.6(3) . . . . ? C19 P2 C13 C14 17.9(3) . . . . ? C11 P2 C13 C14 132.0(3) . . . . ? N2 P2 C13 C18 70.4(3) . . . . ? C19 P2 C13 C18 -171.1(2) . . . . ? C11 P2 C13 C18 -57.0(3) . . . . ? C18 C13 C14 C15 -1.1(5) . . . . ? P2 C13 C14 C15 169.9(3) . . . . ? C13 C14 C15 C16 -0.4(5) . . . . ? C14 C15 C16 C17 1.7(6) . . . . ? C15 C16 C17 C18 -1.5(6) . . . . ? C16 C17 C18 C13 0.0(5) . . . . ? C14 C13 C18 C17 1.2(5) . . . . ? P2 C13 C18 C17 -169.9(2) . . . . ? N2 P2 C19 C24 -138.2(2) . . . . ? C13 P2 C19 C24 99.3(3) . . . . ? C11 P2 C19 C24 -14.9(3) . . . . ? N2 P2 C19 C20 42.4(3) . . . . ? C13 P2 C19 C20 -80.1(3) . . . . ? C11 P2 C19 C20 165.7(2) . . . . ? C24 C19 C20 C21 0.7(4) . . . . ? P2 C19 C20 C21 -179.9(2) . . . . ? C19 C20 C21 C22 0.6(5) . . . . ? C20 C21 C22 C23 -0.8(5) . . . . ? C21 C22 C23 C24 -0.2(5) . . . . ? C22 C23 C24 C19 1.4(5) . . . . ? C20 C19 C24 C23 -1.7(5) . . . . ? P2 C19 C24 C23 178.9(2) . . . . ? P2 N2 C25 C26 90.1(3) . . . . ? Zn1 N2 C25 C26 -97.5(3) . . . . ? P2 N2 C25 C30 -92.6(3) . . . . ? Zn1 N2 C25 C30 79.8(3) . . . . ? C30 C25 C26 C27 3.3(5) . . . . ? N2 C25 C26 C27 -179.4(3) . . . . ? C30 C25 C26 C31 -177.1(3) . . . . ? N2 C25 C26 C31 0.2(5) . . . . ? C25 C26 C27 C28 -2.2(5) . . . . ? C31 C26 C27 C28 178.2(3) . . . . ? C26 C27 C28 C29 -0.6(6) . . . . ? C27 C28 C29 C30 2.3(5) . . . . ? C28 C29 C30 C25 -1.1(5) . . . . ? C26 C25 C30 C29 -1.8(5) . . . . ? N2 C25 C30 C29 -179.1(3) . . . . ? N1 P1 C32 C33 -144.7(2) . . . . ? C38 P1 C32 C33 93.3(3) . . . . ? C2 P1 C32 C33 -19.6(3) . . . . ? N1 P1 C32 C37 39.3(3) . . . . ? C38 P1 C32 C37 -82.7(2) . . . . ? C2 P1 C32 C37 164.4(2) . . . . ? C37 C32 C33 C34 -0.9(4) . . . . ? P1 C32 C33 C34 -176.9(2) . . . . ? C32 C33 C34 C35 0.1(4) . . . . ? C33 C34 C35 C36 1.2(5) . . . . ? C34 C35 C36 C37 -1.5(5) . . . . ? C35 C36 C37 C32 0.7(5) . . . . ? C33 C32 C37 C36 0.6(4) . . . . ? P1 C32 C37 C36 176.6(2) . . . . ? N1 P1 C38 C43 72.3(3) . . . . ? C32 P1 C38 C43 -169.4(2) . . . . ? C2 P1 C38 C43 -55.4(3) . . . . ? N1 P1 C38 C39 -102.7(2) . . . . ? C32 P1 C38 C39 15.6(3) . . . . ? C2 P1 C38 C39 129.6(2) . . . . ? C43 C38 C39 C40 -0.7(4) . . . . ? P1 C38 C39 C40 174.3(2) . . . . ? C38 C39 C40 C41 0.4(4) . . . . ? C39 C40 C41 C42 0.3(5) . . . . ? C40 C41 C42 C43 -0.6(5) . . . . ? C41 C42 C43 C38 0.3(5) . . . . ? C39 C38 C43 C42 0.3(4) . . . . ? P1 C38 C43 C42 -174.8(2) . . . . ? P1 N1 C44 C45 93.1(3) . . . . ? Zn1 N1 C44 C45 -92.8(3) . . . . ? P1 N1 C44 C49 -88.2(3) . . . . ? Zn1 N1 C44 C49 85.9(3) . . . . ? C49 C44 C45 C46 2.1(4) . . . . ? N1 C44 C45 C46 -179.2(3) . . . . ? C49 C44 C45 C50 -178.1(3) . . . . ? N1 C44 C45 C50 0.6(4) . . . . ? C44 C45 C46 C47 -0.7(5) . . . . ? C50 C45 C46 C47 179.5(3) . . . . ? C45 C46 C47 C48 -1.2(5) . . . . ? C46 C47 C48 C49 1.7(5) . . . . ? C47 C48 C49 C44 -0.3(5) . . . . ? C45 C44 C49 C48 -1.6(4) . . . . ? N1 C44 C49 C48 179.7(3) . . . . ? C57 B1 C51 C56 -69.5(3) . . . . ? C63 B1 C51 C56 170.8(3) . . . . ? C69 B1 C51 C56 50.2(3) . . . . ? C57 B1 C51 C52 109.2(3) . . . . ? C63 B1 C51 C52 -10.5(4) . . . . ? C69 B1 C51 C52 -131.1(3) . . . . ? C56 C51 C52 C53 1.6(4) . . . . ? B1 C51 C52 C53 -177.2(3) . . . . ? C51 C52 C53 C54 -0.9(4) . . . . ? C52 C53 C54 C55 -0.2(5) . . . . ? C53 C54 C55 C56 0.6(5) . . . . ? C54 C55 C56 C51 0.1(5) . . . . ? C52 C51 C56 C55 -1.2(5) . . . . ? B1 C51 C56 C55 177.6(3) . . . . ? C51 B1 C57 C58 17.9(4) . . . . ? C63 B1 C57 C58 137.8(3) . . . . ? C69 B1 C57 C58 -101.8(3) . . . . ? C51 B1 C57 C62 -164.9(3) . . . . ? C63 B1 C57 C62 -44.9(3) . . . . ? C69 B1 C57 C62 75.5(3) . . . . ? C62 C57 C58 C59 -0.4(4) . . . . ? B1 C57 C58 C59 176.9(3) . . . . ? C57 C58 C59 C60 0.7(5) . . . . ? C58 C59 C60 C61 -0.3(6) . . . . ? C59 C60 C61 C62 -0.2(6) . . . . ? C60 C61 C62 C57 0.5(6) . . . . ? C58 C57 C62 C61 -0.1(5) . . . . ? B1 C57 C62 C61 -177.7(3) . . . . ? C51 B1 C63 C64 -91.6(3) . . . . ? C57 B1 C63 C64 147.0(3) . . . . ? C69 B1 C63 C64 27.8(4) . . . . ? C51 B1 C63 C68 81.9(3) . . . . ? C57 B1 C63 C68 -39.5(3) . . . . ? C69 B1 C63 C68 -158.7(3) . . . . ? C68 C63 C64 C65 -1.3(5) . . . . ? B1 C63 C64 C65 172.6(3) . . . . ? C63 C64 C65 C66 0.5(5) . . . . ? C64 C65 C66 C67 0.8(5) . . . . ? C65 C66 C67 C68 -1.3(5) . . . . ? C66 C67 C68 C63 0.5(5) . . . . ? C64 C63 C68 C67 0.8(4) . . . . ? B1 C63 C68 C67 -173.3(3) . . . . ? C51 B1 C69 C70 -130.0(3) . . . . ? C57 B1 C69 C70 -8.7(4) . . . . ? C63 B1 C69 C70 110.5(3) . . . . ? C51 B1 C69 C74 50.8(3) . . . . ? C57 B1 C69 C74 172.2(3) . . . . ? C63 B1 C69 C74 -68.7(3) . . . . ? C74 C69 C70 C71 2.8(4) . . . . ? B1 C69 C70 C71 -176.4(3) . . . . ? C69 C70 C71 C72 0.2(5) . . . . ? C70 C71 C72 C73 -2.5(5) . . . . ? C71 C72 C73 C74 1.7(5) . . . . ? C72 C73 C74 C69 1.5(5) . . . . ? C70 C69 C74 C73 -3.6(4) . . . . ? B1 C69 C74 C73 175.6(3) . . . . ? C75 Zn1 C75B C76B -164(6) . . . . ? N1 Zn1 C75B C76B -145.3(4) . . . . ? N2 Zn1 C75B C76B 33.7(7) . . . . ? C75 Zn1 C75B C80B 22(5) . . . . ? N1 Zn1 C75B C80B 40.9(7) . . . . ? N2 Zn1 C75B C80B -140.1(5) . . . . ? C80B C75B C76B C77B 0.0 . . . . ? Zn1 C75B C76B C77B -173.7(9) . . . . ? C75B C76B C77B C78B 0.0 . . . . ? C76B C77B C78B C79B 0.0 . . . . ? C77B C78B C79B C80B 0.0 . . . . ? C78B C79B C80B C75B 0.0 . . . . ? C76B C75B C80B C79B 0.0 . . . . ? Zn1 C75B C80B C79B 173.9(9) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.338 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.052 #===END data_6c _database_code_depnum_ccdc_archive 'CCDC 833328' #TrackingRef '6184_web_deposit_cif_file_0_PaulG.Hayes_ #1310063407.Chem Eur J_AllCifs - Paul G Hayes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80.65 H63.86 B N2 O P2 Zn' _chemical_formula_weight 1215.12 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' B B 0.0013 0.0007 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9023(5) _cell_length_b 16.8670(9) _cell_length_c 20.7112(11) _cell_angle_alpha 101.9740(10) _cell_angle_beta 91.1140(10) _cell_angle_gamma 95.2960(10) _cell_volume 3366.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9956 _cell_measurement_theta_min 4.607 _cell_measurement_theta_max 56.676 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1270 _exptl_absorpt_coefficient_mu 0.459 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6873 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40833 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.03 _reflns_number_total 11870 _reflns_number_gt 10042 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0543P)^2^+1.5755P] 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 11870 _refine_ls_number_parameters 829 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1073 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.004 _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 0.87340(2) 0.663868(14) 0.662342(11) 0.03189(8) Uani 1 1 d . . . P1 P 0.99960(9) 0.50388(5) 0.68936(4) 0.02700(19) Uani 0.80 1 d P A 1 N1 N 0.8715(2) 0.55457(12) 0.68619(10) 0.0289(4) Uani 0.80 1 d P A 1 P1B P 0.9434(4) 0.4954(2) 0.70594(18) 0.0298(8) Uani 0.20 1 d P A 2 N1B N 0.9843(8) 0.5628(5) 0.6626(4) 0.0278(17) Uani 0.20 1 d P A 2 P2 P 0.96175(9) 0.81708(4) 0.78274(4) 0.02732(16) Uani 0.85 1 d P A 1 N2 N 0.9820(2) 0.76595(12) 0.70998(9) 0.0298(4) Uani 0.85 1 d P A 1 P2B P 1.0220(4) 0.8232(2) 0.7638(2) 0.0244(8) Uani 0.15 1 d P A 2 N2B N 0.8833(9) 0.7626(6) 0.7434(5) 0.019(2) Uani 0.15 1 d P A 2 O1 O 1.05172(16) 0.65586(8) 0.79533(7) 0.0389(4) Uani 1 1 d . A . C1 C 1.0951(2) 0.58731(12) 0.81230(10) 0.0327(4) Uani 1 1 d . A . B1 B 0.4682(2) 0.23107(15) 0.85998(12) 0.0336(5) Uani 1 1 d . . . C1S C -0.0984(3) 0.94151(15) 0.01040(13) 0.0585(7) Uani 1 1 d . . . H1S H -0.1665 0.9011 0.0176 0.070 Uiso 1 1 calc R . . C2 C 1.0710(2) 0.51094(12) 0.77210(11) 0.0349(5) Uani 1 1 d . . . C2S C 0.0193(3) 0.95738(15) 0.04863(13) 0.0577(7) Uani 1 1 d . . . H2S H 0.0327 0.9279 0.0822 0.069 Uiso 1 1 calc R . . C3 C 1.1238(2) 0.44840(13) 0.79653(11) 0.0354(5) Uani 1 1 d . A . H3 H 1.1099 0.3941 0.7716 0.042 Uiso 1 1 calc R . . C3S C 0.1186(3) 1.01594(16) 0.03858(13) 0.0581(7) Uani 1 1 d . . . H3S H 0.2002 1.0269 0.0651 0.070 Uiso 1 1 calc R . . C4 C 1.1965(2) 0.46446(13) 0.85706(11) 0.0353(5) Uani 1 1 d . . . H4 H 1.2301 0.4205 0.8726 0.042 Uiso 1 1 calc R A . C5 C 1.2210(2) 0.54215(13) 0.89490(10) 0.0340(5) Uani 1 1 d . A . H5 H 1.2713 0.5520 0.9358 0.041 Uiso 1 1 calc R . . C6 C 1.1704(2) 0.60607(12) 0.87186(10) 0.0311(4) Uani 1 1 d . . . C7 C 1.1764(2) 0.69427(12) 0.89283(10) 0.0308(4) Uani 1 1 d . A . C8 C 1.2372(2) 0.75328(13) 0.94514(10) 0.0361(5) Uani 1 1 d . . . H8 H 1.2883 0.7385 0.9794 0.043 Uiso 1 1 calc R A . C9 C 1.2212(2) 0.83355(14) 0.94572(11) 0.0403(5) Uani 1 1 d . A . H9 H 1.2641 0.8744 0.9806 0.048 Uiso 1 1 calc R . . C10 C 1.1447(2) 0.85733(13) 0.89725(11) 0.0398(5) Uani 1 1 d . . . H10 H 1.1355 0.9135 0.9001 0.048 Uiso 1 1 calc R A . C11 C 1.0813(2) 0.79998(13) 0.84449(11) 0.0366(5) Uani 1 1 d . A . C12 C 1.1033(2) 0.72007(12) 0.84463(10) 0.0332(5) Uani 1 1 d . . . C13 C 0.9745(2) 0.92528(12) 0.78461(10) 0.0323(4) Uani 1 1 d . . . C14 C 1.0976(2) 0.97078(14) 0.78234(11) 0.0405(5) Uani 1 1 d . A . H14 H 1.1800 0.9464 0.7840 0.049 Uiso 1 1 calc R . . C15 C 1.1008(3) 1.05124(15) 0.77761(12) 0.0484(6) Uani 1 1 d . . . H15 H 1.1852 1.0822 0.7756 0.058 Uiso 1 1 calc R A . C16 C 0.9810(3) 1.08654(14) 0.77576(13) 0.0496(6) Uani 1 1 d . A . H16 H 0.9831 1.1419 0.7723 0.059 Uiso 1 1 calc R . . C17 C 0.8580(2) 1.04195(14) 0.77890(13) 0.0474(6) Uani 1 1 d . . . H17 H 0.7759 1.0668 0.7783 0.057 Uiso 1 1 calc R A . C18 C 0.8546(2) 0.96145(13) 0.78297(11) 0.0389(5) Uani 1 1 d . A . H18 H 0.7700 0.9306 0.7846 0.047 Uiso 1 1 calc R . . C19 C 0.7920(2) 0.78108(13) 0.80425(12) 0.0396(5) Uani 1 1 d . . . C20 C 0.7706(2) 0.77593(13) 0.86786(12) 0.0401(5) Uani 1 1 d . A . H20 H 0.8447 0.7878 0.8993 0.048 Uiso 1 1 calc R . . C21 C 0.6433(2) 0.75387(15) 0.88760(12) 0.0461(6) Uani 1 1 d . . . H21 H 0.6294 0.7517 0.9325 0.055 Uiso 1 1 calc R A . C22 C 0.5358(2) 0.73488(15) 0.84178(15) 0.0520(6) Uani 1 1 d . A . H22 H 0.4477 0.7189 0.8548 0.062 Uiso 1 1 calc R . . C23 C 0.5572(3) 0.73926(16) 0.77718(14) 0.0549(7) Uani 1 1 d . . . H23 H 0.4839 0.7253 0.7453 0.066 Uiso 1 1 calc R A . C24 C 0.6845(3) 0.76376(16) 0.75839(12) 0.0485(6) Uani 1 1 d . A . H24 H 0.6982 0.7687 0.7141 0.058 Uiso 1 1 calc R . . C25 C 1.0966(2) 0.79661(13) 0.67620(12) 0.0434(6) Uani 1 1 d . . . C26 C 1.0692(3) 0.82936(17) 0.62371(13) 0.0561(7) Uani 1 1 d . A . H26 H 0.9778 0.8353 0.6123 0.067 Uiso 1 1 calc R . . C27 C 1.1722(3) 0.8542(2) 0.58657(14) 0.0713(9) Uani 1 1 d . . . H27 H 1.1512 0.8760 0.5492 0.086 Uiso 1 1 calc R A . C28 C 1.3048(3) 0.8479(2) 0.60318(15) 0.0671(8) Uani 1 1 d . A . H28 H 1.3757 0.8662 0.5779 0.081 Uiso 1 1 calc R . . C29 C 1.3348(3) 0.81514(18) 0.65608(15) 0.0601(7) Uani 1 1 d . . . H29 H 1.4265 0.8098 0.6674 0.072 Uiso 1 1 calc R A . C30 C 1.2313(3) 0.78969(17) 0.69319(14) 0.0572(7) Uani 1 1 d . A . H30 H 1.2520 0.7675 0.7303 0.069 Uiso 1 1 calc R . . C31 C 0.9632(2) 0.39573(12) 0.65600(10) 0.0334(5) Uani 1 1 d . . . C32 C 0.8764(2) 0.34510(14) 0.68478(12) 0.0416(5) Uani 1 1 d . A . H32 H 0.8359 0.3662 0.7252 0.050 Uiso 1 1 calc R . . C33 C 0.8488(3) 0.26476(16) 0.65503(14) 0.0553(7) Uani 1 1 d . . . H33 H 0.7881 0.2304 0.6745 0.066 Uiso 1 1 calc R A . C34 C 0.9082(3) 0.23360(15) 0.59732(15) 0.0625(8) Uani 1 1 d . A . H34 H 0.8876 0.1779 0.5767 0.075 Uiso 1 1 calc R . . C35 C 0.9975(3) 0.28251(16) 0.56901(13) 0.0573(7) Uani 1 1 d . . . H35 H 1.0401 0.2602 0.5296 0.069 Uiso 1 1 calc R A . C36 C 1.0252(2) 0.36410(14) 0.59795(11) 0.0427(5) Uani 1 1 d . A . H36 H 1.0861 0.3982 0.5783 0.051 Uiso 1 1 calc R . . C37 C 1.1254(2) 0.55158(16) 0.64204(12) 0.0479(6) Uani 1 1 d . . . C38 C 1.2578(2) 0.56236(15) 0.66437(13) 0.0493(6) Uani 1 1 d . A . H38 H 1.2811 0.5474 0.7046 0.059 Uiso 1 1 calc R . . C39 C 1.3577(3) 0.59430(17) 0.62971(17) 0.0635(8) Uani 1 1 d . . . H39 H 1.4497 0.5999 0.6453 0.076 Uiso 1 1 calc R A . C40 C 1.3250(4) 0.61813(18) 0.57248(18) 0.0770(10) Uani 1 1 d . A . H40 H 1.3937 0.6415 0.5488 0.092 Uiso 1 1 calc R . . C41 C 1.1899(4) 0.60781(19) 0.54924(16) 0.0746(9) Uani 1 1 d . . . H41 H 1.1661 0.6247 0.5099 0.089 Uiso 1 1 calc R A . C42 C 1.0907(3) 0.57275(18) 0.58383(14) 0.0589(7) Uani 1 1 d . A . H42 H 0.9992 0.5634 0.5673 0.071 Uiso 1 1 calc R . . C43 C 0.7484(2) 0.52411(15) 0.71313(12) 0.0457(6) Uani 1 1 d . . . C44 C 0.7206(3) 0.55189(15) 0.77963(12) 0.0482(6) Uani 1 1 d . A . H44 H 0.7873 0.5865 0.8085 0.058 Uiso 1 1 calc R . . C45 C 0.5986(3) 0.52966(16) 0.80310(13) 0.0489(6) Uani 1 1 d . . . H45 H 0.5783 0.5507 0.8476 0.059 Uiso 1 1 calc R A . C46 C 0.5046(3) 0.4763(2) 0.76175(14) 0.0595(7) Uani 1 1 d . A . H46 H 0.4208 0.4588 0.7784 0.071 Uiso 1 1 calc R . . C47 C 0.5313(2) 0.44855(18) 0.69697(14) 0.0549(7) Uani 1 1 d . . . H47 H 0.4649 0.4131 0.6685 0.066 Uiso 1 1 calc R A . C48 C 0.6542(2) 0.47166(14) 0.67265(12) 0.0450(6) Uani 1 1 d . A . H48 H 0.6732 0.4511 0.6278 0.054 Uiso 1 1 calc R . . C49 C 0.7561(2) 0.66941(13) 0.58538(10) 0.0334(5) Uani 0.93 1 d P A 1 C50 C 0.7119(2) 0.74402(15) 0.57628(12) 0.0390(5) Uani 0.93 1 d P A 1 H50 H 0.7382 0.7924 0.6082 0.047 Uiso 0.93 1 calc PR A 1 C51 C 0.6312(3) 0.74798(18) 0.52178(13) 0.0477(6) Uani 0.93 1 d P A 1 H51 H 0.6039 0.7988 0.5164 0.057 Uiso 0.93 1 calc PR A 1 C52 C 0.5909(3) 0.6783(2) 0.47562(12) 0.0513(7) Uani 0.93 1 d P A 1 H52 H 0.5352 0.6809 0.4384 0.062 Uiso 0.93 1 calc PR A 1 C53 C 0.6310(3) 0.60524(18) 0.48335(12) 0.0498(7) Uani 0.93 1 d P A 1 H53 H 0.6038 0.5571 0.4513 0.060 Uiso 0.93 1 calc PR A 1 C54 C 0.7116(2) 0.60139(16) 0.53822(12) 0.0413(6) Uani 0.93 1 d P A 1 H54 H 0.7367 0.5499 0.5432 0.050 Uiso 0.93 1 calc PR A 1 C49B C 0.7561(2) 0.66941(13) 0.58538(10) 0.0334(5) Uani 0.07 1 d P A 2 H49A H 0.7600 0.6201 0.5510 0.050 Uiso 0.07 1 calc P B 2 H49B H 0.7877 0.7173 0.5680 0.050 Uiso 0.07 1 calc P C 2 H49C H 0.6623 0.6735 0.5990 0.050 Uiso 0.07 1 calc P D 2 C55 C 0.4064(2) 0.24049(13) 0.78781(10) 0.0342(5) Uani 1 1 d . . . C56 C 0.2712(2) 0.25037(12) 0.77493(11) 0.0344(5) Uani 1 1 d . . . H56 H 0.2123 0.2588 0.8108 0.041 Uiso 1 1 calc R . . C57 C 0.2188(2) 0.24842(14) 0.71198(11) 0.0419(5) Uani 1 1 d . . . H57 H 0.1258 0.2555 0.7057 0.050 Uiso 1 1 calc R . . C58 C 0.3002(3) 0.23642(16) 0.65881(12) 0.0512(6) Uani 1 1 d . . . H58 H 0.2643 0.2345 0.6156 0.061 Uiso 1 1 calc R . . C59 C 0.4352(3) 0.22722(19) 0.66935(13) 0.0599(7) Uani 1 1 d . . . H59 H 0.4932 0.2190 0.6331 0.072 Uiso 1 1 calc R . . C60 C 0.4867(3) 0.22988(17) 0.73244(12) 0.0520(6) Uani 1 1 d . . . H60 H 0.5804 0.2243 0.7384 0.062 Uiso 1 1 calc R . . C61 C 0.4547(2) 0.13317(13) 0.86096(12) 0.0384(5) Uani 1 1 d . . . C62 C 0.4702(2) 0.07364(15) 0.80433(14) 0.0495(6) Uani 1 1 d . . . H62 H 0.4786 0.0898 0.7632 0.059 Uiso 1 1 calc R . . C63 C 0.4737(3) -0.00820(17) 0.80558(18) 0.0651(8) Uani 1 1 d . . . H63 H 0.4870 -0.0462 0.7660 0.078 Uiso 1 1 calc R . . C64 C 0.4581(3) -0.03443(18) 0.8635(2) 0.0758(10) Uani 1 1 d . . . H64 H 0.4607 -0.0903 0.8645 0.091 Uiso 1 1 calc R . . C65 C 0.4387(3) 0.0217(2) 0.92023(19) 0.0717(9) Uani 1 1 d . . . H65 H 0.4246 0.0043 0.9606 0.086 Uiso 1 1 calc R . . C66 C 0.4397(3) 0.10377(16) 0.91876(14) 0.0516(6) Uani 1 1 d . . . H66 H 0.4295 0.1415 0.9589 0.062 Uiso 1 1 calc R . . C67 C 0.6301(2) 0.26396(13) 0.86678(10) 0.0323(4) Uani 1 1 d . . . C68 C 0.7314(2) 0.21960(13) 0.88422(10) 0.0343(5) Uani 1 1 d . . . H68 H 0.7068 0.1663 0.8910 0.041 Uiso 1 1 calc R . . C69 C 0.8673(2) 0.25031(14) 0.89207(12) 0.0430(5) Uani 1 1 d . . . H69 H 0.9334 0.2177 0.9035 0.052 Uiso 1 1 calc R . . C70 C 0.9067(2) 0.32765(15) 0.88332(12) 0.0459(6) Uani 1 1 d . . . H70 H 0.9991 0.3494 0.8899 0.055 Uiso 1 1 calc R . . C71 C 0.8097(2) 0.37292(15) 0.86491(12) 0.0465(6) Uani 1 1 d . . . H71 H 0.8353 0.4262 0.8582 0.056 Uiso 1 1 calc R . . C72 C 0.6752(2) 0.34142(14) 0.85611(12) 0.0420(5) Uani 1 1 d . . . H72 H 0.6107 0.3734 0.8423 0.050 Uiso 1 1 calc R . . C73 C 0.3859(2) 0.28303(13) 0.92034(10) 0.0342(5) Uani 1 1 d . . . C74 C 0.4368(2) 0.35867(14) 0.95883(11) 0.0413(5) Uani 1 1 d . . . H74 H 0.5268 0.3794 0.9522 0.050 Uiso 1 1 calc R . . C75 C 0.3626(3) 0.40493(15) 1.00622(12) 0.0511(6) Uani 1 1 d . . . H75 H 0.4016 0.4563 1.0305 0.061 Uiso 1 1 calc R . . C76 C 0.2331(3) 0.37668(18) 1.01803(12) 0.0541(7) Uani 1 1 d . . . H76 H 0.1813 0.4084 1.0500 0.065 Uiso 1 1 calc R . . C77 C 0.1792(2) 0.30147(17) 0.98281(12) 0.0496(6) Uani 1 1 d . . . H77 H 0.0904 0.2805 0.9912 0.060 Uiso 1 1 calc R . . C78 C 0.2539(2) 0.25644(15) 0.93523(11) 0.0407(5) Uani 1 1 d . . . H78 H 0.2138 0.2050 0.9115 0.049 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 0.03598(14) 0.02827(13) 0.03152(14) 0.00824(10) -0.00475(10) 0.00045(10) P1 0.0268(5) 0.0245(4) 0.0295(4) 0.0054(3) -0.0005(3) 0.0026(4) N1 0.0278(11) 0.0275(11) 0.0315(11) 0.0071(9) 0.0003(9) 0.0021(8) P1B 0.0276(19) 0.0298(16) 0.0308(18) 0.0041(13) -0.0010(14) 0.0023(15) N1B 0.030(4) 0.033(5) 0.022(4) 0.005(3) 0.000(3) 0.008(3) P2 0.0292(4) 0.0236(3) 0.0290(4) 0.0050(3) -0.0006(3) 0.0029(3) N2 0.0319(11) 0.0273(10) 0.0300(10) 0.0061(8) 0.0007(9) 0.0018(8) P2B 0.019(2) 0.0269(19) 0.028(2) 0.0079(15) 0.0064(16) 0.0002(16) N2B 0.017(5) 0.019(5) 0.022(5) 0.003(4) -0.001(4) 0.003(4) O1 0.0522(9) 0.0248(7) 0.0377(8) 0.0021(6) -0.0173(7) 0.0074(6) C1 0.0342(11) 0.0284(10) 0.0367(11) 0.0093(9) -0.0066(9) 0.0048(8) B1 0.0297(12) 0.0351(13) 0.0369(13) 0.0111(10) -0.0016(10) 0.0005(10) C1S 0.080(2) 0.0355(13) 0.0532(16) -0.0019(12) 0.0279(15) -0.0107(13) C2 0.0359(11) 0.0295(11) 0.0390(12) 0.0068(9) -0.0080(9) 0.0051(9) C2S 0.094(2) 0.0388(14) 0.0396(14) 0.0035(11) 0.0203(14) 0.0078(14) C3 0.0351(11) 0.0282(11) 0.0436(12) 0.0096(9) -0.0027(9) 0.0036(9) C3S 0.0681(18) 0.0514(16) 0.0461(15) -0.0091(12) 0.0109(13) 0.0034(13) C4 0.0335(11) 0.0341(11) 0.0428(12) 0.0182(10) -0.0028(9) 0.0048(9) C5 0.0318(11) 0.0403(12) 0.0330(11) 0.0153(9) -0.0031(9) 0.0025(9) C6 0.0276(10) 0.0340(11) 0.0320(11) 0.0085(9) -0.0010(8) 0.0022(8) C7 0.0292(10) 0.0339(11) 0.0292(10) 0.0065(9) -0.0001(8) 0.0036(8) C8 0.0343(11) 0.0435(12) 0.0292(11) 0.0049(9) -0.0030(9) 0.0040(9) C9 0.0437(13) 0.0379(12) 0.0337(11) -0.0032(9) -0.0089(10) 0.0013(10) C10 0.0465(13) 0.0297(11) 0.0394(12) 0.0000(9) -0.0066(10) 0.0026(9) C11 0.0433(12) 0.0299(11) 0.0354(11) 0.0038(9) -0.0068(9) 0.0053(9) C12 0.0371(11) 0.0283(11) 0.0317(11) 0.0017(8) -0.0067(9) 0.0013(9) C13 0.0373(11) 0.0257(10) 0.0324(11) 0.0020(8) -0.0019(9) 0.0049(8) C14 0.0345(12) 0.0419(13) 0.0441(13) 0.0058(10) 0.0026(10) 0.0052(10) C15 0.0458(14) 0.0444(14) 0.0541(15) 0.0143(11) -0.0004(11) -0.0092(11) C16 0.0626(16) 0.0266(11) 0.0597(16) 0.0117(11) -0.0026(12) 0.0002(11) C17 0.0451(14) 0.0387(13) 0.0602(15) 0.0095(11) 0.0001(11) 0.0155(11) C18 0.0343(11) 0.0350(12) 0.0463(13) 0.0072(10) 0.0007(10) 0.0014(9) C19 0.0346(12) 0.0377(12) 0.0532(14) 0.0203(10) 0.0119(10) 0.0124(9) C20 0.0356(12) 0.0322(11) 0.0500(14) 0.0044(10) -0.0044(10) 0.0013(9) C21 0.0499(14) 0.0513(14) 0.0402(13) 0.0128(11) 0.0140(11) 0.0119(11) C22 0.0315(12) 0.0476(14) 0.0812(19) 0.0221(13) 0.0143(12) 0.0035(10) C23 0.0487(15) 0.0506(15) 0.0610(17) 0.0026(13) -0.0195(13) 0.0074(12) C24 0.0520(15) 0.0587(16) 0.0392(13) 0.0120(11) 0.0077(11) 0.0227(12) C25 0.0476(13) 0.0328(12) 0.0544(14) 0.0150(11) 0.0210(11) 0.0101(10) C26 0.0459(14) 0.0639(17) 0.0599(16) 0.0223(14) -0.0016(12) -0.0080(12) C27 0.0672(19) 0.103(3) 0.0481(16) 0.0338(16) 0.0021(14) -0.0083(17) C28 0.0587(18) 0.084(2) 0.0624(18) 0.0266(16) 0.0227(14) -0.0042(15) C29 0.0420(14) 0.0680(18) 0.0744(19) 0.0235(15) 0.0146(13) 0.0051(13) C30 0.0594(16) 0.0640(17) 0.0619(17) 0.0342(14) 0.0234(13) 0.0255(13) C31 0.0320(11) 0.0289(10) 0.0378(11) 0.0033(9) -0.0055(9) 0.0054(8) C32 0.0326(11) 0.0487(14) 0.0436(13) 0.0086(11) 0.0036(10) 0.0060(10) C33 0.0516(15) 0.0463(15) 0.0660(17) 0.0163(13) -0.0059(13) -0.0145(12) C34 0.084(2) 0.0286(13) 0.0666(18) -0.0051(12) -0.0147(16) -0.0007(13) C35 0.0737(18) 0.0499(16) 0.0449(14) -0.0040(12) 0.0066(13) 0.0194(14) C36 0.0434(13) 0.0418(13) 0.0438(13) 0.0106(10) 0.0053(10) 0.0037(10) C37 0.0379(13) 0.0544(15) 0.0441(14) -0.0028(11) 0.0105(10) -0.0049(11) C38 0.0445(14) 0.0440(14) 0.0575(15) 0.0091(12) 0.0066(12) -0.0029(11) C39 0.0382(14) 0.0537(16) 0.095(2) 0.0102(16) 0.0152(14) -0.0026(12) C40 0.088(2) 0.0531(18) 0.093(2) 0.0243(17) 0.049(2) -0.0043(16) C41 0.112(3) 0.0592(18) 0.0622(19) 0.0239(15) 0.0159(19) 0.0321(19) C42 0.0518(16) 0.0688(18) 0.0570(17) 0.0067(14) 0.0119(13) 0.0228(14) C43 0.0374(12) 0.0439(13) 0.0500(14) -0.0011(11) 0.0113(10) -0.0041(10) C44 0.0496(14) 0.0421(13) 0.0474(14) -0.0013(11) 0.0130(11) -0.0017(11) C45 0.0486(14) 0.0594(16) 0.0469(14) 0.0232(12) 0.0172(12) 0.0173(12) C46 0.0314(13) 0.094(2) 0.0618(17) 0.0353(16) 0.0091(12) 0.0077(13) C47 0.0308(12) 0.0709(18) 0.0646(17) 0.0214(14) -0.0076(11) -0.0011(12) C48 0.0407(13) 0.0441(13) 0.0468(13) 0.0036(11) 0.0037(10) 0.0000(10) C49 0.0319(11) 0.0382(11) 0.0319(11) 0.0114(9) -0.0012(9) 0.0032(9) C50 0.0390(13) 0.0424(13) 0.0375(13) 0.0122(11) 0.0037(10) 0.0043(10) C51 0.0431(14) 0.0623(17) 0.0476(15) 0.0313(14) 0.0054(12) 0.0110(12) C52 0.0424(14) 0.082(2) 0.0328(13) 0.0218(14) -0.0024(11) 0.0029(14) C53 0.0481(15) 0.0649(18) 0.0306(13) -0.0011(12) -0.0007(11) 0.0008(13) C54 0.0403(13) 0.0472(14) 0.0361(13) 0.0065(11) 0.0018(10) 0.0070(11) C49B 0.0319(11) 0.0382(11) 0.0319(11) 0.0114(9) -0.0012(9) 0.0032(9) C55 0.0341(11) 0.0315(11) 0.0371(11) 0.0082(9) -0.0009(9) 0.0015(9) C56 0.0368(11) 0.0290(11) 0.0375(11) 0.0068(9) -0.0009(9) 0.0045(9) C57 0.0421(12) 0.0379(12) 0.0457(13) 0.0077(10) -0.0072(10) 0.0085(10) C58 0.0580(16) 0.0587(16) 0.0372(13) 0.0122(11) -0.0073(11) 0.0049(12) C59 0.0526(16) 0.090(2) 0.0406(14) 0.0195(14) 0.0084(12) 0.0109(14) C60 0.0386(13) 0.0757(18) 0.0443(14) 0.0179(13) 0.0012(11) 0.0071(12) C61 0.0231(10) 0.0374(12) 0.0552(14) 0.0134(10) -0.0032(9) -0.0027(9) C62 0.0359(12) 0.0419(13) 0.0671(17) 0.0042(12) 0.0012(11) 0.0020(10) C63 0.0406(14) 0.0411(15) 0.106(2) -0.0013(16) 0.0017(15) 0.0019(11) C64 0.0508(17) 0.0395(16) 0.140(3) 0.027(2) -0.0001(19) 0.0020(13) C65 0.0657(19) 0.0604(19) 0.101(3) 0.0483(19) -0.0020(17) -0.0038(15) C66 0.0512(15) 0.0445(14) 0.0630(16) 0.0234(12) -0.0020(12) -0.0025(11) C67 0.0307(11) 0.0348(11) 0.0321(11) 0.0102(9) 0.0005(8) 0.0002(9) C68 0.0326(11) 0.0323(11) 0.0380(11) 0.0090(9) -0.0005(9) -0.0009(9) C69 0.0329(12) 0.0445(13) 0.0531(14) 0.0142(11) -0.0053(10) 0.0038(10) C70 0.0318(12) 0.0526(14) 0.0546(14) 0.0196(12) -0.0025(10) -0.0079(10) C71 0.0436(13) 0.0426(13) 0.0572(15) 0.0249(12) 0.0010(11) -0.0078(10) C72 0.0344(12) 0.0437(13) 0.0535(14) 0.0242(11) -0.0018(10) 0.0017(10) C73 0.0333(11) 0.0365(11) 0.0352(11) 0.0134(9) -0.0043(9) 0.0036(9) C74 0.0450(13) 0.0406(13) 0.0385(12) 0.0110(10) -0.0025(10) -0.0004(10) C75 0.0706(18) 0.0419(14) 0.0402(13) 0.0065(11) -0.0041(12) 0.0080(12) C76 0.0612(17) 0.0693(18) 0.0342(13) 0.0079(12) 0.0003(12) 0.0260(14) C77 0.0363(12) 0.0762(18) 0.0382(13) 0.0148(13) -0.0002(10) 0.0095(12) C78 0.0349(12) 0.0514(14) 0.0354(12) 0.0097(10) -0.0045(9) 0.0015(10) _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 C49 1.977(2) . ? Zn1 N2 2.0015(19) . ? Zn1 N1 2.004(2) . ? Zn1 N2B 2.099(9) . ? Zn1 N1B 2.112(8) . ? P1 N1 1.601(2) . ? P1 C31 1.811(2) . ? P1 C2 1.817(2) . ? P1 C37 1.830(3) . ? N1 C43 1.446(3) . ? P1B N1B 1.618(9) . ? P1B C2 1.807(4) . ? P1B C31 1.811(4) . ? P1B C43 2.035(5) . ? N1B C37 1.485(8) . ? P2 N2 1.600(2) . ? P2 C13 1.810(2) . ? P2 C11 1.810(2) . ? P2 C19 1.829(2) . ? N2 C25 1.455(3) . ? P2B N2B 1.628(10) . ? P2B C13 1.794(4) . ? P2B C11 1.888(4) . ? P2B C25 1.953(5) . ? N2B C19 1.560(10) . ? O1 C12 1.376(2) . ? O1 C1 1.378(2) . ? C1 C2 1.378(3) . ? C1 C6 1.392(3) . ? B1 C67 1.641(3) . ? B1 C73 1.647(3) . ? B1 C55 1.648(3) . ? B1 C61 1.649(3) . ? C1S C2S 1.370(4) . ? C1S C3S 1.380(4) 2_575 ? C1S H1S 0.9500 . ? C2 C3 1.398(3) . ? C2S C3S 1.378(4) . ? C2S H2S 0.9500 . ? C3 C4 1.397(3) . ? C3 H3 0.9500 . ? C3S C1S 1.380(4) 2_575 ? C3S H3S 0.9500 . ? C4 C5 1.378(3) . ? C4 H4 0.9500 . ? C5 C6 1.395(3) . ? C5 H5 0.9500 . ? C6 C7 1.456(3) . ? C7 C12 1.386(3) . ? C7 C8 1.394(3) . ? C8 C9 1.375(3) . ? C8 H8 0.9500 . ? C9 C10 1.392(3) . ? C9 H9 0.9500 . ? C10 C11 1.395(3) . ? C10 H10 0.9500 . ? C11 C12 1.386(3) . ? C13 C14 1.386(3) . ? C13 C18 1.387(3) . ? C14 C15 1.378(3) . ? C14 H14 0.9500 . ? C15 C16 1.379(4) . ? C15 H15 0.9500 . ? C16 C17 1.381(3) . ? C16 H16 0.9500 . ? C17 C18 1.375(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.358(3) . ? C19 C24 1.382(3) . ? C20 C21 1.375(3) . ? C20 H20 0.9500 . ? C21 C22 1.382(4) . ? C21 H21 0.9500 . ? C22 C23 1.375(4) . ? C22 H22 0.9500 . ? C23 C24 1.379(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.351(3) . ? C25 C30 1.395(4) . ? C26 C27 1.376(4) . ? C26 H26 0.9500 . ? C27 C28 1.371(4) . ? C27 H27 0.9500 . ? C28 C29 1.365(4) . ? C28 H28 0.9500 . ? C29 C30 1.382(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.386(3) . ? C31 C36 1.389(3) . ? C32 C33 1.367(3) . ? C32 H32 0.9500 . ? C33 C34 1.369(4) . ? C33 H33 0.9500 . ? C34 C35 1.376(4) . ? C34 H34 0.9500 . ? C35 C36 1.382(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.366(3) . ? C37 C42 1.373(4) . ? C38 C39 1.369(4) . ? C38 H38 0.9500 . ? C39 C40 1.371(5) . ? C39 H39 0.9500 . ? C40 C41 1.395(5) . ? C40 H40 0.9500 . ? C41 C42 1.387(4) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48 1.366(3) . ? C43 C44 1.401(3) . ? C44 C45 1.360(3) . ? C44 H44 0.9500 . ? C45 C46 1.380(4) . ? C45 H45 0.9500 . ? C46 C47 1.366(4) . ? C46 H46 0.9500 . ? C47 C48 1.380(3) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C54 1.375(3) . ? C49 C50 1.417(3) . ? C50 C51 1.387(3) . ? C50 H50 0.9500 . ? C51 C52 1.373(4) . ? C51 H51 0.9500 . ? C52 C53 1.369(4) . ? C52 H52 0.9500 . ? C53 C54 1.392(3) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.392(3) . ? C55 C60 1.398(3) . ? C56 C57 1.387(3) . ? C56 H56 0.9500 . ? C57 C58 1.369(3) . ? C57 H57 0.9500 . ? C58 C59 1.378(4) . ? C58 H58 0.9500 . ? C59 C60 1.384(3) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C66 1.393(3) . ? C61 C62 1.398(3) . ? C62 C63 1.390(4) . ? C62 H62 0.9500 . ? C63 C64 1.368(5) . ? C63 H63 0.9500 . ? C64 C65 1.377(5) . ? C64 H64 0.9500 . ? C65 C66 1.389(4) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C68 1.390(3) . ? C67 C72 1.404(3) . ? C68 C69 1.391(3) . ? C68 H68 0.9500 . ? C69 C70 1.376(3) . ? C69 H69 0.9500 . ? C70 C71 1.376(3) . ? C70 H70 0.9500 . ? C71 C72 1.381(3) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.400(3) . ? C73 C78 1.404(3) . ? C74 C75 1.389(3) . ? C74 H74 0.9500 . ? C75 C76 1.371(4) . ? C75 H75 0.9500 . ? C76 C77 1.379(4) . ? C76 H76 0.9500 . ? C77 C78 1.384(3) . ? C77 H77 0.9500 . ? C78 H78 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 C49 Zn1 N2 118.36(8) . . ? C49 Zn1 N1 116.12(8) . . ? N2 Zn1 N1 125.52(8) . . ? C49 Zn1 N2B 117.2(3) . . ? N2 Zn1 N2B 34.3(3) . . ? N1 Zn1 N2B 114.6(3) . . ? C49 Zn1 N1B 121.2(2) . . ? N2 Zn1 N1B 109.8(2) . . ? N1 Zn1 N1B 34.8(2) . . ? N2B Zn1 N1B 121.6(3) . . ? N1 P1 C31 113.63(11) . . ? N1 P1 C2 114.52(11) . . ? C31 P1 C2 104.89(10) . . ? N1 P1 C37 103.21(12) . . ? C31 P1 C37 112.13(11) . . ? C2 P1 C37 108.58(11) . . ? C43 N1 P1 115.95(17) . . ? C43 N1 Zn1 116.99(15) . . ? P1 N1 Zn1 126.30(12) . . ? N1B P1B C2 106.4(4) . . ? N1B P1B C31 108.2(4) . . ? C2 P1B C31 105.3(2) . . ? N1B P1B C43 92.8(3) . . ? C2 P1B C43 127.1(2) . . ? C31 P1B C43 114.7(2) . . ? C37 N1B P1B 106.6(5) . . ? C37 N1B Zn1 128.5(5) . . ? P1B N1B Zn1 122.7(5) . . ? N2 P2 C13 111.26(10) . . ? N2 P2 C11 113.92(11) . . ? C13 P2 C11 107.94(10) . . ? N2 P2 C19 105.21(11) . . ? C13 P2 C19 110.82(10) . . ? C11 P2 C19 107.64(11) . . ? C25 N2 P2 115.13(16) . . ? C25 N2 Zn1 117.07(15) . . ? P2 N2 Zn1 127.75(12) . . ? N2B P2B C13 107.4(4) . . ? N2B P2B C11 103.8(4) . . ? C13 P2B C11 105.3(2) . . ? N2B P2B C25 94.4(4) . . ? C13 P2B C25 113.1(2) . . ? C11 P2B C25 129.9(2) . . ? C19 N2B P2B 105.2(6) . . ? C19 N2B Zn1 131.4(5) . . ? P2B N2B Zn1 121.4(5) . . ? C12 O1 C1 105.55(15) . . ? O1 C1 C2 122.56(18) . . ? O1 C1 C6 111.81(17) . . ? C2 C1 C6 125.54(19) . . ? C67 B1 C73 110.31(17) . . ? C67 B1 C55 108.99(17) . . ? C73 B1 C55 110.44(17) . . ? C67 B1 C61 107.87(17) . . ? C73 B1 C61 111.59(17) . . ? C55 B1 C61 107.54(17) . . ? C2S C1S C3S 120.2(2) . 2_575 ? C2S C1S H1S 119.9 . . ? C3S C1S H1S 119.9 2_575 . ? C1 C2 C3 115.02(19) . . ? C1 C2 P1B 118.45(19) . . ? C3 C2 P1B 124.6(2) . . ? C1 C2 P1 117.70(15) . . ? C3 C2 P1 126.52(17) . . ? P1B C2 P1 21.60(11) . . ? C1S C2S C3S 120.3(3) . . ? C1S C2S H2S 119.8 . . ? C3S C2S H2S 119.8 . . ? C4 C3 C2 121.1(2) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C2S C3S C1S 119.4(3) . 2_575 ? C2S C3S H3S 120.3 . . ? C1S C3S H3S 120.3 2_575 . ? C5 C4 C3 121.90(19) . . ? C5 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? C4 C5 C6 118.54(19) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C1 C6 C5 117.84(19) . . ? C1 C6 C7 105.14(17) . . ? C5 C6 C7 136.99(19) . . ? C12 C7 C8 118.00(19) . . ? C12 C7 C6 105.65(17) . . ? C8 C7 C6 136.32(19) . . ? C9 C8 C7 118.02(19) . . ? C9 C8 H8 121.0 . . ? C7 C8 H8 121.0 . . ? C8 C9 C10 122.6(2) . . ? C8 C9 H9 118.7 . . ? C10 C9 H9 118.7 . . ? C9 C10 C11 121.1(2) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C12 C11 C10 114.60(19) . . ? C12 C11 P2 117.43(15) . . ? C10 C11 P2 127.60(17) . . ? C12 C11 P2B 117.35(19) . . ? C10 C11 P2B 124.9(2) . . ? P2 C11 P2B 22.68(12) . . ? O1 C12 C11 122.45(18) . . ? O1 C12 C7 111.82(17) . . ? C11 C12 C7 125.72(19) . . ? C14 C13 C18 119.63(19) . . ? C14 C13 P2B 101.7(2) . . ? C18 C13 P2B 135.5(2) . . ? C14 C13 P2 122.55(16) . . ? C18 C13 P2 117.62(16) . . ? P2B C13 P2 23.41(13) . . ? C15 C14 C13 120.2(2) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 119.7(2) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C17 120.5(2) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 119.9(2) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C13 120.1(2) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C20 C19 C24 119.7(2) . . ? C20 C19 N2B 147.6(4) . . ? C24 C19 N2B 85.4(4) . . ? C20 C19 P2 118.63(18) . . ? C24 C19 P2 121.61(18) . . ? N2B C19 P2 43.6(3) . . ? C19 C20 C21 121.1(2) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C21 C22 119.6(2) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 119.5(2) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 120.3(2) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C19 119.8(2) . . ? C23 C24 H24 120.1 . . ? C19 C24 H24 120.1 . . ? C26 C25 C30 119.1(2) . . ? C26 C25 N2 117.6(2) . . ? C30 C25 N2 123.2(2) . . ? C26 C25 P2B 127.0(2) . . ? C30 C25 P2B 100.4(2) . . ? N2 C25 P2B 43.35(15) . . ? C25 C26 C27 120.8(3) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C28 C27 C26 120.4(3) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C29 C28 C27 119.8(3) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 119.8(3) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C29 C30 C25 120.1(2) . . ? C29 C30 H30 119.9 . . ? C25 C30 H30 119.9 . . ? C32 C31 C36 119.8(2) . . ? C32 C31 P1 123.31(17) . . ? C36 C31 P1 116.87(17) . . ? C32 C31 P1B 102.3(2) . . ? C36 C31 P1B 137.3(2) . . ? P1 C31 P1B 21.62(11) . . ? C33 C32 C31 120.0(2) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120.4(2) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C33 C34 C35 120.4(2) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C34 C35 C36 120.0(2) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 119.4(2) . . ? C35 C36 H36 120.3 . . ? C31 C36 H36 120.3 . . ? C38 C37 C42 119.9(2) . . ? C38 C37 N1B 143.6(4) . . ? C42 C37 N1B 87.9(3) . . ? C38 C37 P1 118.2(2) . . ? C42 C37 P1 121.8(2) . . ? N1B C37 P1 42.9(3) . . ? C37 C38 C39 121.1(3) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.4 . . ? C38 C39 C40 119.9(3) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C39 C40 C41 119.5(3) . . ? C39 C40 H40 120.2 . . ? C41 C40 H40 120.2 . . ? C42 C41 C40 119.7(3) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C37 C42 C41 119.7(3) . . ? C37 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C48 C43 C44 119.4(2) . . ? C48 C43 N1 119.9(2) . . ? C44 C43 N1 120.6(2) . . ? C48 C43 P1B 115.9(2) . . ? C44 C43 P1B 109.7(2) . . ? N1 C43 P1B 43.45(15) . . ? C45 C44 C43 120.4(2) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C44 C45 C46 119.5(2) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C47 C46 C45 120.3(2) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C46 C47 C48 120.4(2) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C43 C48 C47 119.9(2) . . ? C43 C48 H48 120.1 . . ? C47 C48 H48 120.1 . . ? C54 C49 C50 116.3(2) . . ? C54 C49 Zn1 122.15(17) . . ? C50 C49 Zn1 121.58(16) . . ? C51 C50 C49 121.5(2) . . ? C51 C50 H50 119.3 . . ? C49 C50 H50 119.3 . . ? C52 C51 C50 119.9(2) . . ? C52 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? C53 C52 C51 119.9(2) . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C54 120.0(3) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C49 C54 C53 122.3(2) . . ? C49 C54 H54 118.8 . . ? C53 C54 H54 118.8 . . ? C56 C55 C60 114.9(2) . . ? C56 C55 B1 124.28(19) . . ? C60 C55 B1 120.50(19) . . ? C57 C56 C55 122.9(2) . . ? C57 C56 H56 118.6 . . ? C55 C56 H56 118.6 . . ? C58 C57 C56 120.5(2) . . ? C58 C57 H57 119.7 . . ? C56 C57 H57 119.7 . . ? C57 C58 C59 118.6(2) . . ? C57 C58 H58 120.7 . . ? C59 C58 H58 120.7 . . ? C58 C59 C60 120.4(2) . . ? C58 C59 H59 119.8 . . ? C60 C59 H59 119.8 . . ? C59 C60 C55 122.7(2) . . ? C59 C60 H60 118.6 . . ? C55 C60 H60 118.6 . . ? C66 C61 C62 114.7(2) . . ? C66 C61 B1 123.0(2) . . ? C62 C61 B1 122.1(2) . . ? C63 C62 C61 122.9(3) . . ? C63 C62 H62 118.6 . . ? C61 C62 H62 118.6 . . ? C64 C63 C62 120.4(3) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C63 C64 C65 118.7(3) . . ? C63 C64 H64 120.6 . . ? C65 C64 H64 120.6 . . ? C64 C65 C66 120.3(3) . . ? C64 C65 H65 119.9 . . ? C66 C65 H65 119.9 . . ? C65 C66 C61 122.9(3) . . ? C65 C66 H66 118.5 . . ? C61 C66 H66 118.5 . . ? C68 C67 C72 115.16(19) . . ? C68 C67 B1 123.81(18) . . ? C72 C67 B1 121.03(18) . . ? C67 C68 C69 122.5(2) . . ? C67 C68 H68 118.7 . . ? C69 C68 H68 118.7 . . ? C70 C69 C68 120.4(2) . . ? C70 C69 H69 119.8 . . ? C68 C69 H69 119.8 . . ? C71 C70 C69 118.7(2) . . ? C71 C70 H70 120.6 . . ? C69 C70 H70 120.6 . . ? C70 C71 C72 120.4(2) . . ? C70 C71 H71 119.8 . . ? C72 C71 H71 119.8 . . ? C71 C72 C67 122.6(2) . . ? C71 C72 H72 118.7 . . ? C67 C72 H72 118.7 . . ? C74 C73 C78 114.0(2) . . ? C74 C73 B1 123.84(19) . . ? C78 C73 B1 122.05(19) . . ? C75 C74 C73 123.4(2) . . ? C75 C74 H74 118.3 . . ? C73 C74 H74 118.3 . . ? C76 C75 C74 120.1(2) . . ? C76 C75 H75 119.9 . . ? C74 C75 H75 119.9 . . ? C75 C76 C77 118.9(2) . . ? C75 C76 H76 120.6 . . ? C77 C76 H76 120.6 . . ? C76 C77 C78 120.3(2) . . ? C76 C77 H77 119.9 . . ? C78 C77 H77 119.9 . . ? C77 C78 C73 123.2(2) . . ? C77 C78 H78 118.4 . . ? C73 C78 H78 118.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C31 P1 N1 C43 51.2(2) . . . . ? C2 P1 N1 C43 -69.3(2) . . . . ? C37 P1 N1 C43 172.85(17) . . . . ? C31 P1 N1 Zn1 -139.21(13) . . . . ? C2 P1 N1 Zn1 100.28(15) . . . . ? C37 P1 N1 Zn1 -17.54(17) . . . . ? C49 Zn1 N1 C43 -69.53(18) . . . . ? N2 Zn1 N1 C43 110.04(17) . . . . ? N2B Zn1 N1 C43 72.2(3) . . . . ? N1B Zn1 N1 C43 -177.3(4) . . . . ? C49 Zn1 N1 P1 120.96(14) . . . . ? N2 Zn1 N1 P1 -59.47(18) . . . . ? N2B Zn1 N1 P1 -97.3(3) . . . . ? N1B Zn1 N1 P1 13.1(4) . . . . ? C2 P1B N1B C37 55.8(5) . . . . ? C31 P1B N1B C37 -57.0(5) . . . . ? C43 P1B N1B C37 -174.2(4) . . . . ? C2 P1B N1B Zn1 -108.8(4) . . . . ? C31 P1B N1B Zn1 138.5(4) . . . . ? C43 P1B N1B Zn1 21.3(5) . . . . ? C49 Zn1 N1B C37 92.0(6) . . . . ? N2 Zn1 N1B C37 -51.9(6) . . . . ? N1 Zn1 N1B C37 -176.3(8) . . . . ? N2B Zn1 N1B C37 -87.8(6) . . . . ? C49 Zn1 N1B P1B -107.1(5) . . . . ? N2 Zn1 N1B P1B 109.1(5) . . . . ? N1 Zn1 N1B P1B -15.3(3) . . . . ? N2B Zn1 N1B P1B 73.1(6) . . . . ? C13 P2 N2 C25 46.49(19) . . . . ? C11 P2 N2 C25 -75.79(18) . . . . ? C19 P2 N2 C25 166.55(16) . . . . ? C13 P2 N2 Zn1 -136.01(13) . . . . ? C11 P2 N2 Zn1 101.71(15) . . . . ? C19 P2 N2 Zn1 -15.94(16) . . . . ? C49 Zn1 N2 C25 -71.47(18) . . . . ? N1 Zn1 N2 C25 108.97(17) . . . . ? N2B Zn1 N2 C25 -169.0(5) . . . . ? N1B Zn1 N2 C25 73.6(3) . . . . ? C49 Zn1 N2 P2 111.07(14) . . . . ? N1 Zn1 N2 P2 -68.49(17) . . . . ? N2B Zn1 N2 P2 13.5(4) . . . . ? N1B Zn1 N2 P2 -103.9(3) . . . . ? C13 P2B N2B C19 -56.5(5) . . . . ? C11 P2B N2B C19 54.7(5) . . . . ? C25 P2B N2B C19 -172.3(4) . . . . ? C13 P2B N2B Zn1 138.0(4) . . . . ? C11 P2B N2B Zn1 -110.8(5) . . . . ? C25 P2B N2B Zn1 22.2(6) . . . . ? C49 Zn1 N2B C19 86.5(7) . . . . ? N2 Zn1 N2B C19 -172.3(10) . . . . ? N1 Zn1 N2B C19 -54.7(7) . . . . ? N1B Zn1 N2B C19 -93.6(7) . . . . ? C49 Zn1 N2B P2B -112.3(5) . . . . ? N2 Zn1 N2B P2B -11.1(3) . . . . ? N1 Zn1 N2B P2B 106.4(5) . . . . ? N1B Zn1 N2B P2B 67.5(7) . . . . ? C12 O1 C1 C2 -175.5(2) . . . . ? C12 O1 C1 C6 1.3(2) . . . . ? O1 C1 C2 C3 179.13(19) . . . . ? C6 C1 C2 C3 2.8(3) . . . . ? O1 C1 C2 P1B -16.1(3) . . . . ? C6 C1 C2 P1B 167.6(2) . . . . ? O1 C1 C2 P1 8.4(3) . . . . ? C6 C1 C2 P1 -167.90(18) . . . . ? N1B P1B C2 C1 54.9(4) . . . . ? C31 P1B C2 C1 169.7(2) . . . . ? C43 P1B C2 C1 -51.8(4) . . . . ? N1B P1B C2 C3 -141.9(4) . . . . ? C31 P1B C2 C3 -27.1(3) . . . . ? C43 P1B C2 C3 111.5(3) . . . . ? N1B P1B C2 P1 -39.0(4) . . . . ? C31 P1B C2 P1 75.8(3) . . . . ? C43 P1B C2 P1 -145.7(5) . . . . ? N1 P1 C2 C1 -47.9(2) . . . . ? C31 P1 C2 C1 -173.15(17) . . . . ? C37 P1 C2 C1 66.8(2) . . . . ? N1 P1 C2 C3 142.6(2) . . . . ? C31 P1 C2 C3 17.4(2) . . . . ? C37 P1 C2 C3 -102.7(2) . . . . ? N1 P1 C2 P1B 49.9(3) . . . . ? C31 P1 C2 P1B -75.4(3) . . . . ? C37 P1 C2 P1B 164.6(4) . . . . ? C3S C1S C2S C3S 0.1(4) 2_575 . . . ? C1 C2 C3 C4 -0.7(3) . . . . ? P1B C2 C3 C4 -164.5(2) . . . . ? P1 C2 C3 C4 168.99(17) . . . . ? C1S C2S C3S C1S -0.1(4) . . . 2_575 ? C2 C3 C4 C5 -0.8(3) . . . . ? C3 C4 C5 C6 0.5(3) . . . . ? O1 C1 C6 C5 -179.84(18) . . . . ? C2 C1 C6 C5 -3.2(3) . . . . ? O1 C1 C6 C7 -1.2(2) . . . . ? C2 C1 C6 C7 175.4(2) . . . . ? C4 C5 C6 C1 1.4(3) . . . . ? C4 C5 C6 C7 -176.7(2) . . . . ? C1 C6 C7 C12 0.7(2) . . . . ? C5 C6 C7 C12 178.9(2) . . . . ? C1 C6 C7 C8 -177.3(2) . . . . ? C5 C6 C7 C8 0.9(4) . . . . ? C12 C7 C8 C9 -0.1(3) . . . . ? C6 C7 C8 C9 177.7(2) . . . . ? C7 C8 C9 C10 1.5(3) . . . . ? C8 C9 C10 C11 -0.9(4) . . . . ? C9 C10 C11 C12 -1.0(3) . . . . ? C9 C10 C11 P2 171.76(19) . . . . ? C9 C10 C11 P2B -160.2(2) . . . . ? N2 P2 C11 C12 -46.3(2) . . . . ? C13 P2 C11 C12 -170.35(17) . . . . ? C19 P2 C11 C12 70.0(2) . . . . ? N2 P2 C11 C10 141.1(2) . . . . ? C13 P2 C11 C10 17.1(3) . . . . ? C19 P2 C11 C10 -102.6(2) . . . . ? N2 P2 C11 P2B 49.5(3) . . . . ? C13 P2 C11 P2B -74.6(3) . . . . ? C19 P2 C11 P2B 165.8(3) . . . . ? N2B P2B C11 C12 57.0(5) . . . . ? C13 P2B C11 C12 169.7(2) . . . . ? C25 P2B C11 C12 -51.0(4) . . . . ? N2B P2B C11 C10 -144.3(4) . . . . ? C13 P2B C11 C10 -31.6(4) . . . . ? C25 P2B C11 C10 107.7(3) . . . . ? N2B P2B C11 P2 -39.2(4) . . . . ? C13 P2B C11 P2 73.5(3) . . . . ? C25 P2B C11 P2 -147.2(5) . . . . ? C1 O1 C12 C11 179.7(2) . . . . ? C1 O1 C12 C7 -0.9(2) . . . . ? C10 C11 C12 O1 -178.1(2) . . . . ? P2 C11 C12 O1 8.4(3) . . . . ? P2B C11 C12 O1 -17.2(3) . . . . ? C10 C11 C12 C7 2.5(3) . . . . ? P2 C11 C12 C7 -171.01(18) . . . . ? P2B C11 C12 C7 163.4(2) . . . . ? C8 C7 C12 O1 178.50(18) . . . . ? C6 C7 C12 O1 0.1(2) . . . . ? C8 C7 C12 C11 -2.0(3) . . . . ? C6 C7 C12 C11 179.6(2) . . . . ? N2B P2B C13 C14 -163.7(4) . . . . ? C11 P2B C13 C14 86.1(2) . . . . ? C25 P2B C13 C14 -61.0(3) . . . . ? N2B P2B C13 C18 -4.9(5) . . . . ? C11 P2B C13 C18 -115.1(3) . . . . ? C25 P2B C13 C18 97.8(3) . . . . ? N2B P2B C13 P2 41.6(4) . . . . ? C11 P2B C13 P2 -68.6(3) . . . . ? C25 P2B C13 P2 144.3(5) . . . . ? N2 P2 C13 C14 -75.5(2) . . . . ? C11 P2 C13 C14 50.2(2) . . . . ? C19 P2 C13 C14 167.79(18) . . . . ? N2 P2 C13 C18 99.27(19) . . . . ? C11 P2 C13 C18 -135.05(18) . . . . ? C19 P2 C13 C18 -17.4(2) . . . . ? N2 P2 C13 P2B -45.7(3) . . . . ? C11 P2 C13 P2B 79.9(3) . . . . ? C19 P2 C13 P2B -162.4(3) . . . . ? C18 C13 C14 C15 -0.8(3) . . . . ? P2B C13 C14 C15 162.2(2) . . . . ? P2 C13 C14 C15 173.86(18) . . . . ? C13 C14 C15 C16 0.6(4) . . . . ? C14 C15 C16 C17 0.3(4) . . . . ? C15 C16 C17 C18 -0.9(4) . . . . ? C16 C17 C18 C13 0.7(4) . . . . ? C14 C13 C18 C17 0.2(3) . . . . ? P2B C13 C18 C17 -155.8(3) . . . . ? P2 C13 C18 C17 -174.76(18) . . . . ? P2B N2B C19 C20 -70.0(9) . . . . ? Zn1 N2B C19 C20 93.4(9) . . . . ? P2B N2B C19 C24 146.8(5) . . . . ? Zn1 N2B C19 C24 -49.8(6) . . . . ? P2B N2B C19 P2 -1.06(17) . . . . ? Zn1 N2B C19 P2 162.4(10) . . . . ? N2 P2 C19 C20 144.52(18) . . . . ? C13 P2 C19 C20 -95.13(19) . . . . ? C11 P2 C19 C20 22.7(2) . . . . ? N2 P2 C19 C24 -39.3(2) . . . . ? C13 P2 C19 C24 81.1(2) . . . . ? C11 P2 C19 C24 -161.12(19) . . . . ? N2 P2 C19 N2B -0.8(5) . . . . ? C13 P2 C19 N2B 119.6(5) . . . . ? C11 P2 C19 N2B -122.6(5) . . . . ? C24 C19 C20 C21 -0.1(3) . . . . ? N2B C19 C20 C21 -136.7(7) . . . . ? P2 C19 C20 C21 176.14(18) . . . . ? C19 C20 C21 C22 1.4(4) . . . . ? C20 C21 C22 C23 -0.8(4) . . . . ? C21 C22 C23 C24 -1.1(4) . . . . ? C22 C23 C24 C19 2.4(4) . . . . ? C20 C19 C24 C23 -1.8(4) . . . . ? N2B C19 C24 C23 156.6(4) . . . . ? P2 C19 C24 C23 -177.93(19) . . . . ? P2 N2 C25 C26 -111.1(2) . . . . ? Zn1 N2 C25 C26 71.1(3) . . . . ? P2 N2 C25 C30 72.5(3) . . . . ? Zn1 N2 C25 C30 -105.3(3) . . . . ? P2 N2 C25 P2B 4.72(18) . . . . ? Zn1 N2 C25 P2B -173.1(2) . . . . ? N2B P2B C25 C26 83.5(4) . . . . ? C13 P2B C25 C26 -27.5(4) . . . . ? C11 P2B C25 C26 -164.4(3) . . . . ? N2B P2B C25 C30 -137.2(4) . . . . ? C13 P2B C25 C30 111.8(2) . . . . ? C11 P2B C25 C30 -25.1(3) . . . . ? N2B P2B C25 N2 -9.2(3) . . . . ? C13 P2B C25 N2 -120.2(3) . . . . ? C11 P2B C25 N2 103.0(3) . . . . ? C30 C25 C26 C27 1.2(4) . . . . ? N2 C25 C26 C27 -175.3(3) . . . . ? P2B C25 C26 C27 134.0(3) . . . . ? C25 C26 C27 C28 -1.5(5) . . . . ? C26 C27 C28 C29 1.4(5) . . . . ? C27 C28 C29 C30 -1.0(5) . . . . ? C28 C29 C30 C25 0.7(5) . . . . ? C26 C25 C30 C29 -0.8(4) . . . . ? N2 C25 C30 C29 175.5(2) . . . . ? P2B C25 C30 C29 -144.2(3) . . . . ? N1 P1 C31 C32 -66.6(2) . . . . ? C2 P1 C31 C32 59.2(2) . . . . ? C37 P1 C31 C32 176.84(18) . . . . ? N1 P1 C31 C36 112.19(18) . . . . ? C2 P1 C31 C36 -122.01(18) . . . . ? C37 P1 C31 C36 -4.4(2) . . . . ? N1 P1 C31 P1B -51.1(3) . . . . ? C2 P1 C31 P1B 74.7(3) . . . . ? C37 P1 C31 P1B -167.7(4) . . . . ? N1B P1B C31 C32 -156.2(4) . . . . ? C2 P1B C31 C32 90.3(2) . . . . ? C43 P1B C31 C32 -54.1(3) . . . . ? N1B P1B C31 C36 14.8(5) . . . . ? C2 P1B C31 C36 -98.7(3) . . . . ? C43 P1B C31 C36 116.9(3) . . . . ? N1B P1B C31 P1 37.1(4) . . . . ? C2 P1B C31 P1 -76.4(3) . . . . ? C43 P1B C31 P1 139.1(5) . . . . ? C36 C31 C32 C33 -1.9(3) . . . . ? P1 C31 C32 C33 176.88(19) . . . . ? P1B C31 C32 C33 171.1(2) . . . . ? C31 C32 C33 C34 1.0(4) . . . . ? C32 C33 C34 C35 0.8(4) . . . . ? C33 C34 C35 C36 -1.6(4) . . . . ? C34 C35 C36 C31 0.7(4) . . . . ? C32 C31 C36 C35 1.1(3) . . . . ? P1 C31 C36 C35 -177.78(19) . . . . ? P1B C31 C36 C35 -168.8(3) . . . . ? P1B N1B C37 C38 -72.1(8) . . . . ? Zn1 N1B C37 C38 91.2(7) . . . . ? P1B N1B C37 C42 145.4(4) . . . . ? Zn1 N1B C37 C42 -51.3(5) . . . . ? P1B N1B C37 P1 1.04(16) . . . . ? Zn1 N1B C37 P1 164.4(8) . . . . ? N1 P1 C37 C38 140.7(2) . . . . ? C31 P1 C37 C38 -96.7(2) . . . . ? C2 P1 C37 C38 18.8(2) . . . . ? N1 P1 C37 C42 -42.5(2) . . . . ? C31 P1 C37 C42 80.2(2) . . . . ? C2 P1 C37 C42 -164.4(2) . . . . ? N1 P1 C37 N1B 0.8(5) . . . . ? C31 P1 C37 N1B 123.4(5) . . . . ? C2 P1 C37 N1B -121.1(5) . . . . ? C42 C37 C38 C39 0.2(4) . . . . ? N1B C37 C38 C39 -135.3(6) . . . . ? P1 C37 C38 C39 177.0(2) . . . . ? C37 C38 C39 C40 1.8(4) . . . . ? C38 C39 C40 C41 -1.5(5) . . . . ? C39 C40 C41 C42 -0.7(5) . . . . ? C38 C37 C42 C41 -2.4(4) . . . . ? N1B C37 C42 C41 153.0(4) . . . . ? P1 C37 C42 C41 -179.1(2) . . . . ? C40 C41 C42 C37 2.7(4) . . . . ? P1 N1 C43 C48 -93.0(3) . . . . ? Zn1 N1 C43 C48 96.4(2) . . . . ? P1 N1 C43 C44 91.1(3) . . . . ? Zn1 N1 C43 C44 -79.5(3) . . . . ? P1 N1 C43 P1B 4.26(17) . . . . ? Zn1 N1 C43 P1B -166.4(2) . . . . ? N1B P1B C43 C48 102.5(4) . . . . ? C2 P1B C43 C48 -144.5(3) . . . . ? C31 P1B C43 C48 -9.1(3) . . . . ? N1B P1B C43 C44 -118.6(3) . . . . ? C2 P1B C43 C44 -5.5(4) . . . . ? C31 P1B C43 C44 129.8(2) . . . . ? N1B P1B C43 N1 -4.5(3) . . . . ? C2 P1B C43 N1 108.6(3) . . . . ? C31 P1B C43 N1 -116.1(3) . . . . ? C48 C43 C44 C45 -2.8(4) . . . . ? N1 C43 C44 C45 173.1(2) . . . . ? P1B C43 C44 C45 -140.0(2) . . . . ? C43 C44 C45 C46 3.1(4) . . . . ? C44 C45 C46 C47 -2.7(4) . . . . ? C45 C46 C47 C48 1.9(4) . . . . ? C44 C43 C48 C47 2.0(4) . . . . ? N1 C43 C48 C47 -174.0(2) . . . . ? P1B C43 C48 C47 136.7(2) . . . . ? C46 C47 C48 C43 -1.6(4) . . . . ? N2 Zn1 C49 C54 159.58(17) . . . . ? N1 Zn1 C49 C54 -20.8(2) . . . . ? N2B Zn1 C49 C54 -161.5(3) . . . . ? N1B Zn1 C49 C54 18.7(3) . . . . ? N2 Zn1 C49 C50 -21.2(2) . . . . ? N1 Zn1 C49 C50 158.45(17) . . . . ? N2B Zn1 C49 C50 17.8(3) . . . . ? N1B Zn1 C49 C50 -162.1(3) . . . . ? C54 C49 C50 C51 -1.6(3) . . . . ? Zn1 C49 C50 C51 179.07(18) . . . . ? C49 C50 C51 C52 0.9(4) . . . . ? C50 C51 C52 C53 -0.3(4) . . . . ? C51 C52 C53 C54 0.6(4) . . . . ? C50 C49 C54 C53 1.9(3) . . . . ? Zn1 C49 C54 C53 -178.83(19) . . . . ? C52 C53 C54 C49 -1.4(4) . . . . ? C67 B1 C55 C56 -153.1(2) . . . . ? C73 B1 C55 C56 -31.8(3) . . . . ? C61 B1 C55 C56 90.2(2) . . . . ? C67 B1 C55 C60 34.1(3) . . . . ? C73 B1 C55 C60 155.4(2) . . . . ? C61 B1 C55 C60 -82.6(2) . . . . ? C60 C55 C56 C57 1.1(3) . . . . ? B1 C55 C56 C57 -172.1(2) . . . . ? C55 C56 C57 C58 0.0(3) . . . . ? C56 C57 C58 C59 -0.7(4) . . . . ? C57 C58 C59 C60 0.2(4) . . . . ? C58 C59 C60 C55 1.0(5) . . . . ? C56 C55 C60 C59 -1.6(4) . . . . ? B1 C55 C60 C59 171.9(2) . . . . ? C67 B1 C61 C66 91.4(2) . . . . ? C73 B1 C61 C66 -30.0(3) . . . . ? C55 B1 C61 C66 -151.2(2) . . . . ? C67 B1 C61 C62 -82.6(2) . . . . ? C73 B1 C61 C62 156.05(19) . . . . ? C55 B1 C61 C62 34.8(3) . . . . ? C66 C61 C62 C63 -1.6(3) . . . . ? B1 C61 C62 C63 172.9(2) . . . . ? C61 C62 C63 C64 1.8(4) . . . . ? C62 C63 C64 C65 0.1(4) . . . . ? C63 C64 C65 C66 -2.2(4) . . . . ? C64 C65 C66 C61 2.4(4) . . . . ? C62 C61 C66 C65 -0.5(4) . . . . ? B1 C61 C66 C65 -174.9(2) . . . . ? C73 B1 C67 C68 109.9(2) . . . . ? C55 B1 C67 C68 -128.7(2) . . . . ? C61 B1 C67 C68 -12.2(3) . . . . ? C73 B1 C67 C72 -69.0(3) . . . . ? C55 B1 C67 C72 52.4(3) . . . . ? C61 B1 C67 C72 168.9(2) . . . . ? C72 C67 C68 C69 1.4(3) . . . . ? B1 C67 C68 C69 -177.5(2) . . . . ? C67 C68 C69 C70 0.7(4) . . . . ? C68 C69 C70 C71 -1.8(4) . . . . ? C69 C70 C71 C72 0.7(4) . . . . ? C70 C71 C72 C67 1.6(4) . . . . ? C68 C67 C72 C71 -2.6(3) . . . . ? B1 C67 C72 C71 176.4(2) . . . . ? C67 B1 C73 C74 18.0(3) . . . . ? C55 B1 C73 C74 -102.6(2) . . . . ? C61 B1 C73 C74 137.9(2) . . . . ? C67 B1 C73 C78 -165.45(18) . . . . ? C55 B1 C73 C78 74.0(2) . . . . ? C61 B1 C73 C78 -45.6(3) . . . . ? C78 C73 C74 C75 -1.9(3) . . . . ? B1 C73 C74 C75 174.9(2) . . . . ? C73 C74 C75 C76 0.9(4) . . . . ? C74 C75 C76 C77 0.9(4) . . . . ? C75 C76 C77 C78 -1.6(4) . . . . ? C76 C77 C78 C73 0.5(4) . . . . ? C74 C73 C78 C77 1.2(3) . . . . ? B1 C73 C78 C77 -175.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.684 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.045 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.012 0.000 0.500 365 70 ' ' 2 0.000 0.500 0.000 23 1 ' ' _platon_squeeze_details ; ; #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 833329' #TrackingRef '6184_web_deposit_cif_file_0_PaulG.Hayes_ #1310063407.Chem Eur J_AllCifs - Paul G Hayes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86.83 H60.66 B Cl1.66 F24 N2 O4 P2 Zn' _chemical_formula_weight 1848.96 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4655(17) _cell_length_b 19.564(3) _cell_length_c 19.662(3) _cell_angle_alpha 99.640(2) _cell_angle_beta 103.416(2) _cell_angle_gamma 92.916(2) _cell_volume 4210.9(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2598 _cell_measurement_theta_min 4.360 _cell_measurement_theta_max 36.413 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1874 _exptl_absorpt_coefficient_mu 0.487 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8476 _exptl_absorpt_correction_T_max 0.9770 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41317 _diffrn_reflns_av_R_equivalents 0.1034 _diffrn_reflns_av_sigmaI/netI 0.1423 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.12 _reflns_number_total 14955 _reflns_number_gt 7374 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0941P)^2^+0.4499P] 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 14955 _refine_ls_number_parameters 1170 _refine_ls_number_restraints 225 _refine_ls_R_factor_all 0.1704 _refine_ls_R_factor_gt 0.0785 _refine_ls_wR_factor_ref 0.2148 _refine_ls_wR_factor_gt 0.1742 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.017 _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 1.46234(6) 0.30389(4) 1.33887(4) 0.0357(2) Uani 1 1 d . A . P1 P 1.24929(14) 0.22241(8) 1.20201(8) 0.0332(4) Uani 1 1 d . . . N2 N 1.6313(4) 0.3208(2) 1.3281(2) 0.0335(12) Uani 1 1 d . . . O1 O 1.4974(3) 0.25914(19) 1.17874(19) 0.0337(9) Uani 1 1 d . . . B1 B 1.4121(6) -0.2093(4) 1.2019(4) 0.0353(17) Uani 1 1 d . . . C1 C 1.4203(5) 0.2133(3) 1.1229(3) 0.0356(15) Uani 1 1 d . . . P2 P 1.68675(14) 0.36464(8) 1.27983(8) 0.0329(4) Uani 1 1 d . . . O2 O 1.5058(4) 0.2628(2) 1.4330(2) 0.0411(10) Uani 1 1 d . A . N1 N 1.3404(4) 0.2284(2) 1.2783(2) 0.0324(11) Uani 1 1 d . . . C2 C 1.3065(5) 0.1896(3) 1.1256(3) 0.0336(14) Uani 1 1 d . . . C3 C 1.2397(6) 0.1456(3) 1.0645(3) 0.0385(15) Uani 1 1 d . . . H3 H 1.1612 0.1266 1.0633 0.046 Uiso 1 1 calc R . . O3 O 1.4002(4) 0.3749(2) 1.3970(2) 0.0491(11) Uani 1 1 d . . . C4 C 1.2863(6) 0.1289(3) 1.0050(3) 0.0444(17) Uani 1 1 d . . . H4 H 1.2378 0.0996 0.9636 0.053 Uiso 1 1 calc R . . O4 O 1.4839(5) 0.2873(3) 1.5434(2) 0.0732(15) Uani 1 1 d . A . C5 C 1.4018(6) 0.1540(3) 1.0046(3) 0.0456(17) Uani 1 1 d . . . H5 H 1.4325 0.1420 0.9637 0.055 Uiso 1 1 calc R . . C6 C 1.4710(5) 0.1970(3) 1.0656(3) 0.0316(14) Uani 1 1 d . . . C7 C 1.5910(5) 0.2337(3) 1.0869(3) 0.0339(14) Uani 1 1 d . . . C8 C 1.6877(6) 0.2414(3) 1.0564(3) 0.0400(16) Uani 1 1 d . . . H8 H 1.6847 0.2173 1.0098 0.048 Uiso 1 1 calc R . . C9 C 1.7872(6) 0.2843(3) 1.0952(3) 0.0422(16) Uani 1 1 d . . . H9 H 1.8541 0.2892 1.0749 0.051 Uiso 1 1 calc R . . C10 C 1.7937(5) 0.3210(3) 1.1632(3) 0.0377(15) Uani 1 1 d . . . H10 H 1.8642 0.3507 1.1879 0.045 Uiso 1 1 calc R . . C11 C 1.6995(5) 0.3150(3) 1.1955(3) 0.0341(14) Uani 1 1 d . . . C12 C 1.6003(5) 0.2699(3) 1.1550(3) 0.0343(14) Uani 1 1 d . . . C13 C 1.1157(5) 0.1666(3) 1.1941(3) 0.0387(15) Uani 1 1 d . . . C14 C 1.0080(6) 0.1945(3) 1.1964(3) 0.0465(17) Uani 1 1 d . . . H14 H 1.0019 0.2428 1.1966 0.056 Uiso 1 1 calc R . . C15 C 0.9098(6) 0.1524(4) 1.1983(4) 0.062(2) Uani 1 1 d . . . H15 H 0.8350 0.1710 1.1990 0.074 Uiso 1 1 calc R . . C16 C 0.9207(7) 0.0828(5) 1.1994(4) 0.067(2) Uani 1 1 d . . . H16 H 0.8536 0.0541 1.2026 0.081 Uiso 1 1 calc R . . C17 C 1.0244(7) 0.0544(4) 1.1959(4) 0.0550(19) Uani 1 1 d . . . H17 H 1.0295 0.0061 1.1962 0.066 Uiso 1 1 calc R . . C18 C 1.1247(6) 0.0960(3) 1.1917(3) 0.0469(17) Uani 1 1 d . . . H18 H 1.1971 0.0762 1.1873 0.056 Uiso 1 1 calc R . . C19 C 1.2087(5) 0.3071(3) 1.1897(3) 0.0348(14) Uani 1 1 d . . . C20 C 1.1979(5) 0.3564(3) 1.2466(3) 0.0427(16) Uani 1 1 d . . . H20 H 1.2187 0.3468 1.2934 0.051 Uiso 1 1 calc R . . C21 C 1.1568(6) 0.4196(3) 1.2351(4) 0.0527(18) Uani 1 1 d . . . H21 H 1.1481 0.4531 1.2742 0.063 Uiso 1 1 calc R . . C22 C 1.1284(6) 0.4345(3) 1.1679(4) 0.0567(19) Uani 1 1 d . . . H22 H 1.1003 0.4781 1.1605 0.068 Uiso 1 1 calc R . . C23 C 1.1407(6) 0.3858(4) 1.1107(4) 0.0571(19) Uani 1 1 d . . . H23 H 1.1207 0.3961 1.0641 0.068 Uiso 1 1 calc R . . C24 C 1.1816(6) 0.3228(3) 1.1213(3) 0.0480(17) Uani 1 1 d . . . H24 H 1.1916 0.2898 1.0821 0.058 Uiso 1 1 calc R . . C25 C 1.3525(6) 0.1649(3) 1.3075(3) 0.0380(15) Uani 1 1 d . . . C26 C 1.4308(6) 0.1188(3) 1.2869(4) 0.0487(17) Uani 1 1 d . . . H26 H 1.4732 0.1287 1.2530 0.058 Uiso 1 1 calc R . . C27 C 1.4481(7) 0.0601(4) 1.3140(4) 0.067(2) Uani 1 1 d . . . H27 H 1.5019 0.0291 1.2988 0.081 Uiso 1 1 calc R . . C28 C 1.3886(8) 0.0451(4) 1.3632(5) 0.076(2) Uani 1 1 d . . . H28 H 1.4019 0.0043 1.3831 0.091 Uiso 1 1 calc R . . C29 C 1.3082(7) 0.0905(4) 1.3839(4) 0.059(2) Uani 1 1 d . . . H29 H 1.2653 0.0797 1.4173 0.071 Uiso 1 1 calc R . . C30 C 1.2897(6) 0.1504(3) 1.3569(3) 0.0456(17) Uani 1 1 d . . . C31 C 1.2034(6) 0.1990(4) 1.3793(3) 0.0541(19) Uani 1 1 d . . . H31A H 1.2337 0.2471 1.3805 0.081 Uiso 1 1 calc R . . H31B H 1.1955 0.1939 1.4268 0.081 Uiso 1 1 calc R . . H31C H 1.1246 0.1880 1.3454 0.081 Uiso 1 1 calc R . . C32 C 1.5913(5) 0.4307(3) 1.2568(3) 0.0366(15) Uani 1 1 d . . . C33 C 1.5225(6) 0.4597(3) 1.3014(4) 0.0503(18) Uani 1 1 d . . . H33 H 1.5254 0.4445 1.3451 0.060 Uiso 1 1 calc R . . C34 C 1.4497(7) 0.5106(4) 1.2823(5) 0.073(2) Uani 1 1 d . . . H34 H 1.4013 0.5298 1.3125 0.088 Uiso 1 1 calc R . . C35 C 1.4465(7) 0.5339(4) 1.2202(5) 0.072(2) Uani 1 1 d . . . H35 H 1.3956 0.5688 1.2072 0.086 Uiso 1 1 calc R . . C36 C 1.5162(9) 0.5070(4) 1.1770(5) 0.088(3) Uani 1 1 d . . . H36 H 1.5154 0.5243 1.1345 0.105 Uiso 1 1 calc R . . C37 C 1.5874(7) 0.4555(3) 1.1938(4) 0.059(2) Uani 1 1 d . . . H37 H 1.6344 0.4364 1.1626 0.071 Uiso 1 1 calc R . . C38 C 1.8367(5) 0.4037(3) 1.3245(3) 0.0368(15) Uani 1 1 d . . . C39 C 1.9306(5) 0.3625(3) 1.3394(3) 0.0412(16) Uani 1 1 d . . . H39 H 1.9196 0.3140 1.3203 0.049 Uiso 1 1 calc R . . C40 C 2.0400(6) 0.3925(4) 1.3821(4) 0.0547(19) Uani 1 1 d . . . H40 H 2.1055 0.3650 1.3922 0.066 Uiso 1 1 calc R . . C41 C 2.0542(7) 0.4634(4) 1.4103(4) 0.058(2) Uani 1 1 d . . . H41 H 2.1295 0.4836 1.4405 0.070 Uiso 1 1 calc R . . C42 C 1.9635(6) 0.5043(4) 1.3960(4) 0.057(2) Uani 1 1 d . . . H42 H 1.9756 0.5528 1.4151 0.069 Uiso 1 1 calc R . . C43 C 1.8529(6) 0.4750(3) 1.3532(3) 0.0457(17) Uani 1 1 d . . . H43 H 1.7882 0.5032 1.3434 0.055 Uiso 1 1 calc R . . C44 C 1.7102(5) 0.2753(3) 1.3638(3) 0.0368(15) Uani 1 1 d . . . C45 C 1.7182(6) 0.2089(3) 1.3278(4) 0.0468(17) Uani 1 1 d . . . H45 H 1.6740 0.1945 1.2797 0.056 Uiso 1 1 calc R . . C46 C 1.7891(8) 0.1641(4) 1.3609(5) 0.070(2) Uani 1 1 d . . . H46 H 1.7926 0.1184 1.3363 0.084 Uiso 1 1 calc R . . C47 C 1.8547(8) 0.1851(5) 1.4292(6) 0.082(3) Uani 1 1 d . . . H47 H 1.9049 0.1542 1.4520 0.098 Uiso 1 1 calc R . . C48 C 1.8484(7) 0.2507(5) 1.4653(4) 0.072(2) Uani 1 1 d . . . H48 H 1.8945 0.2645 1.5130 0.086 Uiso 1 1 calc R . . C49 C 1.7757(6) 0.2976(4) 1.4334(4) 0.0503(18) Uani 1 1 d . . . C50 C 1.7699(7) 0.3685(4) 1.4751(4) 0.065(2) Uani 1 1 d . . . H50A H 1.6957 0.3876 1.4535 0.098 Uiso 1 1 calc R . . H50B H 1.8396 0.3994 1.4747 0.098 Uiso 1 1 calc R . . H50C H 1.7705 0.3648 1.5243 0.098 Uiso 1 1 calc R . . C51A C 1.4178(9) 0.3679(4) 1.4661(4) 0.087(3) Uani 0.50 1 d P A 1 H51A H 1.3334 0.3564 1.4691 0.104 Uiso 0.50 1 calc PR A 1 C52A C 1.4551(15) 0.4258(8) 1.5216(8) 0.067(4) Uani 0.50 1 d P A 1 H52A H 1.5395 0.4413 1.5256 0.100 Uiso 0.50 1 calc PR A 1 H52B H 1.4471 0.4127 1.5664 0.100 Uiso 0.50 1 calc PR A 1 H52C H 1.4048 0.4636 1.5114 0.100 Uiso 0.50 1 calc PR A 1 C51B C 1.4178(9) 0.3679(4) 1.4661(4) 0.087(3) Uani 0.50 1 d P A 2 H51B H 1.4910 0.4016 1.4868 0.104 Uiso 0.50 1 calc PR A 2 C52B C 1.3448(16) 0.3956(10) 1.5080(9) 0.085(6) Uani 0.50 1 d P A 2 H52D H 1.3388 0.4449 1.5051 0.128 Uiso 0.50 1 calc PR A 2 H52E H 1.3792 0.3913 1.5575 0.128 Uiso 0.50 1 calc PR A 2 H52F H 1.2644 0.3704 1.4914 0.128 Uiso 0.50 1 calc PR A 2 C53 C 1.4730(6) 0.3020(4) 1.4789(4) 0.0509(18) Uani 1 1 d . . . C54 C 1.5358(7) 0.2230(4) 1.5553(4) 0.069(2) Uani 1 1 d . . . H54A H 1.4863 0.1838 1.5218 0.104 Uiso 1 1 calc R A . H54B H 1.5387 0.2169 1.6041 0.104 Uiso 1 1 calc R . . H54C H 1.6176 0.2250 1.5482 0.104 Uiso 1 1 calc R . . C55 C 1.5382(5) -0.2020(3) 1.2626(3) 0.0357(15) Uani 1 1 d . . . C56 C 1.5822(6) -0.1393(3) 1.3096(3) 0.0434(16) Uani 1 1 d . . . H56 H 1.5393 -0.0995 1.3036 0.052 Uiso 1 1 calc R . . C57 C 1.6852(6) -0.1322(3) 1.3644(3) 0.0450(17) Uani 1 1 d . . . C58 C 1.7492(6) -0.1878(4) 1.3760(3) 0.0475(17) Uani 1 1 d . . . H58 H 1.8205 -0.1832 1.4131 0.057 Uiso 1 1 calc R . . C59 C 1.7058(6) -0.2521(3) 1.3313(4) 0.0469(17) Uani 1 1 d . . . C60 C 1.6027(5) -0.2587(3) 1.2767(3) 0.0380(15) Uani 1 1 d . . . H60 H 1.5751 -0.3032 1.2479 0.046 Uiso 1 1 calc R . . C61 C 1.7262(8) -0.0627(4) 1.4100(4) 0.071(2) Uani 1 1 d D . . F1 F 1.6449(5) -0.0370(3) 1.4416(3) 0.1097(19) Uani 1 1 d D . . F2 F 1.8225(4) -0.0627(2) 1.4617(2) 0.0940(16) Uani 1 1 d D . . F3 F 1.7528(6) -0.0165(2) 1.3734(3) 0.127(2) Uani 1 1 d D . . C62 C 1.7728(8) -0.3127(5) 1.3431(5) 0.071(2) Uani 1 1 d . . . F4 F 1.8277(7) -0.3320(4) 1.2899(4) 0.163(3) Uani 1 1 d . . . F5 F 1.8588(6) -0.3059(3) 1.3973(4) 0.157(3) Uani 1 1 d . . . F6 F 1.7077(5) -0.3692(3) 1.3386(4) 0.148(3) Uani 1 1 d . . . C63 C 1.3927(5) -0.1427(3) 1.1622(3) 0.0304(14) Uani 1 1 d . . . C64 C 1.2810(5) -0.1338(3) 1.1204(3) 0.0373(15) Uani 1 1 d . . . H64 H 1.2143 -0.1654 1.1188 0.045 Uiso 1 1 calc R . . C65 C 1.2617(5) -0.0814(3) 1.0810(3) 0.0375(15) Uani 1 1 d . . . C66 C 1.3559(6) -0.0330(3) 1.0834(3) 0.0452(16) Uani 1 1 d . . . H66 H 1.3434 0.0041 1.0577 0.054 Uiso 1 1 calc R . . C67 C 1.4692(6) -0.0404(3) 1.1247(3) 0.0388(15) Uani 1 1 d . B . C68 C 1.4876(5) -0.0940(3) 1.1625(3) 0.0356(15) Uani 1 1 d . . . H68 H 1.5664 -0.0980 1.1895 0.043 Uiso 1 1 calc R . . C69 C 1.1395(6) -0.0770(4) 1.0353(4) 0.0543(19) Uani 1 1 d . . . F7 F 1.1321(4) -0.0253(3) 1.0025(3) 0.126(2) Uani 1 1 d . . . F8 F 1.1019(4) -0.1336(3) 0.9882(3) 0.1081(19) Uani 1 1 d . . . F9 F 1.0560(4) -0.0717(3) 1.0711(3) 0.1009(17) Uani 1 1 d . . . C70 C 1.5728(7) 0.0107(4) 1.1293(5) 0.057(2) Uani 1 1 d . . . F10 F 1.5929(11) 0.0621(5) 1.1737(8) 0.091(4) Uani 0.61 1 d PDU B 1 F11 F 1.6753(10) -0.0224(5) 1.1304(6) 0.057(3) Uani 0.61 1 d PDU B 1 F12 F 1.5633(8) 0.0326(6) 1.0623(5) 0.094(3) Uani 0.61 1 d PDU B 1 F10B F 1.6351(14) 0.0321(8) 1.2044(7) 0.065(4) Uani 0.39 1 d PDU B 2 F11B F 1.5365(13) 0.0759(7) 1.1248(11) 0.085(6) Uani 0.39 1 d PDU B 2 F12B F 1.647(2) -0.0021(9) 1.0987(10) 0.082(7) Uani 0.39 1 d PDU B 2 C71 C 1.3083(5) -0.2176(3) 1.2460(3) 0.0330(14) Uani 1 1 d . . . C72 C 1.2754(6) -0.2821(3) 1.2614(3) 0.0430(16) Uani 1 1 d . . . H72 H 1.3117 -0.3217 1.2439 0.052 Uiso 1 1 calc R . . C73 C 1.1918(6) -0.2907(3) 1.3016(3) 0.0442(17) Uani 1 1 d . . . C74 C 1.1421(6) -0.2346(3) 1.3296(3) 0.0474(17) Uani 1 1 d . . . H74 H 1.0847 -0.2403 1.3567 0.057 Uiso 1 1 calc R . . C75 C 1.1754(6) -0.1694(3) 1.3187(3) 0.0475(17) Uani 1 1 d . . . C76 C 1.2554(6) -0.1622(3) 1.2768(3) 0.0417(16) Uani 1 1 d . . . H76 H 1.2751 -0.1169 1.2687 0.050 Uiso 1 1 calc R . . C77 C 1.1592(9) -0.3619(4) 1.3107(5) 0.075(3) Uani 1 1 d . . . F13 F 1.1168(9) -0.4052(3) 1.2512(3) 0.195(4) Uani 1 1 d . . . F14 F 1.2520(5) -0.3909(3) 1.3445(4) 0.130(3) Uani 1 1 d . . . F15 F 1.0813(4) -0.3652(2) 1.3498(2) 0.0744(13) Uani 1 1 d . . . C78 C 1.1281(8) -0.1072(4) 1.3535(5) 0.068(2) Uani 1 1 d . . . F16 F 1.2055(5) -0.0741(2) 1.4130(3) 0.1023(17) Uani 1 1 d . . . F17 F 1.1050(5) -0.0600(2) 1.3135(3) 0.0905(16) Uani 1 1 d . . . F18 F 1.0270(5) -0.1224(2) 1.3723(3) 0.1061(19) Uani 1 1 d . . . C79 C 1.4046(5) -0.2763(3) 1.1381(3) 0.0345(14) Uani 1 1 d . . . C80 C 1.5037(6) -0.2905(3) 1.1089(3) 0.0383(15) Uani 1 1 d . . . H80 H 1.5763 -0.2608 1.1274 0.046 Uiso 1 1 calc R . . C81 C 1.4998(6) -0.3461(3) 1.0542(3) 0.0444(16) Uani 1 1 d . C . C82 C 1.3954(7) -0.3892(3) 1.0239(3) 0.0492(18) Uani 1 1 d . . . H82 H 1.3924 -0.4271 0.9861 0.059 Uiso 1 1 calc R . . C83 C 1.2953(6) -0.3757(3) 1.0500(3) 0.0421(16) Uani 1 1 d . . . C84 C 1.2996(6) -0.3203(3) 1.1047(3) 0.0388(15) Uani 1 1 d . . . H84 H 1.2283 -0.3116 1.1202 0.047 Uiso 1 1 calc R . . C85 C 1.6078(8) -0.3608(5) 1.0263(5) 0.069(2) Uani 1 1 d . . . F19 F 1.6519(13) -0.4145(7) 1.0364(9) 0.110(5) Uani 0.64 1 d PDU C 1 F20 F 1.5796(8) -0.3644(7) 0.9526(4) 0.090(3) Uani 0.64 1 d PDU C 1 F21 F 1.6912(16) -0.3073(8) 1.0446(8) 0.106(7) Uani 0.64 1 d PDU C 1 F19B F 1.6986(16) -0.3776(15) 1.0864(8) 0.107(8) Uani 0.36 1 d PDU C 2 F20B F 1.6005(18) -0.4189(13) 0.9833(15) 0.125(9) Uani 0.36 1 d PDU C 2 F21B F 1.664(3) -0.3129(11) 1.0137(17) 0.101(11) Uani 0.36 1 d PDU C 2 C86 C 1.1838(7) -0.4224(4) 1.0195(4) 0.064(2) Uani 1 1 d D . . F22 F 1.1803(6) -0.4765(3) 1.0467(4) 0.173(4) Uani 1 1 d DU . . F23 F 1.1634(6) -0.4477(3) 0.9520(3) 0.141(3) Uani 1 1 d DU . . F24 F 1.0866(5) -0.3942(3) 1.0240(4) 0.169(3) Uani 1 1 d DU . . C87 C 1.9258(3) -0.2495(2) 1.16546(19) 0.214(6) Uani 0.83 1 d PU . . H87A H 1.9979 -0.2484 1.2049 0.257 Uiso 0.83 1 calc PR . . H87B H 1.8742 -0.2931 1.1602 0.257 Uiso 0.83 1 calc PR . . Cl1 Cl 1.8395(3) -0.1708(2) 1.18413(19) 0.201(2) Uani 0.83 1 d PRU . . Cl2 Cl 1.9664(3) -0.2449(2) 1.08887(19) 0.204(2) Uani 0.83 1 d PRU . . 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 0.0383(4) 0.0363(4) 0.0327(4) 0.0060(3) 0.0107(3) -0.0023(3) P1 0.0325(9) 0.0315(9) 0.0354(9) 0.0061(7) 0.0086(7) -0.0010(7) N2 0.036(3) 0.035(3) 0.028(3) 0.008(2) 0.006(2) -0.001(2) O1 0.032(2) 0.037(2) 0.031(2) 0.0017(18) 0.0089(19) -0.0015(19) B1 0.038(4) 0.037(4) 0.030(4) 0.008(3) 0.004(3) 0.002(3) C1 0.045(4) 0.029(3) 0.026(3) -0.003(3) 0.001(3) -0.001(3) P2 0.0332(9) 0.0294(8) 0.0364(9) 0.0057(7) 0.0099(7) -0.0013(7) O2 0.039(3) 0.046(3) 0.039(3) 0.010(2) 0.012(2) -0.009(2) N1 0.038(3) 0.030(3) 0.029(3) 0.008(2) 0.006(2) -0.001(2) C2 0.034(4) 0.035(3) 0.033(3) 0.006(3) 0.011(3) 0.003(3) C3 0.044(4) 0.032(3) 0.037(4) 0.003(3) 0.008(3) -0.003(3) O3 0.065(3) 0.042(3) 0.046(3) 0.011(2) 0.021(2) 0.010(2) C4 0.054(5) 0.039(4) 0.031(4) -0.002(3) 0.001(3) -0.004(3) O4 0.098(4) 0.096(4) 0.033(3) 0.021(3) 0.023(3) 0.013(3) C5 0.052(4) 0.045(4) 0.039(4) 0.004(3) 0.011(3) 0.009(3) C6 0.039(4) 0.031(3) 0.025(3) 0.003(3) 0.010(3) 0.005(3) C7 0.041(4) 0.032(3) 0.029(3) 0.005(3) 0.010(3) 0.003(3) C8 0.049(4) 0.048(4) 0.027(3) 0.005(3) 0.017(3) 0.009(3) C9 0.041(4) 0.050(4) 0.041(4) 0.014(3) 0.019(3) 0.001(3) C10 0.031(4) 0.041(4) 0.044(4) 0.017(3) 0.007(3) 0.002(3) C11 0.037(4) 0.030(3) 0.036(4) 0.004(3) 0.012(3) 0.000(3) C12 0.038(4) 0.033(3) 0.037(4) 0.010(3) 0.017(3) 0.003(3) C13 0.037(4) 0.039(4) 0.036(4) 0.009(3) -0.001(3) -0.002(3) C14 0.038(4) 0.048(4) 0.053(4) 0.012(3) 0.010(3) -0.001(3) C15 0.037(4) 0.077(6) 0.073(5) 0.018(4) 0.017(4) -0.003(4) C16 0.041(5) 0.081(6) 0.071(6) 0.013(5) 0.002(4) -0.021(4) C17 0.060(5) 0.043(4) 0.056(5) 0.013(3) 0.004(4) -0.014(4) C18 0.046(4) 0.041(4) 0.050(4) 0.006(3) 0.007(3) -0.006(3) C19 0.025(3) 0.035(3) 0.044(4) 0.010(3) 0.006(3) 0.003(3) C20 0.044(4) 0.037(4) 0.048(4) 0.008(3) 0.012(3) 0.010(3) C21 0.060(5) 0.037(4) 0.061(5) 0.005(4) 0.016(4) 0.011(3) C22 0.061(5) 0.035(4) 0.077(6) 0.020(4) 0.016(4) 0.016(4) C23 0.070(5) 0.056(5) 0.051(5) 0.023(4) 0.017(4) 0.017(4) C24 0.054(4) 0.044(4) 0.048(4) 0.013(3) 0.011(4) 0.006(3) C25 0.043(4) 0.032(3) 0.037(4) 0.014(3) 0.001(3) -0.007(3) C26 0.051(4) 0.037(4) 0.061(5) 0.009(3) 0.018(4) 0.003(3) C27 0.069(6) 0.050(5) 0.082(6) 0.016(4) 0.013(5) 0.010(4) C28 0.084(6) 0.056(5) 0.087(6) 0.035(5) 0.007(5) -0.002(5) C29 0.060(5) 0.060(5) 0.054(5) 0.022(4) 0.005(4) -0.011(4) C30 0.051(4) 0.044(4) 0.038(4) 0.010(3) 0.005(3) -0.016(3) C31 0.052(4) 0.069(5) 0.041(4) 0.005(4) 0.015(4) 0.000(4) C32 0.036(4) 0.025(3) 0.044(4) 0.004(3) 0.004(3) -0.005(3) C33 0.048(4) 0.029(4) 0.081(5) 0.008(4) 0.031(4) 0.001(3) C34 0.061(5) 0.037(4) 0.123(8) 0.008(5) 0.029(5) 0.010(4) C35 0.069(6) 0.039(5) 0.097(7) 0.008(5) -0.001(5) 0.019(4) C36 0.128(8) 0.055(5) 0.068(6) 0.017(4) -0.010(6) 0.037(6) C37 0.088(6) 0.046(4) 0.045(4) 0.012(4) 0.017(4) 0.018(4) C38 0.040(4) 0.037(4) 0.033(3) 0.007(3) 0.010(3) -0.010(3) C39 0.033(4) 0.042(4) 0.045(4) 0.004(3) 0.007(3) -0.004(3) C40 0.041(4) 0.070(5) 0.051(4) 0.011(4) 0.008(4) 0.006(4) C41 0.042(4) 0.063(5) 0.056(5) -0.004(4) 0.002(4) -0.025(4) C42 0.050(5) 0.048(4) 0.070(5) 0.008(4) 0.013(4) -0.020(4) C43 0.047(4) 0.039(4) 0.050(4) 0.012(3) 0.010(3) -0.010(3) C44 0.030(4) 0.044(4) 0.037(4) 0.014(3) 0.006(3) 0.001(3) C45 0.054(4) 0.035(4) 0.056(4) 0.013(3) 0.018(4) 0.010(3) C46 0.082(6) 0.054(5) 0.083(6) 0.028(5) 0.027(5) 0.017(5) C47 0.078(6) 0.089(7) 0.100(8) 0.059(6) 0.030(6) 0.032(6) C48 0.054(5) 0.098(7) 0.072(6) 0.046(5) 0.007(4) 0.010(5) C49 0.041(4) 0.065(5) 0.049(4) 0.021(4) 0.014(4) 0.000(4) C50 0.066(5) 0.073(5) 0.051(5) 0.000(4) 0.015(4) -0.018(4) C51A 0.142(9) 0.078(6) 0.046(5) 0.007(5) 0.031(6) 0.044(6) C52A 0.064(11) 0.070(11) 0.061(10) 0.002(9) 0.012(9) 0.002(9) C51B 0.142(9) 0.078(6) 0.046(5) 0.007(5) 0.031(6) 0.044(6) C52B 0.068(12) 0.125(16) 0.062(11) 0.001(11) 0.020(10) 0.028(12) C53 0.047(4) 0.066(5) 0.036(4) 0.004(4) 0.009(3) -0.005(4) C54 0.070(5) 0.094(6) 0.047(5) 0.031(4) 0.011(4) 0.001(5) C55 0.037(4) 0.034(4) 0.038(4) 0.005(3) 0.015(3) -0.001(3) C56 0.053(4) 0.039(4) 0.040(4) 0.008(3) 0.016(3) 0.003(3) C57 0.052(4) 0.042(4) 0.039(4) 0.007(3) 0.007(3) -0.001(3) C58 0.035(4) 0.060(5) 0.046(4) 0.012(4) 0.007(3) -0.003(4) C59 0.039(4) 0.050(4) 0.054(4) 0.018(4) 0.011(4) 0.009(3) C60 0.032(4) 0.042(4) 0.039(4) 0.011(3) 0.006(3) -0.005(3) C61 0.076(6) 0.063(6) 0.056(5) 0.000(5) -0.008(5) -0.005(5) F1 0.100(4) 0.096(4) 0.101(4) -0.044(3) 0.002(3) 0.020(3) F2 0.088(4) 0.081(3) 0.082(3) -0.010(3) -0.022(3) -0.001(3) F3 0.210(7) 0.059(3) 0.081(4) 0.010(3) -0.013(4) -0.060(4) C62 0.059(6) 0.070(6) 0.078(6) 0.015(5) 0.005(5) 0.008(5) F4 0.174(7) 0.183(7) 0.169(7) 0.062(5) 0.070(6) 0.125(6) F5 0.151(5) 0.085(4) 0.165(6) 0.003(4) -0.097(5) 0.048(4) F6 0.076(4) 0.060(3) 0.309(9) 0.084(4) 0.007(5) 0.017(3) C63 0.035(4) 0.029(3) 0.026(3) 0.000(3) 0.008(3) 0.001(3) C64 0.039(4) 0.038(4) 0.034(4) 0.006(3) 0.009(3) -0.001(3) C65 0.039(4) 0.039(4) 0.033(3) 0.004(3) 0.005(3) 0.007(3) C66 0.045(4) 0.044(4) 0.051(4) 0.020(3) 0.011(3) 0.010(3) C67 0.041(4) 0.035(4) 0.043(4) 0.010(3) 0.014(3) -0.001(3) C68 0.037(4) 0.035(3) 0.035(4) 0.013(3) 0.004(3) 0.006(3) C69 0.043(5) 0.053(5) 0.063(5) 0.017(4) 0.000(4) 0.006(4) F7 0.068(3) 0.125(4) 0.174(5) 0.111(4) -0.043(3) -0.018(3) F8 0.077(3) 0.108(4) 0.096(4) -0.027(3) -0.035(3) 0.024(3) F9 0.053(3) 0.162(5) 0.091(4) 0.022(3) 0.018(3) 0.040(3) C70 0.047(5) 0.047(5) 0.081(6) 0.036(5) 0.007(5) -0.001(4) F10 0.100(12) 0.040(7) 0.137(13) -0.029(7) 0.077(10) -0.033(6) F11 0.035(4) 0.044(5) 0.092(8) 0.011(5) 0.023(5) -0.011(4) F12 0.070(6) 0.126(8) 0.107(8) 0.078(7) 0.031(5) -0.012(6) F10B 0.062(9) 0.070(11) 0.058(8) 0.023(7) 0.006(6) -0.035(7) F11B 0.065(10) 0.048(8) 0.133(15) 0.039(9) -0.005(10) -0.015(6) F12B 0.102(18) 0.060(13) 0.092(16) -0.017(10) 0.073(15) -0.033(11) C71 0.036(4) 0.036(3) 0.030(3) 0.012(3) 0.009(3) 0.001(3) C72 0.051(4) 0.038(4) 0.044(4) 0.011(3) 0.016(3) 0.007(3) C73 0.061(5) 0.033(4) 0.046(4) 0.015(3) 0.022(4) -0.002(3) C74 0.057(4) 0.042(4) 0.050(4) 0.009(3) 0.027(4) 0.000(3) C75 0.057(5) 0.036(4) 0.051(4) 0.006(3) 0.019(4) 0.000(3) C76 0.047(4) 0.035(4) 0.044(4) 0.005(3) 0.016(3) -0.002(3) C77 0.117(8) 0.045(5) 0.083(6) 0.024(5) 0.059(6) 0.006(5) F13 0.441(13) 0.055(3) 0.084(4) -0.018(3) 0.106(6) -0.104(5) F14 0.126(5) 0.086(4) 0.257(8) 0.110(5) 0.136(5) 0.062(4) F15 0.076(3) 0.055(3) 0.112(4) 0.044(2) 0.044(3) -0.001(2) C78 0.080(6) 0.054(5) 0.084(6) 0.008(5) 0.052(5) 0.003(5) F16 0.124(4) 0.079(3) 0.091(4) -0.030(3) 0.035(3) 0.000(3) F17 0.125(4) 0.059(3) 0.116(4) 0.034(3) 0.067(3) 0.040(3) F18 0.115(4) 0.058(3) 0.181(5) 0.012(3) 0.114(4) 0.011(3) C79 0.036(4) 0.033(3) 0.038(4) 0.014(3) 0.008(3) 0.008(3) C80 0.044(4) 0.033(3) 0.036(4) 0.004(3) 0.009(3) 0.000(3) C81 0.047(4) 0.045(4) 0.041(4) 0.007(3) 0.011(3) 0.011(3) C82 0.069(5) 0.043(4) 0.032(4) 0.007(3) 0.005(4) 0.006(4) C83 0.050(4) 0.029(3) 0.044(4) 0.010(3) 0.004(3) 0.002(3) C84 0.040(4) 0.037(4) 0.041(4) 0.012(3) 0.010(3) 0.005(3) C85 0.073(6) 0.054(6) 0.081(7) 0.000(6) 0.031(6) 0.007(5) F19 0.128(13) 0.122(11) 0.140(12) 0.085(10) 0.090(11) 0.089(10) F20 0.099(7) 0.117(8) 0.059(5) -0.001(6) 0.040(5) 0.017(7) F21 0.074(7) 0.124(12) 0.103(11) -0.038(9) 0.040(7) -0.025(7) F19B 0.058(10) 0.21(2) 0.062(10) 0.028(13) 0.020(9) 0.057(12) F20B 0.106(16) 0.102(15) 0.14(2) -0.072(16) 0.053(16) 0.009(13) F21B 0.13(2) 0.081(17) 0.17(3) 0.086(17) 0.12(2) 0.067(16) C86 0.067(6) 0.060(5) 0.057(5) 0.006(4) 0.006(4) -0.017(5) F22 0.137(5) 0.142(5) 0.215(7) 0.127(5) -0.053(5) -0.093(5) F23 0.146(5) 0.169(6) 0.067(4) -0.025(4) 0.002(3) -0.096(5) F24 0.051(3) 0.134(5) 0.259(8) -0.093(5) 0.010(4) -0.021(4) C87 0.216(17) 0.222(16) 0.122(10) 0.063(11) -0.133(7) -0.041(10) Cl1 0.163(4) 0.292(7) 0.120(3) 0.036(4) -0.005(3) -0.031(4) Cl2 0.083(3) 0.204(5) 0.309(7) 0.041(5) 0.029(4) -0.016(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 Zn1 O3 1.921(4) . ? Zn1 N1 1.996(4) . ? Zn1 N2 2.014(5) . ? Zn1 O2 2.105(4) . ? P1 N1 1.599(5) . ? P1 C19 1.783(6) . ? P1 C13 1.796(6) . ? P1 C2 1.811(6) . ? N2 C44 1.449(7) . ? N2 P2 1.593(5) . ? O1 C12 1.384(6) . ? O1 C1 1.389(6) . ? B1 C63 1.627(8) . ? B1 C55 1.630(9) . ? B1 C79 1.639(9) . ? B1 C71 1.642(9) . ? C1 C2 1.377(8) . ? C1 C6 1.382(7) . ? P2 C32 1.784(6) . ? P2 C38 1.803(6) . ? P2 C11 1.816(6) . ? O2 C53 1.224(7) . ? N1 C25 1.453(7) . ? C2 C3 1.389(8) . ? C3 C4 1.393(8) . ? C3 H3 0.9500 . ? O3 C51A 1.357(8) . ? C4 C5 1.391(9) . ? C4 H4 0.9500 . ? O4 C53 1.326(8) . ? O4 C54 1.449(8) . ? C5 C6 1.390(8) . ? C5 H5 0.9500 . ? C6 C7 1.454(8) . ? C7 C12 1.384(7) . ? C7 C8 1.390(8) . ? C8 C9 1.368(8) . ? C8 H8 0.9500 . ? C9 C10 1.391(8) . ? C9 H9 0.9500 . ? C10 C11 1.385(8) . ? C10 H10 0.9500 . ? C11 C12 1.396(8) . ? C13 C14 1.383(8) . ? C13 C18 1.384(8) . ? C14 C15 1.373(9) . ? C14 H14 0.9500 . ? C15 C16 1.375(10) . ? C15 H15 0.9500 . ? C16 C17 1.350(10) . ? C16 H16 0.9500 . ? C17 C18 1.400(9) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.383(8) . ? C19 C24 1.398(8) . ? C20 C21 1.380(8) . ? C20 H20 0.9500 . ? C21 C22 1.370(9) . ? C21 H21 0.9500 . ? C22 C23 1.385(9) . ? C22 H22 0.9500 . ? C23 C24 1.372(8) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.382(8) . ? C25 C30 1.392(8) . ? C26 C27 1.350(9) . ? C26 H26 0.9500 . ? C27 C28 1.367(10) . ? C27 H27 0.9500 . ? C28 C29 1.391(10) . ? C28 H28 0.9500 . ? C29 C30 1.372(9) . ? C29 H29 0.9500 . ? C30 C31 1.495(9) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.383(8) . ? C32 C37 1.396(8) . ? C33 C34 1.376(9) . ? C33 H33 0.9500 . ? C34 C35 1.366(11) . ? C34 H34 0.9500 . ? C35 C36 1.358(11) . ? C35 H35 0.9500 . ? C36 C37 1.365(9) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.384(8) . ? C38 C43 1.401(8) . ? C39 C40 1.376(8) . ? C39 H39 0.9500 . ? C40 C41 1.392(9) . ? C40 H40 0.9500 . ? C41 C42 1.350(9) . ? C41 H41 0.9500 . ? C42 C43 1.384(9) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C49 1.386(8) . ? C44 C45 1.389(8) . ? C45 C46 1.368(9) . ? C45 H45 0.9500 . ? C46 C47 1.361(11) . ? C46 H46 0.9500 . ? C47 C48 1.372(11) . ? C47 H47 0.9500 . ? C48 C49 1.400(9) . ? C48 H48 0.9500 . ? C49 C50 1.501(9) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51A C52A 1.406(16) . ? C51A C53 1.499(10) . ? C51A H51A 1.0000 . ? C52A H52A 0.9800 . ? C52A H52B 0.9800 . ? C52A H52C 0.9800 . ? C52B H52D 0.9800 . ? C52B H52E 0.9800 . ? C52B H52F 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C60 1.395(8) . ? C55 C56 1.398(8) . ? C56 C57 1.385(8) . ? C56 H56 0.9500 . ? C57 C58 1.364(8) . ? C57 C61 1.484(10) . ? C58 C59 1.401(9) . ? C58 H58 0.9500 . ? C59 C60 1.383(8) . ? C59 C62 1.466(10) . ? C60 H60 0.9500 . ? C61 F1 1.312(9) . ? C61 F3 1.313(8) . ? C61 F2 1.316(8) . ? C62 F5 1.256(9) . ? C62 F6 1.280(9) . ? C62 F4 1.353(10) . ? C63 C64 1.389(8) . ? C63 C68 1.407(8) . ? C64 C65 1.381(8) . ? C64 H64 0.9500 . ? C65 C66 1.386(8) . ? C65 C69 1.494(9) . ? C66 C67 1.392(8) . ? C66 H66 0.9500 . ? C67 C68 1.380(8) . ? C67 C70 1.490(9) . ? C68 H68 0.9500 . ? C69 F7 1.285(8) . ? C69 F8 1.302(8) . ? C69 F9 1.311(8) . ? C70 F12B 1.162(17) . ? C70 F10 1.189(11) . ? C70 F11 1.367(14) . ? C70 F11B 1.371(15) . ? C70 F12 1.435(11) . ? C70 F10B 1.462(16) . ? C71 C76 1.388(8) . ? C71 C72 1.400(8) . ? C72 C73 1.396(8) . ? C72 H72 0.9500 . ? C73 C74 1.357(8) . ? C73 C77 1.474(9) . ? C74 C75 1.380(8) . ? C74 H74 0.9500 . ? C75 C76 1.385(8) . ? C75 C78 1.484(9) . ? C76 H76 0.9500 . ? C77 F13 1.298(9) . ? C77 F15 1.312(8) . ? C77 F14 1.325(10) . ? C78 F17 1.309(8) . ? C78 F18 1.331(8) . ? C78 F16 1.336(9) . ? C79 C84 1.399(8) . ? C79 C80 1.408(8) . ? C80 C81 1.386(8) . ? C80 H80 0.9500 . ? C81 C82 1.377(9) . ? C81 C85 1.488(10) . ? C82 C83 1.382(9) . ? C82 H82 0.9500 . ? C83 C84 1.384(8) . ? C83 C86 1.473(9) . ? C84 H84 0.9500 . ? C85 F21B 1.20(2) . ? C85 F19 1.216(12) . ? C85 F20B 1.285(17) . ? C85 F21 1.324(16) . ? C85 F20 1.398(12) . ? C85 F19B 1.478(19) . ? C86 F22 1.266(8) . ? C86 F24 1.284(8) . ? C86 F23 1.298(8) . ? C87 Cl2 1.6911 . ? C87 Cl1 1.9015 . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? 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 O3 Zn1 N1 115.28(19) . . ? O3 Zn1 N2 118.59(19) . . ? N1 Zn1 N2 124.84(18) . . ? O3 Zn1 O2 83.22(17) . . ? N1 Zn1 O2 99.56(16) . . ? N2 Zn1 O2 97.59(17) . . ? N1 P1 C19 109.1(3) . . ? N1 P1 C13 111.3(3) . . ? C19 P1 C13 109.3(3) . . ? N1 P1 C2 116.4(3) . . ? C19 P1 C2 104.5(3) . . ? C13 P1 C2 105.8(3) . . ? C44 N2 P2 116.0(4) . . ? C44 N2 Zn1 110.9(3) . . ? P2 N2 Zn1 132.4(3) . . ? C12 O1 C1 104.6(4) . . ? C63 B1 C55 114.0(5) . . ? C63 B1 C79 105.2(5) . . ? C55 B1 C79 111.4(5) . . ? C63 B1 C71 110.3(5) . . ? C55 B1 C71 103.8(5) . . ? C79 B1 C71 112.4(5) . . ? C2 C1 C6 125.7(5) . . ? C2 C1 O1 122.6(5) . . ? C6 C1 O1 111.7(5) . . ? N2 P2 C32 109.4(3) . . ? N2 P2 C38 111.6(3) . . ? C32 P2 C38 109.8(3) . . ? N2 P2 C11 114.9(3) . . ? C32 P2 C11 105.2(3) . . ? C38 P2 C11 105.6(3) . . ? C53 O2 Zn1 107.5(4) . . ? C25 N1 P1 116.6(4) . . ? C25 N1 Zn1 110.1(3) . . ? P1 N1 Zn1 132.7(3) . . ? C1 C2 C3 115.4(5) . . ? C1 C2 P1 119.8(4) . . ? C3 C2 P1 124.6(5) . . ? C2 C3 C4 120.8(6) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C51A O3 Zn1 114.5(4) . . ? C5 C4 C3 121.9(6) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C53 O4 C54 116.1(6) . . ? C6 C5 C4 118.1(6) . . ? C6 C5 H5 120.9 . . ? C4 C5 H5 120.9 . . ? C1 C6 C5 118.0(6) . . ? C1 C6 C7 106.2(5) . . ? C5 C6 C7 135.7(6) . . ? C12 C7 C8 118.3(6) . . ? C12 C7 C6 104.8(5) . . ? C8 C7 C6 136.9(5) . . ? C9 C8 C7 118.5(5) . . ? C9 C8 H8 120.8 . . ? C7 C8 H8 120.8 . . ? C8 C9 C10 122.2(6) . . ? C8 C9 H9 118.9 . . ? C10 C9 H9 118.9 . . ? C11 C10 C9 121.3(6) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 115.0(5) . . ? C10 C11 P2 127.1(5) . . ? C12 C11 P2 117.6(4) . . ? O1 C12 C7 112.7(5) . . ? O1 C12 C11 122.5(5) . . ? C7 C12 C11 124.7(5) . . ? C14 C13 C18 120.6(6) . . ? C14 C13 P1 120.4(5) . . ? C18 C13 P1 118.8(5) . . ? C15 C14 C13 119.9(6) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 119.3(7) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C17 C16 C15 121.6(7) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 C18 120.0(7) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C13 C18 C17 118.5(6) . . ? C13 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? C20 C19 C24 119.4(6) . . ? C20 C19 P1 120.8(5) . . ? C24 C19 P1 119.7(5) . . ? C21 C20 C19 120.0(6) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 120.5(6) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 120.0(6) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.2(6) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C19 119.9(6) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C26 C25 C30 119.4(6) . . ? C26 C25 N1 118.9(5) . . ? C30 C25 N1 121.6(6) . . ? C27 C26 C25 121.4(7) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C26 C27 C28 120.3(8) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C29 119.1(7) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C30 C29 C28 121.2(7) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C25 118.6(7) . . ? C29 C30 C31 121.1(6) . . ? C25 C30 C31 120.4(6) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C37 118.7(6) . . ? C33 C32 P2 121.2(5) . . ? C37 C32 P2 120.1(5) . . ? C34 C33 C32 119.9(7) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C35 C34 C33 120.6(8) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C36 C35 C34 119.9(8) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 120.8(8) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C36 C37 C32 120.1(7) . . ? C36 C37 H37 120.0 . . ? C32 C37 H37 120.0 . . ? C39 C38 C43 120.2(6) . . ? C39 C38 P2 120.5(5) . . ? C43 C38 P2 118.7(5) . . ? C40 C39 C38 119.3(6) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? C39 C40 C41 119.7(7) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C42 C41 C40 121.6(7) . . ? C42 C41 H41 119.2 . . ? C40 C41 H41 119.2 . . ? C41 C42 C43 119.5(7) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? C42 C43 C38 119.7(6) . . ? C42 C43 H43 120.1 . . ? C38 C43 H43 120.1 . . ? C49 C44 C45 120.5(6) . . ? C49 C44 N2 120.1(6) . . ? C45 C44 N2 119.4(5) . . ? C46 C45 C44 120.6(7) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C47 C46 C45 119.9(8) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 120.2(8) . . ? C46 C47 H47 119.9 . . ? C48 C47 H47 119.9 . . ? C47 C48 C49 121.5(8) . . ? C47 C48 H48 119.2 . . ? C49 C48 H48 119.2 . . ? C44 C49 C48 117.3(7) . . ? C44 C49 C50 122.8(6) . . ? C48 C49 C50 119.9(7) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O3 C51A C52A 121.2(10) . . ? O3 C51A C53 111.7(6) . . ? C52A C51A C53 115.9(9) . . ? O3 C51A H51A 101.3 . . ? C52A C51A H51A 101.3 . . ? C53 C51A H51A 101.3 . . ? H52D C52B H52E 109.5 . . ? H52D C52B H52F 109.5 . . ? H52E C52B H52F 109.5 . . ? O2 C53 O4 120.9(7) . . ? O2 C53 C51A 122.9(6) . . ? O4 C53 C51A 116.3(7) . . ? O4 C54 H54A 109.5 . . ? O4 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O4 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C60 C55 C56 115.1(6) . . ? C60 C55 B1 122.9(5) . . ? C56 C55 B1 121.7(5) . . ? C57 C56 C55 123.2(6) . . ? C57 C56 H56 118.4 . . ? C55 C56 H56 118.4 . . ? C58 C57 C56 120.8(6) . . ? C58 C57 C61 120.2(6) . . ? C56 C57 C61 118.9(6) . . ? C57 C58 C59 117.6(6) . . ? C57 C58 H58 121.2 . . ? C59 C58 H58 121.2 . . ? C60 C59 C58 121.2(6) . . ? C60 C59 C62 120.3(7) . . ? C58 C59 C62 118.5(6) . . ? C59 C60 C55 122.1(6) . . ? C59 C60 H60 119.0 . . ? C55 C60 H60 119.0 . . ? F1 C61 F3 105.9(7) . . ? F1 C61 F2 105.2(7) . . ? F3 C61 F2 106.3(7) . . ? F1 C61 C57 113.2(7) . . ? F3 C61 C57 111.9(7) . . ? F2 C61 C57 113.7(7) . . ? F5 C62 F6 108.5(8) . . ? F5 C62 F4 102.1(8) . . ? F6 C62 F4 100.2(8) . . ? F5 C62 C59 118.0(8) . . ? F6 C62 C59 115.1(7) . . ? F4 C62 C59 110.7(7) . . ? C64 C63 C68 115.4(5) . . ? C64 C63 B1 121.1(5) . . ? C68 C63 B1 123.2(5) . . ? C65 C64 C63 123.5(6) . . ? C65 C64 H64 118.3 . . ? C63 C64 H64 118.3 . . ? C64 C65 C66 120.1(6) . . ? C64 C65 C69 120.1(6) . . ? C66 C65 C69 119.8(6) . . ? C65 C66 C67 118.0(6) . . ? C65 C66 H66 121.0 . . ? C67 C66 H66 121.0 . . ? C68 C67 C66 121.3(6) . . ? C68 C67 C70 119.0(6) . . ? C66 C67 C70 119.8(6) . . ? C67 C68 C63 121.7(6) . . ? C67 C68 H68 119.1 . . ? C63 C68 H68 119.1 . . ? F7 C69 F8 107.9(7) . . ? F7 C69 F9 105.7(6) . . ? F8 C69 F9 103.3(6) . . ? F7 C69 C65 114.4(6) . . ? F8 C69 C65 111.7(6) . . ? F9 C69 C65 113.0(6) . . ? F12B C70 F10 116.8(12) . . ? F12B C70 F11 36.2(10) . . ? F10 C70 F11 110.2(10) . . ? F12B C70 F11B 111.9(12) . . ? F10 C70 F11B 50.8(9) . . ? F11 C70 F11B 138.0(10) . . ? F12B C70 F12 61.1(11) . . ? F10 C70 F12 106.8(9) . . ? F11 C70 F12 97.2(9) . . ? F11B C70 F12 63.4(8) . . ? F12B C70 F10B 106.5(13) . . ? F10 C70 F10B 41.7(8) . . ? F11 C70 F10B 79.9(9) . . ? F11B C70 F10B 92.4(12) . . ? F12 C70 F10B 140.3(9) . . ? F12B C70 C67 122.4(12) . . ? F10 C70 C67 119.8(9) . . ? F11 C70 C67 110.2(7) . . ? F11B C70 C67 111.4(9) . . ? F12 C70 C67 110.2(7) . . ? F10B C70 C67 107.7(8) . . ? C76 C71 C72 114.5(5) . . ? C76 C71 B1 124.1(5) . . ? C72 C71 B1 121.1(5) . . ? C73 C72 C71 122.9(6) . . ? C73 C72 H72 118.5 . . ? C71 C72 H72 118.5 . . ? C74 C73 C72 119.8(6) . . ? C74 C73 C77 122.3(6) . . ? C72 C73 C77 117.9(6) . . ? C73 C74 C75 119.6(6) . . ? C73 C74 H74 120.2 . . ? C75 C74 H74 120.2 . . ? C74 C75 C76 119.7(6) . . ? C74 C75 C78 119.9(6) . . ? C76 C75 C78 120.4(6) . . ? C75 C76 C71 123.4(6) . . ? C75 C76 H76 118.3 . . ? C71 C76 H76 118.3 . . ? F13 C77 F15 107.5(8) . . ? F13 C77 F14 104.7(8) . . ? F15 C77 F14 103.2(7) . . ? F13 C77 C73 113.7(7) . . ? F15 C77 C73 113.9(7) . . ? F14 C77 C73 112.9(8) . . ? F17 C78 F18 106.5(7) . . ? F17 C78 F16 105.0(7) . . ? F18 C78 F16 105.6(7) . . ? F17 C78 C75 113.3(6) . . ? F18 C78 C75 113.1(6) . . ? F16 C78 C75 112.7(7) . . ? C84 C79 C80 114.5(5) . . ? C84 C79 B1 124.0(5) . . ? C80 C79 B1 121.2(5) . . ? C81 C80 C79 122.7(6) . . ? C81 C80 H80 118.6 . . ? C79 C80 H80 118.6 . . ? C82 C81 C80 120.8(6) . . ? C82 C81 C85 118.0(6) . . ? C80 C81 C85 121.1(7) . . ? C81 C82 C83 118.1(6) . . ? C81 C82 H82 121.0 . . ? C83 C82 H82 121.0 . . ? C82 C83 C84 120.9(6) . . ? C82 C83 C86 118.8(6) . . ? C84 C83 C86 120.3(6) . . ? C83 C84 C79 122.8(6) . . ? C83 C84 H84 118.6 . . ? C79 C84 H84 118.6 . . ? F21B C85 F19 122.1(15) . . ? F21B C85 F20B 115.5(18) . . ? F19 C85 F20B 50.1(12) . . ? F21B C85 F21 27.1(16) . . ? F19 C85 F21 111.1(13) . . ? F20B C85 F21 130.5(14) . . ? F21B C85 F20 71.8(17) . . ? F19 C85 F20 105.7(10) . . ? F20B C85 F20 58.6(14) . . ? F21 C85 F20 98.6(10) . . ? F21B C85 F19B 99.3(16) . . ? F19 C85 F19B 47.9(10) . . ? F20B C85 F19B 97.5(16) . . ? F21 C85 F19B 75.2(13) . . ? F20 C85 F19B 143.2(10) . . ? F21B C85 C81 117.9(14) . . ? F19 C85 C81 116.8(9) . . ? F20B C85 C81 116.2(12) . . ? F21 C85 C81 112.9(10) . . ? F20 C85 C81 110.0(8) . . ? F19B C85 C81 105.6(9) . . ? F22 C86 F24 105.9(8) . . ? F22 C86 F23 102.9(7) . . ? F24 C86 F23 102.5(7) . . ? F22 C86 C83 113.8(7) . . ? F24 C86 C83 114.7(7) . . ? F23 C86 C83 115.6(7) . . ? Cl2 C87 Cl1 106.4 . . ? Cl2 C87 H87A 110.4 . . ? Cl1 C87 H87A 110.4 . . ? Cl2 C87 H87B 110.4 . . ? Cl1 C87 H87B 110.4 . . ? H87A C87 H87B 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Zn1 N2 C44 111.0(4) . . . . ? N1 ZN1 N2 C44 -82.7(4) . . . . ? O2 Zn1 N2 C44 24.6(4) . . . . ? O3 Zn1 N2 P2 -79.7(4) . . . . ? N1 Zn1 N2 P2 86.7(4) . . . . ? O2 Zn1 N2 P2 -166.1(3) . . . . ? C12 O1 C1 C2 -179.7(5) . . . . ? C12 O1 C1 C6 -1.4(6) . . . . ? C44 N2 P2 C32 -167.2(4) . . . . ? Zn1 N2 P2 C32 23.9(4) . . . . ? C44 N2 P2 C38 -45.4(5) . . . . ? Zn1 N2 P2 C38 145.6(3) . . . . ? C44 N2 P2 C11 74.8(5) . . . . ? Zn1 N2 P2 C11 -94.1(4) . . . . ? O3 Zn1 O2 C53 -0.4(4) . . . . ? N1 Zn1 O2 C53 -114.9(4) . . . . ? N2 Zn1 O2 C53 117.7(4) . . . . ? C19 P1 N1 C25 160.4(4) . . . . ? C13 P1 N1 C25 39.7(5) . . . . ? C2 P1 N1 C25 -81.7(5) . . . . ? C19 P1 N1 Zn1 -29.6(4) . . . . ? C13 P1 N1 Zn1 -150.3(4) . . . . ? C2 P1 N1 Zn1 88.3(4) . . . . ? O3 Zn1 N1 C25 -105.9(4) . . . . ? N2 Zn1 N1 C25 87.3(4) . . . . ? O2 Zn1 N1 C25 -18.9(4) . . . . ? O3 Zn1 N1 P1 83.7(4) . . . . ? N2 Zn1 N1 P1 -83.1(4) . . . . ? O2 Zn1 N1 P1 170.6(3) . . . . ? C6 C1 C2 C3 0.1(9) . . . . ? O1 C1 C2 C3 178.2(5) . . . . ? C6 C1 C2 P1 -174.4(5) . . . . ? O1 C1 C2 P1 3.7(8) . . . . ? N1 P1 C2 C1 -43.9(6) . . . . ? C19 P1 C2 C1 76.5(5) . . . . ? C13 P1 C2 C1 -168.1(5) . . . . ? N1 P1 C2 C3 142.2(5) . . . . ? C19 P1 C2 C3 -97.4(5) . . . . ? C13 P1 C2 C3 18.0(6) . . . . ? C1 C2 C3 C4 -1.4(8) . . . . ? P1 C2 C3 C4 172.8(5) . . . . ? N1 Zn1 O3 C51A 100.6(6) . . . . ? N2 Zn1 O3 C51A -91.8(6) . . . . ? O2 Zn1 O3 C51A 3.2(6) . . . . ? C2 C3 C4 C5 1.5(9) . . . . ? C3 C4 C5 C6 -0.3(9) . . . . ? C2 C1 C6 C5 1.1(9) . . . . ? O1 C1 C6 C5 -177.2(5) . . . . ? C2 C1 C6 C7 179.9(6) . . . . ? O1 C1 C6 C7 1.6(6) . . . . ? C4 C5 C6 C1 -1.0(8) . . . . ? C4 C5 C6 C7 -179.2(6) . . . . ? C1 C6 C7 C12 -1.1(6) . . . . ? C5 C6 C7 C12 177.3(6) . . . . ? C1 C6 C7 C8 -179.1(7) . . . . ? C5 C6 C7 C8 -0.7(12) . . . . ? C12 C7 C8 C9 -0.1(9) . . . . ? C6 C7 C8 C9 177.8(6) . . . . ? C7 C8 C9 C10 -0.9(9) . . . . ? C8 C9 C10 C11 0.8(9) . . . . ? C9 C10 C11 C12 0.3(8) . . . . ? C9 C10 C11 P2 -173.9(5) . . . . ? N2 P2 C11 C10 -139.9(5) . . . . ? C32 P2 C11 C10 99.7(6) . . . . ? C38 P2 C11 C10 -16.4(6) . . . . ? N2 P2 C11 C12 46.1(5) . . . . ? C32 P2 C11 C12 -74.3(5) . . . . ? C38 P2 C11 C12 169.6(4) . . . . ? C1 O1 C12 C7 0.7(6) . . . . ? C1 O1 C12 C11 178.2(5) . . . . ? C8 C7 C12 O1 178.7(5) . . . . ? C6 C7 C12 O1 0.2(6) . . . . ? C8 C7 C12 C11 1.3(9) . . . . ? C6 C7 C12 C11 -177.2(5) . . . . ? C10 C11 C12 O1 -178.6(5) . . . . ? P2 C11 C12 O1 -3.8(7) . . . . ? C10 C11 C12 C7 -1.4(9) . . . . ? P2 C11 C12 C7 173.4(5) . . . . ? N1 P1 C13 C14 106.1(5) . . . . ? C19 P1 C13 C14 -14.5(6) . . . . ? C2 P1 C13 C14 -126.5(5) . . . . ? N1 P1 C13 C18 -68.6(5) . . . . ? C19 P1 C13 C18 170.8(5) . . . . ? C2 P1 C13 C18 58.7(5) . . . . ? C18 C13 C14 C15 1.9(10) . . . . ? P1 C13 C14 C15 -172.7(5) . . . . ? C13 C14 C15 C16 1.2(11) . . . . ? C14 C15 C16 C17 -2.5(12) . . . . ? C15 C16 C17 C18 0.6(11) . . . . ? C14 C13 C18 C17 -3.7(9) . . . . ? P1 C13 C18 C17 171.0(5) . . . . ? C16 C17 C18 C13 2.5(10) . . . . ? N1 P1 C19 C20 -34.1(6) . . . . ? C13 P1 C19 C20 87.9(5) . . . . ? C2 P1 C19 C20 -159.2(5) . . . . ? N1 P1 C19 C24 149.2(5) . . . . ? C13 P1 C19 C24 -88.9(5) . . . . ? C2 P1 C19 C24 24.0(6) . . . . ? C24 C19 C20 C21 2.2(9) . . . . ? P1 C19 C20 C21 -174.6(5) . . . . ? C19 C20 C21 C22 -1.1(10) . . . . ? C20 C21 C22 C23 0.1(11) . . . . ? C21 C22 C23 C24 -0.2(11) . . . . ? C22 C23 C24 C19 1.3(10) . . . . ? C20 C19 C24 C23 -2.3(9) . . . . ? P1 C19 C24 C23 174.6(5) . . . . ? P1 N1 C25 C26 83.7(6) . . . . ? Zn1 N1 C25 C26 -88.5(6) . . . . ? P1 N1 C25 C30 -97.9(6) . . . . ? Zn1 N1 C25 C30 89.9(6) . . . . ? C30 C25 C26 C27 -0.4(10) . . . . ? N1 C25 C26 C27 178.0(6) . . . . ? C25 C26 C27 C28 -0.4(11) . . . . ? C26 C27 C28 C29 1.3(12) . . . . ? C27 C28 C29 C30 -1.4(11) . . . . ? C28 C29 C30 C25 0.5(10) . . . . ? C28 C29 C30 C31 -179.8(6) . . . . ? C26 C25 C30 C29 0.3(9) . . . . ? N1 C25 C30 C29 -178.1(5) . . . . ? C26 C25 C30 C31 -179.3(6) . . . . ? N1 C25 C30 C31 2.3(9) . . . . ? N2 P2 C32 C33 29.5(6) . . . . ? C38 P2 C32 C33 -93.4(5) . . . . ? C11 P2 C32 C33 153.4(5) . . . . ? N2 P2 C32 C37 -152.3(5) . . . . ? C38 P2 C32 C37 84.9(6) . . . . ? C11 P2 C32 C37 -28.4(6) . . . . ? C37 C32 C33 C34 1.7(9) . . . . ? P2 C32 C33 C34 179.9(5) . . . . ? C32 C33 C34 C35 -1.3(11) . . . . ? C33 C34 C35 C36 -0.5(12) . . . . ? C34 C35 C36 C37 1.8(13) . . . . ? C35 C36 C37 C32 -1.4(12) . . . . ? C33 C32 C37 C36 -0.4(10) . . . . ? P2 C32 C37 C36 -178.6(6) . . . . ? N2 P2 C38 C39 66.9(5) . . . . ? C32 P2 C38 C39 -171.6(5) . . . . ? C11 P2 C38 C39 -58.6(5) . . . . ? N2 P2 C38 C43 -103.7(5) . . . . ? C32 P2 C38 C43 17.9(6) . . . . ? C11 P2 C38 C43 130.8(5) . . . . ? C43 C38 C39 C40 -0.5(9) . . . . ? P2 C38 C39 C40 -171.0(5) . . . . ? C38 C39 C40 C41 0.8(10) . . . . ? C39 C40 C41 C42 -1.2(11) . . . . ? C40 C41 C42 C43 1.2(11) . . . . ? C41 C42 C43 C38 -0.9(10) . . . . ? C39 C38 C43 C42 0.6(9) . . . . ? P2 C38 C43 C42 171.2(5) . . . . ? P2 N2 C44 C49 95.8(6) . . . . ? Zn1 N2 C44 C49 -92.9(6) . . . . ? P2 N2 C44 C45 -85.1(6) . . . . ? Zn1 N2 C44 C45 86.2(6) . . . . ? C49 C44 C45 C46 1.2(10) . . . . ? N2 C44 C45 C46 -178.0(6) . . . . ? C44 C45 C46 C47 -1.5(11) . . . . ? C45 C46 C47 C48 1.0(13) . . . . ? C46 C47 C48 C49 -0.2(13) . . . . ? C45 C44 C49 C48 -0.4(9) . . . . ? N2 C44 C49 C48 178.8(6) . . . . ? C45 C44 C49 C50 -179.5(6) . . . . ? N2 C44 C49 C50 -0.3(9) . . . . ? C47 C48 C49 C44 -0.1(11) . . . . ? C47 C48 C49 C50 179.0(7) . . . . ? Zn1 O3 C51A C52A 137.2(10) . . . . ? Zn1 O3 C51A C53 -5.0(9) . . . . ? Zn1 O2 C53 O4 176.8(5) . . . . ? Zn1 O2 C53 C51A -2.5(8) . . . . ? C54 O4 C53 O2 -0.2(9) . . . . ? C54 O4 C53 C51A 179.2(7) . . . . ? O3 C51A C53 O2 5.2(12) . . . . ? C52A C51A C53 O2 -139.2(10) . . . . ? O3 C51A C53 O4 -174.2(7) . . . . ? C52A C51A C53 O4 41.5(13) . . . . ? C63 B1 C55 C60 -146.0(5) . . . . ? C79 B1 C55 C60 -27.2(8) . . . . ? C71 B1 C55 C60 93.9(6) . . . . ? C63 B1 C55 C56 41.2(8) . . . . ? C79 B1 C55 C56 160.0(5) . . . . ? C71 B1 C55 C56 -78.8(7) . . . . ? C60 C55 C56 C57 2.8(9) . . . . ? B1 C55 C56 C57 176.1(6) . . . . ? C55 C56 C57 C58 -1.0(10) . . . . ? C55 C56 C57 C61 178.3(6) . . . . ? C56 C57 C58 C59 -0.9(9) . . . . ? C61 C57 C58 C59 179.8(7) . . . . ? C57 C58 C59 C60 0.9(10) . . . . ? C57 C58 C59 C62 -179.7(7) . . . . ? C58 C59 C60 C55 1.1(10) . . . . ? C62 C59 C60 C55 -178.3(7) . . . . ? C56 C55 C60 C59 -2.8(9) . . . . ? B1 C55 C60 C59 -176.0(6) . . . . ? C58 C57 C61 F1 -122.7(7) . . . . ? C56 C57 C61 F1 58.0(9) . . . . ? C58 C57 C61 F3 117.7(8) . . . . ? C56 C57 C61 F3 -61.6(10) . . . . ? C58 C57 C61 F2 -2.8(11) . . . . ? C56 C57 C61 F2 177.9(6) . . . . ? C60 C59 C62 F5 -173.2(8) . . . . ? C58 C59 C62 F5 7.4(12) . . . . ? C60 C59 C62 F6 -42.9(11) . . . . ? C58 C59 C62 F6 137.7(8) . . . . ? C60 C59 C62 F4 69.8(10) . . . . ? C58 C59 C62 F4 -109.6(8) . . . . ? C55 B1 C63 C64 -166.4(5) . . . . ? C79 B1 C63 C64 71.3(7) . . . . ? C71 B1 C63 C64 -50.1(7) . . . . ? C55 B1 C63 C68 19.1(8) . . . . ? C79 B1 C63 C68 -103.2(6) . . . . ? C71 B1 C63 C68 135.4(5) . . . . ? C68 C63 C64 C65 0.3(8) . . . . ? B1 C63 C64 C65 -174.6(5) . . . . ? C63 C64 C65 C66 -1.8(9) . . . . ? C63 C64 C65 C69 177.8(6) . . . . ? C64 C65 C66 C67 1.9(9) . . . . ? C69 C65 C66 C67 -177.8(6) . . . . ? C65 C66 C67 C68 -0.4(9) . . . . ? C65 C66 C67 C70 -179.5(7) . . . . ? C66 C67 C68 C63 -1.1(9) . . . . ? C70 C67 C68 C63 178.0(7) . . . . ? C64 C63 C68 C67 1.2(8) . . . . ? B1 C63 C68 C67 176.0(5) . . . . ? C64 C65 C69 F7 178.6(6) . . . . ? C66 C65 C69 F7 -1.8(10) . . . . ? C64 C65 C69 F8 -58.5(9) . . . . ? C66 C65 C69 F8 121.2(7) . . . . ? C64 C65 C69 F9 57.5(9) . . . . ? C66 C65 C69 F9 -122.8(7) . . . . ? C68 C67 C70 F12B 77.1(16) . . . . ? C66 C67 C70 F12B -103.8(16) . . . . ? C68 C67 C70 F10 -90.6(13) . . . . ? C66 C67 C70 F10 88.5(13) . . . . ? C68 C67 C70 F11 38.8(11) . . . . ? C66 C67 C70 F11 -142.1(8) . . . . ? C68 C67 C70 F11B -146.7(12) . . . . ? C66 C67 C70 F11B 32.5(15) . . . . ? C68 C67 C70 F12 145.0(9) . . . . ? C66 C67 C70 F12 -35.9(12) . . . . ? C68 C67 C70 F10B -46.7(11) . . . . ? C66 C67 C70 F10B 132.4(9) . . . . ? C63 B1 C71 C76 -31.4(8) . . . . ? C55 B1 C71 C76 91.1(6) . . . . ? C79 B1 C71 C76 -148.3(6) . . . . ? C63 B1 C71 C72 155.4(5) . . . . ? C55 B1 C71 C72 -82.1(6) . . . . ? C79 B1 C71 C72 38.5(7) . . . . ? C76 C71 C72 C73 3.1(9) . . . . ? B1 C71 C72 C73 176.9(6) . . . . ? C71 C72 C73 C74 -2.6(10) . . . . ? C71 C72 C73 C77 176.4(7) . . . . ? C72 C73 C74 C75 -0.5(10) . . . . ? C77 C73 C74 C75 -179.4(7) . . . . ? C73 C74 C75 C76 2.6(10) . . . . ? C73 C74 C75 C78 -175.7(7) . . . . ? C74 C75 C76 C71 -2.0(10) . . . . ? C78 C75 C76 C71 176.3(7) . . . . ? C72 C71 C76 C75 -0.8(9) . . . . ? B1 C71 C76 C75 -174.4(6) . . . . ? C74 C73 C77 F13 121.7(9) . . . . ? C72 C73 C77 F13 -57.2(12) . . . . ? C74 C73 C77 F15 -1.9(12) . . . . ? C72 C73 C77 F15 179.2(7) . . . . ? C74 C73 C77 F14 -119.1(8) . . . . ? C72 C73 C77 F14 61.9(9) . . . . ? C74 C75 C78 F17 -143.0(7) . . . . ? C76 C75 C78 F17 38.7(10) . . . . ? C74 C75 C78 F18 -21.7(11) . . . . ? C76 C75 C78 F18 160.0(7) . . . . ? C74 C75 C78 F16 98.0(8) . . . . ? C76 C75 C78 F16 -80.3(9) . . . . ? C63 B1 C79 C84 -95.0(6) . . . . ? C55 B1 C79 C84 141.1(6) . . . . ? C71 B1 C79 C84 25.0(8) . . . . ? C63 B1 C79 C80 79.9(6) . . . . ? C55 B1 C79 C80 -44.1(7) . . . . ? C71 B1 C79 C80 -160.2(5) . . . . ? C84 C79 C80 C81 -3.7(8) . . . . ? B1 C79 C80 C81 -179.0(5) . . . . ? C79 C80 C81 C82 2.3(9) . . . . ? C79 C80 C81 C85 -177.9(7) . . . . ? C80 C81 C82 C83 -0.5(9) . . . . ? C85 C81 C82 C83 179.7(7) . . . . ? C81 C82 C83 C84 0.5(9) . . . . ? C81 C82 C83 C86 -178.4(6) . . . . ? C82 C83 C84 C79 -2.2(9) . . . . ? C86 C83 C84 C79 176.7(6) . . . . ? C80 C79 C84 C83 3.6(8) . . . . ? B1 C79 C84 C83 178.8(5) . . . . ? C82 C81 C85 F21B 133(2) . . . . ? C80 C81 C85 F21B -47(2) . . . . ? C82 C81 C85 F19 -66.6(15) . . . . ? C80 C81 C85 F19 113.5(14) . . . . ? C82 C81 C85 F20B -10(2) . . . . ? C80 C81 C85 F20B 170(2) . . . . ? C82 C81 C85 F21 162.8(11) . . . . ? C80 C81 C85 F21 -17.0(14) . . . . ? C82 C81 C85 F20 53.8(11) . . . . ? C80 C81 C85 F20 -126.0(9) . . . . ? C82 C81 C85 F19B -116.9(14) . . . . ? C80 C81 C85 F19B 63.2(16) . . . . ? C82 C83 C86 F22 84.1(9) . . . . ? C84 C83 C86 F22 -94.8(9) . . . . ? C82 C83 C86 F24 -153.7(7) . . . . ? C84 C83 C86 F24 27.4(10) . . . . ? C82 C83 C86 F23 -34.7(10) . . . . ? C84 C83 C86 F23 146.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.12 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.724 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.078 #===END data_9 _database_code_depnum_ccdc_archive 'CCDC 833330' #TrackingRef '6184_web_deposit_cif_file_0_PaulG.Hayes_ #1310063407.Chem Eur J_AllCifs - Paul G Hayes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H60 B Br0.38 F24 N2 O4 P2 Zn' _chemical_formula_weight 1857.89 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.7810(11) _cell_length_b 27.1179(16) _cell_length_c 18.6506(11) _cell_angle_alpha 90.00 _cell_angle_beta 116.7850(10) _cell_angle_gamma 90.00 _cell_volume 8479.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9767 _cell_measurement_theta_min 4.374 _cell_measurement_theta_max 48.202 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3761 _exptl_absorpt_coefficient_mu 0.612 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7608 _exptl_absorpt_correction_T_max 0.8489 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 101702 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.03 _reflns_number_total 14960 _reflns_number_gt 11787 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0540P)^2^+15.4673P] 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 14960 _refine_ls_number_parameters 1339 _refine_ls_number_restraints 815 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1617 _refine_ls_wR_factor_gt 0.1516 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.010 _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 1.01356(2) 0.462792(16) 0.26089(2) 0.03670(13) Uani 1 1 d . A . P1 P 0.84069(5) 0.49812(3) 0.19297(6) 0.0338(2) Uani 1 1 d . . . P2 P 1.17929(6) 0.51112(4) 0.27625(6) 0.0356(2) Uani 1 1 d . A . O1 O 0.98851(13) 0.52292(8) 0.16034(13) 0.0324(5) Uani 1 1 d . . . N1 N 0.92543(17) 0.49992(11) 0.27079(17) 0.0347(7) Uani 1 1 d . . . O3 O 0.9930(2) 0.41618(10) 0.17749(16) 0.0560(8) Uani 1 1 d . . . N2 N 1.12106(18) 0.49368(13) 0.31263(18) 0.0447(8) Uani 1 1 d . . . C1 C 0.9130(2) 0.53130(12) 0.0988(2) 0.0348(8) Uani 1 1 d . . . C2 C 0.8425(2) 0.52315(13) 0.1042(2) 0.0371(8) Uani 1 1 d . . . C3 C 0.7727(2) 0.53588(15) 0.0350(2) 0.0506(10) Uani 1 1 d . . . H3 H 0.7224 0.5316 0.0349 0.061 Uiso 1 1 calc R . . C4 C 0.7752(3) 0.55458(17) -0.0332(2) 0.0565(11) Uani 1 1 d . . . H4 H 0.7267 0.5626 -0.0789 0.068 Uiso 1 1 calc R . . C5 C 0.8464(3) 0.56176(15) -0.0361(2) 0.0503(10) Uani 1 1 d . . . H5 H 0.8473 0.5744 -0.0832 0.060 Uiso 1 1 calc R . . C6 C 0.9171(2) 0.55022(13) 0.0311(2) 0.0391(9) Uani 1 1 d . . . C7 C 1.0008(2) 0.55349(13) 0.0523(2) 0.0372(8) Uani 1 1 d . . . C8 C 1.0455(3) 0.56916(14) 0.0134(2) 0.0454(10) Uani 1 1 d . . . H8 H 1.0199 0.5802 -0.0407 0.054 Uiso 1 1 calc R . . C9 C 1.1268(3) 0.56810(15) 0.0553(3) 0.0506(11) Uani 1 1 d . . . H9 H 1.1577 0.5794 0.0299 0.061 Uiso 1 1 calc R . . C10 C 1.1657(3) 0.55103(15) 0.1339(2) 0.0461(10) Uani 1 1 d . A . H10 H 1.2223 0.5507 0.1605 0.055 Uiso 1 1 calc R . . C11 C 1.1237(2) 0.53428(13) 0.1749(2) 0.0355(8) Uani 1 1 d . . . C12 C 1.0418(2) 0.53671(12) 0.1315(2) 0.0331(8) Uani 1 1 d . A . C13 C 0.7622(2) 0.53035(13) 0.2038(2) 0.0395(8) Uani 1 1 d . . . C14 C 0.7011(2) 0.50547(15) 0.2105(2) 0.0450(9) Uani 1 1 d . . . H14 H 0.6987 0.4705 0.2067 0.054 Uiso 1 1 calc R . . C15 C 0.6439(3) 0.53069(18) 0.2224(3) 0.0553(11) Uani 1 1 d . . . H15 H 0.6023 0.5130 0.2264 0.066 Uiso 1 1 calc R . . C16 C 0.6462(3) 0.58045(19) 0.2284(3) 0.0618(12) Uani 1 1 d . . . H16 H 0.6075 0.5976 0.2385 0.074 Uiso 1 1 calc R . . C17 C 0.7046(3) 0.60571(18) 0.2198(4) 0.0858(18) Uani 1 1 d . . . H17 H 0.7055 0.6407 0.2226 0.103 Uiso 1 1 calc R . . C18 C 0.7625(3) 0.58148(17) 0.2070(4) 0.0757(16) Uani 1 1 d . . . H18 H 0.8023 0.5997 0.2004 0.091 Uiso 1 1 calc R . . C19 C 0.8101(2) 0.43492(13) 0.1737(2) 0.0373(8) Uani 1 1 d . . . C20 C 0.8266(3) 0.40435(14) 0.2399(3) 0.0484(10) Uani 1 1 d . . . H20 H 0.8568 0.4164 0.2930 0.058 Uiso 1 1 calc R . . C21 C 0.7981(3) 0.35622(16) 0.2269(3) 0.0601(12) Uani 1 1 d . . . H21 H 0.8087 0.3352 0.2713 0.072 Uiso 1 1 calc R . . C22 C 0.7545(3) 0.33881(17) 0.1498(3) 0.0640(13) Uani 1 1 d . . . H22 H 0.7356 0.3058 0.1414 0.077 Uiso 1 1 calc R . . C23 C 0.7382(3) 0.36879(17) 0.0853(3) 0.0649(13) Uani 1 1 d . . . H23 H 0.7077 0.3565 0.0324 0.078 Uiso 1 1 calc R . . C24 C 0.7659(2) 0.41665(15) 0.0966(3) 0.0473(10) Uani 1 1 d . . . H24 H 0.7546 0.4372 0.0514 0.057 Uiso 1 1 calc R . . C25 C 0.9471(2) 0.54124(14) 0.3246(2) 0.0405(9) Uani 1 1 d . . . C26 C 0.9720(3) 0.58586(17) 0.3063(3) 0.0634(13) Uani 1 1 d . . . H26 H 0.9744 0.5896 0.2568 0.076 Uiso 1 1 calc R . . C27 C 0.9932(4) 0.6245(2) 0.3598(4) 0.0881(19) Uani 1 1 d . . . H27 H 1.0103 0.6548 0.3471 0.106 Uiso 1 1 calc R . . C28 C 0.9896(4) 0.6194(2) 0.4318(4) 0.092(2) Uani 1 1 d . . . H28 H 1.0044 0.6461 0.4686 0.111 Uiso 1 1 calc R . . C29 C 0.9650(3) 0.5762(2) 0.4500(3) 0.0776(16) Uani 1 1 d . . . H29 H 0.9623 0.5728 0.4994 0.093 Uiso 1 1 calc R . . C30 C 0.9437(3) 0.53706(18) 0.3966(3) 0.0572(11) Uani 1 1 d . . . H30 H 0.9266 0.5070 0.4099 0.069 Uiso 1 1 calc R . . C31 C 1.2438(2) 0.55840(15) 0.3370(2) 0.0436(9) Uani 1 1 d . . . C32 C 1.2193(3) 0.60659(16) 0.3228(3) 0.0572(11) Uani 1 1 d . A . H32 H 1.1729 0.6153 0.2754 0.069 Uiso 1 1 calc R . . C33 C 1.2629(4) 0.6428(2) 0.3784(4) 0.0833(18) Uani 1 1 d . . . H33 H 1.2465 0.6764 0.3691 0.100 Uiso 1 1 calc R A . C34 C 1.3288(4) 0.6298(3) 0.4458(4) 0.090(2) Uani 1 1 d . A . H34 H 1.3581 0.6547 0.4835 0.107 Uiso 1 1 calc R . . C35 C 1.3547(4) 0.5819(2) 0.4613(3) 0.0814(17) Uani 1 1 d . . . H35 H 1.4014 0.5738 0.5088 0.098 Uiso 1 1 calc R A . C36 C 1.3120(3) 0.54546(19) 0.4070(3) 0.0581(11) Uani 1 1 d . A . H36 H 1.3288 0.5120 0.4170 0.070 Uiso 1 1 calc R . . C37 C 1.2431(2) 0.46366(15) 0.2682(2) 0.0431(9) Uani 1 1 d . . . C38 C 1.3166(3) 0.47424(19) 0.2703(3) 0.0599(12) Uani 1 1 d . A . H38 H 1.3364 0.5070 0.2786 0.072 Uiso 1 1 calc R . . C39 C 1.3608(4) 0.4357(3) 0.2598(3) 0.0834(19) Uani 1 1 d . . . H39 H 1.4116 0.4421 0.2623 0.100 Uiso 1 1 calc R A . C40 C 1.3302(5) 0.3883(3) 0.2459(3) 0.098(2) Uani 1 1 d . A . H40 H 1.3592 0.3622 0.2373 0.118 Uiso 1 1 calc R . . C41 C 1.2590(5) 0.3794(2) 0.2447(4) 0.093(2) Uani 1 1 d . . . H41 H 1.2393 0.3465 0.2368 0.112 Uiso 1 1 calc R A . C42 C 1.2147(3) 0.41587(16) 0.2544(3) 0.0641(13) Uani 1 1 d . A . H42 H 1.1641 0.4085 0.2516 0.077 Uiso 1 1 calc R . . C43 C 1.1570(2) 0.4911(2) 0.4008(3) 0.0712(16) Uani 1 1 d . A . C44 C 1.1937(3) 0.4490(3) 0.4395(3) 0.109(3) Uani 1 1 d . . . H44 H 1.1970 0.4215 0.4097 0.131 Uiso 1 1 calc R A . C45 C 1.2263(4) 0.4462(5) 0.5224(5) 0.162(6) Uani 1 1 d . A . H45 H 1.2518 0.4168 0.5497 0.194 Uiso 1 1 calc R . . C46 C 1.2215(5) 0.4856(7) 0.5637(5) 0.196(8) Uani 1 1 d . . . H46 H 1.2434 0.4834 0.6205 0.235 Uiso 1 1 calc R A . C47 C 1.1860(4) 0.5295(5) 0.5267(4) 0.155(5) Uani 1 1 d . A . H47 H 1.1846 0.5570 0.5576 0.186 Uiso 1 1 calc R . . C48 C 1.1523(3) 0.5325(3) 0.4431(3) 0.092(2) Uani 1 1 d . . . H48 H 1.1269 0.5619 0.4157 0.111 Uiso 1 1 calc R A . C49A C 0.9943(6) 0.36877(19) 0.1986(4) 0.110(3) Uani 0.50 1 d P A 1 H49A H 1.0468 0.3596 0.2005 0.132 Uiso 0.50 1 calc PR A 1 C50A C 0.9524(7) 0.3332(4) 0.1528(6) 0.062(2) Uani 0.50 1 d P A 1 H50A H 0.8967 0.3368 0.1428 0.092 Uiso 0.50 1 calc PR A 1 H50B H 0.9734 0.3016 0.1793 0.092 Uiso 0.50 1 calc PR A 1 H50C H 0.9553 0.3344 0.1017 0.092 Uiso 0.50 1 calc PR A 1 C49B C 0.9943(6) 0.36877(19) 0.1986(4) 0.110(3) Uani 0.50 1 d P A 2 H49B H 0.9356 0.3632 0.1769 0.132 Uiso 0.50 1 calc PR A 2 C50B C 1.0110(7) 0.3324(4) 0.1578(6) 0.065(3) Uani 0.50 1 d P A 2 H50D H 0.9795 0.3376 0.0999 0.098 Uiso 0.50 1 calc PR A 2 H50E H 0.9975 0.3003 0.1726 0.098 Uiso 0.50 1 calc PR A 2 H50F H 1.0679 0.3332 0.1717 0.098 Uiso 0.50 1 calc PR A 2 C51 C 1.0183(3) 0.36327(16) 0.2881(3) 0.0647(13) Uani 1 1 d . . . C52 C 1.0520(7) 0.3126(2) 0.4007(4) 0.150(4) Uani 1 1 d . . . H52A H 1.0947 0.3362 0.4306 0.225 Uiso 1 1 calc R A . H52B H 1.0715 0.2790 0.4177 0.225 Uiso 1 1 calc R . . H52C H 1.0064 0.3191 0.4115 0.225 Uiso 1 1 calc R . . C53 C 0.51943(19) 0.18518(12) 0.4266(2) 0.0326(7) Uani 1 1 d . . . C54 C 0.4920(2) 0.15930(13) 0.4745(2) 0.0362(8) Uani 1 1 d . . . H54 H 0.4675 0.1772 0.5012 0.043 Uiso 1 1 calc R . . C55 C 0.4994(2) 0.10843(13) 0.4842(2) 0.0375(8) Uani 1 1 d . . . C56 C 0.5346(2) 0.08126(13) 0.4466(2) 0.0394(9) Uani 1 1 d . . . H56 H 0.5401 0.0465 0.4535 0.047 Uiso 1 1 calc R . . C57 C 0.5616(2) 0.10536(13) 0.3988(2) 0.0368(8) Uani 1 1 d . B . C58 C 0.5535(2) 0.15603(12) 0.3889(2) 0.0341(8) Uani 1 1 d . . . H58 H 0.5721 0.1716 0.3548 0.041 Uiso 1 1 calc R . . C59 C 0.4684(3) 0.08146(15) 0.5341(3) 0.0496(10) Uani 1 1 d . . . C60 C 0.5986(3) 0.07643(15) 0.3562(3) 0.0504(10) Uani 1 1 d . . . C61 C 0.4167(2) 0.24729(12) 0.3301(2) 0.0392(9) Uani 1 1 d . . . C62 C 0.3469(2) 0.24520(14) 0.3384(3) 0.0498(10) Uani 1 1 d . . . H62 H 0.3506 0.2454 0.3909 0.060 Uiso 1 1 calc R . . C63 C 0.2724(3) 0.24284(16) 0.2735(3) 0.0602(13) Uani 1 1 d . C . C64 C 0.2647(3) 0.24283(18) 0.1966(3) 0.0713(15) Uani 1 1 d . . . H64 H 0.2135 0.2414 0.1517 0.086 Uiso 1 1 calc R . . C65 C 0.3324(3) 0.2450(2) 0.1857(3) 0.0733(15) Uani 1 1 d . D . C66 C 0.4074(2) 0.24696(16) 0.2520(3) 0.0528(11) Uani 1 1 d . . . H66 H 0.4535 0.2481 0.2434 0.063 Uiso 1 1 calc R . . C67 C 0.2000(4) 0.2390(3) 0.2867(5) 0.093(2) Uani 1 1 d . . . C68 C 0.3267(5) 0.2454(5) 0.1027(4) 0.128(4) Uani 1 1 d . . . C69 C 0.5751(2) 0.27130(12) 0.39580(19) 0.0317(7) Uani 1 1 d . . . C70 C 0.6542(2) 0.25640(13) 0.4364(2) 0.0369(8) Uani 1 1 d . . . H70 H 0.6665 0.2272 0.4679 0.044 Uiso 1 1 calc R . . C71 C 0.7161(2) 0.28261(15) 0.4328(3) 0.0481(10) Uani 1 1 d . E . C72 C 0.7001(3) 0.32553(17) 0.3880(3) 0.0587(12) Uani 1 1 d . . . H72 H 0.7420 0.3436 0.3851 0.070 Uiso 1 1 calc R . . C73 C 0.6229(3) 0.34136(16) 0.3480(3) 0.0560(11) Uani 1 1 d . F . C74 C 0.5613(2) 0.31516(14) 0.3518(2) 0.0428(9) Uani 1 1 d . . . H74 H 0.5083 0.3273 0.3237 0.051 Uiso 1 1 calc R . . C75 C 0.7998(3) 0.2646(2) 0.4783(4) 0.0751(15) Uani 1 1 d . . . C76 C 0.6039(5) 0.3883(3) 0.2989(4) 0.102(2) Uani 1 1 d . . . C77 C 0.5059(2) 0.27525(13) 0.4853(2) 0.0386(8) Uani 1 1 d . . . C78 C 0.5596(2) 0.26391(14) 0.5642(2) 0.0411(9) Uani 1 1 d . . . H78 H 0.5893 0.2342 0.5745 0.049 Uiso 1 1 calc R . . C79 C 0.5714(3) 0.29435(16) 0.6282(2) 0.0504(10) Uani 1 1 d . G . C80 C 0.5282(3) 0.33769(19) 0.6162(3) 0.0677(14) Uani 1 1 d . . . H80 H 0.5356 0.3585 0.6601 0.081 Uiso 1 1 calc R . . C81 C 0.4743(3) 0.34960(19) 0.5392(3) 0.0689(14) Uani 1 1 d . H . C82 C 0.4631(3) 0.31927(15) 0.4750(3) 0.0519(11) Uani 1 1 d . . . H82 H 0.4253 0.3286 0.4224 0.062 Uiso 1 1 calc R . . C83 C 0.6294(3) 0.2803(2) 0.7112(3) 0.0715(15) Uani 1 1 d . . . C84 C 0.4256(6) 0.3953(3) 0.5236(5) 0.111(3) Uani 1 1 d . . . O2 O 1.02726(17) 0.39836(10) 0.33137(16) 0.0493(7) Uani 1 1 d . A . O4 O 1.0276(4) 0.31789(13) 0.3154(3) 0.1195(19) Uani 1 1 d . A . B1 B 0.5036(2) 0.24436(14) 0.4090(2) 0.0334(9) Uani 1 1 d . . . F1 F 0.4295(2) 0.10922(11) 0.5617(2) 0.0965(12) Uani 1 1 d DU . . F2 F 0.52495(17) 0.05858(11) 0.59628(15) 0.0716(8) Uani 1 1 d DU . . F3 F 0.41848(18) 0.04466(11) 0.49233(18) 0.0811(9) Uani 1 1 d DU . . F4 F 0.6719(3) 0.0931(2) 0.3754(4) 0.0917(17) Uani 0.80 1 d PDU B 1 F5 F 0.5601(4) 0.0802(2) 0.2789(3) 0.0822(16) Uani 0.80 1 d PDU B 1 F6 F 0.6058(5) 0.0293(2) 0.3741(5) 0.102(3) Uani 0.80 1 d PDU B 1 F4B F 0.6329(19) 0.1008(5) 0.3167(17) 0.089(6) Uani 0.20 1 d PDU B 2 F5B F 0.5451(11) 0.0497(10) 0.2904(16) 0.107(9) Uani 0.20 1 d PDU B 2 F6B F 0.6496(16) 0.0445(10) 0.3951(13) 0.096(10) Uani 0.20 1 d PDU B 2 F7 F 0.2099(5) 0.2073(5) 0.3450(7) 0.151(6) Uani 0.62 1 d PDU C 1 F8 F 0.1912(12) 0.2825(6) 0.3194(13) 0.152(7) Uani 0.62 1 d PDU C 1 F9 F 0.1345(6) 0.2312(5) 0.2283(7) 0.148(6) Uani 0.62 1 d PDU C 1 F7B F 0.1996(14) 0.2664(9) 0.3426(15) 0.117(8) Uani 0.38 1 d PDU C 2 F8B F 0.1797(11) 0.1948(4) 0.2919(18) 0.165(10) Uani 0.38 1 d PDU C 2 F9B F 0.1369(10) 0.2580(9) 0.2196(13) 0.161(10) Uani 0.38 1 d PDU C 2 F10 F 0.3445(14) 0.1948(6) 0.0910(10) 0.184(6) Uani 0.47 1 d PDU D 1 F11 F 0.2549(9) 0.2485(12) 0.0464(10) 0.175(10) Uani 0.47 1 d PDU D 1 F12 F 0.3724(17) 0.2708(9) 0.0935(12) 0.181(11) Uani 0.47 1 d PDU D 1 F10B F 0.2727(15) 0.2188(8) 0.0545(10) 0.207(10) Uani 0.53 1 d PDU D 2 F11B F 0.2962(13) 0.2960(5) 0.0671(9) 0.171(5) Uani 0.53 1 d PDU D 2 F12B F 0.3901(8) 0.2466(11) 0.0957(10) 0.175(11) Uani 0.53 1 d PDU D 2 F13 F 0.8244(4) 0.2632(4) 0.5582(4) 0.121(2) Uani 0.79 1 d PDU E 1 F14 F 0.8533(4) 0.2878(3) 0.4665(6) 0.118(3) Uani 0.79 1 d PDU E 1 F15 F 0.8069(7) 0.2165(3) 0.4633(6) 0.105(3) Uani 0.79 1 d PDU E 1 F13B F 0.8386(12) 0.2983(11) 0.534(2) 0.138(11) Uani 0.21 1 d PDU E 2 F14B F 0.8340(18) 0.2733(15) 0.4272(18) 0.133(13) Uani 0.21 1 d PDU E 2 F15B F 0.8084(18) 0.2243(10) 0.499(2) 0.122(15) Uani 0.21 1 d PDU E 2 F16 F 0.5297(9) 0.3888(6) 0.2373(7) 0.126(7) Uani 0.52 1 d PDU F 1 F17 F 0.5867(7) 0.4283(2) 0.3438(6) 0.110(3) Uani 0.52 1 d PDU F 1 F18 F 0.6510(7) 0.4036(5) 0.2793(9) 0.110(5) Uani 0.52 1 d PDU F 1 F16B F 0.5430(9) 0.4027(5) 0.2724(11) 0.113(6) Uani 0.48 1 d PDU F 2 F17B F 0.6108(10) 0.3700(6) 0.2233(8) 0.178(6) Uani 0.48 1 d PDU F 2 F18B F 0.6664(11) 0.4161(7) 0.3235(13) 0.206(11) Uani 0.48 1 d PDU F 2 F19 F 0.6037(7) 0.2342(4) 0.7312(5) 0.148(4) Uani 0.57 1 d PDU G 1 F20 F 0.6431(8) 0.3076(5) 0.7677(6) 0.131(6) Uani 0.57 1 d PDU G 1 F21 F 0.6987(13) 0.2632(8) 0.7169(16) 0.078(4) Uani 0.57 1 d PDU G 1 F19B F 0.5958(6) 0.2696(5) 0.7535(6) 0.080(3) Uani 0.43 1 d PDU G 2 F20B F 0.6709(10) 0.3249(5) 0.7520(7) 0.097(4) Uani 0.43 1 d PDU G 2 F21B F 0.6834(17) 0.2531(9) 0.716(2) 0.110(10) Uani 0.43 1 d PDU G 2 F22 F 0.4516(6) 0.4297(2) 0.4916(7) 0.260(5) Uani 1 1 d DU H 2 F23 F 0.3543(4) 0.3922(3) 0.4685(3) 0.229(5) Uani 1 1 d DU H 2 F24 F 0.4214(3) 0.41366(19) 0.5837(2) 0.177(3) Uani 1 1 d DU H 2 Br1 Br 0.09167(18) 0.31712(11) 1.06157(18) 0.0780(8) Uani 0.20 1 d PD I 1 C1S C 0.0403(5) 0.3170(3) 0.9600(5) 0.145(6) Uani 0.72 1 d PGD I 1 C2S C -0.0413(5) 0.3086(3) 0.9277(6) 0.137(6) Uani 0.72 1 d PGD I 1 H2S H -0.0660 0.3054 0.9622 0.165 Uiso 0.72 1 calc PR I 1 C3S C -0.0868(4) 0.3048(3) 0.8450(6) 0.191(10) Uani 0.72 1 d PGD I 1 H3S H -0.1426 0.2990 0.8230 0.230 Uiso 0.72 1 calc PR I 1 C4S C -0.0508(6) 0.3094(4) 0.7946(5) 0.146(5) Uani 0.72 1 d PGD I 1 H4S H -0.0819 0.3068 0.7381 0.175 Uiso 0.72 1 calc PR I 1 C5S C 0.0309(6) 0.3179(4) 0.8270(6) 0.162(7) Uani 0.72 1 d PGD I 1 H5S H 0.0555 0.3211 0.7925 0.194 Uiso 0.72 1 calc PR I 1 C6S C 0.0764(4) 0.3217(4) 0.9097(6) 0.142(6) Uani 0.72 1 d PGD I 1 H6S H 0.1322 0.3274 0.9317 0.171 Uiso 0.72 1 calc PR I 1 Br1B Br -0.0975(5) 0.2837(3) 0.7662(9) 0.298(8) Uani 0.18 1 d PDU J 2 C1SB C -0.0205(10) 0.2979(5) 0.8564(12) 0.212(10) Uani 0.28 1 d PGDU J 2 C2SB C -0.0258(12) 0.2881(8) 0.9270(14) 0.243(12) Uani 0.28 1 d PGDU J 2 H2SB H -0.0730 0.2740 0.9248 0.291 Uiso 0.28 1 calc PR J 2 C3SB C 0.0379(16) 0.2992(9) 1.0008(12) 0.216(10) Uani 0.28 1 d PGDU J 2 H3SB H 0.0342 0.2926 1.0491 0.259 Uiso 0.28 1 calc PR J 2 C4SB C 0.1069(13) 0.3199(8) 1.0041(14) 0.159(9) Uani 0.28 1 d PGDU J 2 H4SB H 0.1504 0.3275 1.0546 0.191 Uiso 0.28 1 calc PR J 2 C5SB C 0.1123(12) 0.3297(9) 0.9335(16) 0.157(10) Uani 0.28 1 d PGDU J 2 H5SB H 0.1595 0.3439 0.9357 0.188 Uiso 0.28 1 calc PR J 2 C6SB C 0.0486(12) 0.3186(8) 0.8597(14) 0.169(11) Uani 0.28 1 d PGDU J 2 H6SB H 0.0523 0.3253 0.8114 0.203 Uiso 0.28 1 calc PR J 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 Zn1 0.0350(2) 0.0381(2) 0.0350(2) 0.00867(18) 0.01396(18) -0.00114(18) P1 0.0310(5) 0.0301(5) 0.0366(5) 0.0021(4) 0.0119(4) -0.0043(4) P2 0.0340(5) 0.0405(5) 0.0342(5) 0.0009(4) 0.0172(4) -0.0027(4) O1 0.0322(12) 0.0356(13) 0.0279(12) 0.0046(10) 0.0122(10) -0.0048(10) N1 0.0330(16) 0.0339(16) 0.0353(16) 0.0018(13) 0.0137(13) -0.0043(13) O3 0.087(2) 0.0431(16) 0.0436(16) 0.0015(13) 0.0341(16) -0.0069(15) N2 0.0356(17) 0.065(2) 0.0321(16) 0.0112(15) 0.0139(14) -0.0050(15) C1 0.041(2) 0.0265(18) 0.0302(18) 0.0030(14) 0.0097(15) -0.0041(15) C2 0.0340(19) 0.0329(19) 0.0349(19) 0.0039(15) 0.0070(15) -0.0062(15) C3 0.041(2) 0.050(2) 0.046(2) 0.0112(19) 0.0062(18) -0.0022(19) C4 0.050(3) 0.057(3) 0.039(2) 0.014(2) -0.0005(19) -0.001(2) C5 0.065(3) 0.043(2) 0.031(2) 0.0091(17) 0.0114(19) 0.000(2) C6 0.055(2) 0.0282(18) 0.0289(18) 0.0021(14) 0.0147(17) -0.0045(16) C7 0.055(2) 0.0263(18) 0.0332(19) 0.0028(14) 0.0226(17) -0.0012(16) C8 0.070(3) 0.035(2) 0.042(2) 0.0087(17) 0.035(2) 0.0058(19) C9 0.070(3) 0.047(2) 0.058(3) 0.012(2) 0.049(2) 0.006(2) C10 0.053(2) 0.046(2) 0.054(2) 0.0103(19) 0.037(2) 0.0075(18) C11 0.042(2) 0.0332(19) 0.0373(19) 0.0033(15) 0.0234(17) -0.0008(16) C12 0.047(2) 0.0254(17) 0.0329(18) 0.0009(14) 0.0233(16) -0.0028(15) C13 0.0341(19) 0.035(2) 0.043(2) -0.0003(16) 0.0118(16) -0.0003(15) C14 0.043(2) 0.045(2) 0.048(2) 0.0053(18) 0.0216(19) 0.0013(18) C15 0.046(2) 0.067(3) 0.054(3) 0.005(2) 0.024(2) 0.006(2) C16 0.040(2) 0.071(3) 0.064(3) -0.010(2) 0.013(2) 0.014(2) C17 0.069(3) 0.039(3) 0.147(6) -0.017(3) 0.046(4) 0.004(2) C18 0.051(3) 0.039(3) 0.138(5) -0.010(3) 0.043(3) -0.005(2) C19 0.0337(19) 0.0338(19) 0.044(2) 0.0002(16) 0.0173(16) -0.0045(15) C20 0.059(3) 0.040(2) 0.052(2) 0.0031(18) 0.030(2) -0.0055(19) C21 0.072(3) 0.043(2) 0.081(3) 0.011(2) 0.049(3) -0.007(2) C22 0.053(3) 0.039(2) 0.097(4) -0.007(3) 0.031(3) -0.017(2) C23 0.054(3) 0.045(3) 0.070(3) -0.013(2) 0.006(2) -0.011(2) C24 0.040(2) 0.040(2) 0.051(2) -0.0014(18) 0.0115(19) -0.0022(17) C25 0.036(2) 0.047(2) 0.039(2) -0.0041(17) 0.0174(16) -0.0077(17) C26 0.085(3) 0.052(3) 0.061(3) -0.018(2) 0.041(3) -0.027(2) C27 0.111(5) 0.072(4) 0.098(4) -0.041(3) 0.061(4) -0.049(3) C28 0.100(5) 0.098(5) 0.092(4) -0.057(4) 0.055(4) -0.037(4) C29 0.079(4) 0.109(5) 0.058(3) -0.027(3) 0.042(3) -0.022(3) C30 0.056(3) 0.073(3) 0.050(2) -0.009(2) 0.030(2) -0.013(2) C31 0.049(2) 0.047(2) 0.046(2) -0.0091(18) 0.030(2) -0.0093(18) C32 0.072(3) 0.051(3) 0.064(3) -0.007(2) 0.045(3) -0.008(2) C33 0.133(6) 0.054(3) 0.094(4) -0.024(3) 0.079(4) -0.028(3) C34 0.123(5) 0.088(5) 0.066(4) -0.035(3) 0.049(4) -0.058(4) C35 0.081(4) 0.099(5) 0.057(3) -0.023(3) 0.024(3) -0.042(3) C36 0.051(3) 0.070(3) 0.054(3) -0.011(2) 0.024(2) -0.016(2) C37 0.051(2) 0.045(2) 0.0310(19) 0.0069(17) 0.0162(17) 0.0087(18) C38 0.062(3) 0.071(3) 0.055(3) 0.006(2) 0.034(2) 0.020(2) C39 0.077(4) 0.120(5) 0.060(3) 0.016(3) 0.037(3) 0.053(4) C40 0.139(6) 0.085(5) 0.060(3) 0.016(3) 0.035(4) 0.077(5) C41 0.127(6) 0.053(3) 0.079(4) 0.008(3) 0.028(4) 0.035(4) C42 0.079(3) 0.042(3) 0.057(3) 0.011(2) 0.017(2) 0.014(2) C43 0.028(2) 0.143(5) 0.038(2) 0.020(3) 0.0102(19) -0.012(3) C44 0.045(3) 0.205(8) 0.069(4) 0.078(5) 0.018(3) 0.013(4) C45 0.064(4) 0.351(17) 0.069(5) 0.090(8) 0.028(4) 0.029(7) C46 0.049(4) 0.48(2) 0.055(5) 0.081(9) 0.015(4) -0.002(8) C47 0.051(4) 0.366(16) 0.051(4) -0.046(6) 0.026(3) -0.044(6) C48 0.055(3) 0.188(7) 0.040(3) -0.030(4) 0.026(2) -0.035(4) C49A 0.233(9) 0.044(3) 0.076(4) -0.011(3) 0.091(5) -0.019(4) C50A 0.067(7) 0.061(6) 0.063(6) -0.005(5) 0.034(5) -0.006(5) C49B 0.233(9) 0.044(3) 0.076(4) -0.011(3) 0.091(5) -0.019(4) C50B 0.079(7) 0.055(6) 0.065(6) -0.005(5) 0.035(6) 0.010(5) C51 0.105(4) 0.034(2) 0.072(3) 0.014(2) 0.055(3) 0.010(2) C52 0.321(13) 0.063(4) 0.092(5) 0.040(4) 0.116(7) 0.043(6) C53 0.0257(17) 0.0302(18) 0.0401(19) 0.0028(15) 0.0132(15) 0.0002(14) C54 0.0296(18) 0.0344(19) 0.045(2) 0.0039(16) 0.0177(16) 0.0008(15) C55 0.0293(18) 0.035(2) 0.042(2) 0.0065(16) 0.0113(16) -0.0028(15) C56 0.0357(19) 0.0273(18) 0.048(2) 0.0049(16) 0.0121(17) 0.0000(15) C57 0.0300(18) 0.0297(19) 0.045(2) -0.0012(16) 0.0123(16) -0.0004(14) C58 0.0325(18) 0.0303(18) 0.040(2) 0.0007(15) 0.0173(16) -0.0012(14) C59 0.049(2) 0.042(2) 0.061(3) 0.009(2) 0.027(2) -0.0022(19) C60 0.060(3) 0.035(2) 0.064(3) 0.001(2) 0.034(2) 0.009(2) C61 0.037(2) 0.0243(18) 0.051(2) 0.0026(16) 0.0151(17) 0.0062(15) C62 0.043(2) 0.036(2) 0.067(3) 0.0131(19) 0.021(2) 0.0084(17) C63 0.039(2) 0.039(2) 0.093(4) 0.010(2) 0.022(2) 0.0063(18) C64 0.043(3) 0.060(3) 0.079(4) -0.014(3) -0.001(2) 0.007(2) C65 0.055(3) 0.083(4) 0.058(3) -0.022(3) 0.005(2) 0.012(3) C66 0.041(2) 0.058(3) 0.052(3) -0.011(2) 0.014(2) 0.0081(19) C67 0.053(4) 0.083(5) 0.138(7) 0.024(5) 0.040(4) 0.016(3) C68 0.080(6) 0.225(13) 0.047(4) -0.036(6) 0.001(4) 0.016(7) C69 0.045(2) 0.0264(17) 0.0262(17) -0.0038(13) 0.0189(16) -0.0021(15) C70 0.043(2) 0.0307(19) 0.0373(19) -0.0014(15) 0.0185(17) -0.0042(16) C71 0.050(2) 0.047(2) 0.052(2) -0.0091(19) 0.027(2) -0.0111(19) C72 0.066(3) 0.058(3) 0.064(3) 0.000(2) 0.039(3) -0.021(2) C73 0.076(3) 0.047(2) 0.048(2) 0.011(2) 0.031(2) -0.008(2) C74 0.055(2) 0.039(2) 0.037(2) 0.0064(16) 0.0225(18) 0.0008(18) C75 0.043(3) 0.078(4) 0.105(5) -0.011(4) 0.034(3) -0.015(3) C76 0.110(6) 0.088(5) 0.093(5) 0.044(4) 0.033(5) -0.022(5) C77 0.046(2) 0.0344(19) 0.046(2) 0.0064(16) 0.0298(18) 0.0066(16) C78 0.050(2) 0.039(2) 0.048(2) 0.0081(17) 0.0338(19) 0.0087(17) C79 0.058(3) 0.062(3) 0.042(2) 0.0060(19) 0.032(2) 0.010(2) C80 0.088(4) 0.073(3) 0.056(3) -0.008(2) 0.044(3) 0.022(3) C81 0.086(4) 0.065(3) 0.060(3) -0.002(2) 0.035(3) 0.035(3) C82 0.063(3) 0.049(2) 0.047(2) 0.0060(19) 0.028(2) 0.022(2) C83 0.080(4) 0.103(5) 0.042(3) 0.007(3) 0.036(3) 0.015(3) C84 0.150(7) 0.075(5) 0.104(5) -0.004(4) 0.053(5) 0.058(5) O2 0.0639(18) 0.0366(15) 0.0496(16) 0.0100(13) 0.0275(14) 0.0078(13) O4 0.254(6) 0.043(2) 0.101(3) 0.021(2) 0.115(4) 0.023(3) B1 0.034(2) 0.029(2) 0.040(2) 0.0043(17) 0.0191(18) 0.0041(16) F1 0.139(3) 0.0604(18) 0.154(3) 0.0352(19) 0.122(3) 0.0213(18) F2 0.0811(19) 0.0739(18) 0.0557(16) 0.0234(14) 0.0272(14) 0.0031(15) F3 0.081(2) 0.078(2) 0.0793(19) 0.0061(15) 0.0319(16) -0.0432(16) F4 0.061(3) 0.104(4) 0.131(4) -0.044(4) 0.062(3) 0.000(2) F5 0.112(5) 0.083(3) 0.050(2) -0.005(2) 0.036(3) 0.031(3) F6 0.182(8) 0.033(2) 0.140(7) 0.012(3) 0.117(7) 0.030(4) F4B 0.16(2) 0.038(8) 0.121(15) -0.001(11) 0.108(16) 0.007(12) F5B 0.066(11) 0.112(17) 0.13(2) -0.083(16) 0.037(12) -0.013(13) F6B 0.127(19) 0.11(2) 0.067(11) 0.047(13) 0.055(13) 0.113(17) F7 0.062(5) 0.211(14) 0.190(9) 0.113(9) 0.067(6) 0.023(6) F8 0.107(8) 0.178(13) 0.213(15) 0.021(10) 0.111(9) 0.032(8) F9 0.038(4) 0.217(15) 0.149(8) 0.037(8) 0.007(4) -0.037(7) F7B 0.065(10) 0.132(15) 0.184(18) -0.038(16) 0.081(11) -0.028(11) F8B 0.112(13) 0.040(5) 0.40(3) 0.014(12) 0.161(17) 0.000(7) F9B 0.057(9) 0.24(2) 0.197(17) 0.090(16) 0.069(10) 0.080(12) F10 0.199(14) 0.238(16) 0.135(12) -0.105(12) 0.093(11) -0.008(14) F11 0.083(7) 0.32(3) 0.064(7) 0.016(15) -0.015(5) 0.042(13) F12 0.25(3) 0.22(2) 0.055(7) 0.023(10) 0.062(15) -0.01(2) F10B 0.23(2) 0.234(19) 0.071(9) -0.066(11) -0.015(11) -0.023(15) F11B 0.213(14) 0.212(13) 0.094(8) 0.049(8) 0.074(9) 0.057(12) F12B 0.098(8) 0.37(3) 0.051(5) -0.022(12) 0.026(5) 0.073(13) F13 0.071(4) 0.169(7) 0.086(4) 0.001(5) 0.003(3) 0.039(4) F14 0.053(3) 0.109(5) 0.191(9) 0.018(6) 0.054(5) -0.025(3) F15 0.063(3) 0.082(4) 0.170(8) -0.014(5) 0.051(5) 0.009(3) F13B 0.040(10) 0.14(2) 0.17(3) -0.059(18) -0.012(13) -0.011(12) F14B 0.08(2) 0.22(3) 0.13(2) 0.04(2) 0.077(18) 0.069(19) F15B 0.035(10) 0.10(2) 0.20(3) 0.10(2) 0.031(18) 0.007(15) F16 0.145(10) 0.123(12) 0.083(7) 0.062(6) 0.028(6) -0.003(8) F17 0.203(10) 0.039(3) 0.117(6) 0.023(4) 0.097(6) 0.025(4) F18 0.133(9) 0.090(8) 0.175(13) 0.069(8) 0.129(10) 0.015(7) F16B 0.141(12) 0.078(9) 0.193(17) 0.091(11) 0.139(13) 0.067(9) F17B 0.243(15) 0.205(13) 0.151(10) 0.137(10) 0.145(11) 0.136(12) F18B 0.194(14) 0.111(12) 0.26(2) 0.093(13) 0.059(14) -0.064(10) F19 0.168(9) 0.156(8) 0.076(6) 0.063(6) 0.017(5) -0.060(8) F20 0.142(11) 0.191(15) 0.049(5) -0.030(8) 0.032(5) 0.076(11) F21 0.070(5) 0.111(7) 0.048(6) 0.014(5) 0.021(4) 0.026(5) F19B 0.076(5) 0.120(8) 0.048(5) 0.034(5) 0.033(4) -0.001(6) F20B 0.134(11) 0.088(6) 0.041(6) -0.005(4) 0.016(5) -0.009(6) F21B 0.13(2) 0.136(17) 0.039(7) -0.004(10) 0.017(11) 0.085(15) F22 0.319(11) 0.110(4) 0.427(13) 0.103(6) 0.235(11) 0.143(6) F23 0.233(6) 0.234(7) 0.122(4) -0.044(4) -0.005(4) 0.197(6) F24 0.222(5) 0.177(4) 0.098(3) -0.034(3) 0.042(3) 0.139(4) Br1 0.0762(18) 0.0776(19) 0.0725(17) 0.0034(14) 0.0268(15) 0.0191(15) C1S 0.171(12) 0.055(6) 0.29(2) -0.036(9) 0.182(14) -0.012(7) C2S 0.193(13) 0.059(6) 0.266(16) -0.028(8) 0.197(14) -0.023(7) C3S 0.27(2) 0.176(15) 0.25(2) 0.087(14) 0.22(2) 0.139(15) C4S 0.117(11) 0.160(14) 0.147(12) 0.049(10) 0.049(10) 0.022(10) C5S 0.144(12) 0.183(15) 0.235(17) 0.083(14) 0.154(13) 0.068(11) C6S 0.158(12) 0.072(9) 0.269(19) -0.005(10) 0.160(14) 0.017(8) Br1B 0.109(5) 0.127(6) 0.480(17) 0.058(9) -0.025(8) 0.025(4) C1SB 0.148(16) 0.089(19) 0.369(17) 0.02(2) 0.090(16) 0.031(14) C2SB 0.17(2) 0.15(3) 0.462(19) -0.02(3) 0.194(19) 0.027(19) C3SB 0.23(3) 0.12(2) 0.390(18) -0.04(2) 0.219(19) 0.02(2) C4SB 0.22(2) 0.057(14) 0.27(2) -0.058(17) 0.172(19) 0.005(16) C5SB 0.215(19) 0.044(14) 0.23(2) -0.045(17) 0.113(15) -0.021(17) C6SB 0.179(17) 0.027(13) 0.26(2) 0.029(16) 0.057(15) -0.012(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.904(3) . ? Zn1 N2 1.988(3) . ? Zn1 N1 2.016(3) . ? Zn1 O2 2.131(3) . ? Zn1 O1 2.367(2) . ? P1 N1 1.600(3) . ? P1 C19 1.792(4) . ? P1 C13 1.802(4) . ? P1 C2 1.803(4) . ? P2 N2 1.596(3) . ? P2 C31 1.777(4) . ? P2 C11 1.810(4) . ? P2 C37 1.811(4) . ? O1 C1 1.383(4) . ? O1 C12 1.383(4) . ? N1 C25 1.435(5) . ? O3 C49A 1.341(6) . ? N2 C43 1.471(5) . ? C1 C2 1.390(5) . ? C1 C6 1.397(5) . ? C2 C3 1.407(5) . ? C3 C4 1.390(6) . ? C3 H3 0.9500 . ? C4 C5 1.377(6) . ? C4 H4 0.9500 . ? C5 C6 1.389(5) . ? C5 H5 0.9500 . ? C6 C7 1.441(5) . ? C7 C12 1.398(5) . ? C7 C8 1.400(5) . ? C8 C9 1.367(6) . ? C8 H8 0.9500 . ? C9 C10 1.390(6) . ? C9 H9 0.9500 . ? C10 C11 1.399(5) . ? C10 H10 0.9500 . ? C11 C12 1.381(5) . ? C13 C14 1.384(5) . ? C13 C18 1.388(6) . ? C14 C15 1.373(6) . ? C14 H14 0.9500 . ? C15 C16 1.353(6) . ? C15 H15 0.9500 . ? C16 C17 1.364(7) . ? C16 H16 0.9500 . ? C17 C18 1.379(7) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.388(5) . ? C19 C20 1.401(5) . ? C20 C21 1.390(6) . ? C20 H20 0.9500 . ? C21 C22 1.378(7) . ? C21 H21 0.9500 . ? C22 C23 1.368(7) . ? C22 H22 0.9500 . ? C23 C24 1.378(6) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.378(6) . ? C25 C26 1.394(6) . ? C26 C27 1.377(6) . ? C26 H26 0.9500 . ? C27 C28 1.382(8) . ? C27 H27 0.9500 . ? C28 C29 1.358(8) . ? C28 H28 0.9500 . ? C29 C30 1.384(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.371(6) . ? C31 C36 1.401(6) . ? C32 C33 1.395(7) . ? C32 H32 0.9500 . ? C33 C34 1.354(9) . ? C33 H33 0.9500 . ? C34 C35 1.372(9) . ? C34 H34 0.9500 . ? C35 C36 1.384(7) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.381(6) . ? C37 C38 1.392(6) . ? C38 C39 1.401(7) . ? C38 H38 0.9500 . ? C39 C40 1.385(10) . ? C39 H39 0.9500 . ? C40 C41 1.348(10) . ? C40 H40 0.9500 . ? C41 C42 1.357(8) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.360(9) . ? C43 C48 1.398(9) . ? C44 C45 1.384(9) . ? C44 H44 0.9500 . ? C45 C46 1.345(19) . ? C45 H45 0.9500 . ? C46 C47 1.386(17) . ? C46 H46 0.9500 . ? C47 C48 1.397(8) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49A C50A 1.293(11) . ? C49A C51 1.528(7) . ? C49A H49A 1.0000 . ? C50A H50A 0.9800 . ? C50A H50B 0.9800 . ? C50A H50C 0.9800 . ? C50B H50D 0.9800 . ? C50B H50E 0.9800 . ? C50B H50F 0.9800 . ? C51 O2 1.210(5) . ? C51 O4 1.313(5) . ? C52 O4 1.451(7) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C58 1.391(5) . ? C53 C54 1.405(5) . ? C53 B1 1.638(5) . ? C54 C55 1.390(5) . ? C54 H54 0.9500 . ? C55 C56 1.375(5) . ? C55 C59 1.493(5) . ? C56 C57 1.373(5) . ? C56 H56 0.9500 . ? C57 C58 1.386(5) . ? C57 C60 1.492(5) . ? C58 H58 0.9500 . ? C59 F1 1.306(5) . ? C59 F2 1.322(5) . ? C59 F3 1.350(5) . ? C60 F6B 1.253(16) . ? C60 F5 1.294(6) . ? C60 F6 1.312(7) . ? C60 F4 1.336(6) . ? C60 F4B 1.352(16) . ? C60 F5B 1.389(17) . ? C61 C66 1.387(6) . ? C61 C62 1.388(6) . ? C61 B1 1.635(5) . ? C62 C63 1.379(6) . ? C62 H62 0.9500 . ? C63 C64 1.375(7) . ? C63 C67 1.492(8) . ? C64 C65 1.376(8) . ? C64 H64 0.9500 . ? C65 C66 1.395(6) . ? C65 C68 1.502(10) . ? C66 H66 0.9500 . ? C67 F9 1.239(11) . ? C67 F8B 1.275(14) . ? C67 F7B 1.28(3) . ? C67 F7 1.330(11) . ? C67 F8 1.370(19) . ? C67 F9B 1.378(19) . ? C68 F12 1.17(2) . ? C68 F10B 1.240(18) . ? C68 F12B 1.26(2) . ? C68 F11 1.285(16) . ? C68 F10 1.453(19) . ? C68 F11B 1.518(18) . ? C69 C70 1.389(5) . ? C69 C74 1.402(5) . ? C69 B1 1.642(5) . ? C70 C71 1.389(5) . ? C70 H70 0.9500 . ? C71 C72 1.385(6) . ? C71 C75 1.493(7) . ? C72 C73 1.367(7) . ? C72 H72 0.9500 . ? C73 C74 1.386(6) . ? C73 C76 1.514(7) . ? C74 H74 0.9500 . ? C75 F15B 1.14(2) . ? C75 F14 1.285(8) . ? C75 F13B 1.32(2) . ? C75 F13 1.346(8) . ? C75 F15 1.354(10) . ? C75 F14B 1.39(3) . ? C76 F16B 1.093(13) . ? C76 F18 1.175(12) . ? C76 F18B 1.292(16) . ? C76 F16 1.349(16) . ? C76 F17 1.490(13) . ? C76 F17B 1.556(15) . ? C77 C78 1.393(5) . ? C77 C82 1.403(5) . ? C77 B1 1.635(5) . ? C78 C79 1.384(6) . ? C78 H78 0.9500 . ? C79 C80 1.388(6) . ? C79 C83 1.486(6) . ? C80 C81 1.372(7) . ? C80 H80 0.9500 . ? C81 C82 1.389(6) . ? C81 C84 1.489(7) . ? C82 H82 0.9500 . ? C83 F20 1.216(11) . ? C83 F21B 1.22(2) . ? C83 F19B 1.247(9) . ? C83 F21 1.339(18) . ? C83 F19 1.448(10) . ? C83 F20B 1.454(15) . ? C84 F24 1.262(8) . ? C84 F23 1.271(10) . ? C84 F22 1.315(11) . ? Br1 C1S 1.694(9) . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C2S C3S 1.3900 . ? C2S H2S 0.9500 . ? C3S C4S 1.3900 . ? C3S H3S 0.9500 . ? C4S C5S 1.3900 . ? C4S H4S 0.9500 . ? C5S C6S 1.3900 . ? C5S H5S 0.9500 . ? C6S H6S 0.9500 . ? Br1B C1SB 1.697(18) . ? C1SB C2SB 1.3900 . ? C1SB C6SB 1.3900 . ? C2SB C3SB 1.3900 . ? C2SB H2SB 0.9500 . ? C3SB C4SB 1.3900 . ? C3SB H3SB 0.9500 . ? C4SB C5SB 1.3900 . ? C4SB H4SB 0.9500 . ? C5SB C6SB 1.3900 . ? C5SB H5SB 0.9500 . ? C6SB H6SB 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 O3 Zn1 N2 117.66(14) . . ? O3 Zn1 N1 122.25(13) . . ? N2 Zn1 N1 116.18(13) . . ? O3 Zn1 O2 83.29(11) . . ? N2 Zn1 O2 103.42(12) . . ? N1 Zn1 O2 103.23(11) . . ? O3 Zn1 O1 85.14(10) . . ? N2 Zn1 O1 83.69(10) . . ? N1 Zn1 O1 81.39(10) . . ? O2 Zn1 O1 168.28(10) . . ? N1 P1 C19 108.02(16) . . ? N1 P1 C13 114.40(17) . . ? C19 P1 C13 106.37(17) . . ? N1 P1 C2 113.49(16) . . ? C19 P1 C2 108.22(17) . . ? C13 P1 C2 105.98(17) . . ? N2 P2 C31 110.09(18) . . ? N2 P2 C11 111.31(16) . . ? C31 P2 C11 108.76(18) . . ? N2 P2 C37 115.52(19) . . ? C31 P2 C37 106.21(19) . . ? C11 P2 C37 104.58(16) . . ? C1 O1 C12 106.5(3) . . ? C1 O1 Zn1 122.29(19) . . ? C12 O1 Zn1 125.0(2) . . ? C25 N1 P1 120.7(2) . . ? C25 N1 Zn1 117.9(2) . . ? P1 N1 Zn1 115.08(16) . . ? C49A O3 Zn1 115.3(3) . . ? C43 N2 P2 115.6(3) . . ? C43 N2 Zn1 112.1(2) . . ? P2 N2 Zn1 131.21(19) . . ? O1 C1 C2 124.6(3) . . ? O1 C1 C6 110.9(3) . . ? C2 C1 C6 124.5(3) . . ? C1 C2 C3 114.8(3) . . ? C1 C2 P1 122.6(3) . . ? C3 C2 P1 122.6(3) . . ? C4 C3 C2 121.8(4) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C5 C4 C3 121.4(4) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 C6 118.9(4) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C5 C6 C1 118.6(4) . . ? C5 C6 C7 135.6(4) . . ? C1 C6 C7 105.7(3) . . ? C12 C7 C8 118.3(4) . . ? C12 C7 C6 106.5(3) . . ? C8 C7 C6 135.3(3) . . ? C9 C8 C7 118.2(4) . . ? C9 C8 H8 120.9 . . ? C7 C8 H8 120.9 . . ? C8 C9 C10 122.1(4) . . ? C8 C9 H9 118.9 . . ? C10 C9 H9 118.9 . . ? C9 C10 C11 121.8(4) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C12 C11 C10 114.7(3) . . ? C12 C11 P2 126.5(3) . . ? C10 C11 P2 118.8(3) . . ? C11 C12 O1 124.7(3) . . ? C11 C12 C7 124.9(3) . . ? O1 C12 C7 110.4(3) . . ? C14 C13 C18 118.1(4) . . ? C14 C13 P1 121.8(3) . . ? C18 C13 P1 120.1(3) . . ? C15 C14 C13 120.8(4) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C16 C15 C14 120.9(4) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 119.2(4) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C16 C17 C18 121.3(5) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C17 C18 C13 119.7(5) . . ? C17 C18 H18 120.1 . . ? C13 C18 H18 120.1 . . ? C24 C19 C20 119.6(4) . . ? C24 C19 P1 122.5(3) . . ? C20 C19 P1 117.7(3) . . ? C21 C20 C19 119.2(4) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C22 C21 C20 120.3(4) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C21 120.4(4) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 120.4(4) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C19 120.1(4) . . ? C23 C24 H24 119.9 . . ? C19 C24 H24 119.9 . . ? C30 C25 C26 118.6(4) . . ? C30 C25 N1 119.6(4) . . ? C26 C25 N1 121.8(3) . . ? C27 C26 C25 120.2(5) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 120.2(5) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 120.0(5) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.2(5) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C25 C30 C29 120.8(5) . . ? C25 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C32 C31 C36 120.3(4) . . ? C32 C31 P2 119.5(3) . . ? C36 C31 P2 119.2(3) . . ? C31 C32 C33 119.7(5) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C34 C33 C32 119.4(6) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C33 C34 C35 122.1(5) . . ? C33 C34 H34 119.0 . . ? C35 C34 H34 119.0 . . ? C34 C35 C36 119.3(6) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? C35 C36 C31 119.2(5) . . ? C35 C36 H36 120.4 . . ? C31 C36 H36 120.4 . . ? C42 C37 C38 119.5(4) . . ? C42 C37 P2 117.9(3) . . ? C38 C37 P2 122.4(3) . . ? C37 C38 C39 119.0(5) . . ? C37 C38 H38 120.5 . . ? C39 C38 H38 120.5 . . ? C40 C39 C38 119.8(6) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C41 C40 C39 119.6(5) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C40 C41 C42 122.0(6) . . ? C40 C41 H41 119.0 . . ? C42 C41 H41 119.0 . . ? C41 C42 C37 120.1(6) . . ? C41 C42 H42 120.0 . . ? C37 C42 H42 120.0 . . ? C44 C43 C48 121.3(5) . . ? C44 C43 N2 120.1(6) . . ? C48 C43 N2 118.6(5) . . ? C43 C44 C45 120.2(9) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C46 C45 C44 119.0(11) . . ? C46 C45 H45 120.5 . . ? C44 C45 H45 120.5 . . ? C45 C46 C47 122.6(8) . . ? C45 C46 H46 118.7 . . ? C47 C46 H46 118.7 . . ? C46 C47 C48 118.7(10) . . ? C46 C47 H47 120.6 . . ? C48 C47 H47 120.6 . . ? C47 C48 C43 118.1(8) . . ? C47 C48 H48 120.9 . . ? C43 C48 H48 121.0 . . ? C50A C49A O3 126.5(7) . . ? C50A C49A C51 116.1(6) . . ? O3 C49A C51 111.8(4) . . ? C50A C49A H49A 97.8 . . ? O3 C49A H49A 97.8 . . ? C51 C49A H49A 97.8 . . ? H50D C50B H50E 109.5 . . ? H50D C50B H50F 109.5 . . ? H50E C50B H50F 109.5 . . ? O2 C51 O4 121.7(4) . . ? O2 C51 C49A 122.4(4) . . ? O4 C51 C49A 115.9(4) . . ? O4 C52 H52A 109.5 . . ? O4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C58 C53 C54 115.0(3) . . ? C58 C53 B1 122.6(3) . . ? C54 C53 B1 122.1(3) . . ? C55 C54 C53 122.3(3) . . ? C55 C54 H54 118.8 . . ? C53 C54 H54 118.8 . . ? C56 C55 C54 120.5(3) . . ? C56 C55 C59 117.9(3) . . ? C54 C55 C59 121.5(4) . . ? C57 C56 C55 118.6(3) . . ? C57 C56 H56 120.7 . . ? C55 C56 H56 120.7 . . ? C56 C57 C58 120.6(3) . . ? C56 C57 C60 119.5(3) . . ? C58 C57 C60 119.9(3) . . ? C57 C58 C53 122.9(3) . . ? C57 C58 H58 118.5 . . ? C53 C58 H58 118.5 . . ? F1 C59 F2 107.2(4) . . ? F1 C59 F3 106.7(4) . . ? F2 C59 F3 103.5(3) . . ? F1 C59 C55 114.1(3) . . ? F2 C59 C55 113.0(3) . . ? F3 C59 C55 111.5(4) . . ? F6B C60 F5 126.8(12) . . ? F6B C60 F6 38.2(14) . . ? F5 C60 F6 107.6(5) . . ? F6B C60 F4 69.6(14) . . ? F5 C60 F4 105.2(5) . . ? F6 C60 F4 106.6(5) . . ? F6B C60 F4B 103.1(14) . . ? F5 C60 F4B 61.1(13) . . ? F6 C60 F4B 126.5(8) . . ? F4 C60 F4B 45.0(12) . . ? F6B C60 F5B 102.2(14) . . ? F5 C60 F5B 40.4(13) . . ? F6 C60 F5B 70.6(13) . . ? F4 C60 F5B 131.4(11) . . ? F4B C60 F5B 96.1(13) . . ? F6B C60 C57 118.2(11) . . ? F5 C60 C57 113.0(4) . . ? F6 C60 C57 113.3(5) . . ? F4 C60 C57 110.5(4) . . ? F4B C60 C57 119.0(7) . . ? F5B C60 C57 114.8(9) . . ? C66 C61 C62 116.0(4) . . ? C66 C61 B1 123.1(3) . . ? C62 C61 B1 120.5(4) . . ? C63 C62 C61 122.7(4) . . ? C63 C62 H62 118.7 . . ? C61 C62 H62 118.7 . . ? C64 C63 C62 120.2(4) . . ? C64 C63 C67 119.9(5) . . ? C62 C63 C67 119.9(6) . . ? C63 C64 C65 119.0(4) . . ? C63 C64 H64 120.5 . . ? C65 C64 H64 120.5 . . ? C64 C65 C66 120.1(5) . . ? C64 C65 C68 120.7(5) . . ? C66 C65 C68 119.2(6) . . ? C61 C66 C65 122.0(4) . . ? C61 C66 H66 119.0 . . ? C65 C66 H66 119.0 . . ? F9 C67 F8B 72.2(12) . . ? F9 C67 F7B 116.6(15) . . ? F8B C67 F7B 111.9(17) . . ? F9 C67 F7 109.1(9) . . ? F8B C67 F7 42.9(12) . . ? F7B C67 F7 76.2(16) . . ? F9 C67 F8 105.5(11) . . ? F8B C67 F8 132.5(14) . . ? F7B C67 F8 25.1(18) . . ? F7 C67 F8 101.2(11) . . ? F9 C67 F9B 32.7(11) . . ? F8B C67 F9B 104.8(13) . . ? F7B C67 F9B 101.8(14) . . ? F7 C67 F9B 136.9(10) . . ? F8 C67 F9B 81.8(15) . . ? F9 C67 C63 118.9(9) . . ? F8B C67 C63 113.9(9) . . ? F7B C67 C63 115.6(12) . . ? F7 C67 C63 112.2(6) . . ? F8 C67 C63 108.3(10) . . ? F9B C67 C63 107.3(9) . . ? F12 C68 F10B 130.5(17) . . ? F12 C68 F12B 34.7(15) . . ? F10B C68 F12B 116.4(15) . . ? F12 C68 F11 114.3(17) . . ? F10B C68 F11 39.7(12) . . ? F12B C68 F11 127.5(15) . . ? F12 C68 F10 107.4(16) . . ? F10B C68 F10 60.6(12) . . ? F12B C68 F10 73.4(13) . . ? F11 C68 F10 99.5(14) . . ? F12 C68 C65 116.0(13) . . ? F10B C68 C65 113.4(15) . . ? F12B C68 C65 118.4(9) . . ? F11 C68 C65 113.9(12) . . ? F10 C68 C65 103.5(11) . . ? F12 C68 F11B 64.1(18) . . ? F10B C68 F11B 100.6(11) . . ? F12B C68 F11B 97.0(15) . . ? F11 C68 F11B 62.3(11) . . ? F10 C68 F11B 148.7(9) . . ? C65 C68 F11B 107.2(8) . . ? C70 C69 C74 115.8(3) . . ? C70 C69 B1 122.3(3) . . ? C74 C69 B1 121.2(3) . . ? C71 C70 C69 122.5(3) . . ? C71 C70 H70 118.8 . . ? C69 C70 H70 118.8 . . ? C72 C71 C70 120.1(4) . . ? C72 C71 C75 120.3(4) . . ? C70 C71 C75 119.6(4) . . ? C73 C72 C71 118.8(4) . . ? C73 C72 H72 120.6 . . ? C71 C72 H72 120.6 . . ? C72 C73 C74 121.0(4) . . ? C72 C73 C76 119.8(5) . . ? C74 C73 C76 119.2(5) . . ? C73 C74 C69 121.8(4) . . ? C73 C74 H74 119.1 . . ? C69 C74 H74 119.1 . . ? F15B C75 F14 121.2(17) . . ? F15B C75 F13B 117(2) . . ? F14 C75 F13B 66.3(16) . . ? F15B C75 F13 71(2) . . ? F14 C75 F13 107.4(6) . . ? F13B C75 F13 50.5(17) . . ? F15B C75 F15 30(2) . . ? F14 C75 F15 106.1(7) . . ? F13B C75 F15 139.1(14) . . ? F13 C75 F15 100.7(7) . . ? F15B C75 F14B 110(2) . . ? F14 C75 F14B 32.9(14) . . ? F13B C75 F14B 98.9(16) . . ? F13 C75 F14B 136.9(14) . . ? F15 C75 F14B 84.4(18) . . ? F15B C75 C71 117.2(16) . . ? F14 C75 C71 116.5(7) . . ? F13B C75 C71 106.6(11) . . ? F13 C75 C71 112.7(5) . . ? F15 C75 C71 112.0(6) . . ? F14B C75 C71 104.4(14) . . ? F16B C76 F18 121.0(10) . . ? F16B C76 F18B 123.5(14) . . ? F18 C76 F18B 38.2(11) . . ? F16B C76 F16 30.9(11) . . ? F18 C76 F16 111.4(10) . . ? F18B C76 F16 136.2(12) . . ? F16B C76 F17 63.1(14) . . ? F18 C76 F17 107.7(9) . . ? F18B C76 F17 76.7(12) . . ? F16 C76 F17 93.9(10) . . ? F16B C76 C73 119.1(9) . . ? F18 C76 C73 118.6(10) . . ? F18B C76 C73 110.3(10) . . ? F16 C76 C73 113.2(9) . . ? F17 C76 C73 108.9(6) . . ? F16B C76 F17B 101.6(11) . . ? F18 C76 F17B 56.5(9) . . ? F18B C76 F17B 94.3(12) . . ? F16 C76 F17B 73.0(9) . . ? F17 C76 F17B 150.4(7) . . ? C73 C76 F17B 100.7(8) . . ? C78 C77 C82 115.5(3) . . ? C78 C77 B1 122.0(3) . . ? C82 C77 B1 121.8(3) . . ? C79 C78 C77 122.5(4) . . ? C79 C78 H78 118.7 . . ? C77 C78 H78 118.7 . . ? C78 C79 C80 120.8(4) . . ? C78 C79 C83 120.1(4) . . ? C80 C79 C83 119.1(4) . . ? C81 C80 C79 118.0(4) . . ? C81 C80 H80 121.0 . . ? C79 C80 H80 121.0 . . ? C80 C81 C82 121.2(4) . . ? C80 C81 C84 119.9(5) . . ? C82 C81 C84 118.9(5) . . ? C81 C82 C77 122.1(4) . . ? C81 C82 H82 119.0 . . ? C77 C82 H82 119.0 . . ? F20 C83 F21B 117.1(16) . . ? F20 C83 F19B 64.1(7) . . ? F21B C83 F19B 116.7(16) . . ? F20 C83 F21 108.8(12) . . ? F21B C83 F21 16.9(19) . . ? F19B C83 F21 128.3(12) . . ? F20 C83 F19 105.5(8) . . ? F21B C83 F19 79.6(15) . . ? F19B C83 F19 46.6(6) . . ? F21 C83 F19 96.0(10) . . ? F20 C83 F20B 35.5(7) . . ? F21B C83 F20B 103.5(14) . . ? F19B C83 F20B 99.6(8) . . ? F21 C83 F20B 88.6(12) . . ? F19 C83 F20B 138.1(7) . . ? F20 C83 C79 121.1(8) . . ? F21B C83 C79 115.4(15) . . ? F19B C83 C79 112.1(6) . . ? F21 C83 C79 113.7(12) . . ? F19 C83 C79 108.4(6) . . ? F20B C83 C79 107.5(7) . . ? F24 C84 F23 106.2(7) . . ? F24 C84 F22 107.9(8) . . ? F23 C84 F22 98.7(8) . . ? F24 C84 C81 115.7(6) . . ? F23 C84 C81 115.7(7) . . ? F22 C84 C81 111.0(7) . . ? C51 O2 Zn1 107.0(3) . . ? C51 O4 C52 116.0(4) . . ? C77 B1 C61 112.5(3) . . ? C77 B1 C53 113.4(3) . . ? C61 B1 C53 104.2(3) . . ? C77 B1 C69 101.5(3) . . ? C61 B1 C69 113.3(3) . . ? C53 B1 C69 112.3(3) . . ? C2S C1S C6S 120.0 . . ? C2S C1S Br1 116.5(5) . . ? C6S C1S Br1 123.4(5) . . ? C1S C2S C3S 120.0 . . ? C1S C2S H2S 120.0 . . ? C3S C2S H2S 120.0 . . ? C2S C3S C4S 120.0 . . ? C2S C3S H3S 120.0 . . ? C4S C3S H3S 120.0 . . ? C5S C4S C3S 120.0 . . ? C5S C4S H4S 120.0 . . ? C3S C4S H4S 120.0 . . ? C4S C5S C6S 120.0 . . ? C4S C5S H5S 120.0 . . ? C6S C5S H5S 120.0 . . ? C5S C6S C1S 120.0 . . ? C5S C6S H6S 120.0 . . ? C1S C6S H6S 120.0 . . ? C2SB C1SB C6SB 120.0 . . ? C2SB C1SB Br1B 120.2(8) . . ? C6SB C1SB Br1B 119.8(8) . . ? C1SB C2SB C3SB 120.0 . . ? C1SB C2SB H2SB 120.0 . . ? C3SB C2SB H2SB 120.0 . . ? C2SB C3SB C4SB 120.0 . . ? C2SB C3SB H3SB 120.0 . . ? C4SB C3SB H3SB 120.0 . . ? C5SB C4SB C3SB 120.0 . . ? C5SB C4SB H4SB 120.0 . . ? C3SB C4SB H4SB 120.0 . . ? C4SB C5SB C6SB 120.0 . . ? C4SB C5SB H5SB 120.0 . . ? C6SB C5SB H5SB 120.0 . . ? C5SB C6SB C1SB 120.0 . . ? C5SB C6SB H6SB 120.0 . . ? C1SB C6SB H6SB 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Zn1 O1 C1 70.7(3) . . . . ? N2 Zn1 O1 C1 -170.7(3) . . . . ? N1 Zn1 O1 C1 -53.0(2) . . . . ? O2 Zn1 O1 C1 61.2(6) . . . . ? O3 Zn1 O1 C12 -77.8(2) . . . . ? N2 Zn1 O1 C12 40.8(2) . . . . ? N1 Zn1 O1 C12 158.6(2) . . . . ? O2 Zn1 O1 C12 -87.3(5) . . . . ? C19 P1 N1 C25 -148.0(3) . . . . ? C13 P1 N1 C25 -29.8(3) . . . . ? C2 P1 N1 C25 92.0(3) . . . . ? C19 P1 N1 Zn1 60.4(2) . . . . ? C13 P1 N1 Zn1 178.67(16) . . . . ? C2 P1 N1 Zn1 -59.5(2) . . . . ? O3 Zn1 N1 C25 -167.3(2) . . . . ? N2 Zn1 N1 C25 -10.1(3) . . . . ? O2 Zn1 N1 C25 102.4(3) . . . . ? O1 Zn1 N1 C25 -88.6(2) . . . . ? O3 Zn1 N1 P1 -14.9(2) . . . . ? N2 Zn1 N1 P1 142.35(16) . . . . ? O2 Zn1 N1 P1 -105.24(17) . . . . ? O1 Zn1 N1 P1 63.78(16) . . . . ? N2 Zn1 O3 C49A 103.2(5) . . . . ? N1 Zn1 O3 C49A -99.9(5) . . . . ? O2 Zn1 O3 C49A 1.5(5) . . . . ? O1 Zn1 O3 C49A -176.6(5) . . . . ? C31 P2 N2 C43 -38.4(4) . . . . ? C11 P2 N2 C43 -159.1(4) . . . . ? C37 P2 N2 C43 81.9(4) . . . . ? C31 P2 N2 Zn1 154.6(3) . . . . ? C11 P2 N2 Zn1 33.9(3) . . . . ? C37 P2 N2 Zn1 -85.1(3) . . . . ? O3 Zn1 N2 C43 -130.1(3) . . . . ? N1 Zn1 N2 C43 71.6(4) . . . . ? O2 Zn1 N2 C43 -40.7(4) . . . . ? O1 Zn1 N2 C43 148.8(4) . . . . ? O3 Zn1 N2 P2 37.2(3) . . . . ? N1 Zn1 N2 P2 -121.1(3) . . . . ? O2 Zn1 N2 P2 126.6(3) . . . . ? O1 Zn1 N2 P2 -43.9(3) . . . . ? C12 O1 C1 C2 -178.5(3) . . . . ? Zn1 O1 C1 C2 28.0(4) . . . . ? C12 O1 C1 C6 0.0(4) . . . . ? Zn1 O1 C1 C6 -153.4(2) . . . . ? O1 C1 C2 C3 177.9(3) . . . . ? C6 C1 C2 C3 -0.5(5) . . . . ? O1 C1 C2 P1 -2.2(5) . . . . ? C6 C1 C2 P1 179.4(3) . . . . ? N1 P1 C2 C1 15.5(4) . . . . ? C19 P1 C2 C1 -104.4(3) . . . . ? C13 P1 C2 C1 141.9(3) . . . . ? N1 P1 C2 C3 -164.6(3) . . . . ? C19 P1 C2 C3 75.5(4) . . . . ? C13 P1 C2 C3 -38.3(4) . . . . ? C1 C2 C3 C4 0.7(6) . . . . ? P1 C2 C3 C4 -179.2(3) . . . . ? C2 C3 C4 C5 -0.3(7) . . . . ? C3 C4 C5 C6 -0.3(7) . . . . ? C4 C5 C6 C1 0.6(6) . . . . ? C4 C5 C6 C7 -178.0(4) . . . . ? O1 C1 C6 C5 -178.7(3) . . . . ? C2 C1 C6 C5 -0.2(6) . . . . ? O1 C1 C6 C7 0.2(4) . . . . ? C2 C1 C6 C7 178.8(3) . . . . ? C5 C6 C7 C12 178.3(4) . . . . ? C1 C6 C7 C12 -0.4(4) . . . . ? C5 C6 C7 C8 -1.0(8) . . . . ? C1 C6 C7 C8 -179.7(4) . . . . ? C12 C7 C8 C9 -1.2(5) . . . . ? C6 C7 C8 C9 178.0(4) . . . . ? C7 C8 C9 C10 1.5(6) . . . . ? C8 C9 C10 C11 -0.5(6) . . . . ? C9 C10 C11 C12 -0.7(6) . . . . ? C9 C10 C11 P2 178.4(3) . . . . ? N2 P2 C11 C12 -0.9(4) . . . . ? C31 P2 C11 C12 -122.4(3) . . . . ? C37 P2 C11 C12 124.5(3) . . . . ? N2 P2 C11 C10 -179.8(3) . . . . ? C31 P2 C11 C10 58.7(3) . . . . ? C37 P2 C11 C10 -54.4(3) . . . . ? C10 C11 C12 O1 -178.9(3) . . . . ? P2 C11 C12 O1 2.1(5) . . . . ? C10 C11 C12 C7 1.0(5) . . . . ? P2 C11 C12 C7 -178.0(3) . . . . ? C1 O1 C12 C11 179.6(3) . . . . ? Zn1 O1 C12 C11 -27.8(4) . . . . ? C1 O1 C12 C7 -0.3(4) . . . . ? Zn1 O1 C12 C7 152.2(2) . . . . ? C8 C7 C12 C11 -0.1(5) . . . . ? C6 C7 C12 C11 -179.5(3) . . . . ? C8 C7 C12 O1 179.9(3) . . . . ? C6 C7 C12 O1 0.5(4) . . . . ? N1 P1 C13 C14 -108.2(3) . . . . ? C19 P1 C13 C14 10.9(4) . . . . ? C2 P1 C13 C14 126.0(3) . . . . ? N1 P1 C13 C18 70.8(4) . . . . ? C19 P1 C13 C18 -170.1(4) . . . . ? C2 P1 C13 C18 -55.1(4) . . . . ? C18 C13 C14 C15 -2.0(6) . . . . ? P1 C13 C14 C15 177.0(3) . . . . ? C13 C14 C15 C16 -0.4(7) . . . . ? C14 C15 C16 C17 2.2(7) . . . . ? C15 C16 C17 C18 -1.6(9) . . . . ? C16 C17 C18 C13 -0.8(9) . . . . ? C14 C13 C18 C17 2.6(8) . . . . ? P1 C13 C18 C17 -176.4(5) . . . . ? N1 P1 C19 C24 -146.7(3) . . . . ? C13 P1 C19 C24 90.0(3) . . . . ? C2 P1 C19 C24 -23.5(4) . . . . ? N1 P1 C19 C20 38.4(3) . . . . ? C13 P1 C19 C20 -84.8(3) . . . . ? C2 P1 C19 C20 161.6(3) . . . . ? C24 C19 C20 C21 -0.1(6) . . . . ? P1 C19 C20 C21 174.9(3) . . . . ? C19 C20 C21 C22 0.3(7) . . . . ? C20 C21 C22 C23 -0.5(7) . . . . ? C21 C22 C23 C24 0.6(8) . . . . ? C22 C23 C24 C19 -0.4(7) . . . . ? C20 C19 C24 C23 0.1(6) . . . . ? P1 C19 C24 C23 -174.6(3) . . . . ? P1 N1 C25 C30 102.8(4) . . . . ? Zn1 N1 C25 C30 -106.4(4) . . . . ? P1 N1 C25 C26 -77.5(5) . . . . ? Zn1 N1 C25 C26 73.3(5) . . . . ? C30 C25 C26 C27 0.5(7) . . . . ? N1 C25 C26 C27 -179.3(5) . . . . ? C25 C26 C27 C28 -0.2(9) . . . . ? C26 C27 C28 C29 -0.2(10) . . . . ? C27 C28 C29 C30 0.3(10) . . . . ? C26 C25 C30 C29 -0.3(7) . . . . ? N1 C25 C30 C29 179.4(4) . . . . ? C28 C29 C30 C25 0.0(8) . . . . ? N2 P2 C31 C32 -87.3(3) . . . . ? C11 P2 C31 C32 35.0(4) . . . . ? C37 P2 C31 C32 147.0(3) . . . . ? N2 P2 C31 C36 81.4(4) . . . . ? C11 P2 C31 C36 -156.4(3) . . . . ? C37 P2 C31 C36 -44.4(4) . . . . ? C36 C31 C32 C33 0.2(6) . . . . ? P2 C31 C32 C33 168.7(4) . . . . ? C31 C32 C33 C34 -0.1(7) . . . . ? C32 C33 C34 C35 0.3(9) . . . . ? C33 C34 C35 C36 -0.6(9) . . . . ? C34 C35 C36 C31 0.6(8) . . . . ? C32 C31 C36 C35 -0.4(6) . . . . ? P2 C31 C36 C35 -168.9(4) . . . . ? N2 P2 C37 C42 31.3(4) . . . . ? C31 P2 C37 C42 153.7(3) . . . . ? C11 P2 C37 C42 -91.4(3) . . . . ? N2 P2 C37 C38 -152.9(3) . . . . ? C31 P2 C37 C38 -30.5(4) . . . . ? C11 P2 C37 C38 84.4(4) . . . . ? C42 C37 C38 C39 -1.3(6) . . . . ? P2 C37 C38 C39 -177.0(3) . . . . ? C37 C38 C39 C40 1.4(7) . . . . ? C38 C39 C40 C41 -1.8(8) . . . . ? C39 C40 C41 C42 2.0(9) . . . . ? C40 C41 C42 C37 -1.8(8) . . . . ? C38 C37 C42 C41 1.5(7) . . . . ? P2 C37 C42 C41 177.4(4) . . . . ? P2 N2 C43 C44 -88.4(5) . . . . ? Zn1 N2 C43 C44 81.1(4) . . . . ? P2 N2 C43 C48 91.8(4) . . . . ? Zn1 N2 C43 C48 -98.7(4) . . . . ? C48 C43 C44 C45 1.0(8) . . . . ? N2 C43 C44 C45 -178.8(5) . . . . ? C43 C44 C45 C46 -0.4(12) . . . . ? C44 C45 C46 C47 -0.9(15) . . . . ? C45 C46 C47 C48 1.4(13) . . . . ? C46 C47 C48 C43 -0.8(9) . . . . ? C44 C43 C48 C47 -0.4(7) . . . . ? N2 C43 C48 C47 179.4(4) . . . . ? Zn1 O3 C49A C50A 148.4(8) . . . . ? Zn1 O3 C49A C51 -4.0(8) . . . . ? C50A C49A C51 O2 -149.2(8) . . . . ? O3 C49A C51 O2 6.3(10) . . . . ? C50A C49A C51 O4 29.8(11) . . . . ? O3 C49A C51 O4 -174.6(6) . . . . ? C58 C53 C54 C55 0.8(5) . . . . ? B1 C53 C54 C55 174.5(3) . . . . ? C53 C54 C55 C56 0.1(5) . . . . ? C53 C54 C55 C59 -178.7(3) . . . . ? C54 C55 C56 C57 -0.5(5) . . . . ? C59 C55 C56 C57 178.4(3) . . . . ? C55 C56 C57 C58 0.0(5) . . . . ? C55 C56 C57 C60 -178.9(4) . . . . ? C56 C57 C58 C53 0.9(5) . . . . ? C60 C57 C58 C53 179.8(4) . . . . ? C54 C53 C58 C57 -1.3(5) . . . . ? B1 C53 C58 C57 -175.0(3) . . . . ? C56 C55 C59 F1 -174.1(4) . . . . ? C54 C55 C59 F1 4.8(6) . . . . ? C56 C55 C59 F2 63.1(5) . . . . ? C54 C55 C59 F2 -118.1(4) . . . . ? C56 C55 C59 F3 -53.1(5) . . . . ? C54 C55 C59 F3 125.8(4) . . . . ? C56 C57 C60 F6B -46.4(18) . . . . ? C58 C57 C60 F6B 134.7(18) . . . . ? C56 C57 C60 F5 118.7(5) . . . . ? C58 C57 C60 F5 -60.2(6) . . . . ? C56 C57 C60 F6 -4.1(7) . . . . ? C58 C57 C60 F6 177.0(5) . . . . ? C56 C57 C60 F4 -123.7(5) . . . . ? C58 C57 C60 F4 57.4(6) . . . . ? C56 C57 C60 F4B -172.7(17) . . . . ? C58 C57 C60 F4B 8.4(17) . . . . ? C56 C57 C60 F5B 74.3(17) . . . . ? C58 C57 C60 F5B -104.6(17) . . . . ? C66 C61 C62 C63 0.1(6) . . . . ? B1 C61 C62 C63 -173.7(4) . . . . ? C61 C62 C63 C64 -0.5(7) . . . . ? C61 C62 C63 C67 178.0(5) . . . . ? C62 C63 C64 C65 0.3(7) . . . . ? C67 C63 C64 C65 -178.2(5) . . . . ? C63 C64 C65 C66 0.3(8) . . . . ? C63 C64 C65 C68 -179.6(8) . . . . ? C62 C61 C66 C65 0.5(6) . . . . ? B1 C61 C66 C65 174.1(4) . . . . ? C64 C65 C66 C61 -0.7(8) . . . . ? C68 C65 C66 C61 179.2(7) . . . . ? C64 C63 C67 F9 6.7(11) . . . . ? C62 C63 C67 F9 -171.7(9) . . . . ? C64 C63 C67 F8B 88.8(16) . . . . ? C62 C63 C67 F8B -89.7(16) . . . . ? C64 C63 C67 F7B -139.6(16) . . . . ? C62 C63 C67 F7B 42.0(16) . . . . ? C64 C63 C67 F7 135.6(10) . . . . ? C62 C63 C67 F7 -42.8(11) . . . . ? C64 C63 C67 F8 -113.6(11) . . . . ? C62 C63 C67 F8 68.0(11) . . . . ? C64 C63 C67 F9B -26.8(15) . . . . ? C62 C63 C67 F9B 154.8(13) . . . . ? C64 C65 C68 F12 142(2) . . . . ? C66 C65 C68 F12 -38(2) . . . . ? C64 C65 C68 F10B -37.1(19) . . . . ? C66 C65 C68 F10B 143.1(15) . . . . ? C64 C65 C68 F12B -178.8(17) . . . . ? C66 C65 C68 F12B 1(2) . . . . ? C64 C65 C68 F11 6(2) . . . . ? C66 C65 C68 F11 -173.4(17) . . . . ? C64 C65 C68 F10 -100.6(12) . . . . ? C66 C65 C68 F10 79.6(13) . . . . ? C64 C65 C68 F11B 73.1(14) . . . . ? C66 C65 C68 F11B -106.8(12) . . . . ? C74 C69 C70 C71 -1.1(5) . . . . ? B1 C69 C70 C71 -172.2(3) . . . . ? C69 C70 C71 C72 0.5(6) . . . . ? C69 C70 C71 C75 179.7(4) . . . . ? C70 C71 C72 C73 0.1(6) . . . . ? C75 C71 C72 C73 -179.1(5) . . . . ? C71 C72 C73 C74 0.0(7) . . . . ? C71 C72 C73 C76 179.6(5) . . . . ? C72 C73 C74 C69 -0.7(7) . . . . ? C76 C73 C74 C69 179.7(5) . . . . ? C70 C69 C74 C73 1.2(5) . . . . ? B1 C69 C74 C73 172.3(4) . . . . ? C72 C71 C75 F15B -162(3) . . . . ? C70 C71 C75 F15B 19(3) . . . . ? C72 C71 C75 F14 -7.2(9) . . . . ? C70 C71 C75 F14 173.6(7) . . . . ? C72 C71 C75 F13B 64(2) . . . . ? C70 C71 C75 F13B -115(2) . . . . ? C72 C71 C75 F13 117.6(7) . . . . ? C70 C71 C75 F13 -61.6(8) . . . . ? C72 C71 C75 F15 -129.6(6) . . . . ? C70 C71 C75 F15 51.2(8) . . . . ? C72 C71 C75 F14B -39.9(18) . . . . ? C70 C71 C75 F14B 140.9(18) . . . . ? C72 C73 C76 F16B -173.6(15) . . . . ? C74 C73 C76 F16B 6.1(18) . . . . ? C72 C73 C76 F18 19.0(14) . . . . ? C74 C73 C76 F18 -161.3(11) . . . . ? C72 C73 C76 F18B -22.1(16) . . . . ? C74 C73 C76 F18B 157.5(14) . . . . ? C72 C73 C76 F16 152.5(10) . . . . ? C74 C73 C76 F16 -27.9(12) . . . . ? C72 C73 C76 F17 -104.5(9) . . . . ? C74 C73 C76 F17 75.2(8) . . . . ? C72 C73 C76 F17B 76.6(9) . . . . ? C74 C73 C76 F17B -103.8(10) . . . . ? C82 C77 C78 C79 -1.2(6) . . . . ? B1 C77 C78 C79 169.2(4) . . . . ? C77 C78 C79 C80 1.3(6) . . . . ? C77 C78 C79 C83 179.9(4) . . . . ? C78 C79 C80 C81 -0.7(7) . . . . ? C83 C79 C80 C81 -179.3(5) . . . . ? C79 C80 C81 C82 0.1(8) . . . . ? C79 C80 C81 C84 179.0(6) . . . . ? C80 C81 C82 C77 0.0(8) . . . . ? C84 C81 C82 C77 -179.0(6) . . . . ? C78 C77 C82 C81 0.6(6) . . . . ? B1 C77 C82 C81 -169.8(4) . . . . ? C78 C79 C83 F20 176.7(10) . . . . ? C80 C79 C83 F20 -4.7(12) . . . . ? C78 C79 C83 F21B 25.7(16) . . . . ? C80 C79 C83 F21B -155.7(15) . . . . ? C78 C79 C83 F19B -111.1(9) . . . . ? C80 C79 C83 F19B 67.5(10) . . . . ? C78 C79 C83 F21 44.1(11) . . . . ? C80 C79 C83 F21 -137.3(10) . . . . ? C78 C79 C83 F19 -61.4(9) . . . . ? C80 C79 C83 F19 117.2(9) . . . . ? C78 C79 C83 F20B 140.5(7) . . . . ? C80 C79 C83 F20B -40.9(9) . . . . ? C80 C81 C84 F24 -18.1(12) . . . . ? C82 C81 C84 F24 160.8(7) . . . . ? C80 C81 C84 F23 -143.2(8) . . . . ? C82 C81 C84 F23 35.7(11) . . . . ? C80 C81 C84 F22 105.4(9) . . . . ? C82 C81 C84 F22 -75.7(10) . . . . ? O4 C51 O2 Zn1 176.2(5) . . . . ? C49A C51 O2 Zn1 -4.8(7) . . . . ? O3 Zn1 O2 C51 1.9(3) . . . . ? N2 Zn1 O2 C51 -115.0(3) . . . . ? N1 Zn1 O2 C51 123.5(3) . . . . ? O1 Zn1 O2 C51 11.4(7) . . . . ? O2 C51 O4 C52 -2.2(10) . . . . ? C49A C51 O4 C52 178.7(7) . . . . ? C78 C77 B1 C61 155.5(3) . . . . ? C82 C77 B1 C61 -34.7(5) . . . . ? C78 C77 B1 C53 37.6(5) . . . . ? C82 C77 B1 C53 -152.7(4) . . . . ? C78 C77 B1 C69 -83.1(4) . . . . ? C82 C77 B1 C69 86.7(4) . . . . ? C66 C61 B1 C77 147.1(4) . . . . ? C62 C61 B1 C77 -39.5(5) . . . . ? C66 C61 B1 C53 -89.6(4) . . . . ? C62 C61 B1 C53 83.7(4) . . . . ? C66 C61 B1 C69 32.7(5) . . . . ? C62 C61 B1 C69 -154.0(3) . . . . ? C58 C53 B1 C77 -151.5(3) . . . . ? C54 C53 B1 C77 35.2(5) . . . . ? C58 C53 B1 C61 85.9(4) . . . . ? C54 C53 B1 C61 -87.4(4) . . . . ? C58 C53 B1 C69 -37.2(5) . . . . ? C54 C53 B1 C69 149.5(3) . . . . ? C70 C69 B1 C77 87.6(4) . . . . ? C74 C69 B1 C77 -83.0(4) . . . . ? C70 C69 B1 C61 -151.6(3) . . . . ? C74 C69 B1 C61 37.9(4) . . . . ? C70 C69 B1 C53 -33.8(5) . . . . ? C74 C69 B1 C53 155.6(3) . . . . ? C6S C1S C2S C3S 0.0 . . . . ? Br1 C1S C2S C3S -175.9(5) . . . . ? C1S C2S C3S C4S 0.0 . . . . ? C2S C3S C4S C5S 0.0 . . . . ? C3S C4S C5S C6S 0.0 . . . . ? C4S C5S C6S C1S 0.0 . . . . ? C2S C1S C6S C5S 0.0 . . . . ? Br1 C1S C6S C5S 175.6(5) . . . . ? C6SB C1SB C2SB C3SB 0.0 . . . . ? Br1B C1SB C2SB C3SB 179.1(7) . . . . ? C1SB C2SB C3SB C4SB 0.0 . . . . ? C2SB C3SB C4SB C5SB 0.0 . . . . ? C3SB C4SB C5SB C6SB 0.0 . . . . ? C4SB C5SB C6SB C1SB 0.0 . . . . ? C2SB C1SB C6SB C5SB 0.0 . . . . ? Br1B C1SB C6SB C5SB -179.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.852 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.061