# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Paul Hayes' _publ_contact_author_email P.HAYES@ULETH.CA _publ_section_title ; Cationic organozinc complexes of a bis(phosphinimine) pincer ligand: synthesis and structural studies ; loop_ _publ_author_name 'Paul Hayes' 'Craig Wheaton' # Attachment 'XRay-revised_-_Manuscript_B922543A.cif' data_2b _database_code_depnum_ccdc_archive 'CCDC 753815' #TrackingRef 'XRay-revised_-_Manuscript_B922543A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H74 B N2 O P2 Zn' _chemical_formula_weight 1241.55 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 11.4348(10) _cell_length_b 15.8183(14) _cell_length_c 19.2062(17) _cell_angle_alpha 86.6850(10) _cell_angle_beta 75.8230(10) _cell_angle_gamma 82.7630(10) _cell_volume 3340.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1306 _exptl_absorpt_coefficient_mu 0.464 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8901 _exptl_absorpt_correction_T_max 0.9417 _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 40680 _diffrn_reflns_av_R_equivalents 0.0799 _diffrn_reflns_av_sigmaI/netI 0.0906 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.03 _reflns_number_total 11774 _reflns_number_gt 6513 _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^)+(0.0857P)^2^+1.3364P] 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 11774 _refine_ls_number_parameters 861 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.1351 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1883 _refine_ls_wR_factor_gt 0.1554 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.32750(5) 0.72590(5) 0.34194(3) 0.0680(3) Uani 1 1 d . . . B1 B 0.1896(6) 0.7847(4) 0.8502(3) 0.0551(16) Uani 1 1 d . . . P1 P 0.25758(10) 0.64546(7) 0.20291(6) 0.0349(3) Uani 1 1 d . . . O1 O 0.5187(2) 0.69463(18) 0.18803(13) 0.0364(7) Uani 1 1 d . B . N1 N 0.2824(3) 0.6379(2) 0.28218(17) 0.0368(8) Uani 1 1 d . B . C1 C 0.4960(4) 0.6639(3) 0.1278(2) 0.0331(10) Uani 1 1 d . . . P2 P 0.60418(10) 0.77706(8) 0.30377(6) 0.0405(3) Uani 1 1 d . . . N2 N 0.4606(3) 0.8043(2) 0.31895(18) 0.0421(9) Uani 1 1 d . B . C2 C 0.3884(4) 0.6324(3) 0.1271(2) 0.0343(10) Uani 1 1 d . B . C3 C 0.3828(4) 0.6036(3) 0.0606(2) 0.0390(11) Uani 1 1 d . . . H3 H 0.3120 0.5805 0.0566 0.047 Uiso 1 1 calc R B . C4 C 0.4787(4) 0.6081(3) -0.0002(2) 0.0421(11) Uani 1 1 d . B . H4 H 0.4719 0.5874 -0.0444 0.050 Uiso 1 1 calc R . . C5 C 0.5823(4) 0.6418(3) 0.0022(2) 0.0397(11) Uani 1 1 d . . . H5 H 0.6459 0.6457 -0.0398 0.048 Uiso 1 1 calc R B . C6 C 0.5924(4) 0.6700(3) 0.0674(2) 0.0350(10) Uani 1 1 d . B . C7 C 0.6823(4) 0.7103(3) 0.0928(2) 0.0349(10) Uani 1 1 d . . . C8 C 0.7953(4) 0.7370(3) 0.0623(2) 0.0412(11) Uani 1 1 d . B . H8 H 0.8332 0.7287 0.0130 0.049 Uiso 1 1 calc R . . C9 C 0.8509(4) 0.7760(3) 0.1060(2) 0.0453(12) Uani 1 1 d . . . H9 H 0.9282 0.7945 0.0859 0.054 Uiso 1 1 calc R B . C10 C 0.7979(4) 0.7889(3) 0.1779(2) 0.0420(11) Uani 1 1 d . B . H10 H 0.8400 0.8156 0.2059 0.050 Uiso 1 1 calc R . . C11 C 0.6829(4) 0.7635(3) 0.2109(2) 0.0387(11) Uani 1 1 d . B . C12 C 0.6313(3) 0.7239(3) 0.1656(2) 0.0345(10) Uani 1 1 d . B . C13 C 0.1862(4) 0.7509(3) 0.1883(2) 0.0372(10) Uani 1 1 d . B . C14 C 0.1196(4) 0.7981(3) 0.2473(3) 0.0494(12) Uani 1 1 d . . . H14 H 0.1115 0.7745 0.2946 0.059 Uiso 1 1 calc R B . C15 C 0.0653(5) 0.8799(3) 0.2363(3) 0.0628(15) Uani 1 1 d . B . H15 H 0.0199 0.9119 0.2764 0.075 Uiso 1 1 calc R . . C16 C 0.0762(4) 0.9149(3) 0.1689(3) 0.0586(14) Uani 1 1 d . . . H16 H 0.0390 0.9710 0.1622 0.070 Uiso 1 1 calc R B . C17 C 0.1418(4) 0.8683(3) 0.1096(3) 0.0512(13) Uani 1 1 d . B . H17 H 0.1493 0.8925 0.0625 0.061 Uiso 1 1 calc R . . C18 C 0.1957(4) 0.7870(3) 0.1195(2) 0.0455(12) Uani 1 1 d . . . H18 H 0.2399 0.7552 0.0789 0.055 Uiso 1 1 calc R B . C19 C 0.1643(4) 0.5683(3) 0.1889(2) 0.0409(11) Uani 1 1 d . B . C20 C 0.0473(4) 0.5924(3) 0.1808(2) 0.0478(12) Uani 1 1 d . . . H20 H 0.0154 0.6509 0.1825 0.057 Uiso 1 1 calc R B . C21 C -0.0233(5) 0.5314(4) 0.1702(3) 0.0644(16) Uani 1 1 d . B . H21 H -0.1031 0.5484 0.1644 0.077 Uiso 1 1 calc R . . C22 C 0.0204(6) 0.4480(5) 0.1680(3) 0.0747(19) Uani 1 1 d . . . H22 H -0.0291 0.4070 0.1607 0.090 Uiso 1 1 calc R B . C23 C 0.1373(7) 0.4212(4) 0.1763(3) 0.0764(18) Uani 1 1 d . B . H23 H 0.1675 0.3624 0.1747 0.092 Uiso 1 1 calc R . . C24 C 0.2097(5) 0.4824(3) 0.1870(2) 0.0591(14) Uani 1 1 d . . . H24 H 0.2895 0.4652 0.1928 0.071 Uiso 1 1 calc R B . C25 C 0.6860(4) 0.8500(3) 0.3362(2) 0.0417(11) Uani 1 1 d . B . C26 C 0.7470(4) 0.8243(3) 0.3903(2) 0.0531(13) Uani 1 1 d . . . H26 H 0.7476 0.7674 0.4091 0.064 Uiso 1 1 calc R B . C27 C 0.8062(5) 0.8817(4) 0.4161(3) 0.0628(15) Uani 1 1 d . B . H27 H 0.8482 0.8641 0.4524 0.075 Uiso 1 1 calc R . . C28 C 0.8048(5) 0.9641(4) 0.3896(3) 0.0625(15) Uani 1 1 d . . . H28 H 0.8447 1.0034 0.4083 0.075 Uiso 1 1 calc R B . C29 C 0.7464(5) 0.9900(3) 0.3365(3) 0.0596(14) Uani 1 1 d . B . H29 H 0.7460 1.0472 0.3185 0.072 Uiso 1 1 calc R . . C30 C 0.6878(4) 0.9331(3) 0.3089(2) 0.0491(12) Uani 1 1 d . . . H30 H 0.6487 0.9511 0.2713 0.059 Uiso 1 1 calc R B . C31 C 0.6293(4) 0.6755(3) 0.3469(2) 0.0443(12) Uani 1 1 d . B . C32 C 0.7229(5) 0.6155(3) 0.3170(3) 0.0631(15) Uani 1 1 d . . . H32 H 0.7720 0.6257 0.2704 0.076 Uiso 1 1 calc R B . C33 C 0.7468(5) 0.5396(4) 0.3544(4) 0.0815(19) Uani 1 1 d . B . H33 H 0.8110 0.4980 0.3331 0.098 Uiso 1 1 calc R . . C34 C 0.6772(7) 0.5255(5) 0.4218(4) 0.087(2) Uani 1 1 d . . . H34 H 0.6936 0.4740 0.4476 0.104 Uiso 1 1 calc R B . C35 C 0.5844(7) 0.5847(5) 0.4525(4) 0.091(2) Uani 1 1 d . B . H35 H 0.5366 0.5744 0.4994 0.109 Uiso 1 1 calc R . . C36 C 0.5597(5) 0.6589(4) 0.4160(3) 0.0633(15) Uani 1 1 d . . . H36 H 0.4946 0.6997 0.4378 0.076 Uiso 1 1 calc R B . C37 C 0.2615(4) 0.5600(3) 0.3242(2) 0.0422(11) Uani 1 1 d . . . C38 C 0.3589(4) 0.4965(3) 0.3241(2) 0.0500(12) Uani 1 1 d . B . C39 C 0.3402(6) 0.4235(4) 0.3656(3) 0.0663(15) Uani 1 1 d . . . H39 H 0.4074 0.3815 0.3656 0.080 Uiso 1 1 calc R B . C40 C 0.2270(6) 0.4090(4) 0.4074(3) 0.0717(17) Uani 1 1 d . B . C41 C 0.1304(5) 0.4737(4) 0.4070(3) 0.0635(15) Uani 1 1 d . . . H41 H 0.0519 0.4655 0.4354 0.076 Uiso 1 1 calc R B . C42 C 0.1458(4) 0.5490(3) 0.3667(2) 0.0469(12) Uani 1 1 d . B . C43 C 0.4842(4) 0.5064(4) 0.2784(3) 0.0622(15) Uani 1 1 d . . . H43A H 0.5428 0.4619 0.2921 0.093 Uiso 1 1 calc R B . H43B H 0.5062 0.5626 0.2858 0.093 Uiso 1 1 calc R . . H43C H 0.4850 0.5013 0.2277 0.093 Uiso 1 1 calc R . . C44 C 0.2086(7) 0.3283(4) 0.4539(3) 0.107(3) Uani 1 1 d . . . H44A H 0.2759 0.2841 0.4363 0.160 Uiso 1 1 calc R B . H44B H 0.1319 0.3082 0.4517 0.160 Uiso 1 1 calc R . . H44C H 0.2059 0.3406 0.5038 0.160 Uiso 1 1 calc R . . C45 C 0.0383(4) 0.6154(3) 0.3693(2) 0.0550(14) Uani 1 1 d . . . H45A H -0.0353 0.5932 0.3978 0.082 Uiso 1 1 calc R B . H45B H 0.0292 0.6295 0.3204 0.082 Uiso 1 1 calc R . . H45C H 0.0510 0.6668 0.3913 0.082 Uiso 1 1 calc R . . C46 C 0.4157(4) 0.8958(3) 0.3191(3) 0.0525(13) Uani 1 1 d . . . C47 C 0.3947(5) 0.9403(5) 0.3821(3) 0.0772(18) Uani 1 1 d . B . C48 C 0.3553(8) 1.0276(6) 0.3792(4) 0.136(4) Uani 1 1 d . . . H48 H 0.3414 1.0594 0.4215 0.163 Uiso 1 1 calc R B . C49 C 0.3361(10) 1.0685(6) 0.3179(5) 0.170(5) Uani 1 1 d . B . C50 C 0.3547(7) 1.0227(4) 0.2580(4) 0.112(3) Uani 1 1 d . . . H50 H 0.3406 1.0510 0.2153 0.134 Uiso 1 1 calc R B . C51 C 0.3933(4) 0.9365(3) 0.2566(3) 0.0566(13) Uani 1 1 d . B . C52 C 0.4159(5) 0.8995(4) 0.4521(3) 0.0783(18) Uani 1 1 d . . . H52A H 0.3747 0.8479 0.4630 0.117 Uiso 1 1 calc R B . H52B H 0.3833 0.9398 0.4909 0.117 Uiso 1 1 calc R . . H52C H 0.5032 0.8845 0.4475 0.117 Uiso 1 1 calc R . . C53 C 0.2954(15) 1.1661(6) 0.3153(6) 0.318(11) Uani 1 1 d . . . H53A H 0.3341 1.1903 0.2685 0.477 Uiso 1 1 calc R B . H53B H 0.3195 1.1935 0.3533 0.477 Uiso 1 1 calc R . . H53C H 0.2070 1.1760 0.3226 0.477 Uiso 1 1 calc R . . C54 C 0.4106(4) 0.8911(3) 0.1876(2) 0.0472(12) Uani 1 1 d . . . H54A H 0.3727 0.9277 0.1543 0.071 Uiso 1 1 calc R B . H54B H 0.3729 0.8381 0.1974 0.071 Uiso 1 1 calc R . . H54C H 0.4976 0.8781 0.1660 0.071 Uiso 1 1 calc R . . C55 C 0.2719(4) 0.8429(3) 0.8820(2) 0.0469(12) Uani 1 1 d . A . C56 C 0.2656(4) 0.9309(3) 0.8677(3) 0.0504(12) Uani 1 1 d . . . H56 H 0.2117 0.9559 0.8397 0.060 Uiso 1 1 calc R A . C57 C 0.3336(5) 0.9827(3) 0.8922(3) 0.0611(15) Uani 1 1 d . A . H57 H 0.3254 1.0422 0.8814 0.073 Uiso 1 1 calc R . . C58 C 0.4142(5) 0.9489(4) 0.9327(3) 0.0685(16) Uani 1 1 d . . . H58 H 0.4616 0.9844 0.9498 0.082 Uiso 1 1 calc R A . C59 C 0.4242(5) 0.8620(4) 0.9477(3) 0.0716(16) Uani 1 1 d . A . H59 H 0.4787 0.8372 0.9755 0.086 Uiso 1 1 calc R . . C60 C 0.3550(5) 0.8118(3) 0.9224(3) 0.0618(14) Uani 1 1 d . . . H60 H 0.3643 0.7523 0.9329 0.074 Uiso 1 1 calc R A . C61 C 0.0482(6) 0.8282(3) 0.8684(3) 0.0643(16) Uani 1 1 d . A . C62 C -0.0020(5) 0.8790(3) 0.9270(3) 0.0562(14) Uani 1 1 d . . . H62 H 0.0511 0.8941 0.9541 0.067 Uiso 1 1 calc R A . C63 C -0.1232(5) 0.9092(4) 0.9491(3) 0.0746(17) Uani 1 1 d . A . H63 H -0.1513 0.9431 0.9904 0.089 Uiso 1 1 calc R . . C64 C -0.2028(7) 0.8903(5) 0.9113(6) 0.132(4) Uani 1 1 d . . . H64 H -0.2866 0.9109 0.9255 0.159 Uiso 1 1 calc R A . C65 C -0.1582(10) 0.8406(6) 0.8522(8) 0.199(7) Uani 1 1 d . A . H65 H -0.2110 0.8274 0.8242 0.239 Uiso 1 1 calc R . . C66 C -0.0378(9) 0.8102(5) 0.8337(6) 0.171(5) Uani 1 1 d . . . H66 H -0.0112 0.7740 0.7937 0.206 Uiso 1 1 calc R A . C67 C 0.1919(4) 0.6890(3) 0.8887(2) 0.0428(11) Uani 1 1 d . A . C68 C 0.1099(4) 0.6703(3) 0.9527(2) 0.0417(11) Uani 1 1 d . . . H68 H 0.0519 0.7151 0.9751 0.050 Uiso 1 1 calc R A . C69 C 0.1084(4) 0.5903(3) 0.9853(2) 0.0413(11) Uani 1 1 d . A . H69 H 0.0497 0.5810 1.0287 0.050 Uiso 1 1 calc R . . C70 C 0.1912(4) 0.5243(3) 0.9553(2) 0.0445(11) Uani 1 1 d . . . H70 H 0.1892 0.4687 0.9768 0.053 Uiso 1 1 calc R A . C71 C 0.2766(5) 0.5397(3) 0.8942(3) 0.0595(14) Uani 1 1 d . A . H71 H 0.3360 0.4948 0.8736 0.071 Uiso 1 1 calc R . . C72 C 0.2774(5) 0.6198(3) 0.8621(3) 0.0701(17) Uani 1 1 d . . . H72 H 0.3388 0.6286 0.8198 0.084 Uiso 1 1 calc R A . C73 C 0.2696(6) 0.7686(4) 0.7619(2) 0.057(3) Uani 0.70 1 d PG A 1 C74 C 0.2268(6) 0.7113(4) 0.7246(3) 0.087(3) Uani 0.70 1 d PG A 1 H74 H 0.1618 0.6805 0.7488 0.104 Uiso 0.70 1 calc PR A 1 C75 C 0.2792(8) 0.6991(4) 0.6521(3) 0.122(5) Uani 0.70 1 d PG A 1 H75 H 0.2500 0.6600 0.6266 0.147 Uiso 0.70 1 calc PR A 1 C76 C 0.3744(7) 0.7443(5) 0.6167(3) 0.118(6) Uani 0.70 1 d PG A 1 H76 H 0.4102 0.7359 0.5671 0.142 Uiso 0.70 1 calc PR A 1 C77 C 0.4172(6) 0.8016(5) 0.6540(4) 0.137(7) Uani 0.70 1 d PG A 1 H77 H 0.4823 0.8324 0.6299 0.164 Uiso 0.70 1 calc PR A 1 C78 C 0.3648(7) 0.8138(4) 0.7266(4) 0.086(4) Uani 0.70 1 d PG A 1 H78 H 0.3940 0.8529 0.7521 0.103 Uiso 0.70 1 calc PR A 1 C79 C 0.2060(11) 0.7495(12) 0.4375(5) 0.177(8) Uani 0.70 1 d P B 1 H79A H 0.2390 0.7857 0.4659 0.265 Uiso 0.70 1 calc PR B 1 H79B H 0.1906 0.6955 0.4639 0.265 Uiso 0.70 1 calc PR B 1 H79C H 0.1298 0.7785 0.4288 0.265 Uiso 0.70 1 calc PR B 1 C73B C 0.2103(10) 0.7864(8) 0.7603(5) 0.028(4) Uani 0.30 1 d PG A 2 C74B C 0.1278(9) 0.7908(9) 0.7173(6) 0.081(6) Uani 0.30 1 d PG A 2 H74B H 0.0431 0.7995 0.7385 0.097 Uiso 0.30 1 calc PR A 2 C75B C 0.1694(12) 0.7826(10) 0.6435(6) 0.099(8) Uani 0.30 1 d PG A 2 H75B H 0.1131 0.7856 0.6141 0.118 Uiso 0.30 1 calc PR A 2 C76B C 0.2934(14) 0.7699(9) 0.6125(5) 0.061(6) Uani 0.30 1 d PG A 2 H76B H 0.3218 0.7642 0.5620 0.073 Uiso 0.30 1 calc PR A 2 C77B C 0.3758(10) 0.7654(11) 0.6555(7) 0.096(11) Uani 0.30 1 d PG A 2 H77B H 0.4605 0.7568 0.6344 0.115 Uiso 0.30 1 calc PR A 2 C78B C 0.3342(9) 0.7737(10) 0.7294(7) 0.099(12) Uani 0.30 1 d PG A 2 H78B H 0.3906 0.7706 0.7588 0.119 Uiso 0.30 1 calc PR A 2 C79B C 0.263(3) 0.6761(13) 0.4529(12) 0.100(11) Uani 0.30 1 d P B 2 H79D H 0.3246 0.6802 0.4799 0.150 Uiso 0.30 1 calc PR B 2 H79E H 0.2495 0.6163 0.4517 0.150 Uiso 0.30 1 calc PR B 2 H79F H 0.1871 0.7097 0.4762 0.150 Uiso 0.30 1 calc PR B 2 C1S C 0.9787(9) 1.0284(9) 0.5091(7) 0.190(9) Uani 0.50 1 d PU C -1 H1S H 0.9615 0.9992 0.5545 0.228 Uiso 0.50 1 calc PR C -1 C2S C 0.9245(9) 1.1110(9) 0.5015(7) 0.180(8) Uani 0.50 1 d PRU C -1 H2S H 0.8702 1.1383 0.5416 0.216 Uiso 0.50 1 calc PR C -1 C3S C 0.9497(9) 1.1536(9) 0.4351(7) 0.216(9) Uani 0.50 1 d PRU C -1 H3S H 0.9126 1.2101 0.4299 0.259 Uiso 0.50 1 calc PR C -1 C4S C 1.0290(9) 1.1137(9) 0.3764(7) 0.272(12) Uani 0.50 1 d PRU C -1 H4S H 1.0462 1.1428 0.3310 0.326 Uiso 0.50 1 calc PR C -1 C5S C 1.0832(9) 1.0310(9) 0.3840(7) 0.225(10) Uani 0.50 1 d PRU C -1 H5S H 1.1375 1.0037 0.3439 0.269 Uiso 0.50 1 calc PR C -1 C6S C 1.0581(9) 0.9884(9) 0.4504(7) 0.205(10) Uani 0.50 1 d PRU C -1 H6S H 1.0951 0.9319 0.4556 0.246 Uiso 0.50 1 calc PR C -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0518(4) 0.1246(6) 0.0338(3) -0.0186(3) 0.0010(3) -0.0489(4) B1 0.086(5) 0.037(3) 0.037(3) 0.001(3) -0.006(3) -0.003(3) P1 0.0276(6) 0.0473(7) 0.0308(6) -0.0044(5) -0.0077(5) -0.0053(5) O1 0.0276(16) 0.0566(19) 0.0252(15) -0.0006(13) -0.0049(12) -0.0095(14) N1 0.0279(19) 0.052(2) 0.0306(19) -0.0016(17) -0.0060(15) -0.0060(17) C1 0.031(2) 0.037(2) 0.029(2) -0.0014(19) -0.0061(19) 0.0033(19) P2 0.0330(7) 0.0597(8) 0.0319(6) 0.0050(6) -0.0105(5) -0.0145(6) N2 0.029(2) 0.067(3) 0.032(2) -0.0033(18) -0.0075(16) -0.0136(19) C2 0.034(2) 0.040(3) 0.028(2) 0.0006(19) -0.0076(19) -0.001(2) C3 0.040(3) 0.040(3) 0.036(3) -0.007(2) -0.010(2) 0.004(2) C4 0.053(3) 0.042(3) 0.030(2) -0.009(2) -0.011(2) 0.005(2) C5 0.041(3) 0.039(3) 0.032(2) -0.001(2) -0.001(2) 0.005(2) C6 0.029(2) 0.038(3) 0.033(2) 0.0039(19) -0.0033(19) 0.0063(19) C7 0.028(2) 0.036(3) 0.037(3) 0.0065(19) -0.0057(19) 0.0042(19) C8 0.035(3) 0.047(3) 0.036(3) 0.005(2) 0.000(2) -0.002(2) C9 0.029(2) 0.054(3) 0.046(3) 0.009(2) 0.003(2) -0.006(2) C10 0.030(2) 0.052(3) 0.046(3) 0.010(2) -0.012(2) -0.010(2) C11 0.031(2) 0.048(3) 0.036(2) 0.007(2) -0.007(2) -0.006(2) C12 0.024(2) 0.043(3) 0.035(2) 0.006(2) -0.0067(19) -0.0037(19) C13 0.025(2) 0.045(3) 0.045(3) -0.004(2) -0.013(2) -0.006(2) C14 0.046(3) 0.050(3) 0.049(3) -0.004(2) -0.002(2) -0.010(2) C15 0.055(3) 0.051(4) 0.073(4) -0.011(3) 0.001(3) -0.001(3) C16 0.046(3) 0.045(3) 0.082(4) -0.001(3) -0.013(3) 0.001(2) C17 0.051(3) 0.047(3) 0.061(3) 0.005(3) -0.024(3) -0.008(3) C18 0.046(3) 0.050(3) 0.045(3) -0.005(2) -0.018(2) -0.006(2) C19 0.043(3) 0.046(3) 0.034(3) -0.006(2) -0.005(2) -0.010(2) C20 0.043(3) 0.067(3) 0.038(3) -0.008(2) -0.012(2) -0.017(2) C21 0.060(4) 0.095(5) 0.046(3) -0.009(3) -0.012(3) -0.034(3) C22 0.089(5) 0.096(5) 0.049(3) -0.009(3) -0.012(3) -0.056(4) C23 0.118(6) 0.056(4) 0.053(4) -0.004(3) -0.005(4) -0.030(4) C24 0.075(4) 0.061(4) 0.044(3) -0.007(3) -0.012(3) -0.022(3) C25 0.035(3) 0.058(3) 0.036(3) 0.005(2) -0.011(2) -0.019(2) C26 0.048(3) 0.077(4) 0.040(3) 0.011(3) -0.016(2) -0.023(3) C27 0.057(3) 0.095(5) 0.046(3) 0.000(3) -0.023(3) -0.027(3) C28 0.062(4) 0.078(4) 0.051(3) -0.018(3) -0.010(3) -0.021(3) C29 0.064(4) 0.053(3) 0.060(3) -0.013(3) -0.007(3) -0.009(3) C30 0.045(3) 0.060(3) 0.045(3) -0.004(2) -0.013(2) -0.008(2) C31 0.037(3) 0.059(3) 0.043(3) 0.011(2) -0.017(2) -0.018(2) C32 0.042(3) 0.072(4) 0.073(4) 0.034(3) -0.016(3) -0.012(3) C33 0.056(4) 0.078(4) 0.111(5) 0.044(4) -0.027(4) -0.019(3) C34 0.098(5) 0.082(5) 0.093(5) 0.052(4) -0.046(4) -0.038(4) C35 0.125(6) 0.093(5) 0.065(4) 0.029(4) -0.028(4) -0.054(5) C36 0.084(4) 0.071(4) 0.043(3) 0.011(3) -0.018(3) -0.039(3) C37 0.037(3) 0.061(3) 0.029(2) 0.001(2) -0.007(2) -0.008(2) C38 0.057(3) 0.064(3) 0.026(2) 0.001(2) -0.011(2) 0.001(3) C39 0.084(4) 0.068(4) 0.038(3) -0.004(3) -0.007(3) 0.010(3) C40 0.107(5) 0.056(4) 0.045(3) -0.002(3) -0.005(3) -0.011(4) C41 0.071(4) 0.076(4) 0.035(3) -0.004(3) 0.011(3) -0.023(3) C42 0.042(3) 0.060(3) 0.037(3) -0.005(2) -0.002(2) -0.014(2) C43 0.046(3) 0.081(4) 0.054(3) 0.004(3) -0.012(3) 0.011(3) C44 0.167(7) 0.068(4) 0.062(4) 0.011(3) 0.015(4) -0.016(4) C45 0.031(3) 0.089(4) 0.043(3) -0.007(3) 0.000(2) -0.019(3) C46 0.034(3) 0.076(4) 0.046(3) -0.013(3) -0.008(2) 0.000(3) C47 0.055(4) 0.119(6) 0.053(4) -0.024(4) -0.014(3) 0.019(4) C48 0.168(8) 0.134(7) 0.102(6) -0.077(5) -0.061(6) 0.090(6) C49 0.276(13) 0.121(7) 0.117(7) -0.060(6) -0.115(8) 0.121(8) C50 0.160(7) 0.086(5) 0.095(5) -0.036(4) -0.071(5) 0.059(5) C51 0.047(3) 0.070(4) 0.053(3) -0.009(3) -0.019(3) 0.005(3) C52 0.062(4) 0.124(5) 0.050(3) -0.025(3) -0.012(3) -0.007(4) C53 0.59(3) 0.160(10) 0.228(13) -0.138(9) -0.262(16) 0.247(14) C54 0.042(3) 0.061(3) 0.045(3) 0.007(2) -0.019(2) -0.015(2) C55 0.055(3) 0.037(3) 0.040(3) 0.002(2) 0.003(2) -0.002(2) C56 0.046(3) 0.040(3) 0.060(3) 0.008(2) -0.001(2) -0.010(2) C57 0.047(3) 0.046(3) 0.084(4) 0.007(3) -0.003(3) -0.009(3) C58 0.065(4) 0.068(4) 0.076(4) 0.002(3) -0.014(3) -0.027(3) C59 0.073(4) 0.078(4) 0.069(4) 0.016(3) -0.029(3) -0.015(3) C60 0.081(4) 0.045(3) 0.059(3) 0.007(3) -0.019(3) -0.002(3) C61 0.101(5) 0.036(3) 0.076(4) 0.005(3) -0.061(4) -0.007(3) C62 0.047(3) 0.068(4) 0.057(3) 0.017(3) -0.015(3) -0.020(3) C63 0.058(4) 0.071(4) 0.089(5) 0.034(3) -0.014(3) -0.012(3) C64 0.085(6) 0.067(5) 0.267(13) 0.049(6) -0.098(7) -0.009(4) C65 0.191(11) 0.095(7) 0.389(19) -0.076(9) -0.234(13) 0.049(7) C66 0.217(10) 0.095(6) 0.264(12) -0.090(7) -0.204(10) 0.080(6) C67 0.053(3) 0.034(3) 0.037(3) -0.003(2) -0.002(2) -0.003(2) C68 0.038(3) 0.041(3) 0.046(3) -0.006(2) -0.008(2) -0.006(2) C69 0.036(3) 0.052(3) 0.037(3) 0.004(2) -0.007(2) -0.012(2) C70 0.042(3) 0.041(3) 0.054(3) 0.009(2) -0.018(2) -0.009(2) C71 0.056(3) 0.037(3) 0.071(4) -0.003(3) 0.011(3) 0.003(2) C72 0.084(4) 0.042(3) 0.060(4) 0.001(3) 0.028(3) -0.005(3) C73 0.092(9) 0.030(5) 0.047(6) 0.008(4) -0.030(6) 0.017(5) C74 0.165(10) 0.052(5) 0.036(5) -0.005(4) -0.009(5) -0.015(6) C75 0.269(16) 0.044(6) 0.043(6) -0.009(4) -0.029(8) 0.011(8) C76 0.210(15) 0.068(8) 0.033(6) 0.005(5) 0.015(8) 0.057(9) C77 0.232(16) 0.044(8) 0.078(9) 0.007(6) 0.052(9) 0.017(8) C78 0.131(10) 0.056(6) 0.049(6) 0.013(5) 0.011(6) -0.002(6) C79 0.148(12) 0.37(2) 0.050(6) -0.032(10) -0.012(7) -0.201(15) C73B 0.031(9) 0.010(8) 0.043(10) 0.009(7) -0.016(7) 0.005(7) C74B 0.098(16) 0.107(17) 0.044(11) 0.007(11) -0.017(11) -0.043(14) C75B 0.12(2) 0.15(2) 0.049(13) 0.004(13) -0.035(13) -0.083(18) C76B 0.069(14) 0.073(15) 0.048(12) 0.012(10) -0.018(11) -0.028(12) C77B 0.15(3) 0.055(19) 0.036(15) -0.005(12) 0.039(15) 0.037(18) C78B 0.061(15) 0.13(3) 0.08(2) -0.049(19) 0.051(13) -0.017(18) C79B 0.21(3) 0.057(13) 0.082(16) 0.004(11) -0.117(19) -0.029(15) C1S 0.154(19) 0.27(2) 0.188(16) -0.083(15) -0.106(12) -0.025(16) C2S 0.086(12) 0.245(19) 0.242(17) -0.045(16) -0.077(12) -0.057(12) C3S 0.045(10) 0.31(2) 0.28(2) 0.016(16) -0.012(12) -0.043(12) C4S 0.18(2) 0.30(2) 0.30(2) -0.010(18) 0.037(16) -0.109(17) C5S 0.099(13) 0.30(2) 0.27(2) -0.078(18) 0.023(15) -0.113(13) C6S 0.076(13) 0.30(2) 0.26(3) -0.084(16) -0.062(16) -0.027(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 N2 2.033(3) . ? Zn1 C79 2.034(11) . ? Zn1 N1 2.043(3) . ? Zn1 C79B 2.21(2) . ? B1 C55 1.634(8) . ? B1 C61 1.637(8) . ? B1 C67 1.646(7) . ? B1 C73B 1.683(11) . ? B1 C73 1.734(7) . ? P1 N1 1.611(3) . ? P1 C19 1.790(4) . ? P1 C13 1.800(4) . ? P1 C2 1.814(4) . ? O1 C1 1.373(5) . ? O1 C12 1.383(4) . ? N1 C37 1.447(5) . ? C1 C2 1.387(5) . ? C1 C6 1.399(5) . ? P2 N2 1.603(4) . ? P2 C31 1.787(5) . ? P2 C25 1.799(4) . ? P2 C11 1.803(4) . ? N2 C46 1.472(6) . ? C2 C3 1.400(5) . ? C3 C4 1.398(6) . ? C3 H3 0.9500 . ? C4 C5 1.370(6) . ? C4 H4 0.9500 . ? C5 C6 1.389(6) . ? C5 H5 0.9500 . ? C6 C7 1.466(6) . ? C7 C8 1.389(5) . ? C7 C12 1.394(6) . ? C8 C9 1.382(6) . ? C8 H8 0.9500 . ? C9 C10 1.381(6) . ? C9 H9 0.9500 . ? C10 C11 1.409(5) . ? C10 H10 0.9500 . ? C11 C12 1.381(6) . ? C13 C18 1.394(6) . ? C13 C14 1.398(6) . ? C14 C15 1.391(7) . ? C14 H14 0.9500 . ? C15 C16 1.362(7) . ? C15 H15 0.9500 . ? C16 C17 1.393(7) . ? C16 H16 0.9500 . ? C17 C18 1.378(6) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.388(6) . ? C19 C24 1.392(6) . ? C20 C21 1.388(6) . ? C20 H20 0.9500 . ? C21 C22 1.349(8) . ? C21 H21 0.9500 . ? C22 C23 1.395(8) . ? C22 H22 0.9500 . ? C23 C24 1.405(7) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.387(6) . ? C25 C26 1.403(6) . ? C26 C27 1.378(6) . ? C26 H26 0.9500 . ? C27 C28 1.371(7) . ? C27 H27 0.9500 . ? C28 C29 1.368(7) . ? C28 H28 0.9500 . ? C29 C30 1.386(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.373(7) . ? C31 C36 1.399(6) . ? C32 C33 1.394(7) . ? C32 H32 0.9500 . ? C33 C34 1.366(8) . ? C33 H33 0.9500 . ? C34 C35 1.363(9) . ? C34 H34 0.9500 . ? C35 C36 1.366(8) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.399(6) . ? C37 C38 1.402(6) . ? C38 C39 1.373(7) . ? C38 C43 1.506(6) . ? C39 C40 1.385(8) . ? C39 H39 0.9500 . ? C40 C41 1.408(8) . ? C40 C44 1.523(7) . ? C41 C42 1.390(7) . ? C41 H41 0.9500 . ? C42 C45 1.507(6) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.390(7) . ? C46 C51 1.394(7) . ? C47 C48 1.399(9) . ? C47 C52 1.517(8) . ? C48 C49 1.361(10) . ? C48 H48 0.9500 . ? C49 C50 1.355(9) . ? C49 C53 1.558(11) . ? C50 C51 1.378(8) . ? C50 H50 0.9500 . ? C51 C54 1.501(6) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C60 1.395(7) . ? C55 C56 1.399(6) . ? C56 C57 1.373(6) . ? C56 H56 0.9500 . ? C57 C58 1.386(7) . ? C57 H57 0.9500 . ? C58 C59 1.384(7) . ? C58 H58 0.9500 . ? C59 C60 1.374(7) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C66 1.380(8) . ? C61 C62 1.383(7) . ? C62 C63 1.378(7) . ? C62 H62 0.9500 . ? C63 C64 1.363(9) . ? C63 H63 0.9500 . ? C64 C65 1.373(13) . ? C64 H64 0.9500 . ? C65 C66 1.366(13) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C68 1.393(6) . ? C67 C72 1.402(6) . ? C68 C69 1.379(6) . ? C68 H68 0.9500 . ? C69 C70 1.368(6) . ? C69 H69 0.9500 . ? C70 C71 1.363(6) . ? C70 H70 0.9500 . ? C71 C72 1.377(6) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.3900 . ? C73 C78 1.3900 . ? C74 C75 1.3900 . ? C74 H74 0.9500 . ? C75 C76 1.3900 . ? C75 H75 0.9500 . ? C76 C77 1.3900 . ? C76 H76 0.9500 . ? C77 C78 1.3900 . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C73B C74B 1.3900 . ? C73B C78B 1.3900 . ? C74B C75B 1.3900 . ? C74B H74B 0.9500 . ? C75B C76B 1.3900 . ? C75B H75B 0.9500 . ? C76B C77B 1.3900 . ? C76B H76B 0.9500 . ? C77B C78B 1.3900 . ? C77B H77B 0.9500 . ? C78B H78B 0.9500 . ? C79B H79D 0.9800 . ? C79B H79E 0.9800 . ? C79B H79F 0.9800 . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C1S H1S 0.9500 . ? 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 . ? 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 N2 Zn1 C79 113.5(3) . . ? N2 Zn1 N1 131.83(14) . . ? C79 Zn1 N1 114.2(3) . . ? N2 Zn1 C79B 120.1(6) . . ? C79 Zn1 C79B 35.8(8) . . ? N1 Zn1 C79B 102.4(5) . . ? C55 B1 C61 109.6(4) . . ? C55 B1 C67 110.3(4) . . ? C61 B1 C67 107.4(4) . . ? C55 B1 C73B 116.6(6) . . ? C61 B1 C73B 96.6(5) . . ? C67 B1 C73B 115.0(5) . . ? C55 B1 C73 104.0(4) . . ? C61 B1 C73 120.5(5) . . ? C67 B1 C73 104.8(4) . . ? C73B B1 C73 23.9(4) . . ? N1 P1 C19 112.77(19) . . ? N1 P1 C13 109.33(19) . . ? C19 P1 C13 109.3(2) . . ? N1 P1 C2 117.46(18) . . ? C19 P1 C2 103.68(19) . . ? C13 P1 C2 103.66(19) . . ? C1 O1 C12 105.6(3) . . ? C37 N1 P1 118.7(3) . . ? C37 N1 Zn1 110.1(2) . . ? P1 N1 Zn1 130.9(2) . . ? O1 C1 C2 123.5(3) . . ? O1 C1 C6 112.2(3) . . ? C2 C1 C6 124.3(4) . . ? N2 P2 C31 108.2(2) . . ? N2 P2 C25 114.4(2) . . ? C31 P2 C25 107.9(2) . . ? N2 P2 C11 115.94(18) . . ? C31 P2 C11 105.3(2) . . ? C25 P2 C11 104.45(19) . . ? C46 N2 P2 118.5(3) . . ? C46 N2 Zn1 114.2(3) . . ? P2 N2 Zn1 127.2(2) . . ? C1 C2 C3 115.0(4) . . ? C1 C2 P1 121.2(3) . . ? C3 C2 P1 123.0(3) . . ? C4 C3 C2 121.6(4) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 121.6(4) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 118.7(4) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C5 C6 C1 118.8(4) . . ? C5 C6 C7 136.2(4) . . ? C1 C6 C7 105.0(4) . . ? C8 C7 C12 118.6(4) . . ? C8 C7 C6 136.1(4) . . ? C12 C7 C6 105.3(3) . . ? C9 C8 C7 117.9(4) . . ? C9 C8 H8 121.1 . . ? C7 C8 H8 121.1 . . ? C10 C9 C8 122.3(4) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C9 C10 C11 121.7(4) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C12 C11 C10 114.2(4) . . ? C12 C11 P2 119.9(3) . . ? C10 C11 P2 125.9(3) . . ? C11 C12 O1 122.7(4) . . ? C11 C12 C7 125.4(4) . . ? O1 C12 C7 111.9(3) . . ? C18 C13 C14 118.9(4) . . ? C18 C13 P1 121.7(3) . . ? C14 C13 P1 119.4(4) . . ? C15 C14 C13 119.6(5) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C16 C15 C14 121.1(5) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 119.9(5) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 119.9(5) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C13 120.7(4) . . ? C17 C18 H18 119.6 . . ? C13 C18 H18 119.6 . . ? C20 C19 C24 119.4(4) . . ? C20 C19 P1 121.3(4) . . ? C24 C19 P1 119.2(4) . . ? C21 C20 C19 120.2(5) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C22 C21 C20 120.6(5) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 120.9(5) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C22 C23 C24 119.0(6) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C19 C24 C23 119.8(5) . . ? C19 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C30 C25 C26 119.0(4) . . ? C30 C25 P2 120.4(3) . . ? C26 C25 P2 120.6(4) . . ? C27 C26 C25 119.9(5) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C28 C27 C26 120.3(5) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C29 C28 C27 120.5(5) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 120.2(5) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C29 C30 C25 120.0(5) . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? C32 C31 C36 118.2(5) . . ? C32 C31 P2 121.8(4) . . ? C36 C31 P2 119.7(4) . . ? C31 C32 C33 120.6(5) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C34 C33 C32 119.6(6) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C35 C34 C33 120.5(6) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 120.3(6) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C31 120.7(6) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? C42 C37 C38 120.0(4) . . ? C42 C37 N1 120.4(4) . . ? C38 C37 N1 119.5(4) . . ? C39 C38 C37 119.7(5) . . ? C39 C38 C43 119.1(5) . . ? C37 C38 C43 121.1(4) . . ? C38 C39 C40 122.3(5) . . ? C38 C39 H39 118.8 . . ? C40 C39 H39 118.8 . . ? C39 C40 C41 117.1(5) . . ? C39 C40 C44 121.5(6) . . ? C41 C40 C44 121.4(6) . . ? C42 C41 C40 122.4(5) . . ? C42 C41 H41 118.8 . . ? C40 C41 H41 118.8 . . ? C41 C42 C37 118.4(5) . . ? C41 C42 C45 119.4(4) . . ? C37 C42 C45 122.2(4) . . ? C38 C43 H43A 109.5 . . ? C38 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C38 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 C44 H44A 109.5 . . ? C40 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C40 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 C51 120.7(5) . . ? C47 C46 N2 119.4(5) . . ? C51 C46 N2 119.9(4) . . ? C46 C47 C48 117.4(6) . . ? C46 C47 C52 123.3(6) . . ? C48 C47 C52 119.3(6) . . ? C49 C48 C47 122.3(6) . . ? C49 C48 H48 118.8 . . ? C47 C48 H48 118.8 . . ? C50 C49 C48 118.6(7) . . ? C50 C49 C53 119.8(8) . . ? C48 C49 C53 121.6(7) . . ? C49 C50 C51 122.4(7) . . ? C49 C50 H50 118.8 . . ? C51 C50 H50 118.8 . . ? C50 C51 C46 118.4(5) . . ? C50 C51 C54 118.5(5) . . ? C46 C51 C54 123.1(5) . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C49 C53 H53A 109.5 . . ? C49 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C49 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C60 C55 C56 114.3(5) . . ? C60 C55 B1 125.1(4) . . ? C56 C55 B1 120.6(4) . . ? C57 C56 C55 123.1(5) . . ? C57 C56 H56 118.4 . . ? C55 C56 H56 118.4 . . ? C56 C57 C58 120.4(5) . . ? C56 C57 H57 119.8 . . ? C58 C57 H57 119.8 . . ? C59 C58 C57 118.5(5) . . ? C59 C58 H58 120.8 . . ? C57 C58 H58 120.8 . . ? C60 C59 C58 119.7(5) . . ? C60 C59 H59 120.1 . . ? C58 C59 H59 120.1 . . ? C59 C60 C55 124.0(5) . . ? C59 C60 H60 118.0 . . ? C55 C60 H60 118.0 . . ? C66 C61 C62 112.2(6) . . ? C66 C61 B1 124.5(6) . . ? C62 C61 B1 122.8(4) . . ? C63 C62 C61 124.9(5) . . ? C63 C62 H62 117.5 . . ? C61 C62 H62 117.5 . . ? C64 C63 C62 119.7(7) . . ? C64 C63 H63 120.1 . . ? C62 C63 H63 120.1 . . ? C63 C64 C65 118.0(8) . . ? C63 C64 H64 121.0 . . ? C65 C64 H64 121.0 . . ? C66 C65 C64 120.0(8) . . ? C66 C65 H65 120.0 . . ? C64 C65 H65 120.0 . . ? C65 C66 C61 125.1(8) . . ? C65 C66 H66 117.5 . . ? C61 C66 H66 117.5 . . ? C68 C67 C72 113.8(4) . . ? C68 C67 B1 122.4(4) . . ? C72 C67 B1 123.8(4) . . ? C69 C68 C67 123.5(4) . . ? C69 C68 H68 118.2 . . ? C67 C68 H68 118.2 . . ? C70 C69 C68 120.1(4) . . ? C70 C69 H69 119.9 . . ? C68 C69 H69 119.9 . . ? C71 C70 C69 118.9(4) . . ? C71 C70 H70 120.5 . . ? C69 C70 H70 120.5 . . ? C70 C71 C72 120.5(5) . . ? C70 C71 H71 119.7 . . ? C72 C71 H71 119.7 . . ? C71 C72 C67 123.1(5) . . ? C71 C72 H72 118.5 . . ? C67 C72 H72 118.5 . . ? C74 C73 C78 120.0 . . ? C74 C73 B1 115.8(5) . . ? C78 C73 B1 124.0(5) . . ? C73 C74 C75 120.0 . . ? C73 C74 H74 120.0 . . ? C75 C74 H74 120.0 . . ? C76 C75 C74 120.0 . . ? C76 C75 H75 120.0 . . ? C74 C75 H75 120.0 . . ? C77 C76 C75 120.0 . . ? C77 C76 H76 120.0 . . ? C75 C76 H76 120.0 . . ? C76 C77 C78 120.0 . . ? C76 C77 H77 120.0 . . ? C78 C77 H77 120.0 . . ? C77 C78 C73 120.0 . . ? C77 C78 H78 120.0 . . ? C73 C78 H78 120.0 . . ? Zn1 C79 H79A 109.5 . . ? Zn1 C79 H79B 109.5 . . ? Zn1 C79 H79C 109.5 . . ? C74B C73B C78B 120.0 . . ? C74B C73B B1 131.3(7) . . ? C78B C73B B1 108.4(7) . . ? C75B C74B C73B 120.0 . . ? C75B C74B H74B 120.0 . . ? C73B C74B H74B 120.0 . . ? C76B C75B C74B 120.0 . . ? C76B C75B H75B 120.0 . . ? C74B C75B H75B 120.0 . . ? 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 C73B 120.0 . . ? C77B C78B H78B 120.0 . . ? C73B C78B H78B 120.0 . . ? Zn1 C79B H79D 109.5 . . ? Zn1 C79B H79E 109.5 . . ? H79D C79B H79E 109.5 . . ? Zn1 C79B H79F 109.5 . . ? H79D C79B H79F 109.5 . . ? H79E C79B H79F 109.5 . . ? C2S C1S C6S 120.0 . . ? C2S C1S H1S 120.0 . . ? C6S C1S H1S 120.0 . . ? C3S C2S C1S 120.0 . . ? C3S C2S H2S 120.0 . . ? C1S C2S H2S 120.0 . . ? C2S C3S C4S 120.0 . . ? C2S C3S H3S 120.0 . . ? C4S C3S H3S 120.0 . . ? C3S C4S C5S 120.0 . . ? C3S C4S H4S 120.0 . . ? C5S C4S H4S 120.0 . . ? C6S C5S C4S 120.0 . . ? C6S C5S H5S 120.0 . . ? C4S C5S H5S 120.0 . . ? C5S C6S C1S 120.0 . . ? C5S C6S H6S 120.0 . . ? C1S C6S H6S 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 C19 P1 N1 C37 17.8(4) . . . . ? C13 P1 N1 C37 139.7(3) . . . . ? C2 P1 N1 C37 -102.7(3) . . . . ? C19 P1 N1 Zn1 -156.2(2) . . . . ? C13 P1 N1 Zn1 -34.3(3) . . . . ? C2 P1 N1 Zn1 83.4(3) . . . . ? N2 Zn1 N1 C37 134.2(3) . . . . ? C79 Zn1 N1 C37 -54.1(6) . . . . ? C79B Zn1 N1 C37 -18.4(8) . . . . ? N2 Zn1 N1 P1 -51.5(3) . . . . ? C79 Zn1 N1 P1 120.3(6) . . . . ? C79B Zn1 N1 P1 156.0(8) . . . . ? C12 O1 C1 C2 -176.7(4) . . . . ? C12 O1 C1 C6 1.8(4) . . . . ? C31 P2 N2 C46 152.8(3) . . . . ? C25 P2 N2 C46 32.6(4) . . . . ? C11 P2 N2 C46 -89.2(4) . . . . ? C31 P2 N2 Zn1 -25.0(3) . . . . ? C25 P2 N2 Zn1 -145.3(2) . . . . ? C11 P2 N2 Zn1 93.0(3) . . . . ? C79 Zn1 N2 C46 -56.2(6) . . . . ? N1 Zn1 N2 C46 115.6(3) . . . . ? C79B Zn1 N2 C46 -95.8(8) . . . . ? C79 Zn1 N2 P2 121.7(6) . . . . ? N1 Zn1 N2 P2 -66.5(3) . . . . ? C79B Zn1 N2 P2 82.2(8) . . . . ? O1 C1 C2 C3 -179.8(4) . . . . ? C6 C1 C2 C3 1.9(6) . . . . ? O1 C1 C2 P1 10.3(6) . . . . ? C6 C1 C2 P1 -167.9(3) . . . . ? N1 P1 C2 C1 -37.4(4) . . . . ? C19 P1 C2 C1 -162.5(3) . . . . ? C13 P1 C2 C1 83.3(4) . . . . ? N1 P1 C2 C3 153.6(3) . . . . ? C19 P1 C2 C3 28.5(4) . . . . ? C13 P1 C2 C3 -85.7(4) . . . . ? C1 C2 C3 C4 -1.0(6) . . . . ? P1 C2 C3 C4 168.7(3) . . . . ? C2 C3 C4 C5 -0.7(7) . . . . ? C3 C4 C5 C6 1.5(6) . . . . ? C4 C5 C6 C1 -0.6(6) . . . . ? C4 C5 C6 C7 -178.4(4) . . . . ? O1 C1 C6 C5 -179.6(3) . . . . ? C2 C1 C6 C5 -1.2(6) . . . . ? O1 C1 C6 C7 -1.2(4) . . . . ? C2 C1 C6 C7 177.2(4) . . . . ? C5 C6 C7 C8 -0.1(9) . . . . ? C1 C6 C7 C8 -178.0(5) . . . . ? C5 C6 C7 C12 178.1(5) . . . . ? C1 C6 C7 C12 0.2(4) . . . . ? C12 C7 C8 C9 -0.2(6) . . . . ? C6 C7 C8 C9 177.9(4) . . . . ? C7 C8 C9 C10 0.0(7) . . . . ? C8 C9 C10 C11 -0.5(7) . . . . ? C9 C10 C11 C12 1.3(6) . . . . ? C9 C10 C11 P2 -179.8(3) . . . . ? N2 P2 C11 C12 -41.0(4) . . . . ? C31 P2 C11 C12 78.6(4) . . . . ? C25 P2 C11 C12 -167.9(4) . . . . ? N2 P2 C11 C10 140.1(4) . . . . ? C31 P2 C11 C10 -100.3(4) . . . . ? C25 P2 C11 C10 13.2(4) . . . . ? C10 C11 C12 O1 -179.8(4) . . . . ? P2 C11 C12 O1 1.1(6) . . . . ? C10 C11 C12 C7 -1.6(6) . . . . ? P2 C11 C12 C7 179.4(3) . . . . ? C1 O1 C12 C11 176.8(4) . . . . ? C1 O1 C12 C7 -1.6(4) . . . . ? C8 C7 C12 C11 1.1(6) . . . . ? C6 C7 C12 C11 -177.5(4) . . . . ? C8 C7 C12 O1 179.5(3) . . . . ? C6 C7 C12 O1 0.9(4) . . . . ? N1 P1 C13 C18 154.9(3) . . . . ? C19 P1 C13 C18 -81.2(4) . . . . ? C2 P1 C13 C18 28.8(4) . . . . ? N1 P1 C13 C14 -25.0(4) . . . . ? C19 P1 C13 C14 98.9(4) . . . . ? C2 P1 C13 C14 -151.1(3) . . . . ? C18 C13 C14 C15 -0.5(6) . . . . ? P1 C13 C14 C15 179.4(3) . . . . ? C13 C14 C15 C16 -0.2(7) . . . . ? C14 C15 C16 C17 0.5(8) . . . . ? C15 C16 C17 C18 -0.2(7) . . . . ? C16 C17 C18 C13 -0.5(7) . . . . ? C14 C13 C18 C17 0.8(6) . . . . ? P1 C13 C18 C17 -179.1(3) . . . . ? N1 P1 C19 C20 111.8(4) . . . . ? C13 P1 C19 C20 -10.0(4) . . . . ? C2 P1 C19 C20 -120.1(4) . . . . ? N1 P1 C19 C24 -67.5(4) . . . . ? C13 P1 C19 C24 170.6(4) . . . . ? C2 P1 C19 C24 60.6(4) . . . . ? C24 C19 C20 C21 -0.5(7) . . . . ? P1 C19 C20 C21 -179.9(3) . . . . ? C19 C20 C21 C22 0.3(7) . . . . ? C20 C21 C22 C23 0.0(8) . . . . ? C21 C22 C23 C24 -0.1(8) . . . . ? C20 C19 C24 C23 0.4(7) . . . . ? P1 C19 C24 C23 179.8(4) . . . . ? C22 C23 C24 C19 -0.1(7) . . . . ? N2 P2 C25 C30 -62.8(4) . . . . ? C31 P2 C25 C30 176.8(4) . . . . ? C11 P2 C25 C30 65.0(4) . . . . ? N2 P2 C25 C26 116.0(4) . . . . ? C31 P2 C25 C26 -4.4(4) . . . . ? C11 P2 C25 C26 -116.2(4) . . . . ? C30 C25 C26 C27 0.8(7) . . . . ? P2 C25 C26 C27 -178.0(4) . . . . ? C25 C26 C27 C28 0.6(8) . . . . ? C26 C27 C28 C29 -1.0(8) . . . . ? C27 C28 C29 C30 0.1(8) . . . . ? C28 C29 C30 C25 1.3(7) . . . . ? C26 C25 C30 C29 -1.8(7) . . . . ? P2 C25 C30 C29 177.1(4) . . . . ? N2 P2 C31 C32 144.3(4) . . . . ? C25 P2 C31 C32 -91.4(4) . . . . ? C11 P2 C31 C32 19.7(4) . . . . ? N2 P2 C31 C36 -42.0(4) . . . . ? C25 P2 C31 C36 82.3(4) . . . . ? C11 P2 C31 C36 -166.5(4) . . . . ? C36 C31 C32 C33 0.8(7) . . . . ? P2 C31 C32 C33 174.6(4) . . . . ? C31 C32 C33 C34 -0.9(8) . . . . ? C32 C33 C34 C35 0.4(10) . . . . ? C33 C34 C35 C36 0.1(10) . . . . ? C34 C35 C36 C31 -0.2(9) . . . . ? C32 C31 C36 C35 -0.2(7) . . . . ? P2 C31 C36 C35 -174.2(4) . . . . ? P1 N1 C37 C42 -86.5(4) . . . . ? Zn1 N1 C37 C42 88.7(4) . . . . ? P1 N1 C37 C38 95.8(4) . . . . ? Zn1 N1 C37 C38 -89.1(4) . . . . ? C42 C37 C38 C39 0.3(7) . . . . ? N1 C37 C38 C39 178.0(4) . . . . ? C42 C37 C38 C43 179.5(4) . . . . ? N1 C37 C38 C43 -2.7(6) . . . . ? C37 C38 C39 C40 1.0(8) . . . . ? C43 C38 C39 C40 -178.2(5) . . . . ? C38 C39 C40 C41 -1.3(8) . . . . ? C38 C39 C40 C44 -179.0(5) . . . . ? C39 C40 C41 C42 0.3(8) . . . . ? C44 C40 C41 C42 178.0(5) . . . . ? C40 C41 C42 C37 1.0(7) . . . . ? C40 C41 C42 C45 -179.7(5) . . . . ? C38 C37 C42 C41 -1.3(7) . . . . ? N1 C37 C42 C41 -178.9(4) . . . . ? C38 C37 C42 C45 179.4(4) . . . . ? N1 C37 C42 C45 1.8(6) . . . . ? P2 N2 C46 C47 -86.9(5) . . . . ? Zn1 N2 C46 C47 91.3(5) . . . . ? P2 N2 C46 C51 93.9(5) . . . . ? Zn1 N2 C46 C51 -88.0(5) . . . . ? C51 C46 C47 C48 -2.5(9) . . . . ? N2 C46 C47 C48 178.3(6) . . . . ? C51 C46 C47 C52 179.3(5) . . . . ? N2 C46 C47 C52 0.0(8) . . . . ? C46 C47 C48 C49 0.7(13) . . . . ? C52 C47 C48 C49 179.1(9) . . . . ? C47 C48 C49 C50 0.8(17) . . . . ? C47 C48 C49 C53 -178.4(11) . . . . ? C48 C49 C50 C51 -0.6(16) . . . . ? C53 C49 C50 C51 178.6(10) . . . . ? C49 C50 C51 C46 -1.1(12) . . . . ? C49 C50 C51 C54 179.7(9) . . . . ? C47 C46 C51 C50 2.7(8) . . . . ? N2 C46 C51 C50 -178.1(5) . . . . ? C47 C46 C51 C54 -178.1(5) . . . . ? N2 C46 C51 C54 1.1(7) . . . . ? C61 B1 C55 C60 132.3(5) . . . . ? C67 B1 C55 C60 14.3(7) . . . . ? C73B B1 C55 C60 -119.3(6) . . . . ? C73 B1 C55 C60 -97.6(5) . . . . ? C61 B1 C55 C56 -49.8(6) . . . . ? C67 B1 C55 C56 -167.9(4) . . . . ? C73B B1 C55 C56 58.6(7) . . . . ? C73 B1 C55 C56 80.2(5) . . . . ? C60 C55 C56 C57 -1.1(7) . . . . ? B1 C55 C56 C57 -179.2(5) . . . . ? C55 C56 C57 C58 0.6(8) . . . . ? C56 C57 C58 C59 -0.1(8) . . . . ? C57 C58 C59 C60 0.1(8) . . . . ? C58 C59 C60 C55 -0.7(9) . . . . ? C56 C55 C60 C59 1.2(7) . . . . ? B1 C55 C60 C59 179.2(5) . . . . ? C55 B1 C61 C66 161.3(7) . . . . ? C67 B1 C61 C66 -78.9(8) . . . . ? C73B B1 C61 C66 40.0(9) . . . . ? C73 B1 C61 C66 40.8(9) . . . . ? C55 B1 C61 C62 -27.4(7) . . . . ? C67 B1 C61 C62 92.5(6) . . . . ? C73B B1 C61 C62 -148.7(6) . . . . ? C73 B1 C61 C62 -147.9(5) . . . . ? C66 C61 C62 C63 -0.2(8) . . . . ? B1 C61 C62 C63 -172.5(5) . . . . ? C61 C62 C63 C64 -1.0(8) . . . . ? C62 C63 C64 C65 0.4(11) . . . . ? C63 C64 C65 C66 1.3(16) . . . . ? C64 C65 C66 C61 -2.8(18) . . . . ? C62 C61 C66 C65 2.2(13) . . . . ? B1 C61 C66 C65 174.3(9) . . . . ? C55 B1 C67 C68 87.7(6) . . . . ? C61 B1 C67 C68 -31.7(6) . . . . ? C73B B1 C67 C68 -138.0(6) . . . . ? C73 B1 C67 C68 -160.9(4) . . . . ? C55 B1 C67 C72 -90.4(6) . . . . ? C61 B1 C67 C72 150.2(5) . . . . ? C73B B1 C67 C72 44.0(8) . . . . ? C73 B1 C67 C72 21.0(7) . . . . ? C72 C67 C68 C69 -3.1(7) . . . . ? B1 C67 C68 C69 178.7(4) . . . . ? C67 C68 C69 C70 0.8(7) . . . . ? C68 C69 C70 C71 1.8(7) . . . . ? C69 C70 C71 C72 -1.7(8) . . . . ? C70 C71 C72 C67 -0.8(9) . . . . ? C68 C67 C72 C71 3.1(8) . . . . ? B1 C67 C72 C71 -178.7(5) . . . . ? C55 B1 C73 C74 172.1(4) . . . . ? C61 B1 C73 C74 -64.6(6) . . . . ? C67 B1 C73 C74 56.3(5) . . . . ? C73B B1 C73 C74 -62.7(12) . . . . ? C55 B1 C73 C78 -13.0(6) . . . . ? C61 B1 C73 C78 110.3(5) . . . . ? C67 B1 C73 C78 -128.8(4) . . . . ? C73B B1 C73 C78 112.2(13) . . . . ? C78 C73 C74 C75 0.0 . . . . ? B1 C73 C74 C75 175.1(5) . . . . ? C73 C74 C75 C76 0.0 . . . . ? C74 C75 C76 C77 0.0 . . . . ? C75 C76 C77 C78 0.0 . . . . ? C76 C77 C78 C73 0.0 . . . . ? C74 C73 C78 C77 0.0 . . . . ? B1 C73 C78 C77 -174.7(5) . . . . ? C55 B1 C73B C74B -137.7(9) . . . . ? C61 B1 C73B C74B -21.8(10) . . . . ? C67 B1 C73B C74B 90.9(10) . . . . ? C73 B1 C73B C74B 159.8(19) . . . . ? C55 B1 C73B C78B 48.2(8) . . . . ? C61 B1 C73B C78B 164.1(7) . . . . ? C67 B1 C73B C78B -83.2(8) . . . . ? C73 B1 C73B C78B -14.2(11) . . . . ? C78B C73B C74B C75B 0.0 . . . . ? B1 C73B C74B C75B -173.5(11) . . . . ? C73B C74B C75B C76B 0.0 . . . . ? C74B C75B C76B C77B 0.0 . . . . ? C75B C76B C77B C78B 0.0 . . . . ? C76B C77B C78B C73B 0.0 . . . . ? C74B C73B C78B C77B 0.0 . . . . ? B1 C73B C78B C77B 174.9(9) . . . . ? C6S C1S C2S C3S 0.0 . . . . ? 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 . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.499 _refine_diff_density_min -0.935 _refine_diff_density_rms 0.062 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 753816' #TrackingRef 'XRay-revised_-_Manuscript_B922543A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H77 B N2 O3 P2 Zn' _chemical_formula_weight 1324.62 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 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 17.8781(11) _cell_length_b 21.6874(13) _cell_length_c 19.8464(12) _cell_angle_alpha 90.00 _cell_angle_beta 101.0830(10) _cell_angle_gamma 90.00 _cell_volume 7551.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 0.416 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6748 _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 90217 _diffrn_reflns_av_R_equivalents 0.1224 _diffrn_reflns_av_sigmaI/netI 0.0958 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.03 _reflns_number_total 13330 _reflns_number_gt 8079 _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^)+(0.0715P)^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 13330 _refine_ls_number_parameters 755 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1138 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1544 _refine_ls_wR_factor_gt 0.1378 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.25154(3) 0.68882(2) 0.42366(2) 0.03301(15) Uani 1 1 d . . . P1 P 0.17335(6) 0.63140(4) 0.27718(5) 0.0276(2) Uani 1 1 d . . . O1 O 0.34363(13) 0.66456(11) 0.31142(11) 0.0282(6) Uani 1 1 d . . . N1 N 0.17959(16) 0.68396(13) 0.33502(14) 0.0268(7) Uani 1 1 d . . . C1 C 0.3146(2) 0.65147(16) 0.24343(17) 0.0265(9) Uani 1 1 d . . . B1 B 0.2787(3) 0.4032(2) 0.0290(2) 0.0315(11) Uani 1 1 d . . . P2 P 0.43261(6) 0.71281(4) 0.44959(5) 0.0260(2) Uani 1 1 d . . . N2 N 0.35961(16) 0.67570(13) 0.46530(14) 0.0265(7) Uani 1 1 d . . . C2 C 0.2386(2) 0.63896(15) 0.21874(18) 0.0262(9) Uani 1 1 d . . . C3 C 0.2199(2) 0.62647(17) 0.14830(18) 0.0324(9) Uani 1 1 d . . . H3 H 0.1684 0.6179 0.1280 0.039 Uiso 1 1 calc R . . C4 C 0.2747(2) 0.62634(18) 0.10748(19) 0.0398(10) Uani 1 1 d . . . H4 H 0.2597 0.6184 0.0597 0.048 Uiso 1 1 calc R . . C5 C 0.3513(2) 0.63767(16) 0.13483(19) 0.0344(10) Uani 1 1 d . . . H5 H 0.3886 0.6366 0.1067 0.041 Uiso 1 1 calc R . . C6 C 0.3714(2) 0.65052(16) 0.20468(18) 0.0290(9) Uani 1 1 d . . . C7 C 0.4421(2) 0.66425(15) 0.25221(18) 0.0265(9) Uani 1 1 d . . . C8 C 0.5185(2) 0.67160(16) 0.2489(2) 0.0320(9) Uani 1 1 d . . . H8 H 0.5349 0.6673 0.2064 0.038 Uiso 1 1 calc R . . C9 C 0.5698(2) 0.68519(17) 0.3077(2) 0.0363(10) Uani 1 1 d . . . H9 H 0.6223 0.6893 0.3058 0.044 Uiso 1 1 calc R . . C10 C 0.5464(2) 0.69304(16) 0.3704(2) 0.0322(9) Uani 1 1 d . . . H10 H 0.5834 0.7026 0.4102 0.039 Uiso 1 1 calc R . . C11 C 0.4700(2) 0.68715(15) 0.37614(18) 0.0253(8) Uani 1 1 d . . . C12 C 0.4210(2) 0.67232(15) 0.31600(18) 0.0260(9) Uani 1 1 d . . . C13 C 0.19594(15) 0.55791(9) 0.31728(12) 0.0302(9) Uani 1 1 d G . . C14 C 0.17934(15) 0.54669(11) 0.38179(12) 0.0405(10) Uani 1 1 d G . . H14 H 0.1593 0.5787 0.4057 0.049 Uiso 1 1 calc R . . C15 C 0.19213(17) 0.48859(13) 0.41131(11) 0.0529(12) Uani 1 1 d G . . H15 H 0.1808 0.4809 0.4554 0.064 Uiso 1 1 calc R . . C16 C 0.22152(17) 0.44170(9) 0.37634(15) 0.0569(13) Uani 1 1 d G . . H16 H 0.2303 0.4020 0.3965 0.068 Uiso 1 1 calc R . . C17 C 0.23812(15) 0.45292(10) 0.31184(14) 0.0462(11) Uani 1 1 d G . . H17 H 0.2582 0.4209 0.2879 0.055 Uiso 1 1 calc R . . C18 C 0.22533(15) 0.51102(12) 0.28231(11) 0.0370(10) Uani 1 1 d G . . H18 H 0.2367 0.5187 0.2382 0.044 Uiso 1 1 calc R . . C19 C 0.08122(11) 0.62548(11) 0.22228(11) 0.0295(9) Uani 1 1 d G . . C20 C 0.05327(14) 0.67495(9) 0.18040(13) 0.0374(10) Uani 1 1 d G . . H20 H 0.0809 0.7126 0.1837 0.045 Uiso 1 1 calc R . . C21 C -0.01506(14) 0.66930(11) 0.13365(12) 0.0443(11) Uani 1 1 d G . . H21 H -0.0342 0.7031 0.1050 0.053 Uiso 1 1 calc R . . C22 C -0.05542(11) 0.61419(13) 0.12879(12) 0.0471(11) Uani 1 1 d G . . H22 H -0.1021 0.6103 0.0968 0.057 Uiso 1 1 calc R . . C23 C -0.02747(14) 0.56472(10) 0.17067(14) 0.0421(11) Uani 1 1 d G . . H23 H -0.0551 0.5271 0.1674 0.051 Uiso 1 1 calc R . . C24 C 0.04086(14) 0.57037(9) 0.21742(12) 0.0359(10) Uani 1 1 d G . . H24 H 0.0600 0.5366 0.2460 0.043 Uiso 1 1 calc R . . C25 C 0.1293(2) 0.73757(17) 0.32166(18) 0.0323(9) Uani 1 1 d . . . C26 C 0.1546(2) 0.79129(18) 0.2942(2) 0.0386(10) Uani 1 1 d . . . C27 C 0.1060(3) 0.84197(19) 0.2846(2) 0.0561(13) Uani 1 1 d . . . H27 H 0.1225 0.8787 0.2658 0.067 Uiso 1 1 calc R . . C28 C 0.0346(3) 0.8405(2) 0.3014(3) 0.0673(15) Uani 1 1 d . . . C29 C 0.0110(3) 0.7873(2) 0.3277(2) 0.0554(13) Uani 1 1 d . . . H29 H -0.0385 0.7859 0.3384 0.066 Uiso 1 1 calc R . . C30 C 0.0570(2) 0.73497(18) 0.3395(2) 0.0372(10) Uani 1 1 d . . . C31 C 0.2315(3) 0.79587(19) 0.2761(2) 0.0479(12) Uani 1 1 d . . . H31A H 0.2706 0.7867 0.3167 0.072 Uiso 1 1 calc R . . H31B H 0.2392 0.8377 0.2601 0.072 Uiso 1 1 calc R . . H31C H 0.2354 0.7662 0.2396 0.072 Uiso 1 1 calc R . . C32 C -0.0178(3) 0.8964(2) 0.2883(4) 0.106(2) Uani 1 1 d . . . H32A H -0.0685 0.8833 0.2646 0.160 Uiso 1 1 calc R . . H32B H 0.0031 0.9262 0.2597 0.160 Uiso 1 1 calc R . . H32C H -0.0216 0.9156 0.3322 0.160 Uiso 1 1 calc R . . C33 C 0.0272(2) 0.6789(2) 0.3685(2) 0.0478(12) Uani 1 1 d . . . H33A H -0.0209 0.6887 0.3828 0.072 Uiso 1 1 calc R . . H33B H 0.0644 0.6645 0.4083 0.072 Uiso 1 1 calc R . . H33C H 0.0185 0.6464 0.3336 0.072 Uiso 1 1 calc R . . C34 C 0.40768(14) 0.79180(8) 0.42826(12) 0.0267(9) Uani 1 1 d G . . C35 C 0.44454(13) 0.82451(10) 0.38398(12) 0.0338(10) Uani 1 1 d G . . H35 H 0.4830 0.8051 0.3645 0.041 Uiso 1 1 calc R . . C36 C 0.42505(15) 0.88559(10) 0.36822(12) 0.0399(10) Uani 1 1 d G . . H36 H 0.4502 0.9080 0.3380 0.048 Uiso 1 1 calc R . . C37 C 0.36871(15) 0.91396(8) 0.39673(13) 0.0427(11) Uani 1 1 d G . . H37 H 0.3554 0.9557 0.3860 0.051 Uiso 1 1 calc R . . C38 C 0.33186(14) 0.88124(11) 0.44100(13) 0.0464(11) Uani 1 1 d G . . H38 H 0.2934 0.9006 0.4605 0.056 Uiso 1 1 calc R . . C39 C 0.35135(14) 0.82016(10) 0.45676(12) 0.0363(10) Uani 1 1 d G . . H39 H 0.3262 0.7978 0.4870 0.044 Uiso 1 1 calc R . . C40 C 0.51173(12) 0.70868(10) 0.51984(10) 0.0265(9) Uani 1 1 d G . . C41 C 0.54204(14) 0.65103(9) 0.53988(12) 0.0358(10) Uani 1 1 d G . . H41 H 0.5229 0.6154 0.5145 0.043 Uiso 1 1 calc R . . C42 C 0.60029(14) 0.64557(10) 0.59706(13) 0.0442(11) Uani 1 1 d G . . H42 H 0.6210 0.6062 0.6108 0.053 Uiso 1 1 calc R . . C43 C 0.62823(13) 0.69775(13) 0.63420(11) 0.0453(11) Uani 1 1 d G . . H43 H 0.6680 0.6940 0.6733 0.054 Uiso 1 1 calc R . . C44 C 0.59792(14) 0.75540(11) 0.61416(12) 0.0396(10) Uani 1 1 d G . . H44 H 0.6170 0.7911 0.6395 0.048 Uiso 1 1 calc R . . C45 C 0.53967(14) 0.76087(8) 0.55698(12) 0.0304(9) Uani 1 1 d G . . H45 H 0.5190 0.8003 0.5433 0.037 Uiso 1 1 calc R . . C46 C 0.3715(2) 0.62604(17) 0.51583(18) 0.0281(9) Uani 1 1 d . . . C47 C 0.3704(2) 0.64019(17) 0.58499(19) 0.0345(10) Uani 1 1 d . . . C48 C 0.3823(2) 0.59248(19) 0.6327(2) 0.0438(11) Uani 1 1 d . . . H48 H 0.3829 0.6017 0.6796 0.053 Uiso 1 1 calc R . . C49 C 0.3936(3) 0.5318(2) 0.6142(2) 0.0485(12) Uani 1 1 d . . . C50 C 0.3934(2) 0.51965(18) 0.5457(2) 0.0424(11) Uani 1 1 d . . . H50 H 0.4003 0.4784 0.5321 0.051 Uiso 1 1 calc R . . C51 C 0.3835(2) 0.56552(17) 0.4964(2) 0.0319(9) Uani 1 1 d . . . C52 C 0.3589(2) 0.70403(17) 0.6094(2) 0.0408(11) Uani 1 1 d . . . H52A H 0.3550 0.7028 0.6579 0.061 Uiso 1 1 calc R . . H52B H 0.3119 0.7213 0.5823 0.061 Uiso 1 1 calc R . . H52C H 0.4023 0.7299 0.6038 0.061 Uiso 1 1 calc R . . C53 C 0.4052(3) 0.4809(2) 0.6682(2) 0.0727(16) Uani 1 1 d . . . H53A H 0.3671 0.4484 0.6547 0.109 Uiso 1 1 calc R . . H53B H 0.3994 0.4981 0.7126 0.109 Uiso 1 1 calc R . . H53C H 0.4564 0.4635 0.6721 0.109 Uiso 1 1 calc R . . C54 C 0.3887(2) 0.54920(18) 0.42345(19) 0.0384(10) Uani 1 1 d . . . H54A H 0.4373 0.5641 0.4137 0.058 Uiso 1 1 calc R . . H54B H 0.3465 0.5686 0.3917 0.058 Uiso 1 1 calc R . . H54C H 0.3857 0.5043 0.4176 0.058 Uiso 1 1 calc R . . C57 C 0.21105(13) 0.45849(10) 0.01885(13) 0.0353(10) Uani 1 1 d G . . C58 C 0.16474(16) 0.46165(12) 0.06755(12) 0.0428(11) Uani 1 1 d G . . H58 H 0.1728 0.4341 0.1054 0.051 Uiso 1 1 calc R . . C59 C 0.10670(14) 0.50517(14) 0.06081(14) 0.0547(13) Uani 1 1 d G . . H59 H 0.0751 0.5073 0.0941 0.066 Uiso 1 1 calc R . . C60 C 0.09497(13) 0.54553(11) 0.00537(17) 0.0556(13) Uani 1 1 d G . . H60 H 0.0553 0.5753 0.0008 0.067 Uiso 1 1 calc R . . C61 C 0.14128(16) 0.54237(11) -0.04333(13) 0.0472(12) Uani 1 1 d G . . H61 H 0.1333 0.5700 -0.0812 0.057 Uiso 1 1 calc R . . C62 C 0.19932(14) 0.49885(12) -0.03659(12) 0.0376(10) Uani 1 1 d G . . H62 H 0.2310 0.4967 -0.0699 0.045 Uiso 1 1 calc R . . C63 C 0.33719(13) 0.41247(11) -0.02795(11) 0.0320(9) Uani 1 1 d G . . C64 C 0.30696(12) 0.40533(12) -0.09745(12) 0.0380(10) Uani 1 1 d G . . H64 H 0.2550 0.3940 -0.1119 0.046 Uiso 1 1 calc R . . C65 C 0.35273(16) 0.41475(12) -0.14576(9) 0.0438(11) Uani 1 1 d G . . H65 H 0.3321 0.4099 -0.1933 0.053 Uiso 1 1 calc R . . C66 C 0.42872(15) 0.43132(12) -0.12457(13) 0.0471(12) Uani 1 1 d G . . H66 H 0.4600 0.4378 -0.1576 0.057 Uiso 1 1 calc R . . C67 C 0.45895(11) 0.43846(12) -0.05507(14) 0.0405(11) Uani 1 1 d G . . H67 H 0.5109 0.4498 -0.0406 0.049 Uiso 1 1 calc R . . C68 C 0.41318(14) 0.42903(11) -0.00676(10) 0.0365(10) Uani 1 1 d G . . H68 H 0.4338 0.4339 0.0407 0.044 Uiso 1 1 calc R . . C69 C 0.23784(14) 0.33215(9) 0.01654(13) 0.0341(10) Uani 1 1 d G . . C70 C 0.16201(14) 0.32152(11) 0.02001(13) 0.0387(10) Uani 1 1 d G . . H70 H 0.1304 0.3548 0.0282 0.046 Uiso 1 1 calc R . . C71 C 0.13241(13) 0.26215(14) 0.01154(14) 0.0523(12) Uani 1 1 d G . . H71 H 0.0806 0.2549 0.0139 0.063 Uiso 1 1 calc R . . C72 C 0.17864(18) 0.21341(10) -0.00041(14) 0.0563(13) Uani 1 1 d G . . H72 H 0.1584 0.1728 -0.0062 0.068 Uiso 1 1 calc R . . C73 C 0.25448(17) 0.22404(10) -0.00389(14) 0.0528(12) Uani 1 1 d G . . H73 H 0.2861 0.1907 -0.0121 0.063 Uiso 1 1 calc R . . C74 C 0.28408(12) 0.28342(12) 0.00459(14) 0.0416(11) Uani 1 1 d G . . H74 H 0.3359 0.2907 0.0022 0.050 Uiso 1 1 calc R . . C75 C 0.33094(13) 0.40878(11) 0.10953(10) 0.0306(9) Uani 1 1 d G . . C76 C 0.34776(15) 0.46737(9) 0.13661(12) 0.0412(11) Uani 1 1 d G . . H76 H 0.3278 0.5027 0.1111 0.049 Uiso 1 1 calc R . . C77 C 0.39383(15) 0.47427(10) 0.20107(13) 0.0447(11) Uani 1 1 d G . . H77 H 0.4053 0.5143 0.2196 0.054 Uiso 1 1 calc R . . C78 C 0.42309(14) 0.42256(13) 0.23844(10) 0.0458(11) Uani 1 1 d G . . H78 H 0.4546 0.4273 0.2825 0.055 Uiso 1 1 calc R . . C79 C 0.40627(14) 0.36397(10) 0.21137(12) 0.0417(11) Uani 1 1 d G . . H79 H 0.4263 0.3286 0.2369 0.050 Uiso 1 1 calc R . . C80 C 0.36020(14) 0.35707(9) 0.14691(12) 0.0364(10) Uani 1 1 d G . . H80 H 0.3487 0.3170 0.1284 0.044 Uiso 1 1 calc R . . C1S C 0.20427(19) 0.29490(14) 0.21810(19) 0.0637(14) Uani 1 1 d G . . H1S H 0.2113 0.3353 0.2019 0.076 Uiso 1 1 calc R . . C2S C 0.18154(19) 0.28676(15) 0.28067(18) 0.0712(15) Uani 1 1 d G . . H2S H 0.1730 0.3216 0.3072 0.085 Uiso 1 1 calc R . . C3S C 0.1713(2) 0.22764(19) 0.30439(14) 0.0714(16) Uani 1 1 d G . . H3S H 0.1558 0.2221 0.3472 0.086 Uiso 1 1 calc R . . C4S C 0.1837(2) 0.17667(14) 0.26555(18) 0.0749(16) Uani 1 1 d G . . H4S H 0.1767 0.1363 0.2818 0.090 Uiso 1 1 calc R . . C5S C 0.20647(19) 0.18481(15) 0.20299(17) 0.0681(15) Uani 1 1 d G . . H5S H 0.2150 0.1500 0.1764 0.082 Uiso 1 1 calc R . . C6S C 0.21674(17) 0.24392(18) 0.17926(14) 0.0614(14) Uani 1 1 d G . . H6S H 0.2323 0.2495 0.1365 0.074 Uiso 1 1 calc R . . O2 O 0.18899(18) 0.6592(2) 0.49632(15) 0.0668(10) Uani 1 1 d U . . O3 O 0.20299(18) 0.75770(17) 0.47439(17) 0.0617(9) Uani 1 1 d U . . C55 C 0.1741(3) 0.7160(4) 0.5060(3) 0.0782(18) Uani 1 1 d U . . C56 C 0.1241(4) 0.7321(4) 0.5555(4) 0.148(4) Uani 1 1 d U . . H56A H 0.1557 0.7425 0.6001 0.222 Uiso 1 1 calc R . . H56B H 0.0915 0.6968 0.5609 0.222 Uiso 1 1 calc R . . H56C H 0.0922 0.7676 0.5381 0.222 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 0.0292(3) 0.0398(3) 0.0292(3) -0.0033(2) 0.0034(2) 0.0043(2) P1 0.0281(6) 0.0273(6) 0.0267(5) 0.0001(4) 0.0032(4) -0.0008(4) O1 0.0229(15) 0.0382(15) 0.0235(14) -0.0038(11) 0.0046(11) -0.0016(12) N1 0.0215(17) 0.0281(18) 0.0288(17) -0.0009(14) -0.0004(13) 0.0017(14) C1 0.031(2) 0.025(2) 0.023(2) 0.0015(16) 0.0053(17) -0.0024(17) B1 0.033(3) 0.028(3) 0.035(3) -0.002(2) 0.012(2) -0.004(2) P2 0.0270(6) 0.0234(5) 0.0267(5) -0.0002(4) 0.0032(4) 0.0014(4) N2 0.0299(18) 0.0242(17) 0.0259(16) 0.0031(13) 0.0066(14) 0.0006(14) C2 0.030(2) 0.021(2) 0.029(2) 0.0003(16) 0.0090(17) 0.0032(17) C3 0.037(2) 0.032(2) 0.028(2) -0.0030(17) 0.0046(19) -0.0022(18) C4 0.055(3) 0.040(3) 0.023(2) -0.0016(18) 0.007(2) -0.001(2) C5 0.049(3) 0.028(2) 0.030(2) -0.0007(17) 0.017(2) -0.0009(19) C6 0.036(2) 0.022(2) 0.029(2) 0.0025(16) 0.0071(18) 0.0012(17) C7 0.038(2) 0.0148(19) 0.029(2) -0.0040(16) 0.0126(18) 0.0027(17) C8 0.040(3) 0.025(2) 0.036(2) -0.0039(17) 0.019(2) -0.0023(18) C9 0.031(2) 0.033(2) 0.048(3) -0.002(2) 0.016(2) 0.0018(19) C10 0.032(2) 0.025(2) 0.039(2) -0.0060(18) 0.0061(19) -0.0024(18) C11 0.026(2) 0.0197(19) 0.030(2) -0.0005(16) 0.0064(17) 0.0015(17) C12 0.025(2) 0.022(2) 0.031(2) -0.0003(16) 0.0045(17) 0.0031(16) C13 0.025(2) 0.028(2) 0.037(2) -0.0006(18) 0.0027(18) 0.0009(17) C14 0.045(3) 0.036(3) 0.042(3) 0.006(2) 0.013(2) 0.003(2) C15 0.064(3) 0.048(3) 0.050(3) 0.013(2) 0.019(2) 0.007(2) C16 0.058(3) 0.035(3) 0.076(4) 0.016(3) 0.007(3) 0.003(2) C17 0.044(3) 0.032(3) 0.061(3) 0.000(2) 0.005(2) 0.003(2) C18 0.033(2) 0.038(3) 0.037(2) -0.001(2) 0.0002(19) -0.0006(19) C19 0.029(2) 0.033(2) 0.026(2) -0.0035(17) 0.0022(17) 0.0010(18) C20 0.035(3) 0.041(3) 0.034(2) 0.0011(19) 0.0010(19) -0.004(2) C21 0.035(3) 0.056(3) 0.040(3) 0.004(2) 0.000(2) 0.009(2) C22 0.032(3) 0.062(3) 0.044(3) -0.009(2) 0.000(2) -0.003(2) C23 0.032(3) 0.043(3) 0.049(3) -0.010(2) 0.004(2) -0.009(2) C24 0.033(2) 0.033(2) 0.040(2) -0.0006(19) 0.003(2) -0.0034(19) C25 0.037(3) 0.027(2) 0.030(2) -0.0049(17) -0.0009(19) 0.0054(19) C26 0.041(3) 0.028(2) 0.041(2) -0.0059(19) -0.006(2) -0.002(2) C27 0.049(3) 0.026(2) 0.083(4) 0.000(2) -0.014(3) 0.002(2) C28 0.052(4) 0.037(3) 0.103(4) -0.013(3) -0.011(3) 0.011(3) C29 0.036(3) 0.049(3) 0.077(3) -0.022(3) 0.002(2) 0.008(2) C30 0.028(2) 0.039(3) 0.043(2) -0.006(2) 0.002(2) 0.0066(19) C31 0.055(3) 0.037(3) 0.050(3) 0.008(2) 0.005(2) -0.004(2) C32 0.070(4) 0.039(3) 0.193(7) -0.012(4) -0.018(4) 0.026(3) C33 0.033(3) 0.061(3) 0.051(3) -0.007(2) 0.014(2) 0.001(2) C34 0.030(2) 0.025(2) 0.023(2) -0.0017(16) 0.0007(17) 0.0013(17) C35 0.036(2) 0.028(2) 0.041(2) 0.0035(18) 0.0156(19) -0.0001(18) C36 0.046(3) 0.034(2) 0.042(2) 0.011(2) 0.014(2) -0.001(2) C37 0.060(3) 0.031(2) 0.038(2) 0.0094(19) 0.010(2) 0.007(2) C38 0.061(3) 0.036(3) 0.047(3) 0.004(2) 0.023(2) 0.013(2) C39 0.051(3) 0.027(2) 0.034(2) 0.0080(18) 0.017(2) 0.009(2) C40 0.026(2) 0.030(2) 0.024(2) -0.0023(16) 0.0047(17) -0.0036(17) C41 0.026(2) 0.029(2) 0.049(3) -0.0009(19) -0.0017(19) 0.0023(18) C42 0.031(3) 0.044(3) 0.053(3) 0.016(2) -0.001(2) 0.005(2) C43 0.032(3) 0.065(3) 0.036(2) 0.006(2) -0.001(2) -0.004(2) C44 0.035(3) 0.051(3) 0.032(2) -0.015(2) 0.006(2) -0.010(2) C45 0.034(2) 0.027(2) 0.033(2) -0.0044(17) 0.0108(19) -0.0023(18) C46 0.020(2) 0.032(2) 0.032(2) 0.0042(18) 0.0024(17) -0.0021(17) C47 0.035(2) 0.035(2) 0.033(2) 0.0063(19) 0.0066(19) -0.0033(19) C48 0.051(3) 0.044(3) 0.035(2) 0.008(2) 0.004(2) 0.003(2) C49 0.057(3) 0.037(3) 0.049(3) 0.017(2) 0.004(2) -0.001(2) C50 0.048(3) 0.023(2) 0.053(3) 0.003(2) 0.003(2) 0.000(2) C51 0.031(2) 0.023(2) 0.041(2) 0.0010(18) 0.0029(19) -0.0017(17) C52 0.054(3) 0.037(3) 0.035(2) -0.0018(19) 0.015(2) 0.001(2) C53 0.097(4) 0.044(3) 0.072(4) 0.029(3) 0.005(3) 0.003(3) C54 0.039(3) 0.032(2) 0.043(2) -0.0085(19) 0.004(2) 0.0085(19) C57 0.031(2) 0.036(2) 0.037(2) -0.0097(19) 0.0008(19) -0.0072(19) C58 0.035(3) 0.045(3) 0.050(3) -0.007(2) 0.012(2) 0.004(2) C59 0.038(3) 0.064(3) 0.064(3) -0.025(3) 0.016(2) -0.007(2) C60 0.038(3) 0.043(3) 0.077(4) -0.024(3) -0.010(3) 0.005(2) C61 0.040(3) 0.039(3) 0.056(3) -0.006(2) -0.007(2) -0.002(2) C62 0.033(2) 0.032(2) 0.045(3) 0.001(2) -0.002(2) 0.0006(19) C63 0.041(3) 0.019(2) 0.035(2) 0.0007(17) 0.0062(19) 0.0020(18) C64 0.042(3) 0.035(2) 0.039(2) -0.0084(19) 0.013(2) -0.004(2) C65 0.063(3) 0.034(2) 0.038(2) -0.0058(19) 0.016(2) 0.000(2) C66 0.065(3) 0.028(2) 0.058(3) -0.002(2) 0.036(3) -0.003(2) C67 0.037(3) 0.031(2) 0.057(3) -0.002(2) 0.020(2) -0.0026(19) C68 0.039(3) 0.030(2) 0.041(2) 0.0000(19) 0.010(2) -0.0025(19) C69 0.043(3) 0.040(2) 0.019(2) 0.0040(17) 0.0062(18) -0.002(2) C70 0.034(3) 0.042(3) 0.038(2) 0.0052(19) 0.0022(19) -0.002(2) C71 0.047(3) 0.060(3) 0.045(3) 0.014(2) -0.004(2) -0.014(3) C72 0.084(4) 0.041(3) 0.040(3) 0.002(2) 0.002(3) -0.017(3) C73 0.072(4) 0.044(3) 0.047(3) -0.008(2) 0.022(3) -0.008(3) C74 0.049(3) 0.034(2) 0.046(3) -0.005(2) 0.019(2) -0.006(2) C75 0.030(2) 0.032(2) 0.032(2) -0.0001(18) 0.0133(18) -0.0008(18) C76 0.046(3) 0.037(3) 0.038(2) 0.001(2) 0.001(2) 0.008(2) C77 0.049(3) 0.035(3) 0.048(3) -0.011(2) 0.006(2) 0.002(2) C78 0.040(3) 0.065(3) 0.032(2) -0.004(2) 0.007(2) -0.001(2) C79 0.040(3) 0.045(3) 0.040(3) 0.012(2) 0.008(2) 0.007(2) C80 0.038(3) 0.033(2) 0.041(2) 0.0047(19) 0.015(2) -0.0031(19) C1S 0.054(3) 0.077(4) 0.056(3) 0.012(3) 0.000(3) -0.017(3) C2S 0.050(3) 0.080(4) 0.083(4) -0.014(3) 0.012(3) -0.016(3) C3S 0.064(4) 0.097(5) 0.054(3) 0.003(3) 0.013(3) -0.027(3) C4S 0.087(4) 0.079(4) 0.056(3) 0.019(3) 0.008(3) -0.008(3) C5S 0.065(4) 0.077(4) 0.060(3) 0.007(3) 0.006(3) 0.007(3) C6S 0.043(3) 0.090(4) 0.050(3) 0.022(3) 0.004(2) -0.008(3) O2 0.048(2) 0.115(3) 0.0404(19) -0.012(2) 0.0165(16) -0.022(2) O3 0.041(2) 0.079(2) 0.062(2) -0.0357(19) 0.0030(17) 0.0106(18) C55 0.040(3) 0.135(5) 0.060(4) -0.051(4) 0.010(3) -0.019(4) C56 0.081(5) 0.247(9) 0.134(6) -0.128(6) 0.067(4) -0.052(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 Zn1 N2 1.971(3) . ? Zn1 N1 1.972(3) . ? Zn1 O3 2.082(3) . ? Zn1 O2 2.089(3) . ? Zn1 C55 2.410(6) . ? P1 N1 1.606(3) . ? P1 C13 1.793(2) . ? P1 C19 1.7962(19) . ? P1 C2 1.803(4) . ? O1 C12 1.379(4) . ? O1 C1 1.379(4) . ? N1 C25 1.463(4) . ? C1 C2 1.380(5) . ? C1 C6 1.387(5) . ? B1 C57 1.689(5) . ? B1 C75 1.693(5) . ? B1 C63 1.693(5) . ? B1 C69 1.702(5) . ? P2 N2 1.614(3) . ? P2 C40 1.7873(19) . ? P2 C34 1.7998(19) . ? P2 C11 1.804(4) . ? N2 C46 1.459(4) . ? C2 C3 1.400(5) . ? C3 C4 1.387(5) . ? C3 H3 0.9500 . ? C4 C5 1.394(5) . ? C4 H4 0.9500 . ? C5 C6 1.392(5) . ? C5 H5 0.9500 . ? C6 C7 1.455(5) . ? C7 C8 1.389(5) . ? C7 C12 1.400(5) . ? C8 C9 1.370(5) . ? C8 H8 0.9500 . ? C9 C10 1.398(5) . ? C9 H9 0.9500 . ? C10 C11 1.399(5) . ? C10 H10 0.9500 . ? C11 C12 1.376(5) . ? 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 1.398(5) . ? C25 C30 1.406(5) . ? C26 C27 1.391(6) . ? C26 C31 1.490(6) . ? C27 C28 1.381(7) . ? C27 H27 0.9500 . ? C28 C29 1.367(7) . ? C28 C32 1.522(6) . ? C29 C30 1.395(5) . ? C29 H29 0.9500 . ? C30 C33 1.487(6) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? 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 1.3900 . ? C34 C39 1.3900 . ? C35 C36 1.3900 . ? C35 H35 0.9500 . ? C36 C37 1.3900 . ? C36 H36 0.9500 . ? C37 C38 1.3900 . ? C37 H37 0.9500 . ? C38 C39 1.3900 . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C41 C42 1.3900 . ? C41 H41 0.9500 . ? C42 C43 1.3900 . ? C42 H42 0.9500 . ? C43 C44 1.3900 . ? C43 H43 0.9500 . ? C44 C45 1.3900 . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C51 1.396(5) . ? C46 C47 1.410(5) . ? C47 C48 1.391(5) . ? C47 C52 1.494(5) . ? C48 C49 1.392(6) . ? C48 H48 0.9500 . ? C49 C50 1.385(6) . ? C49 C53 1.524(5) . ? C50 C51 1.383(5) . ? C50 H50 0.9500 . ? C51 C54 1.510(5) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C57 C58 1.3900 . ? C57 C62 1.3900 . ? C58 C59 1.3900 . ? C58 H58 0.9500 . ? C59 C60 1.3900 . ? C59 H59 0.9500 . ? C60 C61 1.3900 . ? C60 H60 0.9500 . ? C61 C62 1.3900 . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 C64 1.3900 . ? C63 C68 1.3900 . ? C64 C65 1.3900 . ? C64 H64 0.9500 . ? C65 C66 1.3900 . ? C65 H65 0.9500 . ? C66 C67 1.3900 . ? C66 H66 0.9500 . ? C67 C68 1.3900 . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C70 1.3900 . ? C69 C74 1.3900 . ? C70 C71 1.3900 . ? C70 H70 0.9500 . ? C71 C72 1.3900 . ? C71 H71 0.9500 . ? C72 C73 1.3900 . ? C72 H72 0.9500 . ? C73 C74 1.3900 . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? C75 C76 1.3900 . ? C75 C80 1.3900 . ? C76 C77 1.3900 . ? C76 H76 0.9500 . ? C77 C78 1.3900 . ? C77 H77 0.9500 . ? C78 C79 1.3900 . ? C78 H78 0.9500 . ? C79 C80 1.3900 . ? C79 H79 0.9500 . ? C80 H80 0.9500 . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C1S H1S 0.9500 . ? 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 . ? O2 C55 1.282(7) . ? O3 C55 1.267(7) . ? C55 C56 1.491(7) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 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 N2 Zn1 N1 141.73(12) . . ? N2 Zn1 O3 111.54(12) . . ? N1 Zn1 O3 102.04(12) . . ? N2 Zn1 O2 106.14(12) . . ? N1 Zn1 O2 104.80(12) . . ? O3 Zn1 O2 63.79(15) . . ? N2 Zn1 C55 113.30(16) . . ? N1 Zn1 C55 104.89(16) . . ? O3 Zn1 C55 31.71(18) . . ? O2 Zn1 C55 32.11(19) . . ? N1 P1 C13 109.57(14) . . ? N1 P1 C19 114.45(14) . . ? C13 P1 C19 107.93(12) . . ? N1 P1 C2 115.49(16) . . ? C13 P1 C2 104.36(14) . . ? C19 P1 C2 104.31(15) . . ? C12 O1 C1 105.9(3) . . ? C25 N1 P1 118.6(2) . . ? C25 N1 Zn1 113.1(2) . . ? P1 N1 Zn1 128.24(16) . . ? O1 C1 C2 123.2(3) . . ? O1 C1 C6 111.5(3) . . ? C2 C1 C6 125.2(3) . . ? C57 B1 C75 108.3(3) . . ? C57 B1 C63 110.8(3) . . ? C75 B1 C63 108.8(3) . . ? C57 B1 C69 110.3(3) . . ? C75 B1 C69 110.3(3) . . ? C63 B1 C69 108.3(3) . . ? N2 P2 C40 111.86(14) . . ? N2 P2 C34 110.32(14) . . ? C40 P2 C34 110.75(12) . . ? N2 P2 C11 116.17(16) . . ? C40 P2 C11 104.74(14) . . ? C34 P2 C11 102.53(14) . . ? C46 N2 P2 119.0(2) . . ? C46 N2 Zn1 113.4(2) . . ? P2 N2 Zn1 127.66(16) . . ? C1 C2 C3 115.0(3) . . ? C1 C2 P1 120.3(3) . . ? C3 C2 P1 124.4(3) . . ? C4 C3 C2 121.6(4) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 121.6(4) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 118.0(4) . . ? C6 C5 H5 121.0 . . ? C4 C5 H5 121.0 . . ? C1 C6 C5 118.6(4) . . ? C1 C6 C7 106.0(3) . . ? C5 C6 C7 135.4(4) . . ? C8 C7 C12 117.8(3) . . ? C8 C7 C6 137.1(3) . . ? C12 C7 C6 105.1(3) . . ? C9 C8 C7 119.3(4) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 121.1(4) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C9 C10 C11 121.8(4) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C12 C11 C10 114.8(3) . . ? C12 C11 P2 120.0(3) . . ? C10 C11 P2 123.8(3) . . ? C11 C12 O1 123.3(3) . . ? C11 C12 C7 125.2(3) . . ? O1 C12 C7 111.5(3) . . ? C14 C13 C18 120.0 . . ? C14 C13 P1 119.65(14) . . ? C18 C13 P1 120.22(14) . . ? 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 . . ? C17 C16 C15 120.0 . . ? C17 C16 H16 120.0 . . ? C15 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 119.34(14) . . ? C24 C19 P1 120.46(14) . . ? C19 C20 C21 120.0 . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 120.0 . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 120.0 . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C19 120.0 . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C26 C25 C30 120.9(4) . . ? C26 C25 N1 120.0(4) . . ? C30 C25 N1 119.0(3) . . ? C27 C26 C25 118.2(4) . . ? C27 C26 C31 119.7(4) . . ? C25 C26 C31 122.2(4) . . ? C28 C27 C26 122.1(4) . . ? C28 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? C29 C28 C27 118.6(4) . . ? C29 C28 C32 120.8(5) . . ? C27 C28 C32 120.6(5) . . ? C28 C29 C30 122.5(5) . . ? C28 C29 H29 118.8 . . ? C30 C29 H29 118.8 . . ? C29 C30 C25 117.7(4) . . ? C29 C30 C33 119.2(4) . . ? C25 C30 C33 123.1(4) . . ? 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 . . ? C28 C32 H32A 109.5 . . ? C28 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C28 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C39 120.0 . . ? C35 C34 P2 120.57(13) . . ? C39 C34 P2 119.43(13) . . ? C34 C35 C36 120.0 . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C37 C36 C35 120.0 . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 120.0 . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C38 C39 C34 120.0 . . ? C38 C39 H39 120.0 . . ? C34 C39 H39 120.0 . . ? C41 C40 C45 120.0 . . ? C41 C40 P2 118.35(13) . . ? C45 C40 P2 121.51(13) . . ? C42 C41 C40 120.0 . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C40 120.0 . . ? C44 C45 H45 120.0 . . ? C40 C45 H45 120.0 . . ? C51 C46 C47 120.4(3) . . ? C51 C46 N2 120.9(3) . . ? C47 C46 N2 118.7(3) . . ? C48 C47 C46 118.1(4) . . ? C48 C47 C52 118.8(4) . . ? C46 C47 C52 123.0(3) . . ? C47 C48 C49 122.4(4) . . ? C47 C48 H48 118.8 . . ? C49 C48 H48 118.8 . . ? C50 C49 C48 117.7(4) . . ? C50 C49 C53 121.9(4) . . ? C48 C49 C53 120.4(4) . . ? C51 C50 C49 122.3(4) . . ? C51 C50 H50 118.8 . . ? C49 C50 H50 118.8 . . ? C50 C51 C46 119.1(4) . . ? C50 C51 C54 119.1(3) . . ? C46 C51 C54 121.8(3) . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C49 C53 H53A 109.5 . . ? C49 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C49 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C58 C57 C62 120.0 . . ? C58 C57 B1 117.4(2) . . ? C62 C57 B1 122.5(2) . . ? C57 C58 C59 120.0 . . ? C57 C58 H58 120.0 . . ? C59 C58 H58 120.0 . . ? C60 C59 C58 120.0 . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? C59 C60 C61 120.0 . . ? C59 C60 H60 120.0 . . ? C61 C60 H60 120.0 . . ? C60 C61 C62 120.0 . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C61 C62 C57 120.0 . . ? C61 C62 H62 120.0 . . ? C57 C62 H62 120.0 . . ? C64 C63 C68 120.0 . . ? C64 C63 B1 118.5(2) . . ? C68 C63 B1 121.4(2) . . ? C65 C64 C63 120.0 . . ? C65 C64 H64 120.0 . . ? C63 C64 H64 120.0 . . ? C64 C65 C66 120.0 . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C67 C66 C65 120.0 . . ? C67 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? C66 C67 C68 120.0 . . ? C66 C67 H67 120.0 . . ? C68 C67 H67 120.0 . . ? C67 C68 C63 120.0 . . ? C67 C68 H68 120.0 . . ? C63 C68 H68 120.0 . . ? C70 C69 C74 120.0 . . ? C70 C69 B1 122.6(2) . . ? C74 C69 B1 117.4(2) . . ? C71 C70 C69 120.0 . . ? C71 C70 H70 120.0 . . ? C69 C70 H70 120.0 . . ? C70 C71 C72 120.0 . . ? C70 C71 H71 120.0 . . ? C72 C71 H71 120.0 . . ? C71 C72 C73 120.0 . . ? C71 C72 H72 120.0 . . ? C73 C72 H72 120.0 . . ? C74 C73 C72 120.0 . . ? C74 C73 H73 120.0 . . ? C72 C73 H73 120.0 . . ? C73 C74 C69 120.0 . . ? C73 C74 H74 120.0 . . ? C69 C74 H74 120.0 . . ? C76 C75 C80 120.0 . . ? C76 C75 B1 118.0(2) . . ? C80 C75 B1 121.9(2) . . ? C75 C76 C77 120.0 . . ? C75 C76 H76 120.0 . . ? C77 C76 H76 120.0 . . ? C76 C77 C78 120.0 . . ? C76 C77 H77 120.0 . . ? C78 C77 H77 120.0 . . ? C79 C78 C77 120.0 . . ? C79 C78 H78 120.0 . . ? C77 C78 H78 120.0 . . ? C78 C79 C80 120.0 . . ? C78 C79 H79 120.0 . . ? C80 C79 H79 120.0 . . ? C79 C80 C75 120.0 . . ? C79 C80 H80 120.0 . . ? C75 C80 H80 120.0 . . ? C2S C1S C6S 120.0 . . ? C2S C1S H1S 120.0 . . ? C6S C1S H1S 120.0 . . ? C3S C2S C1S 120.0 . . ? C3S C2S H2S 120.0 . . ? C1S C2S H2S 120.0 . . ? C2S C3S C4S 120.0 . . ? C2S C3S H3S 120.0 . . ? C4S C3S H3S 120.0 . . ? C3S C4S C5S 120.0 . . ? C3S C4S H4S 120.0 . . ? C5S C4S H4S 120.0 . . ? C6S C5S C4S 120.0 . . ? C6S C5S H5S 120.0 . . ? C4S C5S H5S 120.0 . . ? C5S C6S C1S 120.0 . . ? C5S C6S H6S 120.0 . . ? C1S C6S H6S 120.0 . . ? C55 O2 Zn1 87.9(4) . . ? C55 O3 Zn1 88.5(3) . . ? O3 C55 O2 119.7(5) . . ? O3 C55 C56 120.8(7) . . ? O2 C55 C56 119.5(7) . . ? O3 C55 Zn1 59.7(3) . . ? O2 C55 Zn1 60.0(3) . . ? C56 C55 Zn1 178.2(4) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 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 -148.5(3) . . . . ? C19 P1 N1 C25 -27.1(3) . . . . ? C2 P1 N1 C25 94.1(3) . . . . ? C13 P1 N1 Zn1 34.7(2) . . . . ? C19 P1 N1 Zn1 156.05(17) . . . . ? C2 P1 N1 Zn1 -82.8(2) . . . . ? N2 Zn1 N1 C25 -134.9(2) . . . . ? O3 Zn1 N1 C25 16.3(3) . . . . ? O2 Zn1 N1 C25 82.1(3) . . . . ? C55 Zn1 N1 C25 48.8(3) . . . . ? N2 Zn1 N1 P1 42.1(3) . . . . ? O3 Zn1 N1 P1 -166.7(2) . . . . ? O2 Zn1 N1 P1 -100.9(2) . . . . ? C55 Zn1 N1 P1 -134.2(3) . . . . ? C12 O1 C1 C2 178.1(3) . . . . ? C12 O1 C1 C6 0.2(4) . . . . ? C40 P2 N2 C46 -23.9(3) . . . . ? C34 P2 N2 C46 -147.6(2) . . . . ? C11 P2 N2 C46 96.3(3) . . . . ? C40 P2 N2 Zn1 156.16(16) . . . . ? C34 P2 N2 Zn1 32.4(2) . . . . ? C11 P2 N2 Zn1 -83.7(2) . . . . ? N1 Zn1 N2 C46 -115.7(3) . . . . ? O3 Zn1 N2 C46 94.8(3) . . . . ? O2 Zn1 N2 C46 27.1(3) . . . . ? C55 Zn1 N2 C46 60.4(3) . . . . ? N1 Zn1 N2 P2 64.3(3) . . . . ? O3 Zn1 N2 P2 -85.3(2) . . . . ? O2 Zn1 N2 P2 -152.9(2) . . . . ? C55 Zn1 N2 P2 -119.6(3) . . . . ? O1 C1 C2 C3 -179.7(3) . . . . ? C6 C1 C2 C3 -2.1(5) . . . . ? O1 C1 C2 P1 -6.3(5) . . . . ? C6 C1 C2 P1 171.3(3) . . . . ? N1 P1 C2 C1 46.3(3) . . . . ? C13 P1 C2 C1 -74.0(3) . . . . ? C19 P1 C2 C1 172.8(3) . . . . ? N1 P1 C2 C3 -140.9(3) . . . . ? C13 P1 C2 C3 98.7(3) . . . . ? C19 P1 C2 C3 -14.4(3) . . . . ? C1 C2 C3 C4 0.6(5) . . . . ? P1 C2 C3 C4 -172.5(3) . . . . ? C2 C3 C4 C5 1.1(6) . . . . ? C3 C4 C5 C6 -1.3(6) . . . . ? O1 C1 C6 C5 179.7(3) . . . . ? C2 C1 C6 C5 1.8(6) . . . . ? O1 C1 C6 C7 -0.1(4) . . . . ? C2 C1 C6 C7 -178.0(3) . . . . ? C4 C5 C6 C1 0.0(5) . . . . ? C4 C5 C6 C7 179.7(4) . . . . ? C1 C6 C7 C8 -178.7(4) . . . . ? C5 C6 C7 C8 1.6(8) . . . . ? C1 C6 C7 C12 0.0(4) . . . . ? C5 C6 C7 C12 -179.8(4) . . . . ? C12 C7 C8 C9 1.2(5) . . . . ? C6 C7 C8 C9 179.7(4) . . . . ? C7 C8 C9 C10 -1.4(6) . . . . ? C8 C9 C10 C11 0.3(6) . . . . ? C9 C10 C11 C12 0.9(5) . . . . ? C9 C10 C11 P2 -165.8(3) . . . . ? N2 P2 C11 C12 42.5(3) . . . . ? C40 P2 C11 C12 166.4(3) . . . . ? C34 P2 C11 C12 -77.9(3) . . . . ? N2 P2 C11 C10 -151.4(3) . . . . ? C40 P2 C11 C10 -27.5(3) . . . . ? C34 P2 C11 C10 88.2(3) . . . . ? C10 C11 C12 O1 180.0(3) . . . . ? P2 C11 C12 O1 -12.7(5) . . . . ? C10 C11 C12 C7 -1.1(5) . . . . ? P2 C11 C12 C7 166.1(3) . . . . ? C1 O1 C12 C11 178.8(3) . . . . ? C1 O1 C12 C7 -0.2(4) . . . . ? C8 C7 C12 C11 0.1(5) . . . . ? C6 C7 C12 C11 -178.8(3) . . . . ? C8 C7 C12 O1 179.1(3) . . . . ? C6 C7 C12 O1 0.1(4) . . . . ? N1 P1 C13 C14 31.0(2) . . . . ? C19 P1 C13 C14 -94.21(17) . . . . ? C2 P1 C13 C14 155.24(17) . . . . ? N1 P1 C13 C18 -153.15(16) . . . . ? C19 P1 C13 C18 81.63(17) . . . . ? C2 P1 C13 C18 -28.9(2) . . . . ? C18 C13 C14 C15 0.0 . . . . ? P1 C13 C14 C15 175.9(2) . . . . ? 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 -175.8(2) . . . . ? N1 P1 C19 C20 63.38(19) . . . . ? C13 P1 C19 C20 -174.35(14) . . . . ? C2 P1 C19 C20 -63.77(18) . . . . ? N1 P1 C19 C24 -121.83(17) . . . . ? C13 P1 C19 C24 0.43(18) . . . . ? C2 P1 C19 C24 111.02(17) . . . . ? C24 C19 C20 C21 0.0 . . . . ? P1 C19 C20 C21 174.81(19) . . . . ? 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 -174.75(19) . . . . ? P1 N1 C25 C26 -94.3(4) . . . . ? Zn1 N1 C25 C26 83.0(4) . . . . ? P1 N1 C25 C30 88.4(4) . . . . ? Zn1 N1 C25 C30 -94.3(3) . . . . ? C30 C25 C26 C27 -0.5(6) . . . . ? N1 C25 C26 C27 -177.7(3) . . . . ? C30 C25 C26 C31 178.7(4) . . . . ? N1 C25 C26 C31 1.5(6) . . . . ? C25 C26 C27 C28 0.2(7) . . . . ? C31 C26 C27 C28 -179.1(4) . . . . ? C26 C27 C28 C29 -0.6(8) . . . . ? C26 C27 C28 C32 -178.4(5) . . . . ? C27 C28 C29 C30 1.4(7) . . . . ? C32 C28 C29 C30 179.1(5) . . . . ? C28 C29 C30 C25 -1.7(7) . . . . ? C28 C29 C30 C33 179.8(4) . . . . ? C26 C25 C30 C29 1.2(6) . . . . ? N1 C25 C30 C29 178.5(3) . . . . ? C26 C25 C30 C33 179.6(4) . . . . ? N1 C25 C30 C33 -3.1(6) . . . . ? N2 P2 C34 C35 -150.00(16) . . . . ? C40 P2 C34 C35 85.61(17) . . . . ? C11 P2 C34 C35 -25.66(19) . . . . ? N2 P2 C34 C39 30.36(19) . . . . ? C40 P2 C34 C39 -94.04(16) . . . . ? C11 P2 C34 C39 154.69(17) . . . . ? C39 C34 C35 C36 0.0 . . . . ? P2 C34 C35 C36 -179.64(19) . . . . ? C34 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C38 0.0 . . . . ? C36 C37 C38 C39 0.0 . . . . ? C37 C38 C39 C34 0.0 . . . . ? C35 C34 C39 C38 0.0 . . . . ? P2 C34 C39 C38 179.65(19) . . . . ? N2 P2 C40 C41 61.04(18) . . . . ? C34 P2 C40 C41 -175.45(13) . . . . ? C11 P2 C40 C41 -65.60(17) . . . . ? N2 P2 C40 C45 -114.69(17) . . . . ? C34 P2 C40 C45 8.82(18) . . . . ? C11 P2 C40 C45 118.67(17) . . . . ? C45 C40 C41 C42 0.0 . . . . ? P2 C40 C41 C42 -175.80(18) . . . . ? C40 C41 C42 C43 0.0 . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C40 0.0 . . . . ? C41 C40 C45 C44 0.0 . . . . ? P2 C40 C45 C44 175.66(19) . . . . ? P2 N2 C46 C51 -89.5(4) . . . . ? Zn1 N2 C46 C51 90.5(3) . . . . ? P2 N2 C46 C47 90.7(4) . . . . ? Zn1 N2 C46 C47 -89.3(3) . . . . ? C51 C46 C47 C48 0.7(6) . . . . ? N2 C46 C47 C48 -179.5(3) . . . . ? C51 C46 C47 C52 179.1(4) . . . . ? N2 C46 C47 C52 -1.1(5) . . . . ? C46 C47 C48 C49 -1.4(6) . . . . ? C52 C47 C48 C49 -179.9(4) . . . . ? C47 C48 C49 C50 0.7(7) . . . . ? C47 C48 C49 C53 -179.0(4) . . . . ? C48 C49 C50 C51 0.8(7) . . . . ? C53 C49 C50 C51 -179.5(4) . . . . ? C49 C50 C51 C46 -1.5(6) . . . . ? C49 C50 C51 C54 176.4(4) . . . . ? C47 C46 C51 C50 0.7(5) . . . . ? N2 C46 C51 C50 -179.1(3) . . . . ? C47 C46 C51 C54 -177.1(4) . . . . ? N2 C46 C51 C54 3.2(5) . . . . ? C75 B1 C57 C58 -52.7(3) . . . . ? C63 B1 C57 C58 -172.01(19) . . . . ? C69 B1 C57 C58 68.1(3) . . . . ? C75 B1 C57 C62 129.1(2) . . . . ? C63 B1 C57 C62 9.8(4) . . . . ? C69 B1 C57 C62 -110.1(3) . . . . ? C62 C57 C58 C59 0.0 . . . . ? B1 C57 C58 C59 -178.3(3) . . . . ? C57 C58 C59 C60 0.0 . . . . ? C58 C59 C60 C61 0.0 . . . . ? C59 C60 C61 C62 0.0 . . . . ? C60 C61 C62 C57 0.0 . . . . ? C58 C57 C62 C61 0.0 . . . . ? B1 C57 C62 C61 178.2(3) . . . . ? C57 B1 C63 C64 -65.4(3) . . . . ? C75 B1 C63 C64 175.63(19) . . . . ? C69 B1 C63 C64 55.8(3) . . . . ? C57 B1 C63 C68 112.4(3) . . . . ? C75 B1 C63 C68 -6.6(3) . . . . ? C69 B1 C63 C68 -126.5(2) . . . . ? C68 C63 C64 C65 0.0 . . . . ? B1 C63 C64 C65 177.8(2) . . . . ? C63 C64 C65 C66 0.0 . . . . ? C64 C65 C66 C67 0.0 . . . . ? C65 C66 C67 C68 0.0 . . . . ? C66 C67 C68 C63 0.0 . . . . ? C64 C63 C68 C67 0.0 . . . . ? B1 C63 C68 C67 -177.7(3) . . . . ? C57 B1 C69 C70 -19.1(4) . . . . ? C75 B1 C69 C70 100.6(3) . . . . ? C63 B1 C69 C70 -140.5(2) . . . . ? C57 B1 C69 C74 163.0(2) . . . . ? C75 B1 C69 C74 -77.4(3) . . . . ? C63 B1 C69 C74 41.5(3) . . . . ? C74 C69 C70 C71 0.0 . . . . ? B1 C69 C70 C71 -177.9(3) . . . . ? C69 C70 C71 C72 0.0 . . . . ? C70 C71 C72 C73 0.0 . . . . ? C71 C72 C73 C74 0.0 . . . . ? C72 C73 C74 C69 0.0 . . . . ? C70 C69 C74 C73 0.0 . . . . ? B1 C69 C74 C73 178.0(2) . . . . ? C57 B1 C75 C76 -38.7(3) . . . . ? C63 B1 C75 C76 81.9(3) . . . . ? C69 B1 C75 C76 -159.5(2) . . . . ? C57 B1 C75 C80 144.8(2) . . . . ? C63 B1 C75 C80 -94.6(3) . . . . ? C69 B1 C75 C80 24.0(4) . . . . ? C80 C75 C76 C77 0.0 . . . . ? B1 C75 C76 C77 -176.6(2) . . . . ? C75 C76 C77 C78 0.0 . . . . ? C76 C77 C78 C79 0.0 . . . . ? C77 C78 C79 C80 0.0 . . . . ? C78 C79 C80 C75 0.0 . . . . ? C76 C75 C80 C79 0.0 . . . . ? B1 C75 C80 C79 176.5(3) . . . . ? C6S C1S C2S C3S 0.0 . . . . ? 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 . . . . ? N2 Zn1 O2 C55 108.3(3) . . . . ? N1 Zn1 O2 C55 -94.5(3) . . . . ? O3 Zn1 O2 C55 1.8(3) . . . . ? N2 Zn1 O3 C55 -99.8(3) . . . . ? N1 Zn1 O3 C55 98.9(3) . . . . ? O2 Zn1 O3 C55 -1.8(3) . . . . ? Zn1 O3 C55 O2 3.1(5) . . . . ? Zn1 O3 C55 C56 -178.0(5) . . . . ? Zn1 O2 C55 O3 -3.1(5) . . . . ? Zn1 O2 C55 C56 178.0(5) . . . . ? N2 Zn1 C55 O3 93.6(3) . . . . ? N1 Zn1 C55 O3 -88.9(3) . . . . ? O2 Zn1 C55 O3 176.9(5) . . . . ? N2 Zn1 C55 O2 -83.3(3) . . . . ? N1 Zn1 C55 O2 94.2(3) . . . . ? O3 Zn1 C55 O2 -176.9(5) . . . . ? N2 Zn1 C55 C56 -158(22) . . . . ? N1 Zn1 C55 C56 19(22) . . . . ? O3 Zn1 C55 C56 108(22) . . . . ? O2 Zn1 C55 C56 -75(22) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.880 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.061 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 493 80 ' ' 2 0.000 0.500 0.500 493 80 ' ' _platon_squeeze_details ; ; #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 753817' #TrackingRef 'XRay-revised_-_Manuscript_B922543A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H78 B Br N2 O P2 Zn' _chemical_formula_weight 1421.57 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' Zn Zn 0.2839 1.4301 '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' 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 17.7836(9) _cell_length_b 21.8185(11) _cell_length_c 19.8868(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.5040(10) _cell_angle_gamma 90.00 _cell_volume 7587.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2960 _exptl_absorpt_coefficient_mu 0.941 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6530 _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 90924 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.03 _reflns_number_total 13399 _reflns_number_gt 10529 _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^)+(0.0712P)^2^+7.1680P] 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 13399 _refine_ls_number_parameters 877 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1410 _refine_ls_wR_factor_gt 0.1337 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.011 _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 0.75212(2) 0.680269(18) 0.567308(18) 0.03784(12) Uani 1 1 d . . . P1 P 0.56870(4) 0.71021(3) 0.54950(4) 0.02529(16) Uani 1 1 d . . . O1 O 0.65436(11) 0.66067(9) 0.68610(9) 0.0289(4) Uani 1 1 d . . . N1 N 0.63886(13) 0.67059(10) 0.53327(11) 0.0276(5) Uani 1 1 d . . . C1 C 0.57692(16) 0.66992(12) 0.68198(14) 0.0276(6) Uani 1 1 d . . . B1 B 0.27487(19) 0.59458(15) 0.02738(16) 0.0286(7) Uani 1 1 d . . . P2 P 0.82308(4) 0.62438(3) 0.71800(4) 0.03057(18) Uani 1 1 d . . . N2 N 0.81791(13) 0.67664(11) 0.66095(12) 0.0312(5) Uani 1 1 d . . . C2 C 0.52858(16) 0.68669(12) 0.62231(14) 0.0275(6) Uani 1 1 d . . . C3 C 0.45186(17) 0.69359(13) 0.62795(16) 0.0330(7) Uani 1 1 d . . . H3 H 0.4154 0.7041 0.5886 0.040 Uiso 1 1 calc R . . C4 C 0.42785(18) 0.68534(13) 0.69021(17) 0.0374(7) Uani 1 1 d . . . H4 H 0.3752 0.6901 0.6922 0.045 Uiso 1 1 calc R . . C5 C 0.47852(18) 0.67052(13) 0.74900(16) 0.0356(7) Uani 1 1 d . . . H5 H 0.4613 0.6659 0.7912 0.043 Uiso 1 1 calc R . . C6 C 0.55528(17) 0.66246(12) 0.74539(14) 0.0304(6) Uani 1 1 d . . . C7 C 0.62531(17) 0.64806(12) 0.79276(14) 0.0309(6) Uani 1 1 d . . . C8 C 0.6460(2) 0.63536(13) 0.86238(15) 0.0399(8) Uani 1 1 d . . . H8 H 0.6087 0.6353 0.8910 0.048 Uiso 1 1 calc R . . C9 C 0.7217(2) 0.62288(14) 0.88900(16) 0.0435(8) Uani 1 1 d . . . H9 H 0.7364 0.6154 0.9366 0.052 Uiso 1 1 calc R . . C10 C 0.7771(2) 0.62103(14) 0.84751(15) 0.0388(7) Uani 1 1 d . . . H10 H 0.8285 0.6115 0.8673 0.047 Uiso 1 1 calc R . . C11 C 0.75846(17) 0.63291(13) 0.77777(14) 0.0315(6) Uani 1 1 d . . . C12 C 0.68253(17) 0.64715(12) 0.75349(13) 0.0297(6) Uani 1 1 d . . . C13 C 0.48946(16) 0.71125(13) 0.47925(14) 0.0286(6) Uani 1 1 d . . . C14 C 0.45734(17) 0.65572(14) 0.45463(16) 0.0376(7) Uani 1 1 d . . . H14 H 0.4738 0.6187 0.4779 0.045 Uiso 1 1 calc R . . C15 C 0.40162(19) 0.65433(18) 0.39643(18) 0.0494(9) Uani 1 1 d . . . H15 H 0.3811 0.6162 0.3786 0.059 Uiso 1 1 calc R . . C16 C 0.37598(19) 0.7080(2) 0.36439(17) 0.0516(9) Uani 1 1 d . . . H16 H 0.3377 0.7069 0.3243 0.062 Uiso 1 1 calc R . . C17 C 0.40503(19) 0.76320(18) 0.38967(16) 0.0456(9) Uani 1 1 d . . . H17 H 0.3852 0.8002 0.3683 0.055 Uiso 1 1 calc R . . C18 C 0.46324(18) 0.76524(14) 0.44640(15) 0.0354(7) Uani 1 1 d . . . H18 H 0.4850 0.8034 0.4627 0.043 Uiso 1 1 calc R . . C19 C 0.59937(16) 0.78733(12) 0.57146(14) 0.0280(6) Uani 1 1 d . . . C20 C 0.66225(19) 0.81181(14) 0.54764(15) 0.0370(7) Uani 1 1 d . . . H20 H 0.6895 0.7876 0.5205 0.044 Uiso 1 1 calc R . . C21 C 0.6845(2) 0.87155(15) 0.56390(17) 0.0449(8) Uani 1 1 d . . . H21 H 0.7283 0.8878 0.5491 0.054 Uiso 1 1 calc R . . C22 C 0.6436(2) 0.90782(14) 0.60155(17) 0.0440(8) Uani 1 1 d . . . H22 H 0.6587 0.9490 0.6119 0.053 Uiso 1 1 calc R . . C23 C 0.5808(2) 0.88397(14) 0.62390(17) 0.0437(8) Uani 1 1 d . . . H23 H 0.5522 0.9090 0.6491 0.052 Uiso 1 1 calc R . . C24 C 0.55918(18) 0.82398(14) 0.60994(16) 0.0358(7) Uani 1 1 d . . . H24 H 0.5166 0.8076 0.6267 0.043 Uiso 1 1 calc R . . C25 C 0.62659(15) 0.62368(12) 0.48066(14) 0.0285(6) Uani 1 1 d . . . C26 C 0.62778(16) 0.63885(13) 0.41219(15) 0.0319(6) Uani 1 1 d . . . C27 C 0.61729(18) 0.59212(15) 0.36391(16) 0.0414(8) Uani 1 1 d . . . H27 H 0.6182 0.6020 0.3175 0.050 Uiso 1 1 calc R . . C28 C 0.6055(2) 0.53170(15) 0.38081(18) 0.0458(8) Uani 1 1 d . . . C29 C 0.60413(18) 0.51815(14) 0.44797(18) 0.0425(8) Uani 1 1 d . . . H29 H 0.5962 0.4769 0.4601 0.051 Uiso 1 1 calc R . . C30 C 0.61397(17) 0.56277(13) 0.49907(15) 0.0335(7) Uani 1 1 d . . . C31 C 0.60635(19) 0.54595(14) 0.57057(16) 0.0416(8) Uani 1 1 d . . . H31A H 0.5567 0.5599 0.5793 0.062 Uiso 1 1 calc R . . H31B H 0.6474 0.5656 0.6030 0.062 Uiso 1 1 calc R . . H31C H 0.6101 0.5014 0.5761 0.062 Uiso 1 1 calc R . . C32 C 0.63826(19) 0.70314(14) 0.38931(15) 0.0388(7) Uani 1 1 d . . . H32A H 0.5934 0.7277 0.3942 0.058 Uiso 1 1 calc R . . H32B H 0.6441 0.7029 0.3413 0.058 Uiso 1 1 calc R . . H32C H 0.6841 0.7209 0.4175 0.058 Uiso 1 1 calc R . . C33 C 0.5923(3) 0.48204(18) 0.3260(2) 0.0693(12) Uani 1 1 d . . . H33A H 0.6261 0.4472 0.3406 0.104 Uiso 1 1 calc R . . H33B H 0.6034 0.4985 0.2830 0.104 Uiso 1 1 calc R . . H33C H 0.5389 0.4685 0.3191 0.104 Uiso 1 1 calc R . . C34 C 0.79812(17) 0.55168(13) 0.67704(16) 0.0343(7) Uani 1 1 d . . . C35 C 0.76961(18) 0.50494(13) 0.71318(17) 0.0389(7) Uani 1 1 d . . . H35 H 0.7597 0.5123 0.7578 0.047 Uiso 1 1 calc R . . C36 C 0.7559(2) 0.44782(15) 0.6836(2) 0.0505(9) Uani 1 1 d . . . H36 H 0.7370 0.4156 0.7080 0.061 Uiso 1 1 calc R . . C37 C 0.7698(2) 0.43766(17) 0.6184(2) 0.0644(11) Uani 1 1 d . . . H37 H 0.7594 0.3985 0.5979 0.077 Uiso 1 1 calc R . . C38 C 0.7986(2) 0.48360(19) 0.5826(2) 0.0638(11) Uani 1 1 d . . . H38 H 0.8085 0.4760 0.5380 0.077 Uiso 1 1 calc R . . C39 C 0.8131(2) 0.54101(16) 0.61228(18) 0.0478(8) Uani 1 1 d . . . H39 H 0.8332 0.5728 0.5881 0.057 Uiso 1 1 calc R . . C40 C 0.91589(17) 0.61574(14) 0.77051(16) 0.0369(7) Uani 1 1 d . . . C41 C 0.9451(2) 0.66320(16) 0.81348(18) 0.0484(9) Uani 1 1 d . . . H41 H 0.9173 0.7004 0.8136 0.058 Uiso 1 1 calc R . . C42 C 1.0154(2) 0.65620(18) 0.85651(19) 0.0548(10) Uani 1 1 d . . . H42 H 1.0354 0.6888 0.8860 0.066 Uiso 1 1 calc R . . C43 C 1.0560(2) 0.60325(19) 0.8570(2) 0.0559(10) Uani 1 1 d . . . H43 H 1.1033 0.5986 0.8876 0.067 Uiso 1 1 calc R . . C44 C 1.02859(19) 0.55688(17) 0.8135(2) 0.0531(9) Uani 1 1 d . . . H44 H 1.0577 0.5204 0.8128 0.064 Uiso 1 1 calc R . . C45 C 0.95820(18) 0.56271(15) 0.77001(18) 0.0437(8) Uani 1 1 d . . . H45 H 0.9392 0.5302 0.7399 0.052 Uiso 1 1 calc R . . C46 C 0.86951(16) 0.72922(13) 0.67167(15) 0.0336(7) Uani 1 1 d . . . C47 C 0.94153(17) 0.72549(15) 0.65259(17) 0.0402(8) Uani 1 1 d . . . C48 C 0.9876(2) 0.77680(17) 0.6595(2) 0.0527(10) Uani 1 1 d . . . H48 H 1.0364 0.7744 0.6465 0.063 Uiso 1 1 calc R . . C49 C 0.9651(2) 0.83129(16) 0.6844(2) 0.0614(11) Uani 1 1 d . . . C50 C 0.8942(2) 0.83405(15) 0.7033(2) 0.0526(10) Uani 1 1 d . . . H50 H 0.8781 0.8715 0.7206 0.063 Uiso 1 1 calc R . . C51 C 0.84522(18) 0.78332(14) 0.69776(16) 0.0391(7) Uani 1 1 d . . . C52 C 0.97064(19) 0.66799(17) 0.62471(19) 0.0488(9) Uani 1 1 d . . . H52A H 1.0211 0.6757 0.6133 0.073 Uiso 1 1 calc R . . H52B H 0.9351 0.6552 0.5835 0.073 Uiso 1 1 calc R . . H52C H 0.9747 0.6355 0.6592 0.073 Uiso 1 1 calc R . . C53 C 1.0163(3) 0.8873(2) 0.6893(4) 0.103(2) Uani 1 1 d . . . H53A H 0.9928 0.9182 0.6563 0.154 Uiso 1 1 calc R . . H53B H 1.0663 0.8756 0.6791 0.154 Uiso 1 1 calc R . . H53C H 1.0230 0.9043 0.7356 0.154 Uiso 1 1 calc R . . C54 C 0.77067(19) 0.78846(15) 0.72237(18) 0.0443(8) Uani 1 1 d . . . H54A H 0.7304 0.7680 0.6899 0.066 Uiso 1 1 calc R . . H54B H 0.7575 0.8318 0.7260 0.066 Uiso 1 1 calc R . . H54C H 0.7753 0.7690 0.7673 0.066 Uiso 1 1 calc R . . C55 C 0.8132(2) 0.6914(2) 0.49654(19) 0.0604(11) Uani 1 1 d . . . C56 C 0.8498(3) 0.7426(2) 0.4917(2) 0.0694(12) Uani 1 1 d . . . H56 H 0.8424 0.7756 0.5210 0.083 Uiso 1 1 calc R . . C57 C 0.9004(3) 0.7512(3) 0.4447(3) 0.0844(15) Uani 1 1 d . . . H57 H 0.9268 0.7888 0.4430 0.101 Uiso 1 1 calc R . . C58 C 0.9099(3) 0.7027(3) 0.4012(3) 0.0962(18) Uani 1 1 d . . . H58 H 0.9437 0.7074 0.3696 0.115 Uiso 1 1 calc R . . C59 C 0.8707(3) 0.6472(3) 0.4032(3) 0.0885(15) Uani 1 1 d . . . H59 H 0.8763 0.6144 0.3732 0.106 Uiso 1 1 calc R . . C60 C 0.8222(3) 0.6423(2) 0.4521(2) 0.0729(12) Uani 1 1 d . . . H60 H 0.7952 0.6051 0.4552 0.088 Uiso 1 1 calc R . . C61 C 0.32679(16) 0.59206(13) 0.10480(14) 0.0285(6) Uani 1 1 d . . . C62 C 0.35732(17) 0.64307(14) 0.14257(15) 0.0335(7) Uani 1 1 d . . . H62 H 0.3451 0.6827 0.1239 0.040 Uiso 1 1 calc R . . C63 C 0.40473(18) 0.63859(15) 0.20607(16) 0.0393(7) Uani 1 1 d . . . H63 H 0.4240 0.6747 0.2299 0.047 Uiso 1 1 calc R . . C64 C 0.42393(19) 0.58175(15) 0.23463(16) 0.0403(7) Uani 1 1 d . . . H64 H 0.4564 0.5783 0.2781 0.048 Uiso 1 1 calc R . . C65 C 0.39535(19) 0.53033(15) 0.19923(16) 0.0417(8) Uani 1 1 d . . . H65 H 0.4082 0.4909 0.2183 0.050 Uiso 1 1 calc R . . C66 C 0.34782(18) 0.53534(14) 0.13573(16) 0.0376(7) Uani 1 1 d . . . H66 H 0.3289 0.4989 0.1124 0.045 Uiso 1 1 calc R . . C67 C 0.33087(16) 0.58386(12) -0.02893(14) 0.0279(6) Uani 1 1 d . . . C68 C 0.40814(17) 0.56845(13) -0.01170(15) 0.0329(6) Uani 1 1 d . . . H68 H 0.4305 0.5649 0.0353 0.039 Uiso 1 1 calc R . . C69 C 0.45396(19) 0.55800(14) -0.06057(17) 0.0401(7) Uani 1 1 d . . . H69 H 0.5064 0.5479 -0.0464 0.048 Uiso 1 1 calc R . . C70 C 0.4235(2) 0.56220(14) -0.12930(17) 0.0419(8) Uani 1 1 d . . . H70 H 0.4541 0.5543 -0.1628 0.050 Uiso 1 1 calc R . . C71 C 0.3468(2) 0.57823(14) -0.14843(16) 0.0398(8) Uani 1 1 d . . . H71 H 0.3247 0.5817 -0.1955 0.048 Uiso 1 1 calc R . . C72 C 0.30272(18) 0.58917(13) -0.09927(15) 0.0348(7) Uani 1 1 d . . . H72 H 0.2508 0.6009 -0.1138 0.042 Uiso 1 1 calc R . . C73 C 0.20929(16) 0.54085(13) 0.02068(14) 0.0296(6) Uani 1 1 d . . . C74 C 0.19316(17) 0.49844(13) -0.03256(16) 0.0353(7) Uani 1 1 d . . . H74 H 0.2233 0.4993 -0.0674 0.042 Uiso 1 1 calc R . . C75 C 0.13501(18) 0.45498(15) -0.03710(19) 0.0449(8) Uani 1 1 d . . . H75 H 0.1270 0.4266 -0.0739 0.054 Uiso 1 1 calc R . . C76 C 0.08903(19) 0.45316(16) 0.0118(2) 0.0500(9) Uani 1 1 d . . . H76 H 0.0484 0.4244 0.0084 0.060 Uiso 1 1 calc R . . C77 C 0.10315(18) 0.49364(17) 0.06558(19) 0.0481(9) Uani 1 1 d . . . H77 H 0.0721 0.4928 0.0997 0.058 Uiso 1 1 calc R . . C78 C 0.16241(18) 0.53566(15) 0.07046(16) 0.0401(7) Uani 1 1 d . . . H78 H 0.1718 0.5621 0.1090 0.048 Uiso 1 1 calc R . . C79 C 0.23352(17) 0.66243(13) 0.01293(14) 0.0311(6) Uani 1 1 d . . . C80 C 0.15687(18) 0.67546(15) 0.01367(15) 0.0377(7) Uani 1 1 d . . . H80 H 0.1243 0.6432 0.0229 0.045 Uiso 1 1 calc R . . C81 C 0.1260(2) 0.73445(17) 0.00138(17) 0.0506(9) Uani 1 1 d . . . H81 H 0.0735 0.7413 0.0024 0.061 Uiso 1 1 calc R . . C82 C 0.1710(2) 0.78230(16) -0.01215(17) 0.0519(9) Uani 1 1 d . . . H82 H 0.1501 0.8222 -0.0207 0.062 Uiso 1 1 calc R . . C83 C 0.2471(2) 0.77132(15) -0.01310(18) 0.0501(9) Uani 1 1 d . . . H83 H 0.2792 0.8040 -0.0220 0.060 Uiso 1 1 calc R . . C84 C 0.2770(2) 0.71298(14) -0.00111(16) 0.0395(7) Uani 1 1 d . . . H84 H 0.3296 0.7068 -0.0024 0.047 Uiso 1 1 calc R . . C1S C 0.17995(16) 0.82538(10) 0.25947(13) 0.0680(12) Uani 1 1 d G . . H1S H 0.1720 0.8652 0.2763 0.082 Uiso 1 1 calc R . . C2S C 0.17005(16) 0.77398(14) 0.29822(10) 0.0745(13) Uani 1 1 d G . . H2S H 0.1553 0.7786 0.3415 0.089 Uiso 1 1 calc R . . C3S C 0.18171(15) 0.71578(11) 0.27362(12) 0.0648(11) Uani 1 1 d G . . H3S H 0.1750 0.6806 0.3001 0.078 Uiso 1 1 calc R . . C4S C 0.20326(14) 0.70897(9) 0.21027(13) 0.0554(10) Uani 1 1 d G . . H4S H 0.2112 0.6692 0.1935 0.066 Uiso 1 1 calc R . . C5S C 0.21315(13) 0.76038(11) 0.17152(10) 0.0515(9) Uani 1 1 d G . . H5S H 0.2279 0.7557 0.1282 0.062 Uiso 1 1 calc R . . C6S C 0.20150(14) 0.81858(10) 0.19612(12) 0.0559(10) Uani 1 1 d G . . Br1 Br 0.21338(3) 0.88782(2) 0.14467(3) 0.08479(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0296(2) 0.0499(2) 0.0325(2) -0.00720(16) 0.00164(14) -0.00586(16) P1 0.0268(4) 0.0218(3) 0.0263(4) -0.0005(3) 0.0022(3) -0.0037(3) O1 0.0267(10) 0.0352(11) 0.0243(9) 0.0016(8) 0.0032(8) -0.0015(8) N1 0.0295(13) 0.0251(12) 0.0269(12) -0.0042(9) 0.0016(10) -0.0017(10) C1 0.0268(15) 0.0233(14) 0.0331(15) -0.0025(11) 0.0069(12) -0.0031(11) B1 0.0310(17) 0.0267(16) 0.0286(16) 0.0007(13) 0.0070(13) 0.0038(13) P2 0.0283(4) 0.0262(4) 0.0344(4) -0.0009(3) -0.0017(3) -0.0021(3) N2 0.0272(12) 0.0309(13) 0.0331(13) -0.0020(10) -0.0009(10) -0.0049(10) C2 0.0294(15) 0.0218(13) 0.0317(15) -0.0003(11) 0.0070(12) -0.0047(11) C3 0.0293(16) 0.0264(14) 0.0427(17) 0.0032(12) 0.0046(13) -0.0006(12) C4 0.0331(16) 0.0299(15) 0.0534(19) 0.0033(14) 0.0193(15) 0.0006(13) C5 0.0425(18) 0.0264(15) 0.0429(17) 0.0015(13) 0.0210(14) 0.0017(13) C6 0.0424(17) 0.0188(13) 0.0315(15) 0.0010(11) 0.0109(13) -0.0004(12) C7 0.0440(17) 0.0203(13) 0.0290(15) -0.0011(11) 0.0081(13) -0.0009(12) C8 0.064(2) 0.0265(15) 0.0310(16) 0.0007(12) 0.0141(15) 0.0023(15) C9 0.067(2) 0.0358(17) 0.0255(15) 0.0028(13) 0.0026(15) 0.0030(16) C10 0.050(2) 0.0307(16) 0.0313(16) -0.0006(12) -0.0037(14) 0.0012(14) C11 0.0387(17) 0.0243(14) 0.0298(15) -0.0022(11) 0.0016(12) -0.0034(12) C12 0.0400(17) 0.0239(14) 0.0234(14) -0.0011(11) 0.0015(12) -0.0034(12) C13 0.0288(15) 0.0301(15) 0.0271(14) 0.0001(11) 0.0054(11) 0.0023(12) C14 0.0289(16) 0.0362(17) 0.0455(18) -0.0049(14) 0.0013(13) 0.0009(13) C15 0.0335(18) 0.064(2) 0.0460(19) -0.0180(17) -0.0045(15) 0.0016(16) C16 0.0332(18) 0.088(3) 0.0310(17) -0.0050(18) -0.0010(14) 0.0142(19) C17 0.0371(18) 0.066(2) 0.0363(17) 0.0198(17) 0.0138(14) 0.0215(17) C18 0.0376(17) 0.0359(16) 0.0357(16) 0.0061(13) 0.0141(13) 0.0089(13) C19 0.0335(16) 0.0233(14) 0.0268(14) -0.0015(11) 0.0042(12) -0.0044(12) C20 0.0466(19) 0.0329(16) 0.0346(16) -0.0068(13) 0.0154(14) -0.0088(14) C21 0.060(2) 0.0355(17) 0.0441(18) -0.0070(14) 0.0211(16) -0.0217(16) C22 0.062(2) 0.0252(15) 0.0455(19) -0.0054(14) 0.0109(16) -0.0123(15) C23 0.054(2) 0.0302(16) 0.0482(19) -0.0106(14) 0.0129(16) -0.0013(15) C24 0.0346(17) 0.0328(16) 0.0417(17) -0.0052(13) 0.0114(13) -0.0031(13) C25 0.0243(14) 0.0265(14) 0.0324(15) -0.0055(11) -0.0007(11) 0.0003(11) C26 0.0300(15) 0.0304(15) 0.0331(15) -0.0039(12) 0.0000(12) 0.0033(12) C27 0.0386(18) 0.049(2) 0.0343(17) -0.0127(14) -0.0003(14) 0.0054(15) C28 0.0452(19) 0.0348(17) 0.052(2) -0.0194(15) -0.0058(16) 0.0080(15) C29 0.0422(18) 0.0240(15) 0.055(2) -0.0059(14) -0.0067(15) 0.0028(13) C30 0.0294(15) 0.0269(15) 0.0403(17) -0.0025(13) -0.0039(13) 0.0011(12) C31 0.0450(19) 0.0303(16) 0.0467(19) 0.0069(14) 0.0011(15) -0.0046(14) C32 0.0461(19) 0.0414(17) 0.0291(15) 0.0012(13) 0.0077(14) 0.0027(14) C33 0.081(3) 0.048(2) 0.069(3) -0.032(2) -0.010(2) 0.013(2) C34 0.0282(15) 0.0291(15) 0.0434(17) -0.0057(13) 0.0002(13) -0.0017(12) C35 0.0381(17) 0.0290(16) 0.0473(18) -0.0003(14) 0.0019(14) -0.0036(13) C36 0.049(2) 0.0308(17) 0.071(3) -0.0045(17) 0.0082(18) -0.0072(15) C37 0.074(3) 0.0344(19) 0.088(3) -0.023(2) 0.023(2) -0.0126(19) C38 0.075(3) 0.057(2) 0.064(2) -0.029(2) 0.026(2) -0.015(2) C39 0.049(2) 0.0410(19) 0.056(2) -0.0101(16) 0.0162(17) -0.0082(16) C40 0.0303(16) 0.0350(16) 0.0420(17) 0.0087(13) -0.0027(13) -0.0045(13) C41 0.044(2) 0.0444(19) 0.050(2) 0.0018(16) -0.0091(16) 0.0013(15) C42 0.044(2) 0.060(2) 0.053(2) 0.0016(18) -0.0117(17) -0.0125(18) C43 0.0292(18) 0.071(3) 0.063(2) 0.031(2) -0.0042(16) -0.0017(17) C44 0.0317(18) 0.051(2) 0.074(3) 0.0234(19) 0.0041(17) 0.0012(16) C45 0.0318(17) 0.0376(17) 0.061(2) 0.0096(16) 0.0054(15) -0.0005(14) C46 0.0294(15) 0.0309(15) 0.0359(16) 0.0065(12) -0.0062(12) -0.0051(12) C47 0.0270(16) 0.0437(18) 0.0461(18) 0.0111(15) -0.0036(13) -0.0023(13) C48 0.0318(18) 0.050(2) 0.071(2) 0.0249(18) -0.0048(16) -0.0074(15) C49 0.040(2) 0.039(2) 0.096(3) 0.022(2) -0.014(2) -0.0101(16) C50 0.048(2) 0.0296(17) 0.070(2) 0.0060(16) -0.0141(18) -0.0037(15) C51 0.0375(17) 0.0335(17) 0.0403(17) 0.0052(13) -0.0092(14) -0.0029(13) C52 0.0307(17) 0.059(2) 0.057(2) 0.0079(17) 0.0076(15) 0.0022(16) C53 0.055(3) 0.044(2) 0.195(6) 0.026(3) -0.013(3) -0.019(2) C54 0.0455(19) 0.0342(17) 0.050(2) -0.0069(15) -0.0001(15) 0.0003(14) C55 0.0342(19) 0.106(3) 0.040(2) 0.000(2) 0.0038(15) -0.008(2) C56 0.081(3) 0.080(3) 0.046(2) 0.019(2) 0.009(2) 0.010(3) C57 0.070(3) 0.099(4) 0.091(4) 0.028(3) 0.032(3) 0.008(3) C58 0.097(4) 0.104(4) 0.101(4) 0.036(3) 0.054(3) 0.024(3) C59 0.095(4) 0.103(4) 0.072(3) 0.021(3) 0.027(3) 0.016(3) C60 0.059(3) 0.098(3) 0.064(3) 0.013(3) 0.016(2) 0.008(2) C61 0.0283(15) 0.0307(15) 0.0284(14) 0.0005(12) 0.0104(12) 0.0009(12) C62 0.0366(17) 0.0330(16) 0.0325(15) 0.0004(12) 0.0107(13) 0.0027(13) C63 0.0401(18) 0.0428(18) 0.0349(17) -0.0099(14) 0.0068(14) -0.0012(14) C64 0.0412(18) 0.0494(19) 0.0285(16) 0.0004(14) 0.0013(13) 0.0015(15) C65 0.0435(19) 0.0388(18) 0.0401(18) 0.0098(14) 0.0005(14) -0.0008(14) C66 0.0425(18) 0.0310(16) 0.0367(16) 0.0005(13) 0.0003(14) 0.0003(13) C67 0.0326(15) 0.0210(13) 0.0312(15) 0.0002(11) 0.0083(12) 0.0008(11) C68 0.0363(17) 0.0291(15) 0.0340(16) 0.0012(12) 0.0081(13) 0.0020(13) C69 0.0354(17) 0.0331(16) 0.056(2) 0.0071(14) 0.0186(15) 0.0079(13) C70 0.056(2) 0.0305(16) 0.0469(19) 0.0056(14) 0.0304(16) 0.0071(15) C71 0.058(2) 0.0329(16) 0.0310(16) 0.0058(13) 0.0143(15) 0.0053(15) C72 0.0379(17) 0.0318(16) 0.0340(16) 0.0024(13) 0.0052(13) 0.0056(13) C73 0.0262(15) 0.0276(14) 0.0338(15) 0.0062(12) 0.0026(12) 0.0063(12) C74 0.0311(16) 0.0318(16) 0.0405(17) 0.0047(13) -0.0001(13) 0.0064(13) C75 0.0351(18) 0.0360(17) 0.057(2) 0.0026(15) -0.0081(16) 0.0002(14) C76 0.0273(17) 0.0434(19) 0.074(3) 0.0195(18) -0.0041(17) -0.0032(14) C77 0.0308(17) 0.057(2) 0.059(2) 0.0206(18) 0.0125(16) 0.0038(16) C78 0.0345(17) 0.0463(18) 0.0402(17) 0.0062(14) 0.0086(14) 0.0048(14) C79 0.0373(16) 0.0325(15) 0.0233(14) -0.0017(12) 0.0048(12) 0.0055(13) C80 0.0323(16) 0.0411(17) 0.0376(17) -0.0061(13) 0.0002(13) 0.0069(14) C81 0.043(2) 0.058(2) 0.0457(19) -0.0111(17) -0.0054(16) 0.0230(17) C82 0.076(3) 0.0354(19) 0.0412(19) 0.0011(15) 0.0022(18) 0.0229(18) C83 0.074(3) 0.0334(17) 0.047(2) 0.0080(15) 0.0237(18) 0.0095(17) C84 0.0469(19) 0.0351(17) 0.0409(17) 0.0047(14) 0.0199(15) 0.0071(14) C1S 0.061(3) 0.085(3) 0.054(2) -0.026(2) 0.001(2) 0.020(2) C2S 0.064(3) 0.105(4) 0.055(3) -0.011(3) 0.013(2) 0.029(3) C3S 0.045(2) 0.086(3) 0.060(3) 0.001(2) 0.0024(19) 0.015(2) C4S 0.039(2) 0.070(3) 0.056(2) -0.015(2) 0.0041(17) 0.0074(18) C5S 0.0327(18) 0.070(3) 0.050(2) -0.0185(19) 0.0024(15) 0.0035(17) C6S 0.0360(19) 0.069(3) 0.057(2) -0.0155(19) -0.0079(16) 0.0008(17) Br1 0.0842(4) 0.0719(3) 0.0927(4) -0.0033(3) 0.0013(3) -0.0069(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 C55 1.943(4) . ? Zn1 N2 2.012(2) . ? Zn1 N1 2.016(2) . ? P1 N1 1.598(2) . ? P1 C13 1.795(3) . ? P1 C19 1.798(3) . ? P1 C2 1.801(3) . ? O1 C12 1.374(3) . ? O1 C1 1.380(3) . ? N1 C25 1.451(3) . ? C1 C2 1.382(4) . ? C1 C6 1.393(4) . ? B1 C73 1.642(4) . ? B1 C67 1.645(4) . ? B1 C61 1.646(4) . ? B1 C79 1.655(4) . ? P2 N2 1.599(2) . ? P2 C40 1.795(3) . ? P2 C34 1.801(3) . ? P2 C11 1.807(3) . ? N2 C46 1.460(4) . ? C2 C3 1.397(4) . ? C3 C4 1.393(4) . ? C3 H3 0.9500 . ? C4 C5 1.378(4) . ? C4 H4 0.9500 . ? C5 C6 1.391(4) . ? C5 H5 0.9500 . ? C6 C7 1.452(4) . ? C7 C12 1.391(4) . ? C7 C8 1.394(4) . ? C8 C9 1.380(5) . ? C8 H8 0.9500 . ? C9 C10 1.396(5) . ? C9 H9 0.9500 . ? C10 C11 1.390(4) . ? C10 H10 0.9500 . ? C11 C12 1.384(4) . ? C13 C18 1.386(4) . ? C13 C14 1.390(4) . ? C14 C15 1.380(4) . ? C14 H14 0.9500 . ? C15 C16 1.371(5) . ? C15 H15 0.9500 . ? C16 C17 1.369(5) . ? C16 H16 0.9500 . ? C17 C18 1.386(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.391(4) . ? C19 C20 1.398(4) . ? C20 C21 1.383(4) . ? C20 H20 0.9500 . ? C21 C22 1.384(5) . ? C21 H21 0.9500 . ? C22 C23 1.376(5) . ? C22 H22 0.9500 . ? C23 C24 1.378(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.405(4) . ? C25 C30 1.407(4) . ? C26 C27 1.389(4) . ? C26 C32 1.497(4) . ? C27 C28 1.386(5) . ? C27 H27 0.9500 . ? C28 C29 1.373(5) . ? C28 C33 1.525(4) . ? C29 C30 1.395(4) . ? C29 H29 0.9500 . ? C30 C31 1.498(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? 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 1.381(5) . ? C34 C35 1.395(4) . ? C35 C36 1.381(4) . ? C35 H35 0.9500 . ? C36 C37 1.381(6) . ? C36 H36 0.9500 . ? C37 C38 1.381(6) . ? C37 H37 0.9500 . ? C38 C39 1.388(5) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.381(4) . ? C40 C41 1.382(5) . ? C41 C42 1.388(5) . ? C41 H41 0.9500 . ? C42 C43 1.362(5) . ? C42 H42 0.9500 . ? C43 C44 1.363(6) . ? C43 H43 0.9500 . ? C44 C45 1.391(5) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C51 1.390(4) . ? C46 C47 1.403(4) . ? C47 C48 1.379(5) . ? C47 C52 1.501(5) . ? C48 C49 1.375(6) . ? C48 H48 0.9500 . ? C49 C50 1.382(6) . ? C49 C53 1.517(5) . ? C50 C51 1.400(5) . ? C50 H50 0.9500 . ? C51 C54 1.499(5) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.306(6) . ? C55 C60 1.417(6) . ? C56 C57 1.422(6) . ? C56 H56 0.9500 . ? C57 C58 1.398(8) . ? C57 H57 0.9500 . ? C58 C59 1.402(8) . ? C58 H58 0.9500 . ? C59 C60 1.415(6) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C62 1.396(4) . ? C61 C66 1.402(4) . ? C62 C63 1.388(4) . ? C62 H62 0.9500 . ? C63 C64 1.381(5) . ? C63 H63 0.9500 . ? C64 C65 1.372(5) . ? C64 H64 0.9500 . ? C65 C66 1.390(4) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C68 1.395(4) . ? C67 C72 1.402(4) . ? C68 C69 1.396(4) . ? C68 H68 0.9500 . ? C69 C70 1.379(5) . ? C69 H69 0.9500 . ? C70 C71 1.392(5) . ? C70 H70 0.9500 . ? C71 C72 1.381(4) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.396(4) . ? C73 C78 1.410(4) . ? C74 C75 1.394(4) . ? C74 H74 0.9500 . ? C75 C76 1.381(5) . ? C75 H75 0.9500 . ? C76 C77 1.374(5) . ? C76 H76 0.9500 . ? C77 C78 1.387(5) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 C80 1.395(4) . ? C79 C84 1.404(4) . ? C80 C81 1.403(5) . ? C80 H80 0.9500 . ? C81 C82 1.371(5) . ? C81 H81 0.9500 . ? C82 C83 1.377(5) . ? C82 H82 0.9500 . ? C83 C84 1.383(4) . ? C83 H83 0.9500 . ? C84 H84 0.9500 . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C1S H1S 0.9500 . ? 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 Br1 1.858(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C55 Zn1 N2 111.58(13) . . ? C55 Zn1 N1 115.21(12) . . ? N2 Zn1 N1 133.12(10) . . ? N1 P1 C13 112.37(12) . . ? N1 P1 C19 109.99(13) . . ? C13 P1 C19 109.73(13) . . ? N1 P1 C2 116.52(13) . . ? C13 P1 C2 105.04(13) . . ? C19 P1 C2 102.61(13) . . ? C12 O1 C1 105.8(2) . . ? C25 N1 P1 120.44(18) . . ? C25 N1 Zn1 109.01(17) . . ? P1 N1 Zn1 130.13(13) . . ? O1 C1 C2 123.2(2) . . ? O1 C1 C6 111.5(2) . . ? C2 C1 C6 125.2(3) . . ? C73 B1 C67 110.6(2) . . ? C73 B1 C61 108.7(2) . . ? C67 B1 C61 109.0(2) . . ? C73 B1 C79 109.8(2) . . ? C67 B1 C79 108.3(2) . . ? C61 B1 C79 110.4(2) . . ? N2 P2 C40 114.55(13) . . ? N2 P2 C34 109.24(13) . . ? C40 P2 C34 107.18(14) . . ? N2 P2 C11 115.59(13) . . ? C40 P2 C11 104.82(14) . . ? C34 P2 C11 104.72(14) . . ? C46 N2 P2 120.21(18) . . ? C46 N2 Zn1 110.37(17) . . ? P2 N2 Zn1 129.29(13) . . ? C1 C2 C3 115.0(3) . . ? C1 C2 P1 119.4(2) . . ? C3 C2 P1 124.7(2) . . ? C4 C3 C2 121.3(3) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 121.7(3) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 118.8(3) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C5 C6 C1 117.9(3) . . ? C5 C6 C7 136.7(3) . . ? C1 C6 C7 105.5(3) . . ? C12 C7 C8 117.8(3) . . ? C12 C7 C6 105.5(2) . . ? C8 C7 C6 136.7(3) . . ? C9 C8 C7 118.9(3) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C8 C9 C10 121.5(3) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C11 C10 C9 121.2(3) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C12 C11 C10 115.5(3) . . ? C12 C11 P2 119.4(2) . . ? C10 C11 P2 124.9(2) . . ? O1 C12 C11 123.2(3) . . ? O1 C12 C7 111.7(2) . . ? C11 C12 C7 125.0(3) . . ? C18 C13 C14 119.6(3) . . ? C18 C13 P1 121.8(2) . . ? C14 C13 P1 118.5(2) . . ? C15 C14 C13 120.0(3) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 119.9(3) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C17 C16 C15 120.6(3) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 120.2(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C13 C18 C17 119.6(3) . . ? C13 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C24 C19 C20 119.3(3) . . ? C24 C19 P1 120.5(2) . . ? C20 C19 P1 120.1(2) . . ? C21 C20 C19 119.6(3) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 120.6(3) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 119.7(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.5(3) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C19 120.3(3) . . ? C23 C24 H24 119.9 . . ? C19 C24 H24 119.9 . . ? C26 C25 C30 120.4(3) . . ? C26 C25 N1 120.4(2) . . ? C30 C25 N1 119.2(3) . . ? C27 C26 C25 118.2(3) . . ? C27 C26 C32 119.1(3) . . ? C25 C26 C32 122.7(3) . . ? C28 C27 C26 122.5(3) . . ? C28 C27 H27 118.7 . . ? C26 C27 H27 118.7 . . ? C29 C28 C27 118.1(3) . . ? C29 C28 C33 121.0(3) . . ? C27 C28 C33 120.9(3) . . ? C28 C29 C30 122.5(3) . . ? C28 C29 H29 118.8 . . ? C30 C29 H29 118.8 . . ? C29 C30 C25 118.3(3) . . ? C29 C30 C31 120.0(3) . . ? C25 C30 C31 121.6(3) . . ? 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 . . ? C26 C32 H32A 109.5 . . ? C26 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C26 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C39 C34 C35 120.5(3) . . ? C39 C34 P2 119.8(2) . . ? C35 C34 P2 119.6(2) . . ? C36 C35 C34 119.5(3) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C37 C36 C35 119.8(3) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C38 C37 C36 120.9(3) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C37 C38 C39 119.6(4) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C34 C39 C38 119.7(3) . . ? C34 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C45 C40 C41 119.2(3) . . ? C45 C40 P2 121.9(2) . . ? C41 C40 P2 118.9(2) . . ? C40 C41 C42 119.6(3) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C43 C42 C41 121.0(4) . . ? C43 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C42 C43 C44 119.8(3) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C43 C44 C45 120.3(3) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C40 C45 C44 120.1(3) . . ? C40 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C51 C46 C47 120.8(3) . . ? C51 C46 N2 119.5(3) . . ? C47 C46 N2 119.7(3) . . ? C48 C47 C46 118.8(3) . . ? C48 C47 C52 118.4(3) . . ? C46 C47 C52 122.8(3) . . ? C49 C48 C47 122.0(4) . . ? C49 C48 H48 119.0 . . ? C47 C48 H48 119.0 . . ? C48 C49 C50 118.4(3) . . ? C48 C49 C53 120.6(4) . . ? C50 C49 C53 121.0(4) . . ? C49 C50 C51 122.0(3) . . ? C49 C50 H50 119.0 . . ? C51 C50 H50 119.0 . . ? C46 C51 C50 118.0(3) . . ? C46 C51 C54 122.6(3) . . ? C50 C51 C54 119.3(3) . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C49 C53 H53A 109.5 . . ? C49 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C49 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 C60 119.1(4) . . ? C56 C55 Zn1 120.8(4) . . ? C60 C55 Zn1 120.0(3) . . ? C55 C56 C57 123.0(5) . . ? C55 C56 H56 118.5 . . ? C57 C56 H56 118.5 . . ? C58 C57 C56 118.0(5) . . ? C58 C57 H57 121.0 . . ? C56 C57 H57 121.0 . . ? C57 C58 C59 121.2(5) . . ? C57 C58 H58 119.4 . . ? C59 C58 H58 119.4 . . ? C58 C59 C60 117.1(5) . . ? C58 C59 H59 121.5 . . ? C60 C59 H59 121.5 . . ? C59 C60 C55 121.6(5) . . ? C59 C60 H60 119.2 . . ? C55 C60 H60 119.2 . . ? C62 C61 C66 114.9(3) . . ? C62 C61 B1 125.0(3) . . ? C66 C61 B1 119.9(2) . . ? C63 C62 C61 123.1(3) . . ? C63 C62 H62 118.5 . . ? C61 C62 H62 118.5 . . ? C64 C63 C62 120.1(3) . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C65 C64 C63 118.9(3) . . ? C65 C64 H64 120.6 . . ? C63 C64 H64 120.6 . . ? C64 C65 C66 120.6(3) . . ? C64 C65 H65 119.7 . . ? C66 C65 H65 119.7 . . ? C65 C66 C61 122.5(3) . . ? C65 C66 H66 118.8 . . ? C61 C66 H66 118.8 . . ? C68 C67 C72 114.9(3) . . ? C68 C67 B1 123.9(2) . . ? C72 C67 B1 121.1(3) . . ? C67 C68 C69 122.8(3) . . ? C67 C68 H68 118.6 . . ? C69 C68 H68 118.6 . . ? C70 C69 C68 120.4(3) . . ? C70 C69 H69 119.8 . . ? C68 C69 H69 119.8 . . ? C69 C70 C71 118.5(3) . . ? C69 C70 H70 120.8 . . ? C71 C70 H70 120.8 . . ? C72 C71 C70 120.3(3) . . ? C72 C71 H71 119.9 . . ? C70 C71 H71 119.9 . . ? C71 C72 C67 123.1(3) . . ? C71 C72 H72 118.4 . . ? C67 C72 H72 118.4 . . ? C74 C73 C78 114.4(3) . . ? C74 C73 B1 125.4(3) . . ? C78 C73 B1 120.2(3) . . ? C75 C74 C73 123.2(3) . . ? C75 C74 H74 118.4 . . ? C73 C74 H74 118.4 . . ? C76 C75 C74 120.1(3) . . ? C76 C75 H75 120.0 . . ? C74 C75 H75 120.0 . . ? C77 C76 C75 118.8(3) . . ? C77 C76 H76 120.6 . . ? C75 C76 H76 120.6 . . ? C76 C77 C78 120.6(3) . . ? C76 C77 H77 119.7 . . ? C78 C77 H77 119.7 . . ? C77 C78 C73 122.9(3) . . ? C77 C78 H78 118.6 . . ? C73 C78 H78 118.6 . . ? C80 C79 C84 114.6(3) . . ? C80 C79 B1 125.8(3) . . ? C84 C79 B1 119.6(3) . . ? C79 C80 C81 122.5(3) . . ? C79 C80 H80 118.8 . . ? C81 C80 H80 118.8 . . ? C82 C81 C80 120.6(3) . . ? C82 C81 H81 119.7 . . ? C80 C81 H81 119.7 . . ? C81 C82 C83 118.7(3) . . ? C81 C82 H82 120.7 . . ? C83 C82 H82 120.7 . . ? C82 C83 C84 120.4(3) . . ? C82 C83 H83 119.8 . . ? C84 C83 H83 119.8 . . ? C83 C84 C79 123.3(3) . . ? C83 C84 H84 118.4 . . ? C79 C84 H84 118.4 . . ? C2S C1S C6S 120.0 . . ? C2S C1S H1S 120.0 . . ? C6S C1S H1S 120.0 . . ? C3S C2S C1S 120.0 . . ? C3S C2S H2S 120.0 . . ? C1S C2S H2S 120.0 . . ? C2S C3S C4S 120.0 . . ? C2S C3S H3S 120.0 . . ? C4S C3S H3S 120.0 . . ? C3S C4S C5S 120.0 . . ? C3S C4S H4S 120.0 . . ? C5S C4S H4S 120.0 . . ? C6S C5S C4S 120.0 . . ? C6S C5S H5S 120.0 . . ? C4S C5S H5S 120.0 . . ? C5S C6S C1S 120.0 . . ? C5S C6S Br1 120.65(15) . . ? C1S C6S Br1 119.35(15) . . ? 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 -22.1(3) . . . . ? C19 P1 N1 C25 -144.7(2) . . . . ? C2 P1 N1 C25 99.2(2) . . . . ? C13 P1 N1 Zn1 149.56(16) . . . . ? C19 P1 N1 Zn1 27.0(2) . . . . ? C2 P1 N1 Zn1 -89.17(19) . . . . ? C55 Zn1 N1 C25 50.7(2) . . . . ? N2 Zn1 N1 C25 -125.66(18) . . . . ? C55 Zn1 N1 P1 -121.7(2) . . . . ? N2 Zn1 N1 P1 61.9(2) . . . . ? C12 O1 C1 C2 177.7(2) . . . . ? C12 O1 C1 C6 -0.1(3) . . . . ? C40 P2 N2 C46 -27.3(3) . . . . ? C34 P2 N2 C46 -147.6(2) . . . . ? C11 P2 N2 C46 94.7(2) . . . . ? C40 P2 N2 Zn1 148.05(18) . . . . ? C34 P2 N2 Zn1 27.8(2) . . . . ? C11 P2 N2 Zn1 -89.9(2) . . . . ? C55 Zn1 N2 C46 51.7(3) . . . . ? N1 Zn1 N2 C46 -131.83(19) . . . . ? C55 Zn1 N2 P2 -124.0(2) . . . . ? N1 Zn1 N2 P2 52.4(2) . . . . ? O1 C1 C2 C3 179.6(2) . . . . ? C6 C1 C2 C3 -2.9(4) . . . . ? O1 C1 C2 P1 -10.7(4) . . . . ? C6 C1 C2 P1 166.8(2) . . . . ? N1 P1 C2 C1 42.5(3) . . . . ? C13 P1 C2 C1 167.6(2) . . . . ? C19 P1 C2 C1 -77.7(2) . . . . ? N1 P1 C2 C3 -148.9(2) . . . . ? C13 P1 C2 C3 -23.8(3) . . . . ? C19 P1 C2 C3 90.9(3) . . . . ? C1 C2 C3 C4 1.5(4) . . . . ? P1 C2 C3 C4 -167.5(2) . . . . ? C2 C3 C4 C5 0.5(4) . . . . ? C3 C4 C5 C6 -1.3(4) . . . . ? C4 C5 C6 C1 0.0(4) . . . . ? C4 C5 C6 C7 179.0(3) . . . . ? O1 C1 C6 C5 179.9(2) . . . . ? C2 C1 C6 C5 2.2(4) . . . . ? O1 C1 C6 C7 0.7(3) . . . . ? C2 C1 C6 C7 -177.1(3) . . . . ? C5 C6 C7 C12 -180.0(3) . . . . ? C1 C6 C7 C12 -0.9(3) . . . . ? C5 C6 C7 C8 0.9(6) . . . . ? C1 C6 C7 C8 179.9(3) . . . . ? C12 C7 C8 C9 0.3(4) . . . . ? C6 C7 C8 C9 179.4(3) . . . . ? C7 C8 C9 C10 -1.8(5) . . . . ? C8 C9 C10 C11 1.3(5) . . . . ? C9 C10 C11 C12 0.8(4) . . . . ? C9 C10 C11 P2 -173.5(2) . . . . ? N2 P2 C11 C12 46.0(3) . . . . ? C40 P2 C11 C12 173.1(2) . . . . ? C34 P2 C11 C12 -74.2(2) . . . . ? N2 P2 C11 C10 -139.9(2) . . . . ? C40 P2 C11 C10 -12.8(3) . . . . ? C34 P2 C11 C10 99.9(3) . . . . ? C1 O1 C12 C11 177.8(3) . . . . ? C1 O1 C12 C7 -0.6(3) . . . . ? C10 C11 C12 O1 179.4(2) . . . . ? P2 C11 C12 O1 -6.0(4) . . . . ? C10 C11 C12 C7 -2.4(4) . . . . ? P2 C11 C12 C7 172.2(2) . . . . ? C8 C7 C12 O1 -179.7(2) . . . . ? C6 C7 C12 O1 0.9(3) . . . . ? C8 C7 C12 C11 1.9(4) . . . . ? C6 C7 C12 C11 -177.4(3) . . . . ? N1 P1 C13 C18 -118.2(2) . . . . ? C19 P1 C13 C18 4.5(3) . . . . ? C2 P1 C13 C18 114.1(2) . . . . ? N1 P1 C13 C14 57.4(3) . . . . ? C19 P1 C13 C14 -179.9(2) . . . . ? C2 P1 C13 C14 -70.3(3) . . . . ? C18 C13 C14 C15 2.3(5) . . . . ? P1 C13 C14 C15 -173.4(3) . . . . ? C13 C14 C15 C16 -2.4(5) . . . . ? C14 C15 C16 C17 -0.2(5) . . . . ? C15 C16 C17 C18 2.8(5) . . . . ? C14 C13 C18 C17 0.4(4) . . . . ? P1 C13 C18 C17 175.9(2) . . . . ? C16 C17 C18 C13 -2.9(5) . . . . ? N1 P1 C19 C24 -157.3(2) . . . . ? C13 P1 C19 C24 78.6(3) . . . . ? C2 P1 C19 C24 -32.6(3) . . . . ? N1 P1 C19 C20 25.3(3) . . . . ? C13 P1 C19 C20 -98.8(3) . . . . ? C2 P1 C19 C20 149.9(2) . . . . ? C24 C19 C20 C21 1.4(5) . . . . ? P1 C19 C20 C21 178.9(3) . . . . ? C19 C20 C21 C22 -2.2(5) . . . . ? C20 C21 C22 C23 1.0(5) . . . . ? C21 C22 C23 C24 1.0(5) . . . . ? C22 C23 C24 C19 -1.7(5) . . . . ? C20 C19 C24 C23 0.5(5) . . . . ? P1 C19 C24 C23 -177.0(2) . . . . ? P1 N1 C25 C26 87.1(3) . . . . ? Zn1 N1 C25 C26 -86.2(3) . . . . ? P1 N1 C25 C30 -93.3(3) . . . . ? Zn1 N1 C25 C30 93.4(3) . . . . ? C30 C25 C26 C27 -0.9(4) . . . . ? N1 C25 C26 C27 178.7(3) . . . . ? C30 C25 C26 C32 177.9(3) . . . . ? N1 C25 C26 C32 -2.6(4) . . . . ? C25 C26 C27 C28 0.3(5) . . . . ? C32 C26 C27 C28 -178.5(3) . . . . ? C26 C27 C28 C29 0.1(5) . . . . ? C26 C27 C28 C33 178.5(3) . . . . ? C27 C28 C29 C30 0.1(5) . . . . ? C33 C28 C29 C30 -178.2(3) . . . . ? C28 C29 C30 C25 -0.7(5) . . . . ? C28 C29 C30 C31 175.7(3) . . . . ? C26 C25 C30 C29 1.1(4) . . . . ? N1 C25 C30 C29 -178.5(3) . . . . ? C26 C25 C30 C31 -175.2(3) . . . . ? N1 C25 C30 C31 5.2(4) . . . . ? N2 P2 C34 C39 30.1(3) . . . . ? C40 P2 C34 C39 -94.5(3) . . . . ? C11 P2 C34 C39 154.5(3) . . . . ? N2 P2 C34 C35 -155.1(2) . . . . ? C40 P2 C34 C35 80.3(3) . . . . ? C11 P2 C34 C35 -30.7(3) . . . . ? C39 C34 C35 C36 -0.4(5) . . . . ? P2 C34 C35 C36 -175.2(2) . . . . ? C34 C35 C36 C37 -0.6(5) . . . . ? C35 C36 C37 C38 1.2(6) . . . . ? C36 C37 C38 C39 -0.7(7) . . . . ? C35 C34 C39 C38 0.9(5) . . . . ? P2 C34 C39 C38 175.6(3) . . . . ? C37 C38 C39 C34 -0.3(6) . . . . ? N2 P2 C40 C45 -115.6(3) . . . . ? C34 P2 C40 C45 5.8(3) . . . . ? C11 P2 C40 C45 116.7(3) . . . . ? N2 P2 C40 C41 65.5(3) . . . . ? C34 P2 C40 C41 -173.1(3) . . . . ? C11 P2 C40 C41 -62.2(3) . . . . ? C45 C40 C41 C42 -1.6(5) . . . . ? P2 C40 C41 C42 177.3(3) . . . . ? C40 C41 C42 C43 0.0(6) . . . . ? C41 C42 C43 C44 1.8(6) . . . . ? C42 C43 C44 C45 -2.0(6) . . . . ? C41 C40 C45 C44 1.4(5) . . . . ? P2 C40 C45 C44 -177.4(3) . . . . ? C43 C44 C45 C40 0.3(5) . . . . ? P2 N2 C46 C51 -95.7(3) . . . . ? Zn1 N2 C46 C51 88.1(3) . . . . ? P2 N2 C46 C47 87.3(3) . . . . ? Zn1 N2 C46 C47 -88.9(3) . . . . ? C51 C46 C47 C48 -0.7(5) . . . . ? N2 C46 C47 C48 176.3(3) . . . . ? C51 C46 C47 C52 179.5(3) . . . . ? N2 C46 C47 C52 -3.5(4) . . . . ? C46 C47 C48 C49 0.0(5) . . . . ? C52 C47 C48 C49 179.8(3) . . . . ? C47 C48 C49 C50 0.3(6) . . . . ? C47 C48 C49 C53 -178.2(4) . . . . ? C48 C49 C50 C51 0.0(6) . . . . ? C53 C49 C50 C51 178.5(4) . . . . ? C47 C46 C51 C50 1.0(4) . . . . ? N2 C46 C51 C50 -176.0(3) . . . . ? C47 C46 C51 C54 -176.6(3) . . . . ? N2 C46 C51 C54 6.4(4) . . . . ? C49 C50 C51 C46 -0.7(5) . . . . ? C49 C50 C51 C54 177.0(3) . . . . ? N2 Zn1 C55 C56 -67.9(4) . . . . ? N1 Zn1 C55 C56 115.0(3) . . . . ? N2 Zn1 C55 C60 108.1(3) . . . . ? N1 Zn1 C55 C60 -69.0(4) . . . . ? C60 C55 C56 C57 -1.5(7) . . . . ? Zn1 C55 C56 C57 174.5(3) . . . . ? C55 C56 C57 C58 1.0(7) . . . . ? C56 C57 C58 C59 0.4(8) . . . . ? C57 C58 C59 C60 -1.1(8) . . . . ? C58 C59 C60 C55 0.6(7) . . . . ? C56 C55 C60 C59 0.7(6) . . . . ? Zn1 C55 C60 C59 -175.4(3) . . . . ? C73 B1 C61 C62 -144.2(3) . . . . ? C67 B1 C61 C62 95.1(3) . . . . ? C79 B1 C61 C62 -23.8(4) . . . . ? C73 B1 C61 C66 40.2(4) . . . . ? C67 B1 C61 C66 -80.5(3) . . . . ? C79 B1 C61 C66 160.7(3) . . . . ? C66 C61 C62 C63 -0.2(4) . . . . ? B1 C61 C62 C63 -175.9(3) . . . . ? C61 C62 C63 C64 0.2(5) . . . . ? C62 C63 C64 C65 -0.1(5) . . . . ? C63 C64 C65 C66 -0.1(5) . . . . ? C64 C65 C66 C61 0.0(5) . . . . ? C62 C61 C66 C65 0.1(5) . . . . ? B1 C61 C66 C65 176.1(3) . . . . ? C73 B1 C67 C68 -113.1(3) . . . . ? C61 B1 C67 C68 6.5(4) . . . . ? C79 B1 C67 C68 126.6(3) . . . . ? C73 B1 C67 C72 66.2(3) . . . . ? C61 B1 C67 C72 -174.3(2) . . . . ? C79 B1 C67 C72 -54.1(3) . . . . ? C72 C67 C68 C69 -1.1(4) . . . . ? B1 C67 C68 C69 178.2(3) . . . . ? C67 C68 C69 C70 -0.5(5) . . . . ? C68 C69 C70 C71 1.3(5) . . . . ? C69 C70 C71 C72 -0.4(5) . . . . ? C70 C71 C72 C67 -1.3(5) . . . . ? C68 C67 C72 C71 2.0(4) . . . . ? B1 C67 C72 C71 -177.4(3) . . . . ? C67 B1 C73 C74 -11.1(4) . . . . ? C61 B1 C73 C74 -130.8(3) . . . . ? C79 B1 C73 C74 108.4(3) . . . . ? C67 B1 C73 C78 170.4(2) . . . . ? C61 B1 C73 C78 50.7(3) . . . . ? C79 B1 C73 C78 -70.1(3) . . . . ? C78 C73 C74 C75 0.9(4) . . . . ? B1 C73 C74 C75 -177.7(3) . . . . ? C73 C74 C75 C76 1.3(5) . . . . ? C74 C75 C76 C77 -1.8(5) . . . . ? C75 C76 C77 C78 0.2(5) . . . . ? C76 C77 C78 C73 2.1(5) . . . . ? C74 C73 C78 C77 -2.5(4) . . . . ? B1 C73 C78 C77 176.1(3) . . . . ? C73 B1 C79 C80 16.5(4) . . . . ? C67 B1 C79 C80 137.3(3) . . . . ? C61 B1 C79 C80 -103.4(3) . . . . ? C73 B1 C79 C84 -164.0(3) . . . . ? C67 B1 C79 C84 -43.1(3) . . . . ? C61 B1 C79 C84 76.1(3) . . . . ? C84 C79 C80 C81 0.0(4) . . . . ? B1 C79 C80 C81 179.5(3) . . . . ? C79 C80 C81 C82 0.1(5) . . . . ? C80 C81 C82 C83 -0.3(5) . . . . ? C81 C82 C83 C84 0.5(5) . . . . ? C82 C83 C84 C79 -0.5(5) . . . . ? C80 C79 C84 C83 0.2(5) . . . . ? B1 C79 C84 C83 -179.4(3) . . . . ? C6S C1S C2S C3S 0.0 . . . . ? C1S C2S C3S C4S 0.0 . . . . ? C2S C3S C4S C5S 0.0 . . . . ? C3S C4S C5S C6S 0.0 . . . . ? C4S C5S C6S C1S 0.0 . . . . ? C4S C5S C6S Br1 -179.31(18) . . . . ? C2S C1S C6S C5S 0.0 . . . . ? C2S C1S C6S Br1 179.32(18) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.017 _refine_diff_density_min -0.767 _refine_diff_density_rms 0.061 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 323 71 ' ' 2 0.000 0.500 0.500 323 71 ' ' _platon_squeeze_details ; ; # start Validation Reply Form _vrf_PLAT213_2b ; PROBLEM: Atom C79 has ADP max/min Ratio ..... 5.50 prola RESPONSE: The large thermal parameters are due to the poor ordering of this methyl group, which has been modelled over two sites. ; _vrf_PLAT220_2b ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 8.92 Ratio RESPONSE: This is a result of several poorly ordered atomic positions throughout the structure, some of which could not be explicitly modelled as disordered over two sites. ; _vrf_PLAT222_2b ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 9.41 Ratio RESPONSE: This is a result of several poorly ordered atomic positions throughout the structure, some of which could not be explicitly modelled as disordered over two sites. ; _vrf_PLAT410_2b ; PROBLEM: Short Intra H...H Contact H66 .. H74B .. 1.14 Ang. RESPONSE: This short contact is a result of disorder in one of the phenyl groups of the anion. The secondary position of this phenyl closely approaches a neighbouring phenyl. This second phenyl group shows signs of a concomitant disorder but could not be explicitly refined as such. ; _vrf_PLAT220_3 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.90 Ratio RESPONSE: The acetate moiety of this structure is not well ordered, giving rise to large thermal parameters. However, attempts to model these atomic positions as a two-site disorder were unsuccessful. ; _vrf_PLAT222_3 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 6.00 Ratio RESPONSE: The acetate moiety of this structure is not well ordered, giving rise to large thermal parameters. However, attempts to model these atomic positions as a two-site disorder were unsuccessful. ; # end Validation Reply Form