# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Humphrey, Simon' _publ_contact_author_email SMH49@CAM.AC.UK _publ_section_title ; Metal-Organophosphine and Metal-Organophosphonium Frameworks with Layered Honeycomb-like Structures ; loop_ _publ_author_name S.Humphrey R.J.Allan M.S.Ironside S.E.Oungoulian E.R.Wise # Attachment 'PCM-1_NEW.cif' data_sh0706b _database_code_depnum_ccdc_archive 'CCDC 708772' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C23 H19 N1 O6 P1), 1.5(C3 H7 N O)' _chemical_formula_sum 'C50.50 H48.50 N3.50 O13.50 P2 Zn2' _chemical_formula_weight 1113.11 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 44.1966(5) _cell_length_b 14.25930(10) _cell_length_c 24.4632(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15417.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 103054 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 24.11 _exptl_crystal_description 'hexagonal plate' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.959 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4592 _exptl_absorpt_coefficient_mu 0.709 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.526 _exptl_absorpt_correction_T_max 0.957 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 45898 _diffrn_reflns_av_R_equivalents 0.1661 _diffrn_reflns_av_sigmaI/netI 0.1131 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 22.50 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.985 _reflns_number_total 9944 _reflns_number_gt 5770 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.1648P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9944 _refine_ls_number_parameters 642 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1439 _refine_ls_R_factor_gt 0.0899 _refine_ls_wR_factor_ref 0.2654 _refine_ls_wR_factor_gt 0.2349 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.981 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.130 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 0.065 0.092 0.750 2236 899 ' ' 2 0.343 0.141 0.250 2235 905 ' ' 3 0.750 0.250 0.271 83 35 ' ' 4 0.750 0.250 0.771 83 35 ' ' 5 0.250 0.750 0.729 83 35 ' ' 6 0.250 0.750 0.229 83 36 ' ' _platon_squeeze_details ; ; 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_1 Zn 0.08643(2) 0.48736(6) -0.05589(4) 0.0553(3) Uani 1 1 d . . . P1_1 P 0.01955(5) 0.98931(14) 0.10834(9) 0.0579(6) Uani 1 1 d . . . C1_1 C 0.03616(18) 0.8806(5) 0.0842(3) 0.054(2) Uani 1 1 d . . . O1_1 O 0.06765(12) 0.6042(3) -0.0302(2) 0.0642(15) Uani 1 1 d . . . N1_1 N 0.13208(17) 0.4899(5) -0.0618(3) 0.076(2) Uani 1 1 d . . . H1N_1 H 0.1360 0.4534 -0.0925 0.091 Uiso 1 1 calc R . . C2_1 C 0.0266(2) 0.8439(5) 0.0339(3) 0.068(2) Uani 1 1 d . . . H2A_1 H 0.0110 0.8748 0.0141 0.082 Uiso 1 1 calc R . . O2_1 O 0.09328(13) 0.5826(4) 0.0450(3) 0.0746(17) Uani 1 1 d . . . C3_1 C 0.03963(19) 0.7632(5) 0.0125(3) 0.061(2) Uani 1 1 d . . . H3A_1 H 0.0337 0.7419 -0.0226 0.074 Uiso 1 1 calc R . . O3_1 O 0.07033(13) 1.0091(4) 0.3685(2) 0.0662(15) Uani 1 1 d . . . C4_1 C 0.06039(18) 0.7151(5) 0.0406(3) 0.0483(19) Uani 1 1 d . . . O4_1 O 0.11321(16) 1.0574(4) 0.3272(2) 0.0753(17) Uani 1 1 d . . . O5_1 O 0.06879(13) 1.3868(4) -0.0122(2) 0.0709(16) Uani 1 1 d . . . C5_1 C 0.0698(2) 0.7471(6) 0.0911(3) 0.070(2) Uani 1 1 d . . . H5A_1 H 0.0849 0.7137 0.1107 0.084 Uiso 1 1 calc R . . O6_1 O 0.09520(16) 1.2878(4) -0.0644(3) 0.092(2) Uani 1 1 d . . . C6_1 C 0.05737(18) 0.8274(6) 0.1134(3) 0.060(2) Uani 1 1 d . . . H6A_1 H 0.0633 0.8468 0.1490 0.072 Uiso 1 1 calc R . . C7_1 C 0.07525(18) 0.6272(5) 0.0189(3) 0.051(2) Uani 1 1 d . . . C8_1 C 0.03912(19) 1.0088(5) 0.1719(3) 0.051(2) Uani 1 1 d . . . C9_1 C 0.02548(19) 0.9832(5) 0.2199(3) 0.058(2) Uani 1 1 d . . . H9A_1 H 0.0054 0.9597 0.2188 0.069 Uiso 1 1 calc R . . C10_1 C 0.03978(19) 0.9903(6) 0.2697(3) 0.062(2) Uani 1 1 d . . . H10A_1 H 0.0295 0.9701 0.3018 0.074 Uiso 1 1 calc R . . C11_1 C 0.0688(2) 1.0262(5) 0.2740(3) 0.053(2) Uani 1 1 d . . . C12_1 C 0.0828(2) 1.0564(6) 0.2255(3) 0.067(2) Uani 1 1 d . . . H12A_1 H 0.1024 1.0837 0.2267 0.081 Uiso 1 1 calc R . . C13_1 C 0.0678(2) 1.0464(6) 0.1761(3) 0.072(3) Uani 1 1 d . . . H13A_1 H 0.0778 1.0661 0.1436 0.087 Uiso 1 1 calc R . . C14_1 C 0.0860(3) 1.0314(5) 0.3260(3) 0.059(2) Uani 1 1 d . . . C15_1 C 0.03738(16) 1.0777(5) 0.0639(3) 0.0434(18) Uani 1 1 d . . . C16_1 C 0.02877(18) 1.1715(5) 0.0740(3) 0.060(2) Uani 1 1 d . . . H16A_1 H 0.0137 1.1850 0.1006 0.072 Uiso 1 1 calc R . . C17_1 C 0.04220(18) 1.2435(5) 0.0452(3) 0.056(2) Uani 1 1 d . . . H17A_1 H 0.0377 1.3068 0.0542 0.067 Uiso 1 1 calc R . . C18_1 C 0.06187(18) 1.2245(5) 0.0040(3) 0.053(2) Uani 1 1 d . . . C19_1 C 0.06977(19) 1.1348(5) -0.0053(3) 0.064(2) Uani 1 1 d . . . H19A_1 H 0.0841 1.1219 -0.0332 0.077 Uiso 1 1 calc R . . C20_1 C 0.05820(19) 1.0619(5) 0.0236(3) 0.060(2) Uani 1 1 d . . . H20A_1 H 0.0646 0.9997 0.0157 0.072 Uiso 1 1 calc R . . C21_1 C 0.0775(2) 1.3040(6) -0.0278(4) 0.062(2) Uani 1 1 d . . . C22_1 C 0.1495(2) 0.4440(7) -0.0189(4) 0.098(3) Uani 1 1 d . . . H22A_1 H 0.1712 0.4494 -0.0271 0.147 Uiso 1 1 calc R . . H22B_1 H 0.1439 0.3776 -0.0170 0.147 Uiso 1 1 calc R . . H22C_1 H 0.1453 0.4742 0.0163 0.147 Uiso 1 1 calc R . . C23_1 C 0.1442(3) 0.5833(8) -0.0771(4) 0.109(4) Uani 1 1 d . . . H23A_1 H 0.1663 0.5801 -0.0793 0.164 Uiso 1 1 calc R . . H23B_1 H 0.1384 0.6295 -0.0494 0.164 Uiso 1 1 calc R . . H23C_1 H 0.1360 0.6019 -0.1127 0.164 Uiso 1 1 calc R . . Zn1_2 Zn 0.20309(2) 0.45850(6) 0.14858(4) 0.0555(3) Uani 1 1 d . . . P1_2 P 0.13699(5) 0.95853(14) -0.01759(8) 0.0534(6) Uani 1 1 d . . . C1_2 C 0.15748(18) 0.8661(5) 0.0184(3) 0.049(2) Uani 1 1 d . . . O1_2 O 0.22733(13) 0.6445(4) 0.1184(2) 0.0666(16) Uani 1 1 d . . . N1_2 N 0.24844(19) 0.4494(5) 0.1630(3) 0.086(2) Uani 1 1 d . . . H1N_2 H 0.2535 0.5017 0.1839 0.103 Uiso 1 1 calc R . . O2_2 O 0.18567(13) 0.5611(3) 0.1048(2) 0.0606(14) Uani 1 1 d . . . C2_2 C 0.18723(18) 0.8726(5) 0.0366(3) 0.055(2) Uani 1 1 d . . . H2B_2 H 0.1982 0.9289 0.0303 0.066 Uiso 1 1 calc R . . C3_2 C 0.20139(16) 0.7988(5) 0.0638(3) 0.052(2) Uani 1 1 d . . . H3B_2 H 0.2217 0.8053 0.0757 0.062 Uiso 1 1 calc R . . O3_2 O 0.2087(3) 0.9074(7) -0.2616(3) 0.168(5) Uani 1 1 d . . . C4_2 C 0.1860(2) 0.7168(5) 0.0734(3) 0.050(2) Uani 1 1 d . . . O4_2 O 0.18308(14) 1.0307(4) -0.2783(2) 0.0683(16) Uani 1 1 d . . . C5_2 C 0.1564(2) 0.7076(5) 0.0555(3) 0.058(2) Uani 1 1 d . . . H5B_2 H 0.1458 0.6505 0.0611 0.069 Uiso 1 1 calc R . . O5_2 O 0.21292(16) 1.3593(5) 0.0551(3) 0.087(2) Uani 1 1 d . . . C6_2 C 0.14227(17) 0.7822(5) 0.0293(3) 0.052(2) Uani 1 1 d . . . H6B_2 H 0.1217 0.7759 0.0185 0.062 Uiso 1 1 calc R . . O6_2 O 0.18262(15) 1.3416(4) 0.1264(3) 0.0823(18) Uani 1 1 d . . . C7_2 C 0.2018(2) 0.6362(5) 0.1008(3) 0.0478(19) Uani 1 1 d . . . C8_2 C 0.15359(18) 0.9518(5) -0.0861(3) 0.052(2) Uani 1 1 d . . . C9_2 C 0.1754(2) 0.8929(6) -0.1027(3) 0.084(3) Uani 1 1 d . . . H9B_2 H 0.1831 0.8486 -0.0773 0.101 Uiso 1 1 calc R . . C10_2 C 0.1871(3) 0.8937(7) -0.1550(4) 0.116(5) Uani 1 1 d . . . H10B_2 H 0.2018 0.8487 -0.1654 0.139 Uiso 1 1 calc R . . C11_2 C 0.1774(2) 0.9595(6) -0.1916(3) 0.077(3) Uani 1 1 d . . . C12_2 C 0.1548(2) 1.0201(6) -0.1776(3) 0.068(2) Uani 1 1 d . . . H12B_2 H 0.1473 1.0645 -0.2032 0.081 Uiso 1 1 calc R . . C13_2 C 0.1431(2) 1.0149(6) -0.1252(3) 0.068(2) Uani 1 1 d . . . H13B_2 H 0.1271 1.0564 -0.1154 0.081 Uiso 1 1 calc R . . C14_2 C 0.1910(3) 0.9680(7) -0.2474(4) 0.102(4) Uani 1 1 d . . . C15_2 C 0.15535(17) 1.0638(5) 0.0100(3) 0.0452(18) Uani 1 1 d . . . C16_2 C 0.1769(2) 1.1160(6) -0.0172(4) 0.078(3) Uani 1 1 d . . . H16B_2 H 0.1836 1.0960 -0.0522 0.094 Uiso 1 1 calc R . . C17_2 C 0.1890(2) 1.1971(6) 0.0055(4) 0.075(3) Uani 1 1 d . . . H17B_2 H 0.2037 1.2322 -0.0140 0.090 Uiso 1 1 calc R . . C18_2 C 0.17969(19) 1.2266(5) 0.0564(3) 0.054(2) Uani 1 1 d . . . C19_2 C 0.15733(18) 1.1769(5) 0.0840(3) 0.056(2) Uani 1 1 d . . . H19B_2 H 0.1505 1.1977 0.1188 0.068 Uiso 1 1 calc R . . C20_2 C 0.14497(19) 1.0959(5) 0.0602(3) 0.065(2) Uani 1 1 d . . . H20B_2 H 0.1294 1.0627 0.0787 0.077 Uiso 1 1 calc R . . C21_2 C 0.1930(2) 1.3167(6) 0.0798(4) 0.068(3) Uani 1 1 d . . . C22_2 C 0.2557(4) 0.3708(18) 0.1950(13) 0.44(3) Uani 1 1 d . . . H22D_2 H 0.2777 0.3685 0.2008 0.660 Uiso 1 1 calc R . . H22E_2 H 0.2492 0.3137 0.1762 0.660 Uiso 1 1 calc R . . H22F_2 H 0.2454 0.3753 0.2304 0.660 Uiso 1 1 calc R . . C23_2 C 0.2686(3) 0.4505(12) 0.1161(7) 0.173(7) Uani 1 1 d . . . H23D_2 H 0.2896 0.4499 0.1287 0.260 Uiso 1 1 calc R . . H23E_2 H 0.2649 0.5073 0.0945 0.260 Uiso 1 1 calc R . . H23F_2 H 0.2648 0.3951 0.0934 0.260 Uiso 1 1 calc R . . N100 N 0.2343(3) 0.9547(10) 0.4238(6) 0.080(4) Uiso 0.50 1 d PD . . O100 O 0.2191(5) 0.8420(15) 0.3682(9) 0.199(9) Uiso 0.50 1 d PD . . C100 C 0.2271(6) 0.9229(16) 0.3789(8) 0.156(10) Uiso 0.50 1 d PD . . H10A H 0.2278 0.9655 0.3490 0.187 Uiso 0.50 1 calc PR . . C101 C 0.2309(6) 0.9157(16) 0.4679(8) 0.139(9) Uiso 0.50 1 d PD . . H10C H 0.2248 0.8504 0.4619 0.209 Uiso 0.50 1 calc PR . . H10D H 0.2152 0.9482 0.4888 0.209 Uiso 0.50 1 calc PR . . H10E H 0.2500 0.9172 0.4883 0.209 Uiso 0.50 1 calc PR . . C102 C 0.2419(7) 1.0431(14) 0.4264(11) 0.166(12) Uiso 0.50 1 d PD . . H10F H 0.2420 1.0700 0.3895 0.248 Uiso 0.50 1 calc PR . . H10G H 0.2622 1.0487 0.4424 0.248 Uiso 0.50 1 calc PR . . H10H H 0.2273 1.0769 0.4492 0.248 Uiso 0.50 1 calc PR . . N110 N 0.1492(3) 0.8740(9) 0.2233(5) 0.061(4) Uiso 0.50 1 d PD . . O110 O 0.1696(6) 1.0114(15) 0.2270(10) 0.200(9) Uiso 0.50 1 d PD . . C110 C 0.1617(7) 0.9401(17) 0.2508(10) 0.183(14) Uiso 0.50 1 d PD . . H11A H 0.1647 0.9337 0.2890 0.220 Uiso 0.50 1 calc PR . . C111 C 0.1402(10) 0.803(2) 0.2467(13) 0.28(2) Uiso 0.50 1 d PD . . H11A H 0.1469 0.8047 0.2849 0.418 Uiso 0.50 1 calc PR . . H11B H 0.1486 0.7477 0.2286 0.418 Uiso 0.50 1 calc PR . . H11C H 0.1181 0.8011 0.2454 0.418 Uiso 0.50 1 calc PR . . C112 C 0.1448(5) 0.8903(16) 0.1736(7) 0.122(8) Uiso 0.50 1 d PD . . H11D H 0.1367 0.8340 0.1559 0.184 Uiso 0.50 1 calc PR . . H11E H 0.1640 0.9079 0.1563 0.184 Uiso 0.50 1 calc PR . . H11F H 0.1303 0.9418 0.1698 0.184 Uiso 0.50 1 calc PR . . N120 N 0.0089(4) 0.5441(12) 0.1109(7) 0.114(6) Uiso 0.50 1 d PD . . O120 O 0.0396(5) 0.4834(17) 0.1686(10) 0.200(9) Uiso 0.50 1 d PD . . C120 C 0.0266(4) 0.5552(13) 0.1515(7) 0.097(6) Uiso 0.50 1 d PD . . H12A H 0.0298 0.6149 0.1678 0.116 Uiso 0.50 1 calc PR . . C122 C 0.0049(5) 0.4672(13) 0.0930(10) 0.122(8) Uiso 0.50 1 d PD . . H12C H -0.0087 0.4707 0.0614 0.184 Uiso 0.50 1 calc PR . . H12D H -0.0042 0.4275 0.1212 0.184 Uiso 0.50 1 calc PR . . H12E H 0.0244 0.4404 0.0816 0.184 Uiso 0.50 1 calc PR . . C121 C -0.0057(6) 0.6160(15) 0.0953(12) 0.174(12) Uiso 0.50 1 d PD . . H12F H -0.0188 0.5992 0.0644 0.262 Uiso 0.50 1 calc PR . . H12G H 0.0086 0.6649 0.0839 0.262 Uiso 0.50 1 calc PR . . H12H H -0.0181 0.6394 0.1255 0.262 Uiso 0.50 1 calc PR . . 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_1 0.0714(7) 0.0508(6) 0.0439(6) 0.0009(4) -0.0049(5) 0.0004(5) P1_1 0.0772(17) 0.0501(13) 0.0465(13) -0.0034(10) -0.0069(11) -0.0034(11) C1_1 0.075(6) 0.046(5) 0.041(5) -0.006(4) -0.005(4) -0.010(4) O1_1 0.099(5) 0.043(3) 0.050(3) -0.004(3) -0.012(3) 0.000(3) N1_1 0.076(5) 0.081(5) 0.071(5) -0.003(4) -0.009(4) -0.008(4) C2_1 0.103(7) 0.049(5) 0.053(5) 0.006(4) -0.035(5) -0.002(5) O2_1 0.078(4) 0.056(3) 0.089(4) -0.013(3) -0.026(3) 0.008(3) C3_1 0.096(7) 0.039(5) 0.049(5) -0.008(4) -0.032(5) 0.007(4) O3_1 0.074(4) 0.081(4) 0.043(3) -0.005(3) -0.010(3) 0.000(3) C4_1 0.068(6) 0.030(4) 0.047(5) -0.004(3) -0.012(4) -0.009(4) O4_1 0.087(5) 0.096(5) 0.043(3) 0.002(3) -0.016(3) -0.010(4) O5_1 0.098(5) 0.049(3) 0.066(4) 0.008(3) -0.005(3) -0.004(3) C5_1 0.093(7) 0.062(6) 0.054(5) -0.004(4) -0.021(5) 0.007(5) O6_1 0.119(6) 0.080(4) 0.077(5) 0.002(4) 0.033(4) 0.004(4) C6_1 0.071(6) 0.064(5) 0.045(5) 0.000(4) -0.030(4) 0.002(5) C7_1 0.049(5) 0.046(5) 0.057(6) -0.004(4) -0.019(4) -0.007(4) C8_1 0.063(6) 0.036(4) 0.054(5) 0.007(4) 0.002(4) 0.004(4) C9_1 0.066(6) 0.060(5) 0.048(5) 0.006(4) -0.008(4) -0.002(4) C10_1 0.055(6) 0.074(6) 0.057(6) 0.017(4) 0.009(4) -0.003(5) C11_1 0.073(7) 0.050(5) 0.037(5) -0.010(4) -0.002(4) -0.003(4) C12_1 0.079(6) 0.079(6) 0.043(5) -0.002(4) -0.010(4) -0.036(5) C13_1 0.091(8) 0.090(7) 0.035(5) 0.013(4) 0.001(5) -0.036(6) C14_1 0.099(8) 0.044(5) 0.035(5) -0.002(4) 0.001(5) 0.006(5) C15_1 0.054(5) 0.041(4) 0.036(4) -0.010(3) -0.012(4) 0.001(4) C16_1 0.067(6) 0.058(5) 0.055(5) 0.009(4) 0.010(4) 0.013(4) C17_1 0.064(6) 0.045(5) 0.059(5) -0.002(4) 0.005(4) 0.007(4) C18_1 0.075(6) 0.046(5) 0.039(5) 0.009(4) -0.007(4) 0.009(4) C19_1 0.090(7) 0.045(5) 0.057(5) 0.001(4) -0.001(5) 0.024(4) C20_1 0.092(7) 0.044(5) 0.043(5) 0.012(4) 0.001(5) 0.023(4) C21_1 0.077(7) 0.054(6) 0.056(6) 0.008(5) -0.017(5) -0.001(5) C22_1 0.096(8) 0.126(9) 0.072(7) -0.004(6) -0.039(6) 0.034(7) C23_1 0.114(9) 0.126(10) 0.087(8) -0.009(7) -0.023(6) -0.043(7) Zn1_2 0.0771(8) 0.0396(5) 0.0499(6) -0.0024(4) -0.0074(5) 0.0013(4) P1_2 0.0685(16) 0.0457(12) 0.0461(12) -0.0006(9) -0.0057(10) 0.0036(10) C1_2 0.054(6) 0.056(5) 0.038(4) -0.006(4) -0.012(4) 0.005(4) O1_2 0.056(4) 0.054(3) 0.090(4) 0.020(3) -0.014(3) 0.002(3) N1_2 0.102(7) 0.074(5) 0.081(6) 0.010(4) -0.023(5) 0.002(5) O2_2 0.092(4) 0.036(3) 0.054(3) 0.002(2) -0.014(3) 0.004(3) C2_2 0.055(6) 0.052(5) 0.058(5) 0.009(4) -0.005(4) -0.009(4) C3_2 0.044(5) 0.050(5) 0.061(5) 0.009(4) -0.013(4) -0.011(4) O3_2 0.290(12) 0.140(7) 0.073(5) 0.051(5) 0.078(6) 0.115(8) C4_2 0.067(6) 0.045(5) 0.038(4) 0.001(3) -0.006(4) 0.002(4) O4_2 0.114(5) 0.044(3) 0.047(3) 0.006(3) -0.010(3) 0.000(3) C5_2 0.092(7) 0.031(4) 0.049(5) 0.004(4) -0.001(5) -0.009(4) O5_2 0.102(5) 0.078(4) 0.081(5) 0.001(4) 0.015(4) -0.021(4) C6_2 0.050(5) 0.038(4) 0.068(5) 0.002(4) -0.007(4) -0.002(4) O6_2 0.122(5) 0.059(4) 0.067(4) -0.015(3) -0.012(4) -0.012(3) C7_2 0.064(6) 0.034(4) 0.045(5) 0.003(3) 0.001(4) 0.000(4) C8_2 0.065(6) 0.048(5) 0.044(5) -0.002(4) -0.008(4) 0.000(4) C9_2 0.138(9) 0.059(6) 0.054(6) 0.010(5) -0.001(6) 0.052(6) C10_2 0.217(13) 0.080(7) 0.050(6) 0.017(5) 0.033(7) 0.095(8) C11_2 0.137(9) 0.048(5) 0.047(5) 0.000(4) -0.001(5) 0.050(5) C12_2 0.092(7) 0.058(5) 0.053(6) 0.019(4) -0.014(5) 0.001(5) C13_2 0.081(7) 0.072(6) 0.050(6) 0.009(4) -0.004(5) 0.031(5) C14_2 0.195(12) 0.060(6) 0.050(6) 0.008(5) 0.034(7) 0.068(7) C15_2 0.056(5) 0.042(4) 0.037(4) 0.000(4) -0.003(4) 0.006(4) C16_2 0.102(8) 0.074(6) 0.059(6) -0.011(5) 0.003(5) -0.026(5) C17_2 0.094(7) 0.065(6) 0.065(6) -0.004(5) -0.005(5) -0.010(5) C18_2 0.079(6) 0.049(5) 0.035(5) -0.004(4) -0.012(4) 0.016(4) C19_2 0.066(6) 0.062(5) 0.041(5) -0.007(4) -0.009(4) 0.002(4) C20_2 0.075(6) 0.054(5) 0.065(6) -0.010(4) 0.010(5) -0.011(4) C21_2 0.097(8) 0.043(5) 0.064(7) 0.000(5) -0.024(6) 0.020(5) C22_2 0.125(15) 0.48(4) 0.71(6) 0.51(4) -0.10(2) -0.018(18) C23_2 0.080(10) 0.250(19) 0.188(16) -0.090(14) 0.000(10) 0.033(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1_1 O5_1 1.951(5) 1_545 ? Zn1_1 O1_1 1.965(5) . ? Zn1_1 O3_1 1.982(5) 7_575 ? Zn1_1 N1_1 2.023(8) . ? P1_1 C8_1 1.800(8) . ? P1_1 C1_1 1.814(8) . ? P1_1 C15_1 1.842(7) . ? C1_1 C6_1 1.401(10) . ? C1_1 C2_1 1.403(10) . ? O1_1 C7_1 1.290(8) . ? N1_1 C22_1 1.459(10) . ? N1_1 C23_1 1.483(12) . ? N1_1 H1N_1 0.9300 . ? C2_1 C3_1 1.389(11) . ? C2_1 H2A_1 0.9500 . ? O2_1 C7_1 1.203(8) . ? C3_1 C4_1 1.337(10) . ? C3_1 H3A_1 0.9500 . ? O3_1 C14_1 1.288(10) . ? O3_1 Zn1_1 1.982(5) 7_576 ? C4_1 C5_1 1.381(10) . ? C4_1 C7_1 1.511(10) . ? O4_1 C14_1 1.260(10) . ? O5_1 C21_1 1.300(10) . ? O5_1 Zn1_1 1.951(5) 1_565 ? C5_1 C6_1 1.383(11) . ? C5_1 H5A_1 0.9500 . ? O6_1 C21_1 1.210(10) . ? C6_1 H6A_1 0.9500 . ? C8_1 C9_1 1.370(10) . ? C8_1 C13_1 1.382(10) . ? C9_1 C10_1 1.376(11) . ? C9_1 H9A_1 0.9500 . ? C10_1 C11_1 1.384(11) . ? C10_1 H10A_1 0.9500 . ? C11_1 C12_1 1.405(11) . ? C11_1 C14_1 1.484(11) . ? C12_1 C13_1 1.385(11) . ? C12_1 H12A_1 0.9500 . ? C13_1 H13A_1 0.9500 . ? C15_1 C20_1 1.369(10) . ? C15_1 C16_1 1.411(10) . ? C16_1 C17_1 1.380(10) . ? C16_1 H16A_1 0.9500 . ? C17_1 C18_1 1.359(10) . ? C17_1 H17A_1 0.9500 . ? C18_1 C19_1 1.345(9) . ? C18_1 C21_1 1.540(11) . ? C19_1 C20_1 1.356(10) . ? C19_1 H19A_1 0.9500 . ? C20_1 H20A_1 0.9500 . ? C22_1 H22A_1 0.9800 . ? C22_1 H22B_1 0.9800 . ? C22_1 H22C_1 0.9800 . ? C23_1 H23A_1 0.9800 . ? C23_1 H23B_1 0.9800 . ? C23_1 H23C_1 0.9800 . ? Zn1_2 O2_2 1.970(5) . ? Zn1_2 O6_2 1.973(6) 1_545 ? Zn1_2 O4_2 2.001(6) 7_576 ? Zn1_2 N1_2 2.039(8) . ? P1_2 C1_2 1.825(7) . ? P1_2 C8_2 1.832(8) . ? P1_2 C15_2 1.836(7) . ? C1_2 C2_2 1.391(10) . ? C1_2 C6_2 1.399(10) . ? O1_2 C7_2 1.212(8) . ? N1_2 C22_2 1.405(16) . ? N1_2 C23_2 1.453(15) . ? N1_2 H1N_2 0.9300 . ? O2_2 C7_2 1.291(9) . ? C2_2 C3_2 1.394(10) . ? C2_2 H2B_2 0.9500 . ? C3_2 C4_2 1.372(10) . ? C3_2 H3B_2 0.9500 . ? O3_2 C14_2 1.215(10) . ? C4_2 C5_2 1.388(10) . ? C4_2 C7_2 1.501(10) . ? O4_2 C14_2 1.223(10) . ? O4_2 Zn1_2 2.001(6) 7_575 ? C5_2 C6_2 1.390(10) . ? C5_2 H5B_2 0.9500 . ? O5_2 C21_2 1.229(11) . ? C6_2 H6B_2 0.9500 . ? O6_2 C21_2 1.277(10) . ? O6_2 Zn1_2 1.973(6) 1_565 ? C8_2 C9_2 1.341(10) . ? C8_2 C13_2 1.394(10) . ? C9_2 C10_2 1.378(11) . ? C9_2 H9B_2 0.9500 . ? C10_2 C11_2 1.366(11) . ? C10_2 H10B_2 0.9500 . ? C11_2 C12_2 1.364(11) . ? C11_2 C14_2 1.497(12) . ? C12_2 C13_2 1.385(11) . ? C12_2 H12B_2 0.9500 . ? C13_2 H13B_2 0.9500 . ? C15_2 C16_2 1.380(10) . ? C15_2 C20_2 1.389(10) . ? C16_2 C17_2 1.390(11) . ? C16_2 H16B_2 0.9500 . ? C17_2 C18_2 1.375(11) . ? C17_2 H17B_2 0.9500 . ? C18_2 C19_2 1.391(10) . ? C18_2 C21_2 1.525(11) . ? C19_2 C20_2 1.404(10) . ? C19_2 H19B_2 0.9500 . ? C20_2 H20B_2 0.9500 . ? C22_2 H22D_2 0.9800 . ? C22_2 H22E_2 0.9800 . ? C22_2 H22F_2 0.9800 . ? C23_2 H23D_2 0.9800 . ? C23_2 H23E_2 0.9800 . ? C23_2 H23F_2 0.9800 . ? N100 C101 1.223(15) . ? N100 C100 1.231(16) . ? N100 C102 1.306(16) . ? O100 C100 1.235(17) . ? C100 H10A 0.9500 . ? C101 H10C 0.9800 . ? C101 H10D 0.9800 . ? C101 H10E 0.9800 . ? C102 H10F 0.9800 . ? C102 H10G 0.9800 . ? C102 H10H 0.9800 . ? N110 C111 1.224(16) . ? N110 C112 1.253(15) . ? N110 C110 1.283(16) . ? O110 C110 1.223(18) . ? C110 H11A 0.9500 . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? C112 H11D 0.9800 . ? C112 H11E 0.9800 . ? C112 H11F 0.9800 . ? N120 C122 1.194(15) . ? N120 C121 1.270(15) . ? N120 C120 1.276(15) . ? O120 C120 1.246(17) . ? C120 H12A 0.9500 . ? C122 H12C 0.9800 . ? C122 H12D 0.9800 . ? C122 H12E 0.9800 . ? C121 H12F 0.9800 . ? C121 H12G 0.9800 . ? C121 H12H 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 O5_1 Zn1_1 O1_1 106.2(2) 1_545 . ? O5_1 Zn1_1 O3_1 112.7(2) 1_545 7_575 ? O1_1 Zn1_1 O3_1 97.2(2) . 7_575 ? O5_1 Zn1_1 N1_1 116.8(3) 1_545 . ? O1_1 Zn1_1 N1_1 115.4(3) . . ? O3_1 Zn1_1 N1_1 106.9(3) 7_575 . ? C8_1 P1_1 C1_1 102.6(3) . . ? C8_1 P1_1 C15_1 101.4(3) . . ? C1_1 P1_1 C15_1 102.7(3) . . ? C6_1 C1_1 C2_1 116.6(7) . . ? C6_1 C1_1 P1_1 124.6(6) . . ? C2_1 C1_1 P1_1 118.8(6) . . ? C7_1 O1_1 Zn1_1 113.8(5) . . ? C22_1 N1_1 C23_1 113.1(8) . . ? C22_1 N1_1 Zn1_1 117.9(6) . . ? C23_1 N1_1 Zn1_1 113.3(6) . . ? C22_1 N1_1 H1N_1 103.4 . . ? C23_1 N1_1 H1N_1 103.4 . . ? Zn1_1 N1_1 H1N_1 103.4 . . ? C3_1 C2_1 C1_1 120.9(7) . . ? C3_1 C2_1 H2A_1 119.6 . . ? C1_1 C2_1 H2A_1 119.6 . . ? C4_1 C3_1 C2_1 121.2(7) . . ? C4_1 C3_1 H3A_1 119.4 . . ? C2_1 C3_1 H3A_1 119.4 . . ? C14_1 O3_1 Zn1_1 123.7(6) . 7_576 ? C3_1 C4_1 C5_1 119.8(7) . . ? C3_1 C4_1 C7_1 122.9(7) . . ? C5_1 C4_1 C7_1 117.3(7) . . ? C21_1 O5_1 Zn1_1 112.8(5) . 1_565 ? C4_1 C5_1 C6_1 120.4(8) . . ? C4_1 C5_1 H5A_1 119.8 . . ? C6_1 C5_1 H5A_1 119.8 . . ? C5_1 C6_1 C1_1 120.9(7) . . ? C5_1 C6_1 H6A_1 119.6 . . ? C1_1 C6_1 H6A_1 119.6 . . ? O2_1 C7_1 O1_1 122.1(7) . . ? O2_1 C7_1 C4_1 122.7(7) . . ? O1_1 C7_1 C4_1 115.2(7) . . ? C9_1 C8_1 C13_1 116.3(7) . . ? C9_1 C8_1 P1_1 119.2(6) . . ? C13_1 C8_1 P1_1 124.4(6) . . ? C8_1 C9_1 C10_1 122.5(8) . . ? C8_1 C9_1 H9A_1 118.7 . . ? C10_1 C9_1 H9A_1 118.7 . . ? C9_1 C10_1 C11_1 121.3(8) . . ? C9_1 C10_1 H10A_1 119.4 . . ? C11_1 C10_1 H10A_1 119.4 . . ? C10_1 C11_1 C12_1 117.2(7) . . ? C10_1 C11_1 C14_1 123.9(8) . . ? C12_1 C11_1 C14_1 118.9(8) . . ? C13_1 C12_1 C11_1 119.8(8) . . ? C13_1 C12_1 H12A_1 120.1 . . ? C11_1 C12_1 H12A_1 120.1 . . ? C8_1 C13_1 C12_1 122.8(8) . . ? C8_1 C13_1 H13A_1 118.6 . . ? C12_1 C13_1 H13A_1 118.6 . . ? O4_1 C14_1 O3_1 124.5(8) . . ? O4_1 C14_1 C11_1 121.6(8) . . ? O3_1 C14_1 C11_1 113.9(9) . . ? C20_1 C15_1 C16_1 117.6(7) . . ? C20_1 C15_1 P1_1 126.9(5) . . ? C16_1 C15_1 P1_1 115.5(6) . . ? C17_1 C16_1 C15_1 120.0(7) . . ? C17_1 C16_1 H16A_1 120.0 . . ? C15_1 C16_1 H16A_1 120.0 . . ? C18_1 C17_1 C16_1 120.3(7) . . ? C18_1 C17_1 H17A_1 119.8 . . ? C16_1 C17_1 H17A_1 119.8 . . ? C19_1 C18_1 C17_1 118.8(7) . . ? C19_1 C18_1 C21_1 119.9(8) . . ? C17_1 C18_1 C21_1 121.0(7) . . ? C18_1 C19_1 C20_1 122.9(8) . . ? C18_1 C19_1 H19A_1 118.5 . . ? C20_1 C19_1 H19A_1 118.5 . . ? C19_1 C20_1 C15_1 120.1(7) . . ? C19_1 C20_1 H20A_1 119.9 . . ? C15_1 C20_1 H20A_1 119.9 . . ? O6_1 C21_1 O5_1 125.7(8) . . ? O6_1 C21_1 C18_1 121.5(8) . . ? O5_1 C21_1 C18_1 112.8(8) . . ? N1_1 C22_1 H22A_1 109.5 . . ? N1_1 C22_1 H22B_1 109.5 . . ? H22A_1 C22_1 H22B_1 109.5 . . ? N1_1 C22_1 H22C_1 109.5 . . ? H22A_1 C22_1 H22C_1 109.5 . . ? H22B_1 C22_1 H22C_1 109.5 . . ? N1_1 C23_1 H23A_1 109.5 . . ? N1_1 C23_1 H23B_1 109.5 . . ? H23A_1 C23_1 H23B_1 109.5 . . ? N1_1 C23_1 H23C_1 109.5 . . ? H23A_1 C23_1 H23C_1 109.5 . . ? H23B_1 C23_1 H23C_1 109.5 . . ? O2_2 Zn1_2 O6_2 107.4(2) . 1_545 ? O2_2 Zn1_2 O4_2 104.8(2) . 7_576 ? O6_2 Zn1_2 O4_2 96.2(3) 1_545 7_576 ? O2_2 Zn1_2 N1_2 121.7(3) . . ? O6_2 Zn1_2 N1_2 116.4(3) 1_545 . ? O4_2 Zn1_2 N1_2 106.5(3) 7_576 . ? C1_2 P1_2 C8_2 101.8(3) . . ? C1_2 P1_2 C15_2 101.2(3) . . ? C8_2 P1_2 C15_2 101.7(3) . . ? C2_2 C1_2 C6_2 116.7(7) . . ? C2_2 C1_2 P1_2 125.1(6) . . ? C6_2 C1_2 P1_2 118.1(6) . . ? C22_2 N1_2 C23_2 107.9(15) . . ? C22_2 N1_2 Zn1_2 111.9(9) . . ? C23_2 N1_2 Zn1_2 117.7(7) . . ? C22_2 N1_2 H1N_2 106.2 . . ? C23_2 N1_2 H1N_2 106.2 . . ? Zn1_2 N1_2 H1N_2 106.2 . . ? C7_2 O2_2 Zn1_2 116.2(5) . . ? C3_2 C2_2 C1_2 121.8(7) . . ? C3_2 C2_2 H2B_2 119.1 . . ? C1_2 C2_2 H2B_2 119.1 . . ? C4_2 C3_2 C2_2 120.2(7) . . ? C4_2 C3_2 H3B_2 119.9 . . ? C2_2 C3_2 H3B_2 119.9 . . ? C3_2 C4_2 C5_2 119.6(7) . . ? C3_2 C4_2 C7_2 119.9(8) . . ? C5_2 C4_2 C7_2 120.5(7) . . ? C14_2 O4_2 Zn1_2 118.9(6) . 7_575 ? C4_2 C5_2 C6_2 119.9(7) . . ? C4_2 C5_2 H5B_2 120.1 . . ? C6_2 C5_2 H5B_2 120.1 . . ? C5_2 C6_2 C1_2 121.8(7) . . ? C5_2 C6_2 H6B_2 119.1 . . ? C1_2 C6_2 H6B_2 119.1 . . ? C21_2 O6_2 Zn1_2 108.4(6) . 1_565 ? O1_2 C7_2 O2_2 124.6(7) . . ? O1_2 C7_2 C4_2 121.0(7) . . ? O2_2 C7_2 C4_2 114.3(8) . . ? C9_2 C8_2 C13_2 115.9(7) . . ? C9_2 C8_2 P1_2 126.8(6) . . ? C13_2 C8_2 P1_2 117.4(6) . . ? C8_2 C9_2 C10_2 123.1(8) . . ? C8_2 C9_2 H9B_2 118.5 . . ? C10_2 C9_2 H9B_2 118.5 . . ? C11_2 C10_2 C9_2 119.7(8) . . ? C11_2 C10_2 H10B_2 120.1 . . ? C9_2 C10_2 H10B_2 120.1 . . ? C12_2 C11_2 C10_2 120.0(8) . . ? C12_2 C11_2 C14_2 118.1(7) . . ? C10_2 C11_2 C14_2 121.8(8) . . ? C11_2 C12_2 C13_2 118.2(7) . . ? C11_2 C12_2 H12B_2 120.9 . . ? C13_2 C12_2 H12B_2 120.9 . . ? C12_2 C13_2 C8_2 123.0(8) . . ? C12_2 C13_2 H13B_2 118.5 . . ? C8_2 C13_2 H13B_2 118.5 . . ? O3_2 C14_2 O4_2 121.7(9) . . ? O3_2 C14_2 C11_2 117.6(8) . . ? O4_2 C14_2 C11_2 120.6(8) . . ? C16_2 C15_2 C20_2 118.5(7) . . ? C16_2 C15_2 P1_2 124.7(6) . . ? C20_2 C15_2 P1_2 116.6(6) . . ? C15_2 C16_2 C17_2 121.5(8) . . ? C15_2 C16_2 H16B_2 119.3 . . ? C17_2 C16_2 H16B_2 119.3 . . ? C18_2 C17_2 C16_2 120.0(9) . . ? C18_2 C17_2 H17B_2 120.0 . . ? C16_2 C17_2 H17B_2 120.0 . . ? C17_2 C18_2 C19_2 119.8(7) . . ? C17_2 C18_2 C21_2 118.8(9) . . ? C19_2 C18_2 C21_2 121.3(8) . . ? C18_2 C19_2 C20_2 119.6(7) . . ? C18_2 C19_2 H19B_2 120.2 . . ? C20_2 C19_2 H19B_2 120.2 . . ? C15_2 C20_2 C19_2 120.6(8) . . ? C15_2 C20_2 H20B_2 119.7 . . ? C19_2 C20_2 H20B_2 119.7 . . ? O5_2 C21_2 O6_2 123.9(8) . . ? O5_2 C21_2 C18_2 120.5(9) . . ? O6_2 C21_2 C18_2 115.6(9) . . ? N1_2 C22_2 H22D_2 109.5 . . ? N1_2 C22_2 H22E_2 109.5 . . ? H22D_2 C22_2 H22E_2 109.5 . . ? N1_2 C22_2 H22F_2 109.5 . . ? H22D_2 C22_2 H22F_2 109.5 . . ? H22E_2 C22_2 H22F_2 109.5 . . ? N1_2 C23_2 H23D_2 109.5 . . ? N1_2 C23_2 H23E_2 109.5 . . ? H23D_2 C23_2 H23E_2 109.5 . . ? N1_2 C23_2 H23F_2 109.5 . . ? H23D_2 C23_2 H23F_2 109.5 . . ? H23E_2 C23_2 H23F_2 109.5 . . ? C101 N100 C100 126.0(15) . . ? C101 N100 C102 115.3(15) . . ? C100 N100 C102 117.8(15) . . ? N100 C100 O100 127(2) . . ? N100 C100 H10A 116.3 . . ? O100 C100 H10A 116.3 . . ? N100 C101 H10C 109.5 . . ? N100 C101 H10D 109.5 . . ? H10C C101 H10D 109.5 . . ? N100 C101 H10E 109.5 . . ? H10C C101 H10E 109.5 . . ? H10D C101 H10E 109.5 . . ? N100 C102 H10F 109.5 . . ? N100 C102 H10G 109.5 . . ? H10F C102 H10G 109.5 . . ? N100 C102 H10H 109.5 . . ? H10F C102 H10H 109.5 . . ? H10G C102 H10H 109.5 . . ? C111 N110 C112 123.9(16) . . ? C111 N110 C110 119.9(16) . . ? C112 N110 C110 116.0(13) . . ? O110 C110 N110 119.0(19) . . ? O110 C110 H11A 120.5 . . ? N110 C110 H11A 120.5 . . ? N110 C111 H11A 109.5 . . ? N110 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? N110 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? N110 C112 H11D 109.5 . . ? N110 C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? N110 C112 H11F 109.5 . . ? H11D C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? C122 N120 C121 123.8(16) . . ? C122 N120 C120 119.3(15) . . ? C121 N120 C120 116.5(15) . . ? O120 C120 N120 116.2(17) . . ? O120 C120 H12A 121.9 . . ? N120 C120 H12A 121.9 . . ? N120 C122 H12C 109.5 . . ? N120 C122 H12D 109.5 . . ? H12C C122 H12D 109.5 . . ? N120 C122 H12E 109.5 . . ? H12C C122 H12E 109.5 . . ? H12D C122 H12E 109.5 . . ? N120 C121 H12F 109.5 . . ? N120 C121 H12G 109.5 . . ? H12F C121 H12G 109.5 . . ? N120 C121 H12H 109.5 . . ? H12F C121 H12H 109.5 . . ? H12G C121 H12H 109.5 . . ? # Attachment 'PCM-2_NEW.cif' data_sh0705 _database_code_depnum_ccdc_archive 'CCDC 708773' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H39 N O16 P2 Zn4, C3 H7 N O, 2(H2 O)' _chemical_formula_sum 'C50 H50 N2 O19 P2 Zn4' _chemical_formula_weight 1302.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.5679(3) _cell_length_b 14.4250(2) _cell_length_c 22.2199(4) _cell_angle_alpha 90.00 _cell_angle_beta 130.8320(6) _cell_angle_gamma 90.00 _cell_volume 7898.25(19) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 38003 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 25.03 _exptl_crystal_description Rod _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2648 _exptl_absorpt_coefficient_mu 1.292 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.901 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 29764 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 24.99 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.989 _reflns_number_total 6877 _reflns_number_gt 4885 _reflns_threshold_expression >2sigma(I) _refine_diff_density_max 1.623 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.120 _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.1506P)^2^+20.2014P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6877 _refine_ls_number_parameters 341 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1083 _refine_ls_R_factor_gt 0.0795 _refine_ls_wR_factor_ref 0.2393 _refine_ls_wR_factor_gt 0.2194 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.298 -0.156 0.298 1118 206 ' ' 2 0.318 0.118 0.818 1118 206 ' ' _platon_squeeze_details ; ; 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 -0.04988(3) -0.02517(4) 0.07550(4) 0.0385(3) Uani 1 1 d . . . P1 P -0.21871(7) 0.47612(10) 0.02658(11) 0.0433(4) Uani 1 1 d . . . O1 O -0.09067(19) 0.0849(3) 0.0603(3) 0.0485(11) Uani 1 1 d . . . C1 C -0.1776(2) 0.3870(4) 0.0284(4) 0.0399(14) Uani 1 1 d . . . Zn2 Zn -0.00597(3) 0.10548(5) 0.01428(5) 0.0432(3) Uani 1 1 d . . . O2 O -0.05431(19) 0.1819(3) 0.0265(3) 0.0516(12) Uani 1 1 d . . . C2 C -0.1770(3) 0.2998(4) 0.0559(4) 0.0505(17) Uani 1 1 d . . . H2 H -0.1970 0.2896 0.0727 0.061 Uiso 1 1 calc R . . C3 C -0.1478(3) 0.2288(4) 0.0589(4) 0.0498(17) Uani 1 1 d . . . H3 H -0.1489 0.1692 0.0760 0.060 Uiso 1 1 calc R . . O3 O -0.07270(19) 0.8594(3) 0.0940(3) 0.0490(11) Uani 1 1 d . . . C4 C -0.1171(2) 0.2422(4) 0.0375(4) 0.0395(14) Uani 1 1 d . . . O4 O -0.1435(2) 0.8867(4) -0.0294(4) 0.0760(17) Uani 1 1 d . . . C5 C -0.1180(3) 0.3288(4) 0.0094(5) 0.0548(18) Uani 1 1 d . . . H5 H -0.0982 0.3389 -0.0077 0.066 Uiso 1 1 calc R . . O5 O -0.47749(18) 0.5087(3) -0.3203(3) 0.0483(11) Uani 1 1 d . . . C6 C -0.1475(3) 0.4002(5) 0.0062(5) 0.059(2) Uani 1 1 d . . . H6 H -0.1469 0.4596 -0.0117 0.071 Uiso 1 1 calc R . . O6 O -0.44613(18) 0.4163(3) -0.3623(3) 0.0477(11) Uani 1 1 d . . . O7 O -0.04307(18) -0.0227(3) -0.0055(3) 0.0410(10) Uani 1 1 d . . . H7A H -0.0804 -0.0209 -0.0589 0.049 Uiso 1 1 calc R . . C7 C -0.0845(3) 0.1645(4) 0.0413(4) 0.0451(16) Uani 1 1 d . . . C8 C -0.1906(3) 0.5837(4) 0.0226(4) 0.0448(15) Uani 1 1 d . . . C9 C -0.1349(3) 0.6000(5) 0.0832(5) 0.068(2) Uani 1 1 d . . . H9 H -0.1123 0.5541 0.1227 0.082 Uiso 1 1 calc R . . C10 C -0.1130(3) 0.6827(5) 0.0852(5) 0.066(2) Uani 1 1 d . . . H10 H -0.0754 0.6937 0.1269 0.080 Uiso 1 1 calc R . . C11 C -0.1442(3) 0.7495(4) 0.0284(4) 0.0459(15) Uani 1 1 d . . . C12 C -0.1990(4) 0.7345(5) -0.0275(6) 0.079(3) Uani 1 1 d . . . H12 H -0.2219 0.7821 -0.0645 0.095 Uiso 1 1 calc R . . C13 C -0.2210(3) 0.6531(6) -0.0309(5) 0.076(3) Uani 1 1 d . . . H13 H -0.2589 0.6440 -0.0721 0.091 Uiso 1 1 calc R . . C14 C -0.1193(3) 0.8378(4) 0.0299(5) 0.0501(17) Uani 1 1 d . . . C15 C -0.2844(2) 0.4681(4) -0.0760(4) 0.0382(14) Uani 1 1 d . . . C16 C -0.3280(2) 0.5100(4) -0.0905(4) 0.0421(14) Uani 1 1 d . . . H16 H -0.3235 0.5400 -0.0485 0.051 Uiso 1 1 calc R . . C17 C -0.3784(3) 0.5085(4) -0.1664(4) 0.0417(14) Uani 1 1 d . . . H17 H -0.4082 0.5387 -0.1762 0.050 Uiso 1 1 calc R . . C18 C -0.3860(3) 0.4634(4) -0.2282(4) 0.0393(14) Uani 1 1 d . . . C19 C -0.3424(3) 0.4185(5) -0.2125(4) 0.0477(16) Uani 1 1 d . . . H19 H -0.3473 0.3858 -0.2540 0.057 Uiso 1 1 calc R . . C20 C -0.2919(3) 0.4208(4) -0.1379(4) 0.0507(17) Uani 1 1 d . . . H20 H -0.2621 0.3904 -0.1281 0.061 Uiso 1 1 calc R . . C21 C -0.4405(3) 0.4618(4) -0.3106(4) 0.0426(15) Uani 1 1 d . . . O110 O 0.0377(10) 0.4551(14) 0.2560(14) 0.182(9) Uiso 0.50 1 d PD A -1 N110 N 0.0282(7) 0.2976(11) 0.2378(11) 0.121(7) Uiso 0.50 1 d PD A -1 C110 C 0.0221(8) 0.3746(13) 0.2627(14) 0.136(10) Uiso 0.50 1 d PD A -1 H11G H 0.0060 0.3721 0.2862 0.164 Uiso 0.50 1 calc PR A -1 C111 C 0.0529(11) 0.2977(17) 0.2079(17) 0.140(10) Uiso 0.50 1 d PD A -1 H11A H 0.0427 0.3538 0.1760 0.210 Uiso 0.50 1 calc PR A -1 H11B H 0.0417 0.2429 0.1743 0.210 Uiso 0.50 1 calc PR A -1 H11C H 0.0923 0.2965 0.2515 0.210 Uiso 0.50 1 calc PR A -1 C112 C 0.0141(9) 0.2168(12) 0.2487(15) 0.101(7) Uiso 0.50 1 d PD A -1 H11D H -0.0001 0.2273 0.2757 0.151 Uiso 0.50 1 calc PR A -1 H11E H 0.0460 0.1763 0.2814 0.151 Uiso 0.50 1 calc PR A -1 H11F H -0.0139 0.1875 0.1970 0.151 Uiso 0.50 1 calc PR A -1 O120 O -0.0638(3) 0.1340(5) -0.1072(4) 0.0289(15) Uiso 0.50 1 d PD . . N120 N -0.1222(6) 0.2059(10) -0.2280(8) 0.080(4) Uiso 0.50 1 d PD . . C120 C -0.0765(7) 0.1808(11) -0.1593(8) 0.092(6) Uiso 0.50 1 d PD . . H12G H -0.0461 0.2079 -0.1495 0.138 Uiso 0.50 1 calc PR . . C121 C -0.1690(8) 0.1717(19) -0.2513(15) 0.135(9) Uiso 0.50 1 d PD . . H12A H -0.1996 0.2011 -0.3014 0.202 Uiso 0.50 1 calc PR . . H12B H -0.1715 0.1845 -0.2104 0.202 Uiso 0.50 1 calc PR . . H12C H -0.1702 0.1046 -0.2591 0.202 Uiso 0.50 1 calc PR . . C122 C -0.1223(9) 0.2532(16) -0.2766(13) 0.118(8) Uiso 0.50 1 d PD . . H12D H -0.0853 0.2742 -0.2501 0.176 Uiso 0.50 1 calc PR . . H12E H -0.1461 0.3071 -0.2946 0.176 Uiso 0.50 1 calc PR . . H12F H -0.1356 0.2146 -0.3225 0.176 Uiso 0.50 1 calc PR . . O201 O 0.0000 0.2184(8) 0.7500 0.108(3) Uiso 1 2 d S . . O202 O 0.0106(8) 0.4065(12) 0.7178(11) 0.123(5) Uiso 0.50 1 d P . . O100 O 0.0339(3) 0.2258(4) 0.0281(4) 0.0215(14) Uiso 0.50 1 d PD . . H10F H 0.0078 0.2727 -0.0049 0.026 Uiso 0.50 1 calc PR . . C101 C 0.1458(8) 0.2177(14) 0.1353(11) 0.083(5) Uiso 0.50 1 d PD . . H10A H 0.1750 0.2632 0.1582 0.124 Uiso 0.50 1 calc PR . . H10B H 0.1502 0.1679 0.1100 0.124 Uiso 0.50 1 calc PR . . H10C H 0.1473 0.1918 0.1775 0.124 Uiso 0.50 1 calc PR . . C100 C 0.0907(8) 0.265(3) 0.073(3) 0.30(3) Uiso 0.50 1 d PD . . H10D H 0.0920 0.3221 0.0992 0.358 Uiso 0.50 1 calc PR . . H10E H 0.0911 0.2869 0.0310 0.358 Uiso 0.50 1 calc PR . . 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 0.0388(4) 0.0301(4) 0.0531(5) -0.0005(3) 0.0329(4) -0.0017(3) P1 0.0383(9) 0.0318(9) 0.0596(11) -0.0026(7) 0.0318(9) -0.0002(6) O1 0.053(3) 0.032(2) 0.076(3) 0.002(2) 0.049(3) 0.0019(19) C1 0.031(3) 0.033(3) 0.051(4) -0.002(2) 0.025(3) 0.000(2) Zn2 0.0520(5) 0.0340(4) 0.0574(5) 0.0036(3) 0.0418(4) 0.0030(3) O2 0.059(3) 0.041(2) 0.082(3) 0.005(2) 0.058(3) 0.006(2) C2 0.051(4) 0.038(4) 0.080(5) 0.004(3) 0.051(4) 0.001(3) C3 0.046(4) 0.035(3) 0.076(5) 0.005(3) 0.043(4) 0.001(3) O3 0.050(3) 0.039(2) 0.062(3) -0.012(2) 0.039(3) -0.017(2) C4 0.033(3) 0.033(3) 0.057(4) -0.001(3) 0.032(3) -0.001(2) O4 0.067(4) 0.057(3) 0.079(4) 0.010(3) 0.036(3) -0.012(3) C5 0.050(4) 0.043(4) 0.090(5) 0.006(3) 0.054(4) 0.002(3) O5 0.040(3) 0.052(3) 0.052(3) 0.006(2) 0.030(2) 0.009(2) C6 0.061(5) 0.034(4) 0.098(6) 0.016(3) 0.058(5) 0.013(3) O6 0.047(3) 0.036(2) 0.057(3) 0.001(2) 0.033(2) 0.0049(19) O7 0.042(2) 0.040(2) 0.046(2) -0.0007(17) 0.031(2) 0.0014(18) C7 0.039(4) 0.036(3) 0.050(4) 0.004(3) 0.024(3) 0.008(3) C8 0.036(4) 0.037(3) 0.058(4) -0.013(3) 0.029(3) -0.008(3) C9 0.057(5) 0.056(5) 0.066(5) 0.000(4) 0.029(4) -0.017(4) C10 0.060(5) 0.055(5) 0.071(5) -0.009(4) 0.037(4) -0.022(4) C11 0.048(4) 0.033(3) 0.061(4) -0.007(3) 0.038(4) -0.002(3) C12 0.060(5) 0.046(4) 0.091(6) 0.014(4) 0.031(5) -0.010(4) C13 0.043(4) 0.059(5) 0.088(6) 0.018(4) 0.027(4) -0.006(4) C14 0.052(4) 0.032(3) 0.077(5) -0.008(3) 0.047(4) -0.007(3) C15 0.034(3) 0.034(3) 0.048(4) 0.004(2) 0.027(3) -0.001(2) C16 0.036(4) 0.039(3) 0.054(4) -0.007(3) 0.030(3) 0.000(3) C17 0.034(3) 0.041(3) 0.057(4) 0.002(3) 0.033(3) 0.005(3) C18 0.042(3) 0.029(3) 0.058(4) 0.000(3) 0.037(3) -0.001(2) C19 0.036(4) 0.050(4) 0.058(4) -0.006(3) 0.031(3) 0.003(3) C20 0.043(4) 0.044(4) 0.075(5) -0.008(3) 0.043(4) 0.002(3) C21 0.046(4) 0.034(3) 0.059(4) 0.003(3) 0.039(3) -0.002(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 O7 1.951(4) . ? Zn1 O1 1.953(4) . ? Zn1 O5 1.959(4) 8_556 ? Zn1 O3 1.973(4) 1_545 ? P1 C8 1.832(6) . ? P1 C1 1.838(6) . ? P1 C15 1.846(6) . ? O1 C7 1.283(7) . ? C1 C6 1.369(10) . ? C1 C2 1.392(9) . ? Zn2 O100 2.066(6) . ? Zn2 O2 2.080(4) . ? Zn2 O120 2.087(7) . ? Zn2 O7 2.093(4) . ? Zn2 O7 2.103(4) 5 ? Zn2 O6 2.104(5) 8_556 ? O2 C7 1.250(8) . ? C2 C3 1.369(9) . ? C2 H2 0.9500 . ? C3 C4 1.376(9) . ? C3 H3 0.9500 . ? O3 C14 1.266(8) . ? O3 Zn1 1.973(4) 1_565 ? C4 C5 1.387(9) . ? C4 C7 1.507(8) . ? O4 C14 1.223(9) . ? C5 C6 1.378(9) . ? C5 H5 0.9500 . ? O5 C21 1.272(8) . ? O5 Zn1 1.959(4) 8_455 ? C6 H6 0.9500 . ? O6 C21 1.229(8) . ? O6 Zn2 2.104(5) 8_455 ? O7 Zn2 2.103(4) 5 ? O7 H7A 1.0000 . ? C8 C13 1.363(10) . ? C8 C9 1.403(10) . ? C9 C10 1.375(10) . ? C9 H9 0.9500 . ? C10 C11 1.370(10) . ? C10 H10 0.9500 . ? C11 C12 1.368(10) . ? C11 C14 1.499(9) . ? C12 C13 1.351(11) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C15 C16 1.373(9) . ? C15 C20 1.406(9) . ? C16 C17 1.386(9) . ? C16 H16 0.9500 . ? C17 C18 1.387(9) . ? C17 H17 0.9500 . ? C18 C19 1.384(9) . ? C18 C21 1.500(9) . ? C19 C20 1.374(10) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? O110 C110 1.315(18) . ? N110 C110 1.313(17) . ? N110 C112 1.331(15) . ? N110 C111 1.335(17) . ? C110 H11G 0.9500 . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? C112 H11D 0.9800 . ? C112 H11E 0.9800 . ? C112 H11F 0.9800 . ? O120 C120 1.156(14) . ? N120 C122 1.276(15) . ? N120 C120 1.305(15) . ? N120 C121 1.345(16) . ? C120 H12G 0.9500 . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? C122 H12D 0.9800 . ? C122 H12E 0.9800 . ? C122 H12F 0.9800 . ? O100 C100 1.526(19) . ? O100 H10F 0.9500 . ? C101 C100 1.537(19) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C100 H10D 0.9900 . ? C100 H10E 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Zn1 O1 107.48(18) . . ? O7 Zn1 O5 108.27(19) . 8_556 ? O1 Zn1 O5 105.2(2) . 8_556 ? O7 Zn1 O3 119.50(18) . 1_545 ? O1 Zn1 O3 114.57(19) . 1_545 ? O5 Zn1 O3 100.50(19) 8_556 1_545 ? C8 P1 C1 102.3(3) . . ? C8 P1 C15 101.9(3) . . ? C1 P1 C15 102.9(3) . . ? C7 O1 Zn1 123.3(4) . . ? C6 C1 C2 118.4(6) . . ? C6 C1 P1 125.3(5) . . ? C2 C1 P1 116.2(5) . . ? O100 Zn2 O2 89.5(2) . . ? O100 Zn2 O120 88.5(3) . . ? O2 Zn2 O120 86.8(2) . . ? O100 Zn2 O7 173.6(2) . . ? O2 Zn2 O7 96.49(17) . . ? O120 Zn2 O7 89.6(2) . . ? O100 Zn2 O7 92.8(2) . 5 ? O2 Zn2 O7 177.03(17) . 5 ? O120 Zn2 O7 95.1(2) . 5 ? O7 Zn2 O7 81.29(17) . 5 ? O100 Zn2 O6 88.6(2) . 8_556 ? O2 Zn2 O6 92.55(19) . 8_556 ? O120 Zn2 O6 177.1(2) . 8_556 ? O7 Zn2 O6 93.26(16) . 8_556 ? O7 Zn2 O6 85.63(17) 5 8_556 ? C7 O2 Zn2 136.1(4) . . ? C3 C2 C1 120.5(6) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 121.0(6) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C14 O3 Zn1 108.2(4) . 1_565 ? C3 C4 C5 118.5(6) . . ? C3 C4 C7 121.3(5) . . ? C5 C4 C7 120.2(6) . . ? C6 C5 C4 120.4(6) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C21 O5 Zn1 122.6(4) . 8_455 ? C1 C6 C5 121.1(6) . . ? C1 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C21 O6 Zn2 138.0(4) . 8_455 ? Zn1 O7 Zn2 102.77(18) . . ? Zn1 O7 Zn2 128.8(2) . 5 ? Zn2 O7 Zn2 98.71(17) . 5 ? Zn1 O7 H7A 108.2 . . ? Zn2 O7 H7A 108.2 . . ? Zn2 O7 H7A 108.2 5 . ? O2 C7 O1 125.9(6) . . ? O2 C7 C4 118.7(5) . . ? O1 C7 C4 115.4(6) . . ? C13 C8 C9 117.3(6) . . ? C13 C8 P1 124.4(5) . . ? C9 C8 P1 118.0(5) . . ? C10 C9 C8 119.6(7) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C11 C10 C9 121.7(7) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C12 C11 C10 117.8(6) . . ? C12 C11 C14 121.3(6) . . ? C10 C11 C14 120.9(6) . . ? C13 C12 C11 121.2(7) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C8 122.3(7) . . ? C12 C13 H13 118.9 . . ? C8 C13 H13 118.9 . . ? O4 C14 O3 121.5(6) . . ? O4 C14 C11 120.6(7) . . ? O3 C14 C11 117.9(6) . . ? C16 C15 C20 119.5(6) . . ? C16 C15 P1 116.6(5) . . ? C20 C15 P1 123.9(5) . . ? C15 C16 C17 120.0(6) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C18 121.0(6) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C19 C18 C17 118.7(6) . . ? C19 C18 C21 120.0(6) . . ? C17 C18 C21 121.3(5) . . ? C20 C19 C18 121.0(6) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C15 119.8(6) . . ? C19 C20 H20 120.1 . . ? C15 C20 H20 120.1 . . ? O6 C21 O5 125.5(6) . . ? O6 C21 C18 119.0(6) . . ? O5 C21 C18 115.5(6) . . ? C110 N110 C112 119.9(15) . . ? C110 N110 C111 121.0(15) . . ? C112 N110 C111 118.8(15) . . ? N110 C110 O110 121.4(19) . . ? N110 C110 H11G 119.3 . . ? O110 C110 H11G 119.3 . . ? N110 C111 H11A 109.5 . . ? N110 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? N110 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? N110 C112 H11D 109.5 . . ? N110 C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? N110 C112 H11F 109.5 . . ? H11D C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? C120 O120 Zn2 147.0(10) . . ? C122 N120 C120 120.7(14) . . ? C122 N120 C121 119.7(14) . . ? C120 N120 C121 119.1(13) . . ? O120 C120 N120 136.2(17) . . ? O120 C120 H12G 111.9 . . ? N120 C120 H12G 111.9 . . ? N120 C121 H12A 109.5 . . ? N120 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? N120 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? N120 C122 H12D 109.5 . . ? N120 C122 H12E 109.5 . . ? H12D C122 H12E 109.5 . . ? N120 C122 H12F 109.5 . . ? H12D C122 H12F 109.5 . . ? H12E C122 H12F 109.5 . . ? C100 O100 Zn2 141.9(14) . . ? C100 O100 H10F 109.1 . . ? Zn2 O100 H10F 109.1 . . ? C100 C101 H10A 109.5 . . ? C100 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C100 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? O100 C100 C101 129(3) . . ? O100 C100 H10D 105.2 . . ? C101 C100 H10D 105.2 . . ? O100 C100 H10E 105.2 . . ? C101 C100 H10E 105.2 . . ? H10D C100 H10E 105.9 . . ? # Attachment 'PCM-3_NEW.cif' data_sh0704a _database_code_depnum_ccdc_archive 'CCDC 708774' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H32 N4 O14 P2 Zn4, 2(C3 H7 N O)' _chemical_formula_sum 'C52 H46 N6 O16 P2 Zn4' _chemical_formula_weight 1336.38 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' _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 11.4898(3) _cell_length_b 14.5201(5) _cell_length_c 24.1655(9) _cell_angle_alpha 90.00 _cell_angle_beta 94.3513(9) _cell_angle_gamma 90.00 _cell_volume 4020.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 50848 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 24.11 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.104 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 1.270 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.835 _exptl_absorpt_correction_T_max 1.004 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 22881 _diffrn_reflns_av_R_equivalents 0.1516 _diffrn_reflns_av_sigmaI/netI 0.1423 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 22.50 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.993 _reflns_number_total 5229 _reflns_number_gt 2461 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.1135P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5229 _refine_ls_number_parameters 339 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1585 _refine_ls_R_factor_gt 0.0773 _refine_ls_wR_factor_ref 0.2162 _refine_ls_wR_factor_gt 0.1838 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.919 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.539 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.086 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 0.000 475 105 ' ' 2 0.000 0.500 0.500 475 104 ' ' _platon_squeeze_details ; ; 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 0.24146(10) 0.47931(7) 0.05754(5) 0.0624(4) Uani 1 1 d . . . Zn2 Zn 0.03651(10) 0.60593(8) 0.00440(5) 0.0717(5) Uani 1 1 d . . . P1 P 0.4864(3) 0.97958(17) 0.22643(12) 0.0672(8) Uani 1 1 d . . . O2 O 0.2934(6) 0.5893(4) 0.0975(3) 0.076(2) Uani 1 1 d . . . O7 O 0.0728(5) 0.4833(4) 0.0462(3) 0.0645(17) Uani 1 1 d . . . H7A H 0.0405 0.4875 0.0834 0.077 Uiso 1 1 calc R . . O4 O 0.3088(6) 1.0098(4) 0.4853(3) 0.0720(19) Uani 1 1 d . . . O6 O 0.2115(11) 1.3841(6) 0.1547(4) 0.147(4) Uani 1 1 d . A . O1 O 0.1580(7) 0.6862(4) 0.0569(3) 0.086(2) Uani 1 1 d . . . O5 O 0.3174(7) 1.3684(5) 0.0860(4) 0.086(3) Uani 1 1 d . . . O3 O 0.1645(7) 0.9169(5) 0.4487(3) 0.078(2) Uani 1 1 d . . . C1 C 0.4103(9) 0.8933(7) 0.1825(4) 0.066(3) Uani 1 1 d . A . C2 C 0.3152(11) 0.9073(8) 0.1436(5) 0.099(4) Uani 1 1 d . . . H2 H 0.2854 0.9678 0.1375 0.119 Uiso 1 1 calc R A . C3 C 0.2632(11) 0.8334(8) 0.1137(5) 0.101(4) Uani 1 1 d . A . H3 H 0.1982 0.8443 0.0878 0.121 Uiso 1 1 calc R . . C4 C 0.3041(9) 0.7483(6) 0.1212(4) 0.062(3) Uani 1 1 d . . . C5 C 0.3976(10) 0.7335(7) 0.1592(5) 0.094(4) Uani 1 1 d . A . H5 H 0.4263 0.6725 0.1647 0.112 Uiso 1 1 calc R . . C6 C 0.4497(10) 0.8024(7) 0.1887(5) 0.097(4) Uani 1 1 d . . . H6 H 0.5146 0.7892 0.2142 0.116 Uiso 1 1 calc R A . C7 C 0.2461(10) 0.6684(7) 0.0889(4) 0.068(3) Uani 1 1 d . A . C8 C 0.4174(9) 0.9650(6) 0.2907(4) 0.055(2) Uani 1 1 d . A . C9 C 0.3035(10) 0.9311(7) 0.2944(5) 0.077(3) Uani 1 1 d . . . H9 H 0.2608 0.9079 0.2621 0.092 Uiso 1 1 calc R A . C10 C 0.2542(9) 0.9314(7) 0.3440(5) 0.072(3) Uani 1 1 d . A . H10 H 0.1764 0.9096 0.3450 0.087 Uiso 1 1 calc R . . C11 C 0.3132(8) 0.9624(5) 0.3938(4) 0.053(3) Uani 1 1 d . . . C12 C 0.4255(10) 0.9910(6) 0.3906(4) 0.061(3) Uani 1 1 d . A . H12 H 0.4687 1.0106 0.4236 0.074 Uiso 1 1 calc R . . C13 C 0.4792(9) 0.9925(6) 0.3408(4) 0.061(3) Uani 1 1 d . . . H13 H 0.5581 1.0121 0.3405 0.073 Uiso 1 1 calc R A . C14 C 0.2570(11) 0.9604(6) 0.4452(4) 0.060(3) Uani 1 1 d . A . C15 C 0.4180(8) 1.0887(6) 0.2001(4) 0.060(3) Uiso 0.501(19) 1 d P A 1 C15' C 0.4180(8) 1.0887(6) 0.2001(4) 0.060(3) Uiso 0.499(19) 1 d P A 2 C16 C 0.307(3) 1.1228(18) 0.2108(12) 0.092(9) Uiso 0.501(19) 1 d P A 1 H16 H 0.2626 1.0862 0.2342 0.111 Uiso 0.501(19) 1 calc PR A 1 C16' C 0.3550(18) 1.1377(12) 0.2288(9) 0.048(6) Uiso 0.499(19) 1 d P A 2 H16' H 0.3380 1.1183 0.2649 0.058 Uiso 0.499(19) 1 calc PR A 2 C17 C 0.257(2) 1.1998(15) 0.1918(10) 0.076(7) Uiso 0.501(19) 1 d P A 1 H17 H 0.1812 1.2190 0.2000 0.091 Uiso 0.501(19) 1 calc PR A 1 C17' C 0.3085(19) 1.2246(13) 0.2063(9) 0.056(6) Uiso 0.499(19) 1 d P A 2 H17' H 0.2607 1.2615 0.2278 0.067 Uiso 0.499(19) 1 calc PR A 2 C18 C 0.3322(9) 1.2528(6) 0.1563(4) 0.064(3) Uiso 0.501(19) 1 d P A 1 C18' C 0.3322(9) 1.2528(6) 0.1563(4) 0.064(3) Uiso 0.499(19) 1 d P A 2 C19 C 0.4310(16) 1.2277(12) 0.1441(8) 0.050(6) Uiso 0.501(19) 1 d P A 1 H19' H 0.4726 1.2630 0.1190 0.060 Uiso 0.501(19) 1 calc PR A 1 C19' C 0.393(2) 1.1886(17) 0.1207(12) 0.087(8) Uiso 0.499(19) 1 d P A 2 H19 H 0.4020 1.2039 0.0830 0.104 Uiso 0.499(19) 1 calc PR A 2 C20 C 0.4809(18) 1.1461(13) 0.1680(8) 0.057(6) Uiso 0.501(19) 1 d P A 1 H20 H 0.5592 1.1308 0.1618 0.068 Uiso 0.501(19) 1 calc PR A 1 C20' C 0.439(2) 1.1043(16) 0.1428(11) 0.081(8) Uiso 0.499(19) 1 d P A 2 H20' H 0.4800 1.0617 0.1216 0.097 Uiso 0.499(19) 1 calc PR A 2 C21 C 0.2840(10) 1.3409(7) 0.1290(6) 0.074(3) Uani 1 1 d . . . C100 C 0.350(2) 0.7154(15) 0.4670(11) 0.116(9) Uiso 0.50 1 d PD . . H10D H 0.3192 0.7757 0.4611 0.139 Uiso 0.50 1 calc PR . . C101 C 0.492(2) 0.6294(16) 0.5152(13) 0.153(12) Uiso 0.50 1 d PD . . H10E H 0.4448 0.5787 0.4989 0.230 Uiso 0.50 1 calc PR . . H10F H 0.4877 0.6296 0.5555 0.230 Uiso 0.50 1 calc PR . . H10G H 0.5735 0.6214 0.5066 0.230 Uiso 0.50 1 calc PR . . C102 C 0.5060(19) 0.7895(13) 0.5126(10) 0.096(7) Uiso 0.50 1 d PD . . H10A H 0.4679 0.8441 0.4956 0.144 Uiso 0.50 1 calc PR . . H10B H 0.5874 0.7872 0.5032 0.144 Uiso 0.50 1 calc PR . . H10C H 0.5034 0.7925 0.5530 0.144 Uiso 0.50 1 calc PR . . C110 C 0.092(2) 0.5784(19) 0.1949(12) 0.134(11) Uiso 0.50 1 d PD . . H11B H 0.1500 0.5323 0.2003 0.160 Uiso 0.50 1 calc PR . . C111 C 0.054(5) 0.728(3) 0.218(3) 0.39(4) Uiso 0.50 1 d PD . . H11F H -0.0137 0.7192 0.1918 0.578 Uiso 0.50 1 calc PR . . H11G H 0.1091 0.7706 0.2027 0.578 Uiso 0.50 1 calc PR . . H11H H 0.0287 0.7537 0.2530 0.578 Uiso 0.50 1 calc PR . . C112 C 0.213(2) 0.653(2) 0.2629(13) 0.147(11) Uiso 0.50 1 d PD . . H11C H 0.2578 0.5959 0.2627 0.221 Uiso 0.50 1 calc PR . . H11D H 0.1941 0.6671 0.3009 0.221 Uiso 0.50 1 calc PR . . H11E H 0.2584 0.7036 0.2487 0.221 Uiso 0.50 1 calc PR . . N100 N 0.4497(16) 0.7131(11) 0.4931(8) 0.095(6) Uiso 0.50 1 d PD . . N110 N 0.109(2) 0.6428(18) 0.2294(12) 0.177(11) Uiso 0.50 1 d PD . . O110 O 0.0171(19) 0.5565(14) 0.1543(10) 0.155(8) Uiso 0.50 1 d PD . . O100 O 0.279(2) 0.649(2) 0.4464(13) 0.228(12) Uiso 0.50 1 d PD . . N2 N 0.0028(8) 0.7261(6) -0.0446(4) 0.092(3) Uani 1 1 d D . . N1 N -0.0944(7) 0.6487(6) 0.0572(5) 0.098(3) Uani 1 1 d D . . C23 C -0.091(2) 0.7737(16) -0.0228(10) 0.225(10) Uiso 1 1 d D . . H23A H -0.1624 0.7645 -0.0476 0.270 Uiso 1 1 calc R . . H23B H -0.0731 0.8405 -0.0217 0.270 Uiso 1 1 calc R . . C22 C -0.113(3) 0.7404(17) 0.0362(12) 0.300(14) Uiso 1 1 d D . . H22A H -0.0654 0.7810 0.0620 0.360 Uiso 1 1 calc R . . H22B H -0.1953 0.7551 0.0413 0.360 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 0.0608(8) 0.0645(7) 0.0593(8) 0.0074(6) -0.0116(6) 0.0057(6) Zn2 0.0621(8) 0.0729(8) 0.0768(10) -0.0074(6) -0.0152(7) 0.0132(6) P1 0.081(2) 0.0590(16) 0.0597(19) 0.0026(14) -0.0102(15) 0.0016(14) O2 0.088(5) 0.052(4) 0.083(5) 0.001(3) -0.029(4) 0.003(4) O7 0.054(4) 0.079(4) 0.060(4) 0.000(3) -0.001(3) 0.009(3) O4 0.076(5) 0.082(5) 0.059(5) -0.018(4) 0.012(4) -0.008(4) O6 0.228(12) 0.109(7) 0.110(8) 0.048(6) 0.053(8) 0.082(8) O1 0.091(6) 0.072(5) 0.088(6) -0.008(4) -0.037(5) 0.018(4) O5 0.085(6) 0.092(6) 0.080(6) 0.047(5) -0.003(5) 0.010(4) O3 0.074(5) 0.076(5) 0.082(6) -0.010(4) 0.008(4) -0.022(4) C1 0.072(7) 0.072(7) 0.052(7) -0.004(5) -0.005(6) 0.009(5) C2 0.114(10) 0.085(8) 0.092(10) -0.016(7) -0.045(8) 0.041(7) C3 0.111(10) 0.095(9) 0.088(9) -0.025(7) -0.048(8) 0.033(8) C4 0.079(7) 0.049(6) 0.054(7) -0.005(5) -0.011(6) 0.012(5) C5 0.110(10) 0.035(6) 0.128(11) 0.013(6) -0.041(9) 0.008(6) C6 0.105(10) 0.056(7) 0.121(11) -0.003(7) -0.045(8) 0.009(7) C7 0.095(9) 0.052(7) 0.057(7) -0.002(5) 0.006(6) 0.010(6) C8 0.073(7) 0.050(6) 0.041(6) 0.004(4) -0.003(5) -0.004(5) C9 0.090(9) 0.087(7) 0.049(8) -0.011(6) -0.019(7) -0.024(7) C10 0.052(7) 0.098(8) 0.067(8) -0.017(6) 0.000(6) -0.027(6) C11 0.049(6) 0.048(6) 0.062(8) -0.003(5) -0.007(6) -0.017(5) C12 0.078(8) 0.064(6) 0.040(7) -0.002(5) -0.011(6) 0.014(5) C13 0.056(6) 0.061(6) 0.062(8) 0.004(5) -0.023(6) 0.001(5) C14 0.081(8) 0.055(6) 0.044(7) -0.001(5) -0.004(6) 0.018(6) C21 0.065(8) 0.049(7) 0.102(11) -0.010(7) -0.023(8) 0.006(6) N2 0.085(7) 0.069(6) 0.115(8) -0.003(5) -0.030(6) 0.032(5) N1 0.072(6) 0.076(6) 0.145(10) -0.032(6) 0.004(6) 0.020(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 O5 1.933(7) 1_545 ? Zn1 O2 1.937(6) . ? Zn1 O7 1.937(6) . ? Zn1 O4 1.970(7) 4_575 ? Zn2 O7 2.075(6) . ? Zn2 O3 2.094(8) 4_575 ? Zn2 O7 2.126(6) 3_565 ? Zn2 N2 2.128(8) . ? Zn2 N1 2.138(9) . ? Zn2 O1 2.156(7) . ? P1 C8 1.810(10) . ? P1 C1 1.822(10) . ? P1 C15 1.859(9) . ? O2 C7 1.282(10) . ? O7 Zn2 2.126(6) 3_565 ? O7 H7A 1.0000 . ? O4 C14 1.311(11) . ? O4 Zn1 1.970(7) 4_576 ? O6 C21 1.244(13) . ? O1 C7 1.253(12) . ? O5 C21 1.205(14) . ? O5 Zn1 1.933(7) 1_565 ? O3 C14 1.244(12) . ? O3 Zn2 2.094(8) 4_576 ? C1 C6 1.399(13) . ? C1 C2 1.401(13) . ? C2 C3 1.402(14) . ? C2 H2 0.9500 . ? C3 C4 1.329(13) . ? C3 H3 0.9500 . ? C4 C5 1.377(13) . ? C4 C7 1.523(13) . ? C5 C6 1.343(14) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C8 C9 1.407(13) . ? C8 C13 1.413(12) . ? C9 C10 1.364(13) . ? C9 H9 0.9500 . ? C10 C11 1.411(13) . ? C10 H10 0.9500 . ? C11 C12 1.363(13) . ? C11 C14 1.444(13) . ? C12 C13 1.394(13) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C15 C20 1.38(2) . ? C15 C16 1.41(3) . ? C16 C17 1.32(3) . ? C16 H16 0.9500 . ? C16' C17' 1.46(2) . ? C16' H16' 0.9500 . ? C17 C18 1.48(3) . ? C17 H17 0.9500 . ? C17' H17' 0.9500 . ? C18 C19 1.249(18) . ? C18 C21 1.523(14) . ? C19 C20 1.42(2) . ? C19 H19' 0.9500 . ? C19' C20' 1.42(3) . ? C19' H19 0.9500 . ? C20 H20 0.9500 . ? C20' H20' 0.9500 . ? C100 N100 1.27(2) . ? C100 O100 1.33(2) . ? C100 H10D 0.9500 . ? C101 N100 1.40(2) . ? C101 H10E 0.9800 . ? C101 H10F 0.9800 . ? C101 H10G 0.9800 . ? C102 N100 1.350(19) . ? C102 H10A 0.9800 . ? C102 H10B 0.9800 . ? C102 H10C 0.9800 . ? C110 N110 1.26(3) . ? C110 O110 1.29(2) . ? C110 H11B 0.9500 . ? C111 N110 1.41(2) . ? C111 H11F 0.9800 . ? C111 H11G 0.9800 . ? C111 H11H 0.9800 . ? C112 N110 1.39(2) . ? C112 H11C 0.9800 . ? C112 H11D 0.9800 . ? C112 H11E 0.9800 . ? N2 C23 1.413(18) . ? N1 C22 1.43(2) . ? C23 C22 1.545(17) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn1 O2 113.3(3) 1_545 . ? O5 Zn1 O7 119.7(3) 1_545 . ? O2 Zn1 O7 108.2(3) . . ? O5 Zn1 O4 100.6(3) 1_545 4_575 ? O2 Zn1 O4 104.4(3) . 4_575 ? O7 Zn1 O4 109.2(3) . 4_575 ? O7 Zn2 O3 93.0(3) . 4_575 ? O7 Zn2 O7 81.1(2) . 3_565 ? O3 Zn2 O7 87.0(3) 4_575 3_565 ? O7 Zn2 N2 175.3(3) . . ? O3 Zn2 N2 83.1(3) 4_575 . ? O7 Zn2 N2 96.0(3) 3_565 . ? O7 Zn2 N1 94.8(3) . . ? O3 Zn2 N1 172.0(3) 4_575 . ? O7 Zn2 N1 96.2(3) 3_565 . ? N2 Zn2 N1 89.3(4) . . ? O7 Zn2 O1 94.6(2) . . ? O3 Zn2 O1 90.5(3) 4_575 . ? O7 Zn2 O1 174.9(2) 3_565 . ? N2 Zn2 O1 88.1(3) . . ? N1 Zn2 O1 86.9(3) . . ? C8 P1 C1 101.4(5) . . ? C8 P1 C15 101.1(4) . . ? C1 P1 C15 102.4(5) . . ? C7 O2 Zn1 123.2(6) . . ? Zn1 O7 Zn2 104.9(3) . . ? Zn1 O7 Zn2 127.2(3) . 3_565 ? Zn2 O7 Zn2 98.9(2) . 3_565 ? Zn1 O7 H7A 108.1 . . ? Zn2 O7 H7A 108.1 . . ? Zn2 O7 H7A 108.1 3_565 . ? C14 O4 Zn1 120.7(7) . 4_576 ? C7 O1 Zn2 135.1(6) . . ? C21 O5 Zn1 114.7(8) . 1_565 ? C14 O3 Zn2 140.2(7) . 4_576 ? C6 C1 C2 116.0(10) . . ? C6 C1 P1 116.7(8) . . ? C2 C1 P1 127.3(8) . . ? C1 C2 C3 121.0(10) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C4 C3 C2 120.6(10) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.1(9) . . ? C3 C4 C7 120.2(9) . . ? C5 C4 C7 120.7(9) . . ? C6 C5 C4 122.1(9) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C1 121.2(10) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? O1 C7 O2 126.7(9) . . ? O1 C7 C4 117.4(9) . . ? O2 C7 C4 115.9(10) . . ? C9 C8 C13 117.0(9) . . ? C9 C8 P1 124.4(8) . . ? C13 C8 P1 118.6(8) . . ? C10 C9 C8 120.2(9) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 123.2(10) . . ? C9 C10 H10 118.4 . . ? C11 C10 H10 118.4 . . ? C12 C11 C10 116.4(10) . . ? C12 C11 C14 122.8(9) . . ? C10 C11 C14 120.8(9) . . ? C11 C12 C13 122.5(9) . . ? C11 C12 H12 118.8 . . ? C13 C12 H12 118.8 . . ? C12 C13 C8 120.5(9) . . ? C12 C13 H13 119.7 . . ? C8 C13 H13 119.7 . . ? O3 C14 O4 124.8(10) . . ? O3 C14 C11 120.6(9) . . ? O4 C14 C11 114.6(10) . . ? C20 C15 C16 114.2(15) . . ? C20 C15 P1 118.8(10) . . ? C16 C15 P1 126.9(13) . . ? C17 C16 C15 127(2) . . ? C17 C16 H16 116.4 . . ? C15 C16 H16 116.4 . . ? C17' C16' H16' 120.3 . . ? C16 C17 C18 113(2) . . ? C16 C17 H17 123.7 . . ? C18 C17 H17 123.7 . . ? C16' C17' H17' 119.6 . . ? C19 C18 C17 124.5(15) . . ? C19 C18 C21 116.8(13) . . ? C17 C18 C21 118.6(13) . . ? C18 C19 C20 119.6(17) . . ? C18 C19 H19' 120.2 . . ? C20 C19 H19' 120.2 . . ? C20' C19' H19 120.0 . . ? C15 C20 C19 121.4(16) . . ? C15 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C19' C20' H20' 122.8 . . ? O5 C21 O6 122.2(11) . . ? O5 C21 C18 121.4(12) . . ? O6 C21 C18 116.3(13) . . ? N100 C100 O100 132(2) . . ? N100 C100 H10D 114.0 . . ? O100 C100 H10D 114.0 . . ? N100 C101 H10E 109.5 . . ? N100 C101 H10F 109.5 . . ? H10E C101 H10F 109.5 . . ? N100 C101 H10G 109.5 . . ? H10E C101 H10G 109.5 . . ? H10F C101 H10G 109.5 . . ? N100 C102 H10A 109.5 . . ? N100 C102 H10B 109.5 . . ? H10A C102 H10B 109.5 . . ? N100 C102 H10C 109.5 . . ? H10A C102 H10C 109.5 . . ? H10B C102 H10C 109.5 . . ? N110 C110 O110 139(3) . . ? N110 C110 H11B 110.7 . . ? O110 C110 H11B 110.7 . . ? N110 C111 H11F 109.5 . . ? N110 C111 H11G 109.5 . . ? H11F C111 H11G 109.5 . . ? N110 C111 H11H 109.5 . . ? H11F C111 H11H 109.5 . . ? H11G C111 H11H 109.5 . . ? N110 C112 H11C 109.5 . . ? N110 C112 H11D 109.5 . . ? H11C C112 H11D 109.5 . . ? N110 C112 H11E 109.5 . . ? H11C C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? C100 N100 C102 122.9(16) . . ? C100 N100 C101 119.2(15) . . ? C102 N100 C101 115.9(16) . . ? C110 N110 C112 124(2) . . ? C110 N110 C111 119(2) . . ? C112 N110 C111 112(2) . . ? C23 N2 Zn2 107.7(12) . . ? C22 N1 Zn2 98.6(13) . . ? N2 C23 C22 112(2) . . ? N2 C23 H23A 109.2 . . ? C22 C23 H23A 109.2 . . ? N2 C23 H23B 109.2 . . ? C22 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? N1 C22 C23 126(2) . . ? N1 C22 H22A 105.8 . . ? C23 C22 H22A 105.8 . . ? N1 C22 H22B 105.8 . . ? C23 C22 H22B 105.8 . . ? H22A C22 H22B 106.2 . . ? #===END data_sh0702b _database_code_depnum_ccdc_archive 'CCDC 708775' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H33 N O14 P2 Zn2, C3 H7 N O, 2(H2 O)' _chemical_formula_sum 'C50 H44 N2 O17 P2 Zn2' _chemical_formula_weight 1137.55 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' 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 14.5705(2) _cell_length_b 25.2421(4) _cell_length_c 16.0875(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.1402(6) _cell_angle_gamma 90.00 _cell_volume 5654.03(14) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 36093 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 25.03 _exptl_crystal_description Shard _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 0.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.804 _exptl_absorpt_correction_T_max 0.891 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 36187 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9918 _reflns_number_gt 6483 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0980P)^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 9918 _refine_ls_number_parameters 668 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1690 _refine_ls_wR_factor_gt 0.1555 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.041 _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 -0.22370(4) 0.28185(2) 1.30396(3) 0.05246(19) Uani 1 1 d . . . Zn2 Zn 0.15199(3) 0.02243(2) 0.67243(3) 0.04536(18) Uani 1 1 d . . . P2 P 0.18690(8) 0.23442(5) 1.81270(7) 0.0404(3) Uani 1 1 d . . . P1 P -0.25061(8) 0.00994(5) 0.97555(7) 0.0437(3) Uani 1 1 d . . . C1 C -0.2356(3) 0.07234(17) 1.0329(3) 0.0413(10) Uani 1 1 d . . . C1P C -0.2385(3) -0.04333(18) 1.0501(3) 0.0526(11) Uani 1 1 d . . . H1PA H -0.2854 -0.0392 1.0826 0.079 Uiso 1 1 calc R . . H1PB H -0.1734 -0.0433 1.0907 0.079 Uiso 1 1 calc R . . H1PC H -0.2500 -0.0769 1.0181 0.079 Uiso 1 1 calc R . . C2 C -0.1969(3) 0.07357(19) 1.1223(3) 0.0543(12) Uani 1 1 d . . . H2A H -0.1746 0.0419 1.1537 0.065 Uiso 1 1 calc R . . C2P C 0.1504(3) 0.17075(17) 1.8393(3) 0.0504(11) Uani 1 1 d . . . H2PA H 0.0828 0.1721 1.8382 0.076 Uiso 1 1 calc R . . H2PB H 0.1901 0.1605 1.8976 0.076 Uiso 1 1 calc R . . H2PC H 0.1583 0.1447 1.7968 0.076 Uiso 1 1 calc R . . C3 C -0.1910(3) 0.1215(2) 1.1655(3) 0.0597(13) Uani 1 1 d . . . H3A H -0.1623 0.1228 1.2267 0.072 Uiso 1 1 calc R . . C4 C -0.2261(3) 0.16737(19) 1.1211(3) 0.0497(11) Uani 1 1 d . . . C5 C -0.2626(3) 0.1649(2) 1.0316(3) 0.0559(12) Uani 1 1 d . . . H5A H -0.2848 0.1966 1.0002 0.067 Uiso 1 1 calc R . . C6 C -0.2678(3) 0.11871(19) 0.9872(3) 0.0521(11) Uani 1 1 d . . . H6A H -0.2932 0.1181 0.9256 0.063 Uiso 1 1 calc R . . C7 C -0.2310(4) 0.2184(2) 1.1689(4) 0.0624(14) Uani 1 1 d . . . C8 C -0.1677(3) 0.00369(18) 0.9126(3) 0.0463(11) Uani 1 1 d . . . C9 C -0.1800(4) -0.0364(2) 0.8525(4) 0.0774(17) Uani 1 1 d . . . H9A H -0.2262 -0.0632 0.8508 0.093 Uiso 1 1 calc R . . C10 C -0.1267(4) -0.0385(2) 0.7949(4) 0.0780(18) Uani 1 1 d . . . H10A H -0.1373 -0.0659 0.7526 0.094 Uiso 1 1 calc R . . C11 C -0.0567(3) 0.00028(18) 0.7993(3) 0.0482(11) Uani 1 1 d . . . C12 C -0.0424(3) 0.03869(17) 0.8616(3) 0.0443(10) Uani 1 1 d . . . H12A H 0.0065 0.0643 0.8659 0.053 Uiso 1 1 calc R . . C13 C -0.0968(3) 0.04131(19) 0.9185(3) 0.0485(11) Uani 1 1 d . . . H13A H -0.0859 0.0685 0.9612 0.058 Uiso 1 1 calc R . . C14 C -0.0054(3) 0.0019(2) 0.7315(3) 0.0515(11) Uani 1 1 d . . . C15 C -0.3682(3) 0.00910(18) 0.8977(3) 0.0448(11) Uani 1 1 d . . . C16 C -0.4456(3) -0.0119(2) 0.9192(3) 0.0562(12) Uani 1 1 d . . . H16A H -0.4364 -0.0294 0.9733 0.067 Uiso 1 1 calc R . . C17 C -0.5365(3) -0.0072(2) 0.8615(3) 0.0617(14) Uani 1 1 d . . . H17A H -0.5899 -0.0207 0.8772 0.074 Uiso 1 1 calc R . . C18 C -0.5512(3) 0.0164(2) 0.7822(3) 0.0604(13) Uani 1 1 d . . . C19 C -0.4730(4) 0.0353(3) 0.7595(3) 0.0780(17) Uani 1 1 d . . . H19A H -0.4821 0.0506 0.7038 0.094 Uiso 1 1 calc R . . C20 C -0.3830(3) 0.0321(2) 0.8162(3) 0.0690(15) Uani 1 1 d . . . H20A H -0.3300 0.0457 0.8000 0.083 Uiso 1 1 calc R . . C21 C -0.6517(4) 0.0219(3) 0.7210(4) 0.0778(18) Uani 1 1 d . . . C22 C 0.1136(3) 0.25662(17) 1.7074(2) 0.0406(10) Uani 1 1 d . . . C23 C 0.0202(3) 0.23839(19) 1.6752(3) 0.0501(11) Uani 1 1 d . . . H23A H -0.0054 0.2145 1.7083 0.060 Uiso 1 1 calc R . . C24 C -0.0352(3) 0.25523(19) 1.5946(3) 0.0511(11) Uani 1 1 d . . . H24A H -0.0994 0.2428 1.5724 0.061 Uiso 1 1 calc R . . C25 C 0.0006(3) 0.28983(17) 1.5454(3) 0.0426(10) Uani 1 1 d . . . C26 C 0.0923(3) 0.30976(17) 1.5800(3) 0.0458(10) Uani 1 1 d . . . H26A H 0.1165 0.3355 1.5488 0.055 Uiso 1 1 calc R . . C27 C 0.1488(3) 0.29209(18) 1.6602(3) 0.0494(11) Uani 1 1 d . . . H27A H 0.2128 0.3047 1.6827 0.059 Uiso 1 1 calc R . . C28 C -0.0592(3) 0.30580(17) 1.4541(3) 0.0393(10) Uani 1 1 d . . . C29 C 0.3113(3) 0.23142(17) 1.8159(3) 0.0430(10) Uani 1 1 d . . . C30 C 0.3491(3) 0.1854(2) 1.7912(3) 0.0553(12) Uani 1 1 d . . . H30A H 0.3094 0.1552 1.7730 0.066 Uiso 1 1 calc R . . C31 C 0.4444(3) 0.1837(2) 1.7931(3) 0.0621(13) Uani 1 1 d . . . H31A H 0.4699 0.1522 1.7764 0.074 Uiso 1 1 calc R . . C32 C 0.5029(3) 0.2273(2) 1.8191(3) 0.0594(13) Uani 1 1 d . . . C33 C 0.4660(4) 0.2719(2) 1.8432(4) 0.0694(15) Uani 1 1 d . . . H33A H 0.5063 0.3018 1.8615 0.083 Uiso 1 1 calc R . . C34 C 0.3702(3) 0.2749(2) 1.8418(3) 0.0595(13) Uani 1 1 d . . . H34A H 0.3455 0.3067 1.8585 0.071 Uiso 1 1 calc R . . C35 C 0.6080(4) 0.2262(3) 1.8201(4) 0.0730(17) Uani 1 1 d . . . C36 C 0.1729(3) 0.28116(17) 1.8919(3) 0.0436(10) Uani 1 1 d . . . C37 C 0.2175(4) 0.27221(19) 1.9782(3) 0.0566(12) Uani 1 1 d . . . H37A H 0.2553 0.2412 1.9954 0.068 Uiso 1 1 calc R . . C38 C 0.2081(3) 0.30792(19) 2.0408(3) 0.0562(12) Uani 1 1 d . . . H38A H 0.2399 0.3014 2.1006 0.067 Uiso 1 1 calc R . . C39 C 0.1528(3) 0.35267(17) 2.0166(3) 0.0457(10) Uani 1 1 d . . . C40 C 0.1077(3) 0.36195(19) 1.9296(3) 0.0586(13) Uani 1 1 d . . . H40A H 0.0702 0.3931 1.9126 0.070 Uiso 1 1 calc R . . C41 C 0.1164(3) 0.32669(19) 1.8672(3) 0.0561(12) Uani 1 1 d . . . H41A H 0.0842 0.3332 1.8076 0.067 Uiso 1 1 calc R . . C42 C 0.1469(3) 0.3920(2) 2.0859(3) 0.0473(11) Uani 1 1 d . . . O1 O -0.2766(4) 0.25581(19) 1.1293(3) 0.1088(15) Uani 1 1 d . . . O2 O -0.1883(3) 0.21927(15) 1.2480(3) 0.0804(11) Uani 1 1 d . . . O3 O -0.0440(3) -0.01679(17) 0.6575(3) 0.0852(12) Uani 1 1 d . . . O4 O 0.0743(2) 0.02602(11) 0.75251(18) 0.0458(7) Uani 1 1 d . . . O5 O -0.6617(3) 0.0283(3) 0.6432(3) 0.176(3) Uani 1 1 d . . . O6 O -0.7176(2) 0.01943(13) 0.7547(2) 0.0602(9) Uani 1 1 d . . . O7 O -0.1358(2) 0.27972(13) 1.42390(18) 0.0522(8) Uani 1 1 d . . . O8 O -0.0287(2) 0.34101(13) 1.4172(2) 0.0599(9) Uani 1 1 d . . . O9 O 0.6585(3) 0.2649(2) 1.8466(4) 0.1170(18) Uani 1 1 d . . . O10 O 0.6395(3) 0.1865(2) 1.7942(3) 0.0878(13) Uani 1 1 d . . . O11 O 0.1722(2) 0.37796(13) 2.1624(2) 0.0607(9) Uani 1 1 d . . . O12 O 0.1174(2) 0.43824(13) 2.06070(18) 0.0526(8) Uani 1 1 d . . . O13 O -0.1622(2) 0.34540(14) 1.2646(2) 0.0714(10) Uani 1 1 d . . . N100 N 0.1311(3) -0.10727(17) 0.5153(3) 0.0641(11) Uani 1 1 d . . . O100 O 0.1487(3) -0.05164(14) 0.6271(2) 0.0668(9) Uani 1 1 d . . . C102 C 0.1825(7) -0.1487(3) 0.5702(5) 0.128(3) Uani 1 1 d . . . H10B H 0.2023 -0.1366 0.6308 0.191 Uiso 1 1 calc R . . H10C H 0.2395 -0.1580 0.5528 0.191 Uiso 1 1 calc R . . H10D H 0.1410 -0.1798 0.5646 0.191 Uiso 1 1 calc R . . C101 C 0.0929(5) -0.1174(3) 0.4233(4) 0.0853(17) Uani 1 1 d . . . H10E H 0.0640 -0.0849 0.3935 0.128 Uiso 1 1 calc R . . H10F H 0.0439 -0.1452 0.4135 0.128 Uiso 1 1 calc R . . H10G H 0.1448 -0.1290 0.4003 0.128 Uiso 1 1 calc R . . C100 C 0.1188(3) -0.0617(2) 0.5491(3) 0.0556(12) Uani 1 1 d . . . H100 H 0.0847 -0.0348 0.5111 0.083 Uiso 1 1 calc R . . O110 O 0.3100(3) 0.35051(18) 0.5615(3) 0.1037(15) Uani 1 1 d D . . N110 N 0.4722(3) 0.3478(2) 0.6149(4) 0.1003(17) Uani 1 1 d D . . C110 C 0.3844(4) 0.3551(3) 0.6212(5) 0.097(2) Uani 1 1 d D . . H11A H 0.3788 0.3647 0.6766 0.116 Uiso 1 1 calc R . . C112 C 0.5586(4) 0.3548(3) 0.6884(5) 0.113(2) Uani 1 1 d D . . H11B H 0.5402 0.3609 0.7415 0.169 Uiso 1 1 calc R . . H11C H 0.5950 0.3853 0.6775 0.169 Uiso 1 1 calc R . . H11D H 0.5984 0.3229 0.6954 0.169 Uiso 1 1 calc R . . C111 C 0.4848(6) 0.3345(6) 0.5322(7) 0.245(8) Uani 1 1 d D . . H11E H 0.4217 0.3310 0.4888 0.368 Uiso 1 1 calc R . . H11F H 0.5195 0.3008 0.5370 0.368 Uiso 1 1 calc R . . H11G H 0.5216 0.3625 0.5144 0.368 Uiso 1 1 calc R . . O200 O 0.2420(4) 0.4890(2) 0.9424(3) 0.1210(17) Uani 1 1 d . . . O201 O 0.2755(4) 0.57646(19) 0.8315(3) 0.1140(16) 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 0.0501(3) 0.0594(4) 0.0433(3) -0.0012(3) 0.0068(2) -0.0061(3) Zn2 0.0465(3) 0.0534(4) 0.0371(3) 0.0074(2) 0.0137(2) 0.0016(2) P2 0.0479(6) 0.0400(7) 0.0331(6) -0.0019(5) 0.0115(5) 0.0005(5) P1 0.0391(6) 0.0453(7) 0.0479(7) 0.0029(5) 0.0145(5) 0.0006(5) C1 0.038(2) 0.048(3) 0.040(2) 0.002(2) 0.0149(19) 0.0019(19) C1P 0.050(3) 0.047(3) 0.056(3) 0.011(2) 0.007(2) 0.002(2) C2 0.065(3) 0.051(3) 0.043(3) 0.008(2) 0.009(2) 0.004(2) C2P 0.064(3) 0.042(3) 0.051(3) 0.004(2) 0.025(2) 0.002(2) C3 0.073(3) 0.068(4) 0.037(3) -0.007(3) 0.015(2) -0.006(3) C4 0.050(2) 0.053(3) 0.052(3) -0.004(2) 0.023(2) -0.001(2) C5 0.064(3) 0.056(3) 0.047(3) 0.005(2) 0.015(2) 0.007(2) C6 0.063(3) 0.050(3) 0.042(3) -0.003(2) 0.013(2) 0.005(2) C7 0.069(3) 0.067(4) 0.059(4) -0.014(3) 0.030(3) -0.017(3) C8 0.045(2) 0.040(3) 0.057(3) -0.005(2) 0.019(2) 0.000(2) C9 0.079(4) 0.053(3) 0.121(5) -0.019(3) 0.062(4) -0.026(3) C10 0.075(4) 0.061(4) 0.119(5) -0.036(3) 0.060(4) -0.020(3) C11 0.040(2) 0.047(3) 0.062(3) -0.003(2) 0.021(2) 0.002(2) C12 0.041(2) 0.044(3) 0.049(3) -0.003(2) 0.014(2) -0.0080(19) C13 0.044(2) 0.050(3) 0.052(3) -0.005(2) 0.014(2) -0.001(2) C14 0.050(3) 0.054(3) 0.050(3) -0.006(2) 0.014(2) -0.001(2) C15 0.037(2) 0.052(3) 0.048(3) -0.001(2) 0.016(2) 0.003(2) C16 0.055(3) 0.064(3) 0.050(3) 0.007(2) 0.016(2) 0.004(2) C17 0.041(3) 0.085(4) 0.062(3) 0.009(3) 0.020(2) 0.001(2) C18 0.042(3) 0.089(4) 0.048(3) 0.003(3) 0.009(2) 0.004(2) C19 0.057(3) 0.128(5) 0.052(3) 0.022(3) 0.021(3) 0.005(3) C20 0.049(3) 0.106(5) 0.055(3) 0.012(3) 0.019(2) -0.004(3) C21 0.047(3) 0.127(6) 0.058(4) 0.015(3) 0.013(3) 0.003(3) C22 0.044(2) 0.043(3) 0.035(2) -0.0028(19) 0.0109(19) 0.0010(19) C23 0.051(3) 0.059(3) 0.042(3) 0.000(2) 0.017(2) -0.008(2) C24 0.038(2) 0.065(3) 0.048(3) -0.004(2) 0.010(2) -0.008(2) C25 0.042(2) 0.044(3) 0.042(2) -0.001(2) 0.013(2) 0.008(2) C26 0.041(2) 0.046(3) 0.047(3) 0.009(2) 0.009(2) -0.003(2) C27 0.042(2) 0.055(3) 0.046(3) -0.001(2) 0.005(2) -0.010(2) C28 0.037(2) 0.038(3) 0.040(2) 0.000(2) 0.0066(19) 0.010(2) C29 0.049(2) 0.043(3) 0.030(2) 0.0028(19) 0.0012(18) 0.001(2) C30 0.052(3) 0.058(3) 0.058(3) -0.018(2) 0.018(2) -0.007(2) C31 0.061(3) 0.058(3) 0.069(3) -0.007(3) 0.022(3) 0.008(3) C32 0.049(3) 0.075(4) 0.047(3) 0.023(3) 0.002(2) -0.001(3) C33 0.056(3) 0.066(4) 0.080(4) 0.004(3) 0.011(3) -0.019(3) C34 0.066(3) 0.049(3) 0.061(3) -0.008(2) 0.014(3) -0.004(2) C35 0.051(3) 0.100(5) 0.060(4) 0.037(4) 0.004(3) 0.004(3) C36 0.053(2) 0.040(3) 0.037(2) -0.0019(19) 0.012(2) 0.002(2) C37 0.079(3) 0.048(3) 0.036(3) 0.000(2) 0.006(2) 0.019(2) C38 0.080(3) 0.049(3) 0.037(3) 0.006(2) 0.013(2) 0.017(3) C39 0.060(3) 0.042(3) 0.037(3) 0.001(2) 0.018(2) 0.004(2) C40 0.078(3) 0.048(3) 0.045(3) 0.000(2) 0.010(2) 0.023(3) C41 0.077(3) 0.052(3) 0.035(2) -0.001(2) 0.009(2) 0.014(2) C42 0.049(2) 0.051(3) 0.043(3) -0.001(2) 0.016(2) 0.003(2) O1 0.126(4) 0.072(3) 0.115(4) -0.033(3) 0.015(3) 0.019(3) O2 0.112(3) 0.077(3) 0.060(3) -0.017(2) 0.035(2) -0.019(2) O3 0.075(2) 0.108(3) 0.080(3) -0.031(2) 0.033(2) -0.022(2) O4 0.0426(16) 0.054(2) 0.0433(17) 0.0013(14) 0.0157(13) -0.0052(14) O5 0.054(3) 0.416(11) 0.055(3) 0.043(4) 0.014(2) 0.000(4) O6 0.0425(17) 0.082(3) 0.053(2) 0.0070(17) 0.0098(15) 0.0004(16) O7 0.0475(17) 0.065(2) 0.0386(17) 0.0018(15) 0.0043(14) -0.0106(15) O8 0.0506(18) 0.062(2) 0.061(2) 0.0220(18) 0.0065(16) 0.0009(16) O9 0.048(2) 0.127(4) 0.159(5) 0.043(4) 0.004(3) -0.011(3) O10 0.061(2) 0.132(4) 0.070(3) 0.020(3) 0.018(2) 0.011(2) O11 0.084(2) 0.060(2) 0.0403(19) -0.0016(16) 0.0209(17) 0.0110(17) O12 0.0668(19) 0.047(2) 0.0439(18) -0.0044(15) 0.0159(15) 0.0092(16) O13 0.079(2) 0.076(3) 0.056(2) 0.0041(18) 0.0142(18) -0.0204(19) N100 0.081(3) 0.055(3) 0.054(3) -0.004(2) 0.017(2) 0.004(2) O100 0.094(3) 0.057(2) 0.047(2) -0.0009(17) 0.0181(19) 0.0077(18) C102 0.222(9) 0.057(4) 0.086(5) 0.015(4) 0.017(5) 0.048(5) C101 0.109(4) 0.080(4) 0.060(4) -0.003(3) 0.015(3) 0.013(3) C100 0.058(3) 0.050(3) 0.057(3) 0.002(3) 0.014(2) -0.001(2) O110 0.059(2) 0.081(3) 0.157(4) 0.027(3) 0.010(3) -0.001(2) N110 0.061(3) 0.122(5) 0.116(5) -0.002(4) 0.024(3) 0.009(3) C110 0.070(4) 0.089(5) 0.131(6) 0.043(4) 0.030(4) 0.010(4) C112 0.074(4) 0.127(6) 0.129(6) 0.015(5) 0.018(4) 0.015(4) C111 0.101(6) 0.44(2) 0.180(10) -0.182(13) 0.024(7) 0.009(9) O200 0.096(3) 0.158(5) 0.113(4) 0.020(3) 0.036(3) -0.011(3) O201 0.135(4) 0.107(4) 0.110(4) 0.015(3) 0.051(3) 0.033(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 O2 1.961(4) . ? Zn1 O7 1.977(3) . ? Zn1 O13 2.028(3) . ? Zn1 O10 2.109(4) 4_465 ? Zn1 O9 2.346(5) 4_465 ? Zn1 C35 2.549(6) 4_465 ? Zn2 O4 1.952(3) . ? Zn2 O6 1.971(3) 1_655 ? Zn2 O12 1.984(3) 4_564 ? Zn2 O100 2.002(3) . ? Zn2 C42 2.559(5) 4_564 ? P2 C2P 1.784(4) . ? P2 C36 1.792(4) . ? P2 C29 1.799(4) . ? P2 C22 1.805(4) . ? P1 C1P 1.776(4) . ? P1 C8 1.797(4) . ? P1 C15 1.799(4) . ? P1 C1 1.806(4) . ? C1 C2 1.381(6) . ? C1 C6 1.388(6) . ? C1P H1PA 0.9800 . ? C1P H1PB 0.9800 . ? C1P H1PC 0.9800 . ? C2 C3 1.386(6) . ? C2 H2A 0.9500 . ? C2P H2PA 0.9800 . ? C2P H2PB 0.9800 . ? C2P H2PC 0.9800 . ? C3 C4 1.377(7) . ? C3 H3A 0.9500 . ? C4 C5 1.381(6) . ? C4 C7 1.512(7) . ? C5 C6 1.358(6) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 O1 1.220(7) . ? C7 O2 1.242(6) . ? C8 C9 1.374(7) . ? C8 C13 1.386(6) . ? C9 C10 1.374(7) . ? C9 H9A 0.9500 . ? C10 C11 1.401(7) . ? C10 H10A 0.9500 . ? C11 C12 1.366(6) . ? C11 C14 1.493(6) . ? C12 C13 1.378(6) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 O3 1.249(6) . ? C14 O4 1.266(5) . ? C15 C16 1.379(6) . ? C15 C20 1.391(6) . ? C16 C17 1.380(6) . ? C16 H16A 0.9500 . ? C17 C18 1.366(7) . ? C17 H17A 0.9500 . ? C18 C19 1.380(7) . ? C18 C21 1.511(7) . ? C19 C20 1.361(7) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 O5 1.229(6) . ? C21 O6 1.233(6) . ? C22 C27 1.368(6) . ? C22 C23 1.384(6) . ? C23 C24 1.378(6) . ? C23 H23A 0.9500 . ? C24 C25 1.379(6) . ? C24 H24A 0.9500 . ? C25 C26 1.382(6) . ? C25 C28 1.526(6) . ? C26 C27 1.384(6) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 O8 1.222(5) . ? C28 O7 1.263(5) . ? C29 C34 1.379(6) . ? C29 C30 1.393(6) . ? C30 C31 1.380(6) . ? C30 H30A 0.9500 . ? C31 C32 1.380(7) . ? C31 H31A 0.9500 . ? C32 C33 1.352(7) . ? C32 C35 1.526(8) . ? C33 C34 1.391(7) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 O9 1.223(8) . ? C35 O10 1.226(7) . ? C35 Zn1 2.549(6) 4_666 ? C36 C37 1.366(6) . ? C36 C41 1.401(6) . ? C37 C38 1.389(6) . ? C37 H37A 0.9500 . ? C38 C39 1.375(6) . ? C38 H38A 0.9500 . ? C39 C40 1.380(6) . ? C39 C42 1.515(6) . ? C40 C41 1.375(6) . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? C42 O11 1.228(5) . ? C42 O12 1.268(5) . ? C42 Zn2 2.559(5) 4_567 ? O6 Zn2 1.971(3) 1_455 ? O9 Zn1 2.346(5) 4_666 ? O10 Zn1 2.109(4) 4_666 ? O12 Zn2 1.984(3) 4_567 ? N100 C100 1.307(6) . ? N100 C102 1.430(7) . ? N100 C101 1.443(6) . ? O100 C100 1.228(5) . ? C102 H10B 0.9800 . ? C102 H10C 0.9800 . ? C102 H10D 0.9800 . ? C101 H10E 0.9800 . ? C101 H10F 0.9800 . ? C101 H10G 0.9800 . ? C100 H100 0.9500 . ? O110 C110 1.224(7) . ? N110 C110 1.326(7) . ? N110 C111 1.435(9) . ? N110 C112 1.461(7) . ? C110 H11A 0.9500 . ? C112 H11B 0.9800 . ? C112 H11C 0.9800 . ? C112 H11D 0.9800 . ? C111 H11E 0.9800 . ? C111 H11F 0.9800 . ? C111 H11G 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 O2 Zn1 O7 104.09(16) . . ? O2 Zn1 O13 107.07(15) . . ? O7 Zn1 O13 96.17(13) . . ? O2 Zn1 O10 129.91(18) . 4_465 ? O7 Zn1 O10 114.14(14) . 4_465 ? O13 Zn1 O10 99.90(18) . 4_465 ? O2 Zn1 O9 92.46(16) . 4_465 ? O7 Zn1 O9 91.16(15) . 4_465 ? O13 Zn1 O9 156.66(17) . 4_465 ? O10 Zn1 O9 57.03(18) 4_465 4_465 ? O2 Zn1 C35 111.93(19) . 4_465 ? O7 Zn1 C35 105.35(16) . 4_465 ? O13 Zn1 C35 128.5(2) . 4_465 ? O10 Zn1 C35 28.55(19) 4_465 4_465 ? O9 Zn1 C35 28.54(19) 4_465 4_465 ? O4 Zn2 O6 101.02(13) . 1_655 ? O4 Zn2 O12 122.20(12) . 4_564 ? O6 Zn2 O12 124.35(13) 1_655 4_564 ? O4 Zn2 O100 109.10(13) . . ? O6 Zn2 O100 97.09(14) 1_655 . ? O12 Zn2 O100 99.51(14) 4_564 . ? O4 Zn2 C42 112.97(13) . 4_564 ? O6 Zn2 C42 105.37(14) 1_655 4_564 ? O12 Zn2 C42 29.07(13) 4_564 4_564 ? O100 Zn2 C42 126.63(15) . 4_564 ? C2P P2 C36 108.5(2) . . ? C2P P2 C29 108.9(2) . . ? C36 P2 C29 109.4(2) . . ? C2P P2 C22 111.7(2) . . ? C36 P2 C22 107.66(19) . . ? C29 P2 C22 110.63(18) . . ? C1P P1 C8 111.4(2) . . ? C1P P1 C15 110.2(2) . . ? C8 P1 C15 105.5(2) . . ? C1P P1 C1 110.0(2) . . ? C8 P1 C1 111.36(19) . . ? C15 P1 C1 108.24(19) . . ? C2 C1 C6 120.2(4) . . ? C2 C1 P1 120.1(3) . . ? C6 C1 P1 119.6(3) . . ? P1 C1P H1PA 109.5 . . ? P1 C1P H1PB 109.5 . . ? H1PA C1P H1PB 109.5 . . ? P1 C1P H1PC 109.5 . . ? H1PA C1P H1PC 109.5 . . ? H1PB C1P H1PC 109.5 . . ? C1 C2 C3 119.2(4) . . ? C1 C2 H2A 120.4 . . ? C3 C2 H2A 120.4 . . ? P2 C2P H2PA 109.5 . . ? P2 C2P H2PB 109.5 . . ? H2PA C2P H2PB 109.5 . . ? P2 C2P H2PC 109.5 . . ? H2PA C2P H2PC 109.5 . . ? H2PB C2P H2PC 109.5 . . ? C4 C3 C2 121.0(4) . . ? C4 C3 H3A 119.5 . . ? C2 C3 H3A 119.5 . . ? C3 C4 C5 118.2(4) . . ? C3 C4 C7 121.2(5) . . ? C5 C4 C7 120.4(5) . . ? C6 C5 C4 122.1(5) . . ? C6 C5 H5A 118.9 . . ? C4 C5 H5A 118.9 . . ? C5 C6 C1 119.2(4) . . ? C5 C6 H6A 120.4 . . ? C1 C6 H6A 120.4 . . ? O1 C7 O2 123.6(6) . . ? O1 C7 C4 119.6(5) . . ? O2 C7 C4 116.8(6) . . ? C9 C8 C13 119.5(4) . . ? C9 C8 P1 119.4(3) . . ? C13 C8 P1 120.8(3) . . ? C8 C9 C10 121.4(4) . . ? C8 C9 H9A 119.3 . . ? C10 C9 H9A 119.3 . . ? C9 C10 C11 119.1(5) . . ? C9 C10 H10A 120.5 . . ? C11 C10 H10A 120.5 . . ? C12 C11 C10 119.0(4) . . ? C12 C11 C14 121.1(4) . . ? C10 C11 C14 119.7(4) . . ? C11 C12 C13 121.9(4) . . ? C11 C12 H12A 119.0 . . ? C13 C12 H12A 119.0 . . ? C12 C13 C8 119.0(4) . . ? C12 C13 H13A 120.5 . . ? C8 C13 H13A 120.5 . . ? O3 C14 O4 123.8(4) . . ? O3 C14 C11 120.3(4) . . ? O4 C14 C11 115.7(4) . . ? C16 C15 C20 119.0(4) . . ? C16 C15 P1 120.7(3) . . ? C20 C15 P1 120.2(3) . . ? C15 C16 C17 119.5(4) . . ? C15 C16 H16A 120.3 . . ? C17 C16 H16A 120.3 . . ? C18 C17 C16 121.4(4) . . ? C18 C17 H17A 119.3 . . ? C16 C17 H17A 119.3 . . ? C17 C18 C19 118.9(4) . . ? C17 C18 C21 120.2(4) . . ? C19 C18 C21 120.9(5) . . ? C20 C19 C18 120.7(5) . . ? C20 C19 H19A 119.7 . . ? C18 C19 H19A 119.7 . . ? C19 C20 C15 120.5(4) . . ? C19 C20 H20A 119.7 . . ? C15 C20 H20A 119.7 . . ? O5 C21 O6 125.5(5) . . ? O5 C21 C18 118.5(5) . . ? O6 C21 C18 116.1(5) . . ? C27 C22 C23 119.9(4) . . ? C27 C22 P2 120.6(3) . . ? C23 C22 P2 119.5(3) . . ? C24 C23 C22 119.2(4) . . ? C24 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? C23 C24 C25 121.3(4) . . ? C23 C24 H24A 119.4 . . ? C25 C24 H24A 119.4 . . ? C24 C25 C26 118.9(4) . . ? C24 C25 C28 121.0(4) . . ? C26 C25 C28 120.1(4) . . ? C25 C26 C27 119.8(4) . . ? C25 C26 H26A 120.1 . . ? C27 C26 H26A 120.1 . . ? C22 C27 C26 120.7(4) . . ? C22 C27 H27A 119.6 . . ? C26 C27 H27A 119.6 . . ? O8 C28 O7 126.8(4) . . ? O8 C28 C25 118.3(4) . . ? O7 C28 C25 114.9(4) . . ? C34 C29 C30 119.0(4) . . ? C34 C29 P2 120.5(4) . . ? C30 C29 P2 120.5(3) . . ? C31 C30 C29 120.0(4) . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 120.6(5) . . ? C30 C31 H31A 119.7 . . ? C32 C31 H31A 119.7 . . ? C33 C32 C31 119.2(5) . . ? C33 C32 C35 119.7(6) . . ? C31 C32 C35 121.1(6) . . ? C32 C33 C34 121.5(5) . . ? C32 C33 H33A 119.2 . . ? C34 C33 H33A 119.2 . . ? C29 C34 C33 119.6(5) . . ? C29 C34 H34A 120.2 . . ? C33 C34 H34A 120.2 . . ? O9 C35 O10 121.6(6) . . ? O9 C35 C32 119.3(7) . . ? O10 C35 C32 119.1(6) . . ? O9 C35 Zn1 66.5(4) . 4_666 ? O10 C35 Zn1 55.3(3) . 4_666 ? C32 C35 Zn1 172.9(5) . 4_666 ? C37 C36 C41 119.2(4) . . ? C37 C36 P2 119.6(3) . . ? C41 C36 P2 121.2(3) . . ? C36 C37 C38 120.7(4) . . ? C36 C37 H37A 119.6 . . ? C38 C37 H37A 119.6 . . ? C39 C38 C37 120.1(4) . . ? C39 C38 H38A 120.0 . . ? C37 C38 H38A 120.0 . . ? C38 C39 C40 119.5(4) . . ? C38 C39 C42 119.0(4) . . ? C40 C39 C42 121.5(4) . . ? C41 C40 C39 120.8(4) . . ? C41 C40 H40A 119.6 . . ? C39 C40 H40A 119.6 . . ? C40 C41 C36 119.8(4) . . ? C40 C41 H41A 120.1 . . ? C36 C41 H41A 120.1 . . ? O11 C42 O12 124.0(4) . . ? O11 C42 C39 118.9(4) . . ? O12 C42 C39 117.1(4) . . ? O11 C42 Zn2 75.3(3) . 4_567 ? O12 C42 Zn2 49.5(2) . 4_567 ? C39 C42 Zn2 162.7(3) . 4_567 ? C7 O2 Zn1 111.4(4) . . ? C14 O4 Zn2 117.8(3) . . ? C21 O6 Zn2 115.1(3) . 1_455 ? C28 O7 Zn1 127.3(3) . . ? C35 O9 Zn1 85.0(5) . 4_666 ? C35 O10 Zn1 96.1(4) . 4_666 ? C42 O12 Zn2 101.5(3) . 4_567 ? C100 N100 C102 119.9(5) . . ? C100 N100 C101 121.6(5) . . ? C102 N100 C101 118.5(5) . . ? C100 O100 Zn2 121.9(3) . . ? N100 C102 H10B 109.5 . . ? N100 C102 H10C 109.5 . . ? H10B C102 H10C 109.5 . . ? N100 C102 H10D 109.5 . . ? H10B C102 H10D 109.5 . . ? H10C C102 H10D 109.5 . . ? N100 C101 H10E 109.5 . . ? N100 C101 H10F 109.5 . . ? H10E C101 H10F 109.5 . . ? N100 C101 H10G 109.5 . . ? H10E C101 H10G 109.5 . . ? H10F C101 H10G 109.5 . . ? O100 C100 N100 123.8(5) . . ? O100 C100 H100 118.1 . . ? N100 C100 H100 118.1 . . ? C110 N110 C111 119.5(6) . . ? C110 N110 C112 122.8(6) . . ? C111 N110 C112 117.6(6) . . ? O110 C110 N110 125.4(7) . . ? O110 C110 H11A 117.3 . . ? N110 C110 H11A 117.3 . . ? N110 C112 H11B 109.5 . . ? N110 C112 H11C 109.5 . . ? H11B C112 H11C 109.5 . . ? N110 C112 H11D 109.5 . . ? H11B C112 H11D 109.5 . . ? H11C C112 H11D 109.5 . . ? N110 C111 H11E 109.5 . . ? N110 C111 H11F 109.5 . . ? H11E C111 H11F 109.5 . . ? N110 C111 H11G 109.5 . . ? H11E C111 H11G 109.5 . . ? H11F C111 H11G 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.514 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.075 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.500 374 125 ' ' 2 0.500 0.500 1.000 374 126 ' ' _platon_squeeze_details ; ;