Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_ZnPO-DACH _database_code_CSD 171183 _journal_coden_Cambridge 186 loop_ _publ_author_name 'Yu, Jihong' 'Du, Yu' 'Shi, Zhan' 'Wang, Yu' 'Xu, Ruren' 'Zou, Yongcun' # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof Jihong Yu' _publ_contact_author_address ; Key Lab of Inorg Synth & Preparative Chem Jilin University Changchun 130023 CHINA ; _publ_contact_author_phone '86 431 8922331 2479' _publ_contact_author_fax '86 431 5671974' _publ_contact_author_email 'jihong@mail.jlu.edu.cn' _publ_requested_journal 'Dalton Transactions' _publ_requested_coeditor_name ? #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Hydrothermal Synthesis and Characterization of a New Inorganic-organic Hybrid Layered Zinc Phosphate-phosphite (trans-C6H15N2)2Zn4(PO4)2(HPO3)2 ; #complex ZnPO-DACH _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H32 N4 O14 P4 Zn4' _chemical_formula_weight 841.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.7060(17) _cell_length_b 9.9929(16) _cell_length_c 27.557(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.795(3) _cell_angle_gamma 90.00 _cell_volume 2654.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 3.884 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6974 _exptl_absorpt_correction_T_max 0.7464 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6017 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 23.27 _reflns_number_total 3705 _reflns_number_gt 2382 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0689P)^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 3705 _refine_ls_number_parameters 349 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0835 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1263 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.51425(11) 0.20081(9) 0.35999(4) 0.0308(3) Uani 1 1 d . . . Zn2 Zn 0.01581(11) 0.26321(9) 0.35925(4) 0.0291(3) Uani 1 1 d . . . Zn3 Zn 0.79696(9) 0.41977(8) 0.20795(3) 0.0211(3) Uani 1 1 d . . . Zn4 Zn 0.29609(9) 0.04675(8) 0.20760(3) 0.0214(3) Uani 1 1 d . . . P1 P 0.5979(2) 0.19722(19) 0.25063(7) 0.0201(5) Uani 1 1 d . . . P2 P 0.1008(2) 0.27034(19) 0.25078(8) 0.0204(5) Uani 1 1 d . . . P3 P 0.7175(2) 0.5594(2) 0.10559(8) 0.0278(5) Uani 1 1 d D . . P4 P 0.2183(2) -0.0957(2) 0.10444(8) 0.0278(5) Uani 1 1 d . . . O1 O -0.0835(7) 0.1073(6) 0.3775(2) 0.0480(17) Uani 1 1 d . . . O2 O 0.1797(6) 0.2964(5) 0.4053(2) 0.0334(14) Uani 1 1 d . . . O3 O 0.0983(7) 0.2062(5) 0.3009(2) 0.0387(16) Uani 1 1 d . . . O4 O 0.1398(6) 0.1622(5) 0.21611(19) 0.0285(13) Uani 1 1 d . . . O5 O 0.2928(6) -0.1162(5) 0.24685(19) 0.0302(14) Uani 1 1 d . . . O6 O 0.4610(7) 0.1455(6) 0.2286(3) 0.060(2) Uani 1 1 d . . . O7 O 0.2857(7) 0.0096(5) 0.1382(2) 0.0391(16) Uani 1 1 d . . . O8 O 0.4155(7) 0.3544(6) 0.3801(2) 0.0482(17) Uani 1 1 d . . . O9 O 0.5912(8) 0.2584(6) 0.3006(2) 0.0492(19) Uani 1 1 d . . . O10 O 0.6418(6) 0.3079(5) 0.2168(2) 0.0326(15) Uani 1 1 d . . . O11 O 0.7932(6) 0.5856(5) 0.24515(19) 0.0268(13) Uani 1 1 d . . . O12 O 0.9594(6) 0.3203(6) 0.2309(3) 0.0514(19) Uani 1 1 d . . . O13 O 0.7881(6) 0.4516(5) 0.1386(2) 0.0354(15) Uani 1 1 d . . . O14 O 0.8184(6) 0.6701(5) 0.0957(2) 0.0357(15) Uani 1 1 d . . . N1 N 0.3809(9) 0.0495(8) 0.3450(3) 0.052(2) Uani 1 1 d . . . H1A H 0.3168 0.0776 0.3208 0.080 Uiso 1 1 calc . . . H1B H 0.4282 -0.0170 0.3325 0.080 Uiso 1 1 calc . . . N2 N 0.1172(8) -0.0817(7) 0.3192(3) 0.037(2) Uani 1 1 d . . . H2A H 0.0603 -0.1498 0.3108 0.080 Uiso 1 1 calc . . . H2B H 0.1711 -0.0675 0.2957 0.080 Uiso 1 1 calc . . . H2C H 0.0677 -0.0085 0.3232 0.080 Uiso 1 1 calc . . . N3 N -0.1202(8) 0.4118(7) 0.3423(3) 0.040(2) Uani 1 1 d . . . H3A H -0.0737 0.4780 0.3292 0.080 Uiso 1 1 calc . . . H3B H -0.1832 0.3810 0.3183 0.080 Uiso 1 1 calc . . . N4 N -0.3845(8) 0.5456(7) 0.3169(3) 0.0362(18) Uani 1 1 d . . . H4A H -0.4408 0.6142 0.3087 0.080 Uiso 1 1 calc . . . H4B H -0.4346 0.4728 0.3211 0.080 Uiso 1 1 calc . . . H4C H -0.3311 0.5309 0.2933 0.080 Uiso 1 1 calc . . . C1 C 0.3065(11) -0.0092(10) 0.3820(4) 0.053(3) Uani 1 1 d . . . H1 H 0.2472 0.0645 0.3904 0.080 Uiso 1 1 calc . . . C2 C 0.2057(11) -0.1141(10) 0.3659(4) 0.052(3) Uani 1 1 d . . . H2 H 0.2637 -0.1883 0.3569 0.080 Uiso 1 1 calc . . . C3 C 0.1261(11) -0.1736(10) 0.4036(4) 0.050(3) Uani 1 1 d . . . H3C H 0.0498 -0.1145 0.4086 0.080 Uiso 1 1 calc . . . H3D H 0.0869 -0.2583 0.3915 0.080 Uiso 1 1 calc . . . C4 C 0.2111(17) -0.1964(12) 0.4510(5) 0.086(5) Uani 1 1 d . . . H4D H 0.1489 -0.2034 0.4760 0.080 Uiso 1 1 calc . . . H4E H 0.2572 -0.2822 0.4494 0.080 Uiso 1 1 calc . . . C5 C 0.3155(16) -0.0972(15) 0.4668(5) 0.100(5) Uani 1 1 d . . . H5A H 0.3822 -0.1379 0.4914 0.080 Uiso 1 1 calc . . . H5B H 0.2707 -0.0251 0.4826 0.080 Uiso 1 1 calc . . . C6 C 0.3920(11) -0.0382(10) 0.4294(4) 0.049(3) Uani 1 1 d . . . H6A H 0.4662 -0.0988 0.4233 0.080 Uiso 1 1 calc . . . H6B H 0.4345 0.0445 0.4421 0.080 Uiso 1 1 calc . . . C7 C -0.1991(10) 0.4744(9) 0.3796(3) 0.041(2) Uani 1 1 d . . . H7 H -0.2597 0.4014 0.3877 0.080 Uiso 1 1 calc . . . C8 C -0.2960(11) 0.5769(10) 0.3630(3) 0.053(3) Uani 1 1 d . . . H8 H -0.2373 0.6506 0.3541 0.080 Uiso 1 1 calc . . . C9 C -0.3752(10) 0.6364(9) 0.4009(4) 0.048(3) Uani 1 1 d . . . H9A H -0.4490 0.5753 0.4069 0.080 Uiso 1 1 calc . . . H9B H -0.4181 0.7189 0.3882 0.080 Uiso 1 1 calc . . . C10 C -0.2880(14) 0.6659(11) 0.4489(4) 0.073(4) Uani 1 1 d . . . H10A H -0.2393 0.7497 0.4458 0.080 Uiso 1 1 calc . . . H10B H -0.3491 0.6776 0.4740 0.080 Uiso 1 1 calc . . . C11 C -0.1854(15) 0.5609(13) 0.4648(4) 0.085(5) Uani 1 1 d . . . H11A H -0.1165 0.5993 0.4892 0.080 Uiso 1 1 calc . . . H11B H -0.2325 0.4906 0.4806 0.080 Uiso 1 1 calc . . . C12 C -0.1129(11) 0.4997(9) 0.4269(3) 0.043(2) Uani 1 1 d . . . H12A H -0.0737 0.4153 0.4392 0.080 Uiso 1 1 calc . . . H12B H -0.0363 0.5575 0.4209 0.080 Uiso 1 1 calc . . . H4 H 0.178(11) -0.031(9) 0.064(4) 0.080 Uiso 1 1 d . . . H3 H 0.675(11) 0.495(8) 0.064(2) 0.080 Uiso 1 1 d 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 0.0285(6) 0.0295(6) 0.0351(6) -0.0044(4) 0.0066(5) -0.0027(4) Zn2 0.0279(6) 0.0277(6) 0.0326(6) 0.0036(4) 0.0073(5) 0.0009(4) Zn3 0.0207(6) 0.0171(5) 0.0255(6) -0.0002(4) 0.0028(4) 0.0007(4) Zn4 0.0212(5) 0.0172(5) 0.0258(6) -0.0002(4) 0.0033(4) 0.0011(4) P1 0.0209(12) 0.0148(11) 0.0246(12) 0.0006(8) 0.0028(9) -0.0005(8) P2 0.0180(12) 0.0166(11) 0.0267(13) -0.0004(8) 0.0025(10) 0.0028(8) P3 0.0280(14) 0.0284(13) 0.0269(13) -0.0038(9) 0.0029(10) 0.0041(10) P4 0.0315(14) 0.0296(13) 0.0228(13) 0.0037(9) 0.0054(10) 0.0002(10) O1 0.034(4) 0.038(4) 0.074(5) 0.008(3) 0.014(3) -0.013(3) O2 0.030(4) 0.028(3) 0.042(4) 0.008(3) 0.002(3) -0.002(3) O3 0.057(5) 0.033(4) 0.029(4) 0.001(3) 0.019(3) -0.008(3) O4 0.026(3) 0.026(3) 0.034(3) -0.012(2) 0.004(3) -0.001(2) O5 0.034(4) 0.016(3) 0.041(4) 0.006(2) 0.007(3) 0.008(2) O6 0.028(4) 0.030(4) 0.113(7) 0.014(4) -0.024(4) -0.013(3) O7 0.049(4) 0.039(4) 0.031(4) -0.004(3) 0.013(3) 0.001(3) O8 0.034(4) 0.046(4) 0.067(5) -0.019(3) 0.014(3) 0.005(3) O9 0.075(6) 0.032(4) 0.044(4) -0.002(3) 0.023(4) 0.009(3) O10 0.023(3) 0.024(3) 0.052(4) 0.011(3) 0.007(3) -0.001(3) O11 0.026(3) 0.023(3) 0.032(3) -0.005(2) 0.008(3) -0.004(2) O12 0.032(4) 0.040(4) 0.078(5) -0.009(3) -0.013(3) 0.017(3) O13 0.048(4) 0.032(3) 0.028(3) 0.001(3) 0.009(3) 0.005(3) O14 0.037(4) 0.028(3) 0.041(4) 0.010(3) 0.002(3) -0.001(3) N1 0.047(6) 0.063(5) 0.046(5) -0.011(4) 0.007(4) -0.032(4) N2 0.032(5) 0.035(5) 0.045(5) -0.020(3) 0.005(4) -0.009(3) N3 0.043(5) 0.050(5) 0.031(4) 0.007(3) 0.014(4) 0.020(4) N4 0.033(5) 0.040(4) 0.036(5) 0.010(3) 0.006(4) 0.004(3) C1 0.047(7) 0.064(7) 0.047(7) 0.015(5) -0.003(5) -0.033(5) C2 0.047(7) 0.071(7) 0.038(6) 0.000(5) 0.003(5) -0.034(5) C3 0.062(8) 0.044(6) 0.048(7) 0.000(5) 0.027(6) -0.015(5) C4 0.135(14) 0.069(8) 0.058(9) 0.016(6) 0.032(9) -0.039(9) C5 0.100(13) 0.145(14) 0.052(9) 0.039(8) -0.010(8) -0.049(10) C6 0.046(7) 0.056(6) 0.041(6) -0.001(5) -0.009(5) -0.008(5) C7 0.043(6) 0.048(6) 0.030(5) -0.007(4) 0.002(5) 0.015(5) C8 0.048(7) 0.077(8) 0.032(6) -0.012(5) -0.002(5) 0.030(6) C9 0.043(6) 0.040(6) 0.060(7) 0.001(5) 0.005(5) 0.008(5) C10 0.097(11) 0.069(8) 0.052(8) -0.019(6) 0.013(7) 0.025(7) C11 0.092(11) 0.114(11) 0.044(7) -0.036(7) -0.014(7) 0.041(8) C12 0.042(6) 0.052(6) 0.036(6) -0.001(5) 0.005(5) 0.010(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 O8 1.926(6) . ? Zn1 O14 1.937(6) 2_645 ? Zn1 O9 1.964(6) . ? Zn1 N1 2.001(7) . ? Zn2 O1 1.930(6) . ? Zn2 O2 1.942(6) . ? Zn2 O3 1.962(6) . ? Zn2 N3 2.005(7) . ? Zn3 O12 1.907(6) . ? Zn3 O10 1.914(5) . ? Zn3 O13 1.930(5) . ? Zn3 O11 1.951(5) . ? Zn4 O6 1.912(6) . ? Zn4 O7 1.940(6) . ? Zn4 O4 1.942(5) . ? Zn4 O5 1.957(5) . ? P1 O6 1.486(6) . ? P1 O9 1.515(6) . ? P1 O11 1.532(5) 2_645 ? P1 O10 1.539(6) . ? P2 O12 1.502(6) 1_455 ? P2 O4 1.520(5) . ? P2 O3 1.526(6) . ? P2 O5 1.530(5) 2 ? P3 O1 1.510(6) 2 ? P3 O13 1.519(6) . ? P3 O14 1.523(6) . ? P3 H3 1.33(5) . ? P4 O8 1.499(6) 2_545 ? P4 O7 1.502(6) . ? P4 O2 1.510(6) 2_545 ? P4 H4 1.31(10) . ? O1 P3 1.510(6) 2_545 ? O2 P4 1.510(6) 2 ? O5 P2 1.530(5) 2_545 ? O8 P4 1.499(6) 2 ? O11 P1 1.532(5) 2_655 ? O12 P2 1.502(6) 1_655 ? O14 Zn1 1.937(6) 2_655 ? N1 C1 1.441(12) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C2 1.497(12) . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 H2C 0.8900 . ? N3 C7 1.490(11) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C8 1.480(11) . ? N4 H4A 0.8900 . ? N4 H4B 0.8900 . ? N4 H4C 0.8900 . ? C1 C2 1.467(12) . ? C1 C6 1.491(13) . ? C1 H1 0.9800 . ? C2 C3 1.490(13) . ? C2 H2 0.9800 . ? C3 C4 1.478(16) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 C5 1.447(18) . ? C4 H4D 0.9700 . ? C4 H4E 0.9700 . ? C5 C6 1.465(16) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.428(12) . ? C7 C12 1.485(12) . ? C7 H7 0.9800 . ? C8 C9 1.491(14) . ? C8 H8 0.9800 . ? C9 C10 1.513(14) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.477(16) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.461(15) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Zn1 O14 110.7(3) . 2_645 ? O8 Zn1 O9 104.9(3) . . ? O14 Zn1 O9 101.4(3) 2_645 . ? O8 Zn1 N1 109.3(3) . . ? O14 Zn1 N1 118.9(3) 2_645 . ? O9 Zn1 N1 110.5(3) . . ? O1 Zn2 O2 111.3(3) . . ? O1 Zn2 O3 104.2(3) . . ? O2 Zn2 O3 101.7(3) . . ? O1 Zn2 N3 108.8(3) . . ? O2 Zn2 N3 119.5(3) . . ? O3 Zn2 N3 110.2(3) . . ? O12 Zn3 O10 106.6(3) . . ? O12 Zn3 O13 110.6(3) . . ? O10 Zn3 O13 106.2(2) . . ? O12 Zn3 O11 109.6(2) . . ? O10 Zn3 O11 111.4(2) . . ? O13 Zn3 O11 112.3(2) . . ? O6 Zn4 O7 110.0(3) . . ? O6 Zn4 O4 107.1(3) . . ? O7 Zn4 O4 106.4(2) . . ? O6 Zn4 O5 109.3(3) . . ? O7 Zn4 O5 112.6(2) . . ? O4 Zn4 O5 111.3(2) . . ? O6 P1 O9 112.3(5) . . ? O6 P1 O11 110.7(3) . 2_645 ? O9 P1 O11 109.2(3) . 2_645 ? O6 P1 O10 107.5(4) . . ? O9 P1 O10 107.8(3) . . ? O11 P1 O10 109.3(3) 2_645 . ? O12 P2 O4 107.0(3) 1_455 . ? O12 P2 O3 111.0(4) 1_455 . ? O4 P2 O3 107.6(3) . . ? O12 P2 O5 110.6(3) 1_455 2 ? O4 P2 O5 109.6(3) . 2 ? O3 P2 O5 110.8(3) . 2 ? O1 P3 O13 112.6(4) 2 . ? O1 P3 O14 114.8(4) 2 . ? O13 P3 O14 111.6(3) . . ? O1 P3 H3 103(5) 2 . ? O13 P3 H3 104(4) . . ? O14 P3 H3 110(4) . . ? O8 P4 O7 112.7(4) 2_545 . ? O8 P4 O2 115.0(3) 2_545 2_545 ? O7 P4 O2 111.3(4) . 2_545 ? O8 P4 H4 103(5) 2_545 . ? O7 P4 H4 104(4) . . ? O2 P4 H4 109(4) 2_545 . ? P3 O1 Zn2 144.3(4) 2_545 . ? P4 O2 Zn2 120.6(3) 2 . ? P2 O3 Zn2 132.2(4) . . ? P2 O4 Zn4 139.0(3) . . ? P2 O5 Zn4 125.8(3) 2_545 . ? P1 O6 Zn4 168.3(4) . . ? P4 O7 Zn4 135.4(4) . . ? P4 O8 Zn1 145.5(4) 2 . ? P1 O9 Zn1 134.5(4) . . ? P1 O10 Zn3 140.9(4) . . ? P1 O11 Zn3 127.1(3) 2_655 . ? P2 O12 Zn3 168.0(4) 1_655 . ? P3 O13 Zn3 132.3(4) . . ? P3 O14 Zn1 120.8(3) . 2_655 ? C1 N1 Zn1 121.8(6) . . ? C1 N1 H1A 106.9 . . ? Zn1 N1 H1A 106.9 . . ? C1 N1 H1B 106.9 . . ? Zn1 N1 H1B 106.9 . . ? H1A N1 H1B 106.7 . . ? C2 N2 H2A 109.5 . . ? C2 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C2 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C7 N3 Zn2 121.8(5) . . ? C7 N3 H3A 106.9 . . ? Zn2 N3 H3A 106.9 . . ? C7 N3 H3B 106.9 . . ? Zn2 N3 H3B 106.9 . . ? H3A N3 H3B 106.7 . . ? C8 N4 H4A 109.5 . . ? C8 N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? C8 N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? N1 C1 C2 116.7(9) . . ? N1 C1 C6 115.2(9) . . ? C2 C1 C6 114.1(8) . . ? N1 C1 H1 102.7 . . ? C2 C1 H1 102.7 . . ? C6 C1 H1 102.7 . . ? C1 C2 C3 117.2(9) . . ? C1 C2 N2 113.5(8) . . ? C3 C2 N2 113.2(8) . . ? C1 C2 H2 103.6 . . ? C3 C2 H2 103.6 . . ? N2 C2 H2 103.6 . . ? C4 C3 C2 113.4(10) . . ? C4 C3 H3C 108.9 . . ? C2 C3 H3C 108.9 . . ? C4 C3 H3D 108.9 . . ? C2 C3 H3D 108.9 . . ? H3C C3 H3D 107.7 . . ? C5 C4 C3 117.3(10) . . ? C5 C4 H4D 108.0 . . ? C3 C4 H4D 108.0 . . ? C5 C4 H4E 108.0 . . ? C3 C4 H4E 108.0 . . ? H4D C4 H4E 107.2 . . ? C4 C5 C6 117.3(11) . . ? C4 C5 H5A 108.0 . . ? C6 C5 H5A 108.0 . . ? C4 C5 H5B 108.0 . . ? C6 C5 H5B 108.0 . . ? H5A C5 H5B 107.2 . . ? C5 C6 C1 114.8(10) . . ? C5 C6 H6A 108.6 . . ? C1 C6 H6A 108.6 . . ? C5 C6 H6B 108.6 . . ? C1 C6 H6B 108.6 . . ? H6A C6 H6B 107.5 . . ? C8 C7 C12 116.1(8) . . ? C8 C7 N3 117.0(8) . . ? C12 C7 N3 113.3(8) . . ? C8 C7 H7 102.5 . . ? C12 C7 H7 102.5 . . ? N3 C7 H7 102.5 . . ? C7 C8 N4 114.6(8) . . ? C7 C8 C9 115.9(8) . . ? N4 C8 C9 112.9(8) . . ? C7 C8 H8 103.8 . . ? N4 C8 H8 103.8 . . ? C9 C8 H8 103.8 . . ? C8 C9 C10 114.0(9) . . ? C8 C9 H9A 108.7 . . ? C10 C9 H9A 108.7 . . ? C8 C9 H9B 108.7 . . ? C10 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C11 C10 C9 114.2(9) . . ? C11 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? C11 C10 H10B 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C12 C11 C10 116.7(10) . . ? C12 C11 H11A 108.1 . . ? C10 C11 H11A 108.1 . . ? C12 C11 H11B 108.1 . . ? C10 C11 H11B 108.1 . . ? H11A C11 H11B 107.3 . . ? C11 C12 C7 115.5(9) . . ? C11 C12 H12A 108.4 . . ? C7 C12 H12A 108.4 . . ? C11 C12 H12B 108.4 . . ? C7 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O3 0.90 2.49 3.265(11) 145.2 . N2 H2A O10 0.89 2.06 2.816(9) 141.9 2_545 N2 H2A O6 0.89 2.31 3.083(9) 144.7 2_545 N2 H2B O5 0.89 1.95 2.792(9) 156.3 . N2 H2C O3 0.89 2.26 2.923(9) 131.0 . N2 H2C O1 0.89 2.50 3.271(10) 145.1 . N3 H3A O6 0.90 2.64 3.518(11) 166.5 2 N3 H3B O9 0.90 2.51 3.279(11) 144.3 1_455 N4 H4A O4 0.89 2.03 2.792(9) 143.2 2_455 N4 H4A O12 0.89 2.33 3.094(9) 144.4 2 N4 H4B O9 0.89 2.24 2.910(9) 132.2 1_455 N4 H4B O8 0.89 2.59 3.354(9) 144.0 1_455 N4 H4C O11 0.89 1.97 2.802(9) 154.3 1_455 _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.790 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.132