# 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 'Peng Cheng' _publ_contact_author_email PCHENG@NANKAI.EDU.CN _publ_section_title ; 3D Porous Hetero-metal Phosphonate with Helical Channels ; loop_ _publ_author_name 'Peng Cheng' 'Dai-Zheng Liao' 'Hai-Yang Liu' 'Wei Shi' 'Shi-Ping Yan' ; Zhen-Jie Zhang ; 'Bin Zhao' # Attachment 'R70506B.cif' data_r70506b _database_code_depnum_ccdc_archive 'CCDC 716863' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H32 Cd N3 O17.50 P3 Zn3.50' _chemical_formula_weight 1004.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 21.982(4) _cell_length_b 15.977(3) _cell_length_c 25.818(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.50(3) _cell_angle_gamma 90.00 _cell_volume 8547(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7851 _cell_measurement_theta_min 1.6094 _cell_measurement_theta_max 27.8924 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3992 _exptl_absorpt_coefficient_mu 2.600 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6244 _exptl_absorpt_correction_T_max 0.6244 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _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 dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25984 _diffrn_reflns_av_R_equivalents 0.0945 _diffrn_reflns_av_sigmaI/netI 0.0883 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7526 _reflns_number_gt 5876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0640P)^2^+0.2717P] 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 7526 _refine_ls_number_parameters 425 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1423 _refine_ls_wR_factor_gt 0.1326 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.060 _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 C1 C 0.6247(4) 0.8942(4) 0.8488(3) 0.0338(18) Uani 1 1 d . . . H1A H 0.6467 0.8414 0.8491 0.041 Uiso 1 1 calc R . . H1B H 0.5799 0.8884 0.8258 0.041 Uiso 1 1 calc R . . C2 C 0.6299(4) 0.9201(4) 0.9072(3) 0.0314(17) Uani 1 1 d . . . H2A H 0.5974 0.8926 0.9191 0.038 Uiso 1 1 calc R . . H2B H 0.6724 0.9082 0.9333 0.038 Uiso 1 1 calc R . . C3 C 0.6176(3) 1.0143(4) 0.8998(3) 0.0279(16) Uani 1 1 d . . . H3A H 0.5721 1.0259 0.8819 0.033 Uiso 1 1 calc R . . H3B H 0.6325 1.0431 0.9349 0.033 Uiso 1 1 calc R . . C4 C 0.6296(3) 1.1164(4) 0.8325(2) 0.0210(14) Uani 1 1 d . . . H4A H 0.5834 1.1101 0.8151 0.025 Uiso 1 1 calc R . . H4B H 0.6485 1.1241 0.8038 0.025 Uiso 1 1 calc R . . C5 C 0.6574(3) 0.9650(4) 0.8282(3) 0.0245(15) Uani 1 1 d . . . H5 H 0.6335 0.9773 0.7895 0.029 Uiso 1 1 calc R . . C6 C 0.7266(3) 0.9418(4) 0.8355(3) 0.0235(15) Uani 1 1 d . . . C7 C 0.7818(3) 0.9769(4) 0.7129(3) 0.0260(15) Uani 1 1 d . . . C8 C 0.7517(4) 1.0336(4) 0.6639(2) 0.0292(17) Uani 1 1 d . . . H8 H 0.7767 1.0854 0.6674 0.035 Uiso 1 1 calc R . . C9 C 0.6810(4) 1.0533(5) 0.6576(3) 0.050(2) Uani 1 1 d . . . H9A H 0.6713 1.0356 0.6900 0.060 Uiso 1 1 calc R . . H9B H 0.6726 1.1129 0.6524 0.060 Uiso 1 1 calc R . . C10 C 0.6400(4) 1.0043(5) 0.6068(3) 0.0352(18) Uani 1 1 d . . . H10A H 0.5991 1.0321 0.5886 0.042 Uiso 1 1 calc R . . H10B H 0.6318 0.9477 0.6163 0.042 Uiso 1 1 calc R . . C11 C 0.6836(3) 1.0050(4) 0.5706(3) 0.0251(16) Uani 1 1 d . . . H11A H 0.6710 0.9619 0.5425 0.030 Uiso 1 1 calc R . . H11B H 0.6827 1.0590 0.5532 0.030 Uiso 1 1 calc R . . C12 C 0.8032(3) 1.0113(4) 0.5924(3) 0.0257(16) Uani 1 1 d . . . H12A H 0.8431 1.0120 0.6234 0.031 Uiso 1 1 calc R . . H12B H 0.7960 1.0672 0.5768 0.031 Uiso 1 1 calc R . . C13 C 0.9430(3) 0.8204(4) 0.9237(3) 0.0213(14) Uani 1 1 d . . . C14 C 0.9627(3) 0.7767(4) 0.9799(3) 0.0235(15) Uani 1 1 d . . . H14 H 0.9550 0.8147 1.0068 0.028 Uiso 1 1 calc R . . C15 C 0.9241(3) 0.6932(4) 0.9780(3) 0.0329(18) Uani 1 1 d . . . H15A H 0.8918 0.7002 0.9957 0.039 Uiso 1 1 calc R . . H15B H 0.9031 0.6747 0.9405 0.039 Uiso 1 1 calc R . . C16 C 0.9760(3) 0.6321(4) 1.0095(3) 0.0318(17) Uani 1 1 d . . . H16A H 0.9841 0.6361 1.0487 0.038 Uiso 1 1 calc R . . H16B H 0.9640 0.5750 0.9977 0.038 Uiso 1 1 calc R . . C17 C 1.0342(3) 0.6591(4) 0.9954(3) 0.0239(15) Uani 1 1 d . . . H17A H 1.0311 0.6406 0.9589 0.029 Uiso 1 1 calc R . . H17B H 1.0735 0.6369 1.0217 0.029 Uiso 1 1 calc R . . C18 C 1.0669(3) 0.7823(4) 1.0560(3) 0.0243(15) Uani 1 1 d . . . H18A H 1.0539 0.7479 1.0814 0.029 Uiso 1 1 calc R . . H18B H 1.0551 0.8398 1.0603 0.029 Uiso 1 1 calc R . . Cd1 Cd 0.84432(2) 0.89488(3) 0.81691(2) 0.02585(15) Uani 1 1 d . . . N1 N 0.6563(3) 1.0402(3) 0.8639(2) 0.0207(12) Uani 1 1 d . . . N2 N 1.0328(3) 0.7539(3) 0.9985(2) 0.0247(13) Uani 1 1 d . . . N3 N 0.7483(3) 0.9874(3) 0.6117(2) 0.0271(14) Uani 1 1 d . . . O1 O 0.5866(2) 1.2270(3) 0.89286(18) 0.0236(10) Uani 1 1 d . . . O2 O 0.7038(2) 1.1823(2) 0.92771(17) 0.0199(10) Uani 1 1 d . . . O3 O 0.6617(2) 1.2793(3) 0.84410(18) 0.0276(11) Uani 1 1 d . . . O4 O 0.7739(2) 0.9801(2) 0.86876(17) 0.0216(10) Uani 1 1 d . . . O5 O 0.7350(2) 0.8833(3) 0.80533(18) 0.0242(10) Uani 1 1 d . . . O6 O 0.8419(3) 0.7562(4) 0.7843(3) 0.0383(17) Uani 0.75 1 d PU . . O7 O 0.9037(2) 1.0127(3) 0.8707(2) 0.0442(15) Uani 1 1 d . . . O9 O 0.7853(2) 0.8984(2) 0.70644(18) 0.0274(11) Uani 1 1 d . . . O10 O 0.8024(2) 1.0108(3) 0.75940(17) 0.0275(11) Uani 1 1 d . . . O11 O 0.7731(2) 0.8593(2) 0.54842(16) 0.0195(10) Uani 1 1 d . . . O12 O 0.8826(2) 0.9203(3) 0.55344(18) 0.0259(11) Uani 1 1 d . . . O13 O 0.7801(2) 0.9790(2) 0.48491(17) 0.0202(10) Uani 1 1 d . . . O14 O 0.8827(2) 0.8314(3) 0.9011(2) 0.0298(11) Uani 1 1 d . . . O15 O 0.9856(2) 0.8425(3) 0.90462(18) 0.0242(10) Uani 1 1 d . . . O16 O 1.1817(2) 0.8567(3) 1.10301(17) 0.0239(10) Uani 1 1 d . . . O17 O 1.1791(2) 0.6988(3) 1.10809(18) 0.0253(10) Uani 1 1 d . . . O18 O 1.1632(2) 0.7697(3) 1.01550(16) 0.0208(10) Uani 1 1 d . . . P1 P 0.64610(8) 1.20848(10) 0.87695(7) 0.0202(4) Uani 1 1 d . . . P2 P 0.81059(8) 0.93767(10) 0.54087(7) 0.0203(4) Uani 1 1 d . . . P3 P 1.15408(8) 0.77507(10) 1.07221(7) 0.0197(4) Uani 1 1 d . . . Zn1 Zn 0.57960(4) 1.30709(4) 0.94746(3) 0.02017(19) Uani 1 1 d . . . Zn2 Zn 0.75186(4) 1.07420(4) 0.91295(3) 0.01917(19) Uani 1 1 d . . . Zn3 Zn 0.73694(4) 1.35571(4) 0.87179(3) 0.0218(2) Uani 1 1 d . . . Zn4 Zn 0.7500 1.2500 1.0000 0.0174(2) Uani 1 2 d S . . O8 O 0.9347(4) 0.8993(5) 0.7904(3) 0.051(2) Uani 0.75 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.022(4) 0.024(3) 0.056(5) -0.010(3) 0.015(4) -0.010(3) C2 0.024(4) 0.025(3) 0.047(4) 0.001(3) 0.014(3) -0.009(3) C3 0.021(4) 0.039(4) 0.025(4) -0.005(3) 0.010(3) -0.009(3) C4 0.022(4) 0.029(3) 0.014(3) -0.004(3) 0.008(3) -0.001(3) C5 0.028(4) 0.020(3) 0.024(4) -0.007(3) 0.007(3) -0.004(3) C6 0.022(4) 0.024(3) 0.025(4) 0.004(3) 0.009(3) -0.004(3) C7 0.033(4) 0.029(3) 0.019(3) -0.002(3) 0.013(3) 0.005(3) C8 0.049(5) 0.032(3) 0.008(3) 0.003(3) 0.010(3) 0.015(3) C9 0.045(5) 0.063(5) 0.033(4) -0.012(4) 0.002(4) 0.024(4) C10 0.034(5) 0.041(4) 0.028(4) -0.006(3) 0.007(3) 0.010(3) C11 0.036(4) 0.024(3) 0.016(3) 0.009(3) 0.010(3) 0.012(3) C12 0.024(4) 0.024(3) 0.026(4) -0.002(3) 0.004(3) -0.001(3) C13 0.018(4) 0.024(3) 0.024(3) -0.001(3) 0.010(3) 0.004(3) C14 0.017(4) 0.029(3) 0.026(4) 0.003(3) 0.010(3) -0.005(3) C15 0.021(4) 0.032(4) 0.040(4) 0.001(3) 0.003(3) -0.002(3) C16 0.024(4) 0.035(4) 0.031(4) -0.006(3) 0.002(3) -0.001(3) C17 0.028(4) 0.025(3) 0.020(3) -0.005(3) 0.011(3) -0.002(3) C18 0.031(4) 0.026(3) 0.023(3) -0.002(3) 0.019(3) -0.010(3) Cd1 0.0242(3) 0.0255(3) 0.0261(3) 0.0056(2) 0.0060(2) 0.0012(2) N1 0.019(3) 0.017(2) 0.026(3) -0.001(2) 0.008(2) -0.003(2) N2 0.018(3) 0.027(3) 0.026(3) -0.004(2) 0.004(2) -0.002(2) N3 0.028(3) 0.031(3) 0.017(3) -0.002(2) 0.001(2) 0.004(2) O1 0.014(2) 0.032(2) 0.022(2) -0.006(2) 0.0031(19) 0.0003(19) O2 0.016(2) 0.024(2) 0.017(2) -0.0011(18) 0.0024(19) -0.0028(18) O3 0.036(3) 0.022(2) 0.021(2) 0.0033(19) 0.004(2) -0.006(2) O4 0.019(2) 0.025(2) 0.020(2) -0.0076(19) 0.0067(19) -0.0067(19) O5 0.023(3) 0.026(2) 0.027(2) -0.009(2) 0.012(2) 0.0012(19) O6 0.0366(19) 0.0349(18) 0.0402(19) -0.0008(10) 0.0088(10) 0.0015(10) O7 0.021(3) 0.040(3) 0.055(4) 0.009(3) -0.009(3) -0.006(2) O9 0.043(3) 0.017(2) 0.022(2) -0.0010(19) 0.011(2) 0.006(2) O10 0.040(3) 0.027(2) 0.015(2) -0.0051(19) 0.009(2) 0.002(2) O11 0.024(3) 0.022(2) 0.015(2) 0.0008(18) 0.0101(19) 0.0020(18) O12 0.021(3) 0.028(2) 0.024(2) -0.003(2) 0.002(2) 0.0047(19) O13 0.021(2) 0.020(2) 0.018(2) 0.0024(18) 0.0047(19) 0.0061(18) O14 0.022(3) 0.038(3) 0.032(3) 0.011(2) 0.012(2) 0.008(2) O15 0.020(3) 0.030(2) 0.024(2) 0.004(2) 0.009(2) 0.0041(19) O16 0.022(3) 0.036(2) 0.015(2) -0.0055(19) 0.0074(19) -0.005(2) O17 0.020(3) 0.040(3) 0.021(2) 0.007(2) 0.014(2) 0.001(2) O18 0.015(2) 0.037(2) 0.012(2) -0.0016(19) 0.0061(18) -0.0045(19) P1 0.0180(9) 0.0240(8) 0.0156(8) -0.0029(7) 0.0015(7) -0.0019(7) P2 0.0187(9) 0.0217(8) 0.0200(8) -0.0015(7) 0.0055(7) 0.0028(7) P3 0.0151(9) 0.0278(8) 0.0158(8) -0.0004(7) 0.0046(7) -0.0055(7) Zn1 0.0161(4) 0.0254(4) 0.0185(4) -0.0004(3) 0.0051(3) -0.0024(3) Zn2 0.0168(4) 0.0244(4) 0.0152(4) -0.0015(3) 0.0039(3) -0.0035(3) Zn3 0.0242(4) 0.0235(4) 0.0154(4) 0.0025(3) 0.0036(3) -0.0034(3) Zn4 0.0160(6) 0.0214(5) 0.0131(5) 0.0001(4) 0.0027(4) -0.0019(4) O8 0.050(2) 0.051(2) 0.053(2) 0.0022(10) 0.0179(11) 0.0007(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 C1 C5 1.528(10) . ? C1 C2 1.531(11) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.530(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.509(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N1 1.472(8) . ? C4 P1 1.826(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.515(10) . ? C5 N1 1.519(8) . ? C5 H5 0.9800 . ? C6 O4 1.265(7) . ? C6 O5 1.269(8) . ? C7 O10 1.256(8) . ? C7 O9 1.270(8) . ? C7 C8 1.518(9) . ? C8 N3 1.517(8) . ? C8 C9 1.541(11) . ? C8 H8 0.9800 . ? C9 C10 1.536(10) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.548(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N3 1.489(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N3 1.501(9) . ? C12 P2 1.824(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 O15 1.245(8) . ? C13 O14 1.270(8) . ? C13 C14 1.536(9) . ? C14 N2 1.496(8) . ? C14 C15 1.573(9) . ? C14 H14 0.9800 . ? C15 C16 1.516(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.503(10) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N2 1.518(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N2 1.493(8) . ? C18 P3 1.823(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? Cd1 O14 2.288(5) . ? Cd1 O8 2.310(9) . ? Cd1 O5 2.328(5) . ? Cd1 O10 2.360(4) . ? Cd1 O6 2.365(7) . ? Cd1 O7 2.443(5) . ? N1 Zn2 2.130(5) . ? N2 Zn1 2.104(6) 3_545 ? N3 Zn3 2.150(5) 4_646 ? O1 P1 1.525(5) . ? O1 Zn1 1.947(4) . ? O2 P1 1.547(4) . ? O2 Zn4 2.102(4) . ? O2 Zn2 2.124(4) . ? O3 P1 1.521(5) . ? O3 Zn3 1.986(5) . ? O4 Zn2 2.041(4) . ? O9 Zn3 2.031(4) 4_646 ? O11 P2 1.546(5) . ? O11 Zn4 2.109(4) 4_646 ? O11 Zn3 2.145(4) 4_646 ? O12 P2 1.530(5) . ? O12 Zn1 1.995(4) 4_646 ? O13 P2 1.525(4) . ? O13 Zn2 1.947(4) 6_575 ? O15 Zn1 2.071(4) 3_545 ? O16 P3 1.543(4) . ? O16 Zn2 1.980(5) 5_777 ? O17 P3 1.519(5) . ? O17 Zn3 1.948(5) 5_777 ? O18 P3 1.544(5) . ? O18 Zn4 2.101(4) 3_545 ? O18 Zn1 2.159(4) 3_545 ? Zn1 O12 1.995(4) 4_656 ? Zn1 O15 2.071(4) 3_455 ? Zn1 N2 2.104(6) 3_455 ? Zn1 O18 2.159(4) 3_455 ? Zn2 O13 1.947(4) 6_576 ? Zn2 O16 1.980(5) 5_777 ? Zn3 O17 1.948(5) 5_777 ? Zn3 O9 2.031(4) 4_656 ? Zn3 O11 2.145(4) 4_656 ? Zn3 N3 2.150(5) 4_656 ? Zn4 O18 2.101(5) 5_777 ? Zn4 O18 2.101(5) 3_455 ? Zn4 O2 2.102(4) 7_677 ? Zn4 O11 2.109(4) 6_576 ? Zn4 O11 2.109(4) 4_656 ? 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 C5 C1 C2 104.7(5) . . ? C5 C1 H1A 110.8 . . ? C2 C1 H1A 110.8 . . ? C5 C1 H1B 110.8 . . ? C2 C1 H1B 110.8 . . ? H1A C1 H1B 108.9 . . ? C3 C2 C1 101.0(6) . . ? C3 C2 H2A 111.6 . . ? C1 C2 H2A 111.6 . . ? C3 C2 H2B 111.6 . . ? C1 C2 H2B 111.6 . . ? H2A C2 H2B 109.4 . . ? N1 C3 C2 103.6(6) . . ? N1 C3 H3A 111.0 . . ? C2 C3 H3A 111.0 . . ? N1 C3 H3B 111.0 . . ? C2 C3 H3B 111.0 . . ? H3A C3 H3B 109.0 . . ? N1 C4 P1 111.2(4) . . ? N1 C4 H4A 109.4 . . ? P1 C4 H4A 109.4 . . ? N1 C4 H4B 109.4 . . ? P1 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C6 C5 N1 109.7(5) . . ? C6 C5 C1 110.1(5) . . ? N1 C5 C1 105.6(6) . . ? C6 C5 H5 110.4 . . ? N1 C5 H5 110.4 . . ? C1 C5 H5 110.4 . . ? O4 C6 O5 121.2(6) . . ? O4 C6 C5 122.0(6) . . ? O5 C6 C5 116.7(5) . . ? O10 C7 O9 122.3(6) . . ? O10 C7 C8 117.2(6) . . ? O9 C7 C8 120.6(6) . . ? N3 C8 C7 109.2(5) . . ? N3 C8 C9 104.9(6) . . ? C7 C8 C9 110.7(6) . . ? N3 C8 H8 110.6 . . ? C7 C8 H8 110.6 . . ? C9 C8 H8 110.6 . . ? C10 C9 C8 105.6(6) . . ? C10 C9 H9A 110.6 . . ? C8 C9 H9A 110.6 . . ? C10 C9 H9B 110.6 . . ? C8 C9 H9B 110.6 . . ? H9A C9 H9B 108.7 . . ? C9 C10 C11 102.0(7) . . ? C9 C10 H10A 111.4 . . ? C11 C10 H10A 111.4 . . ? C9 C10 H10B 111.4 . . ? C11 C10 H10B 111.4 . . ? H10A C10 H10B 109.2 . . ? N3 C11 C10 101.8(5) . . ? N3 C11 H11A 111.4 . . ? C10 C11 H11A 111.4 . . ? N3 C11 H11B 111.4 . . ? C10 C11 H11B 111.4 . . ? H11A C11 H11B 109.3 . . ? N3 C12 P2 110.8(4) . . ? N3 C12 H12A 109.5 . . ? P2 C12 H12A 109.5 . . ? N3 C12 H12B 109.5 . . ? P2 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? O15 C13 O14 125.8(6) . . ? O15 C13 C14 119.4(6) . . ? O14 C13 C14 114.8(6) . . ? N2 C14 C13 110.5(6) . . ? N2 C14 C15 106.9(5) . . ? C13 C14 C15 112.1(5) . . ? N2 C14 H14 109.1 . . ? C13 C14 H14 109.1 . . ? C15 C14 H14 109.1 . . ? C16 C15 C14 103.1(6) . . ? C16 C15 H15A 111.1 . . ? C14 C15 H15A 111.1 . . ? C16 C15 H15B 111.1 . . ? C14 C15 H15B 111.1 . . ? H15A C15 H15B 109.1 . . ? C17 C16 C15 103.6(6) . . ? C17 C16 H16A 111.0 . . ? C15 C16 H16A 111.0 . . ? C17 C16 H16B 111.0 . . ? C15 C16 H16B 111.0 . . ? H16A C16 H16B 109.0 . . ? C16 C17 N2 103.9(5) . . ? C16 C17 H17A 111.0 . . ? N2 C17 H17A 111.0 . . ? C16 C17 H17B 111.0 . . ? N2 C17 H17B 111.0 . . ? H17A C17 H17B 109.0 . . ? N2 C18 P3 110.5(5) . . ? N2 C18 H18A 109.6 . . ? P3 C18 H18A 109.6 . . ? N2 C18 H18B 109.6 . . ? P3 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? O14 Cd1 O8 102.3(2) . . ? O14 Cd1 O5 97.16(17) . . ? O8 Cd1 O5 156.6(2) . . ? O14 Cd1 O10 152.60(16) . . ? O8 Cd1 O10 89.0(2) . . ? O5 Cd1 O10 79.20(17) . . ? O14 Cd1 O6 83.1(2) . . ? O8 Cd1 O6 80.9(3) . . ? O5 Cd1 O6 88.9(2) . . ? O10 Cd1 O6 123.6(2) . . ? O14 Cd1 O7 81.02(18) . . ? O8 Cd1 O7 78.2(2) . . ? O5 Cd1 O7 117.87(17) . . ? O10 Cd1 O7 77.00(16) . . ? O6 Cd1 O7 150.3(2) . . ? C4 N1 C3 111.2(5) . . ? C4 N1 C5 113.8(5) . . ? C3 N1 C5 106.4(5) . . ? C4 N1 Zn2 104.4(4) . . ? C3 N1 Zn2 110.6(4) . . ? C5 N1 Zn2 110.5(4) . . ? C18 N2 C14 111.6(5) . . ? C18 N2 C17 110.1(5) . . ? C14 N2 C17 105.2(5) . . ? C18 N2 Zn1 108.1(4) . 3_545 ? C14 N2 Zn1 111.5(4) . 3_545 ? C17 N2 Zn1 110.3(4) . 3_545 ? C11 N3 C12 113.5(5) . . ? C11 N3 C8 107.1(5) . . ? C12 N3 C8 111.3(5) . . ? C11 N3 Zn3 111.8(4) . 4_646 ? C12 N3 Zn3 103.3(4) . 4_646 ? C8 N3 Zn3 109.9(4) . 4_646 ? P1 O1 Zn1 127.2(3) . . ? P1 O2 Zn4 129.0(2) . . ? P1 O2 Zn2 112.6(2) . . ? Zn4 O2 Zn2 117.13(19) . . ? P1 O3 Zn3 124.9(3) . . ? C6 O4 Zn2 116.2(4) . . ? C6 O5 Cd1 102.6(4) . . ? C7 O9 Zn3 117.2(4) . 4_646 ? C7 O10 Cd1 101.7(4) . . ? P2 O11 Zn4 129.0(3) . 4_646 ? P2 O11 Zn3 111.9(2) . 4_646 ? Zn4 O11 Zn3 117.74(19) 4_646 4_646 ? P2 O12 Zn1 124.6(3) . 4_646 ? P2 O13 Zn2 127.9(2) . 6_575 ? C13 O14 Cd1 119.8(4) . . ? C13 O15 Zn1 117.3(4) . 3_545 ? P3 O16 Zn2 123.7(3) . 5_777 ? P3 O17 Zn3 129.7(3) . 5_777 ? P3 O18 Zn4 127.0(2) . 3_545 ? P3 O18 Zn1 114.3(3) . 3_545 ? Zn4 O18 Zn1 117.8(2) 3_545 3_545 ? O3 P1 O1 112.3(3) . . ? O3 P1 O2 113.6(3) . . ? O1 P1 O2 111.0(3) . . ? O3 P1 C4 106.5(3) . . ? O1 P1 C4 108.5(3) . . ? O2 P1 C4 104.4(3) . . ? O13 P2 O12 112.0(3) . . ? O13 P2 O11 112.7(2) . . ? O12 P2 O11 112.5(2) . . ? O13 P2 C12 107.1(3) . . ? O12 P2 C12 107.4(3) . . ? O11 P2 C12 104.5(3) . . ? O17 P3 O16 111.4(3) . . ? O17 P3 O18 113.5(3) . . ? O16 P3 O18 112.4(3) . . ? O17 P3 C18 109.3(3) . . ? O16 P3 C18 105.5(3) . . ? O18 P3 C18 104.2(3) . . ? O1 Zn1 O12 117.0(2) . 4_656 ? O1 Zn1 O15 95.66(18) . 3_455 ? O12 Zn1 O15 95.27(18) 4_656 3_455 ? O1 Zn1 N2 111.2(2) . 3_455 ? O12 Zn1 N2 131.8(2) 4_656 3_455 ? O15 Zn1 N2 80.5(2) 3_455 3_455 ? O1 Zn1 O18 98.99(17) . 3_455 ? O12 Zn1 O18 90.88(17) 4_656 3_455 ? O15 Zn1 O18 159.44(18) 3_455 3_455 ? N2 Zn1 O18 80.79(19) 3_455 3_455 ? O13 Zn2 O16 114.79(18) 6_576 5_777 ? O13 Zn2 O4 98.78(17) 6_576 . ? O16 Zn2 O4 87.99(18) 5_777 . ? O13 Zn2 O2 101.70(17) 6_576 . ? O16 Zn2 O2 91.70(18) 5_777 . ? O4 Zn2 O2 157.55(16) . . ? O13 Zn2 N1 113.1(2) 6_576 . ? O16 Zn2 N1 131.93(19) 5_777 . ? O4 Zn2 N1 81.42(19) . . ? O2 Zn2 N1 82.15(18) . . ? O17 Zn3 O3 114.99(19) 5_777 . ? O17 Zn3 O9 107.9(2) 5_777 4_656 ? O3 Zn3 O9 87.34(18) . 4_656 ? O17 Zn3 O11 98.52(18) 5_777 4_656 ? O3 Zn3 O11 91.24(18) . 4_656 ? O9 Zn3 O11 151.45(18) 4_656 4_656 ? O17 Zn3 N3 108.5(2) 5_777 4_656 ? O3 Zn3 N3 136.5(2) . 4_656 ? O9 Zn3 N3 80.73(18) 4_656 4_656 ? O11 Zn3 N3 80.80(19) 4_656 4_656 ? O18 Zn4 O18 180.000(1) 5_777 3_455 ? O18 Zn4 O2 92.64(17) 5_777 7_677 ? O18 Zn4 O2 87.36(17) 3_455 7_677 ? O18 Zn4 O2 87.36(17) 5_777 . ? O18 Zn4 O2 92.64(17) 3_455 . ? O2 Zn4 O2 180.000(1) 7_677 . ? O18 Zn4 O11 86.21(17) 5_777 6_576 ? O18 Zn4 O11 93.79(17) 3_455 6_576 ? O2 Zn4 O11 87.16(16) 7_677 6_576 ? O2 Zn4 O11 92.84(16) . 6_576 ? O18 Zn4 O11 93.79(17) 5_777 4_656 ? O18 Zn4 O11 86.21(17) 3_455 4_656 ? O2 Zn4 O11 92.84(16) 7_677 4_656 ? O2 Zn4 O11 87.16(16) . 4_656 ? O11 Zn4 O11 180.0(2) 6_576 4_656 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 39.1(7) . . . . ? C1 C2 C3 N1 -42.5(6) . . . . ? C2 C1 C5 C6 97.3(7) . . . . ? C2 C1 C5 N1 -21.0(7) . . . . ? N1 C5 C6 O4 2.5(9) . . . . ? C1 C5 C6 O4 -113.3(7) . . . . ? N1 C5 C6 O5 -175.5(5) . . . . ? C1 C5 C6 O5 68.7(8) . . . . ? O10 C7 C8 N3 163.2(6) . . . . ? O9 C7 C8 N3 -17.0(10) . . . . ? O10 C7 C8 C9 -81.8(8) . . . . ? O9 C7 C8 C9 98.0(8) . . . . ? N3 C8 C9 C10 9.5(8) . . . . ? C7 C8 C9 C10 -108.1(7) . . . . ? C8 C9 C10 C11 -32.1(8) . . . . ? C9 C10 C11 N3 42.7(7) . . . . ? O15 C13 C14 N2 -10.3(8) . . . . ? O14 C13 C14 N2 170.5(5) . . . . ? O15 C13 C14 C15 -129.4(6) . . . . ? O14 C13 C14 C15 51.4(8) . . . . ? N2 C14 C15 C16 13.8(8) . . . . ? C13 C14 C15 C16 135.0(6) . . . . ? C14 C15 C16 C17 -34.2(7) . . . . ? C15 C16 C17 N2 42.5(6) . . . . ? P1 C4 N1 C3 72.5(6) . . . . ? P1 C4 N1 C5 -167.4(4) . . . . ? P1 C4 N1 Zn2 -46.8(5) . . . . ? C2 C3 N1 C4 154.7(5) . . . . ? C2 C3 N1 C5 30.3(6) . . . . ? C2 C3 N1 Zn2 -89.8(5) . . . . ? C6 C5 N1 C4 112.8(6) . . . . ? C1 C5 N1 C4 -128.5(6) . . . . ? C6 C5 N1 C3 -124.3(6) . . . . ? C1 C5 N1 C3 -5.7(7) . . . . ? C6 C5 N1 Zn2 -4.3(6) . . . . ? C1 C5 N1 Zn2 114.4(5) . . . . ? P3 C18 N2 C14 -167.4(4) . . . . ? P3 C18 N2 C17 76.2(6) . . . . ? P3 C18 N2 Zn1 -44.4(5) . . . 3_545 ? C13 C14 N2 C18 130.2(5) . . . . ? C15 C14 N2 C18 -107.6(6) . . . . ? C13 C14 N2 C17 -110.5(6) . . . . ? C15 C14 N2 C17 11.8(7) . . . . ? C13 C14 N2 Zn1 9.1(6) . . . 3_545 ? C15 C14 N2 Zn1 131.4(5) . . . 3_545 ? C16 C17 N2 C18 86.9(6) . . . . ? C16 C17 N2 C14 -33.4(6) . . . . ? C16 C17 N2 Zn1 -153.8(4) . . . 3_545 ? C10 C11 N3 C12 -161.2(5) . . . . ? C10 C11 N3 C8 -38.0(7) . . . . ? C10 C11 N3 Zn3 82.4(5) . . . 4_646 ? P2 C12 N3 C11 -73.6(6) . . . . ? P2 C12 N3 C8 165.6(4) . . . . ? P2 C12 N3 Zn3 47.7(4) . . . 4_646 ? C7 C8 N3 C11 136.7(6) . . . . ? C9 C8 N3 C11 18.0(7) . . . . ? C7 C8 N3 C12 -98.8(7) . . . . ? C9 C8 N3 C12 142.5(6) . . . . ? C7 C8 N3 Zn3 15.1(7) . . . 4_646 ? C9 C8 N3 Zn3 -103.6(5) . . . 4_646 ? O5 C6 O4 Zn2 178.7(5) . . . . ? C5 C6 O4 Zn2 0.8(8) . . . . ? O4 C6 O5 Cd1 -11.1(7) . . . . ? C5 C6 O5 Cd1 166.9(5) . . . . ? O14 Cd1 O5 C6 78.1(4) . . . . ? O8 Cd1 O5 C6 -135.4(6) . . . . ? O10 Cd1 O5 C6 -74.4(4) . . . . ? O6 Cd1 O5 C6 161.0(4) . . . . ? O7 Cd1 O5 C6 -5.5(4) . . . . ? O10 C7 O9 Zn3 -170.4(5) . . . 4_646 ? C8 C7 O9 Zn3 9.8(9) . . . 4_646 ? O9 C7 O10 Cd1 1.4(8) . . . . ? C8 C7 O10 Cd1 -178.8(5) . . . . ? O14 Cd1 O10 C7 -165.9(4) . . . . ? O8 Cd1 O10 C7 78.5(5) . . . . ? O5 Cd1 O10 C7 -81.2(5) . . . . ? O6 Cd1 O10 C7 0.1(5) . . . . ? O7 Cd1 O10 C7 156.7(5) . . . . ? O15 C13 O14 Cd1 1.2(9) . . . . ? C14 C13 O14 Cd1 -179.6(4) . . . . ? O8 Cd1 O14 C13 10.2(5) . . . . ? O5 Cd1 O14 C13 177.3(5) . . . . ? O10 Cd1 O14 C13 -102.4(6) . . . . ? O6 Cd1 O14 C13 89.3(5) . . . . ? O7 Cd1 O14 C13 -65.5(5) . . . . ? O14 C13 O15 Zn1 -174.8(5) . . . 3_545 ? C14 C13 O15 Zn1 6.1(7) . . . 3_545 ? Zn3 O3 P1 O1 109.4(4) . . . . ? Zn3 O3 P1 O2 -17.6(5) . . . . ? Zn3 O3 P1 C4 -131.9(4) . . . . ? Zn1 O1 P1 O3 -72.0(4) . . . . ? Zn1 O1 P1 O2 56.4(4) . . . . ? Zn1 O1 P1 C4 170.6(3) . . . . ? Zn4 O2 P1 O3 67.6(4) . . . . ? Zn2 O2 P1 O3 -99.0(3) . . . . ? Zn4 O2 P1 O1 -60.1(4) . . . . ? Zn2 O2 P1 O1 133.3(3) . . . . ? Zn4 O2 P1 C4 -176.8(3) . . . . ? Zn2 O2 P1 C4 16.5(3) . . . . ? N1 C4 P1 O3 141.3(5) . . . . ? N1 C4 P1 O1 -97.6(5) . . . . ? N1 C4 P1 O2 20.9(5) . . . . ? Zn2 O13 P2 O12 79.8(4) 6_575 . . . ? Zn2 O13 P2 O11 -48.3(4) 6_575 . . . ? Zn2 O13 P2 C12 -162.6(3) 6_575 . . . ? Zn1 O12 P2 O13 -106.9(3) 4_646 . . . ? Zn1 O12 P2 O11 21.3(4) 4_646 . . . ? Zn1 O12 P2 C12 135.8(3) 4_646 . . . ? Zn4 O11 P2 O13 57.2(4) 4_646 . . . ? Zn3 O11 P2 O13 -136.8(2) 4_646 . . . ? Zn4 O11 P2 O12 -70.7(4) 4_646 . . . ? Zn3 O11 P2 O12 95.3(3) 4_646 . . . ? Zn4 O11 P2 C12 173.1(3) 4_646 . . . ? Zn3 O11 P2 C12 -20.9(3) 4_646 . . . ? N3 C12 P2 O13 101.1(4) . . . . ? N3 C12 P2 O12 -138.3(4) . . . . ? N3 C12 P2 O11 -18.6(5) . . . . ? Zn3 O17 P3 O16 -76.5(4) 5_777 . . . ? Zn3 O17 P3 O18 51.6(4) 5_777 . . . ? Zn3 O17 P3 C18 167.4(3) 5_777 . . . ? Zn2 O16 P3 O17 107.3(3) 5_777 . . . ? Zn2 O16 P3 O18 -21.4(4) 5_777 . . . ? Zn2 O16 P3 C18 -134.3(3) 5_777 . . . ? Zn4 O18 P3 O17 -55.8(4) 3_545 . . . ? Zn1 O18 P3 O17 134.9(3) 3_545 . . . ? Zn4 O18 P3 O16 71.7(4) 3_545 . . . ? Zn1 O18 P3 O16 -97.5(3) 3_545 . . . ? Zn4 O18 P3 C18 -174.5(3) 3_545 . . . ? Zn1 O18 P3 C18 16.2(3) 3_545 . . . ? N2 C18 P3 O17 -103.5(4) . . . . ? N2 C18 P3 O16 136.7(4) . . . . ? N2 C18 P3 O18 18.1(5) . . . . ? P1 O1 Zn1 O12 45.3(4) . . . 4_656 ? P1 O1 Zn1 O15 144.1(3) . . . 3_455 ? P1 O1 Zn1 N2 -133.9(3) . . . 3_455 ? P1 O1 Zn1 O18 -50.4(4) . . . 3_455 ? C6 O4 Zn2 O13 109.6(5) . . . 6_576 ? C6 O4 Zn2 O16 -135.6(5) . . . 5_777 ? C6 O4 Zn2 O2 -46.0(7) . . . . ? C6 O4 Zn2 N1 -2.7(4) . . . . ? P1 O2 Zn2 O13 -147.1(3) . . . 6_576 ? Zn4 O2 Zn2 O13 44.6(3) . . . 6_576 ? P1 O2 Zn2 O16 97.1(3) . . . 5_777 ? Zn4 O2 Zn2 O16 -71.2(2) . . . 5_777 ? P1 O2 Zn2 O4 8.3(6) . . . . ? Zn4 O2 Zn2 O4 -160.0(4) . . . . ? P1 O2 Zn2 N1 -35.0(3) . . . . ? Zn4 O2 Zn2 N1 156.7(3) . . . . ? C4 N1 Zn2 O13 145.1(4) . . . 6_576 ? C3 N1 Zn2 O13 25.4(4) . . . 6_576 ? C5 N1 Zn2 O13 -92.1(4) . . . 6_576 ? C4 N1 Zn2 O16 -39.5(5) . . . 5_777 ? C3 N1 Zn2 O16 -159.2(4) . . . 5_777 ? C5 N1 Zn2 O16 83.2(4) . . . 5_777 ? C4 N1 Zn2 O4 -119.0(4) . . . . ? C3 N1 Zn2 O4 121.3(4) . . . . ? C5 N1 Zn2 O4 3.8(4) . . . . ? C4 N1 Zn2 O2 45.7(4) . . . . ? C3 N1 Zn2 O2 -74.0(4) . . . . ? C5 N1 Zn2 O2 168.4(4) . . . . ? P1 O3 Zn3 O17 61.7(4) . . . 5_777 ? P1 O3 Zn3 O9 170.2(4) . . . 4_656 ? P1 O3 Zn3 O11 -38.3(4) . . . 4_656 ? P1 O3 Zn3 N3 -116.2(4) . . . 4_656 ? P1 O2 Zn4 O18 -125.3(4) . . . 5_777 ? Zn2 O2 Zn4 O18 40.8(2) . . . 5_777 ? P1 O2 Zn4 O18 54.7(4) . . . 3_455 ? Zn2 O2 Zn4 O18 -139.2(2) . . . 3_455 ? P1 O2 Zn4 O2 -43(100) . . . 7_677 ? Zn2 O2 Zn4 O2 123(100) . . . 7_677 ? P1 O2 Zn4 O11 148.6(3) . . . 6_576 ? Zn2 O2 Zn4 O11 -45.3(2) . . . 6_576 ? P1 O2 Zn4 O11 -31.4(3) . . . 4_656 ? Zn2 O2 Zn4 O11 134.7(2) . . . 4_656 ? 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 1 -0.003 -0.002 -0.001 2930.7 -39.3 _platon_squeeze_details ; ? ; _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.230 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.175