# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_f61211c #TrackingRef 'web_deposit_cif_file_0_ZhenxiaChen_1363075380.f61211c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H4 O5 P Zn, (H3 O), 0.5(H2 O)' _chemical_formula_sum 'C7 H8 O6.50 P Zn' _chemical_formula_weight 292.47 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' 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 Tetragonal _symmetry_space_group_name_H-M P4/nnc _symmetry_space_group_name_Hall '-P 4a 2bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 23.986(6) _cell_length_b 23.986(6) _cell_length_c 10.481(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6030(3) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.685 _cell_measurement_theta_max 25.003 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 1.742 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5424 _exptl_absorpt_correction_T_max 0.7801 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23600 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2677 _reflns_number_gt 2257 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1383P)^2^+70.0000P] 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 SHELXL _refine_ls_extinction_coef 0.0016(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2677 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0962 _refine_ls_R_factor_gt 0.0866 _refine_ls_wR_factor_ref 0.2740 _refine_ls_wR_factor_gt 0.2631 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.57915(4) 0.02035(4) 0.61049(10) 0.0392(4) Uani 1 1 d . . . P1 P 0.51073(10) 0.08499(9) 0.4110(2) 0.0395(6) Uani 1 1 d . . . O1 O 0.5520(3) 0.0850(2) 0.5206(6) 0.0487(15) Uani 1 1 d . . . O2 O 0.5430(3) 0.0792(3) 0.2875(7) 0.0629(19) Uani 1 1 d . . . O3 O 0.4659(3) 0.0428(3) 0.4260(9) 0.071(2) Uani 1 1 d . . . O4 O 0.5652(4) 0.3029(3) 0.4151(12) 0.107(4) Uani 1 1 d . . . O5 O 0.4876(3) 0.3493(3) 0.4360(8) 0.067(2) Uani 1 1 d . . . C1 C 0.4764(3) 0.1520(3) 0.4114(8) 0.0379(18) Uani 1 1 d . . . C2 C 0.4191(4) 0.1554(4) 0.4090(12) 0.063(3) Uani 1 1 d . . . H2A H 0.3980 0.1229 0.4052 0.076 Uiso 1 1 calc R . . C3 C 0.3927(5) 0.2062(5) 0.4121(15) 0.088(5) Uani 1 1 d . . . H3A H 0.3540 0.2080 0.4082 0.106 Uiso 1 1 calc R . . C4 C 0.4238(5) 0.2544(4) 0.4211(13) 0.071(3) Uani 1 1 d . . . H4A H 0.4058 0.2886 0.4277 0.086 Uiso 1 1 calc R . . C5 C 0.4805(4) 0.2526(4) 0.4203(8) 0.046(2) Uani 1 1 d . . . C6 C 0.5066(4) 0.2002(3) 0.4161(8) 0.042(2) Uani 1 1 d . . . H6A H 0.5454 0.1983 0.4165 0.051 Uiso 1 1 calc R . . C7 C 0.5142(5) 0.3054(4) 0.4229(11) 0.059(3) Uani 1 1 d . . . O6 O 0.4329(12) 0.0671(12) 0.7500 0.267(16) Uiso 1 2 d S . . O7 O 0.6597(17) 0.1263(14) 0.319(3) 0.356(17) Uiso 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 0.0306(6) 0.0387(6) 0.0482(7) -0.0006(4) -0.0043(4) -0.0037(4) P1 0.0436(12) 0.0297(11) 0.0451(13) -0.0047(9) -0.0104(9) -0.0038(9) O1 0.057(4) 0.035(3) 0.055(4) -0.001(3) -0.016(3) -0.007(3) O2 0.072(5) 0.066(5) 0.051(4) -0.013(3) -0.005(4) 0.022(4) O3 0.063(4) 0.033(3) 0.117(6) 0.012(4) -0.027(4) -0.019(3) O4 0.076(6) 0.044(4) 0.200(12) -0.025(6) 0.022(7) -0.015(4) O5 0.085(5) 0.030(3) 0.086(5) -0.003(3) 0.021(4) -0.002(3) C1 0.042(4) 0.034(4) 0.037(4) -0.005(3) 0.001(3) -0.001(3) C2 0.047(5) 0.040(5) 0.102(9) 0.013(5) 0.000(5) -0.005(4) C3 0.046(6) 0.058(7) 0.162(15) -0.009(8) 0.008(7) 0.004(5) C4 0.065(7) 0.039(5) 0.109(9) -0.003(6) 0.005(6) 0.014(5) C5 0.059(6) 0.035(4) 0.044(5) 0.001(4) 0.002(4) 0.000(4) C6 0.041(5) 0.035(4) 0.051(5) -0.005(4) -0.004(4) -0.002(3) C7 0.074(7) 0.035(5) 0.069(7) 0.000(5) 0.005(6) -0.004(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 O3 1.899(6) 9_656 ? Zn1 O1 1.928(6) . ? Zn1 O2 1.933(7) 16_656 ? Zn1 O5 1.949(7) 12_656 ? P1 O3 1.485(7) . ? P1 O2 1.514(8) . ? P1 O1 1.516(6) . ? P1 C1 1.805(8) . ? O2 Zn1 1.933(7) 16_655 ? O3 Zn1 1.899(6) 9_656 ? O4 C7 1.229(14) . ? O5 C7 1.239(12) . ? O5 Zn1 1.949(7) 11_666 ? C1 C6 1.367(12) . ? C1 C2 1.378(13) . ? C2 C3 1.373(15) . ? C2 H2A 0.9300 . ? C3 C4 1.381(16) . ? C3 H3A 0.9300 . ? C4 C5 1.360(14) . ? C4 H4A 0.9300 . ? C5 C6 1.405(12) . ? C5 C7 1.501(13) . ? C6 H6A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O1 110.5(3) 9_656 . ? O3 Zn1 O2 114.7(4) 9_656 16_656 ? O1 Zn1 O2 104.1(3) . 16_656 ? O3 Zn1 O5 97.5(3) 9_656 12_656 ? O1 Zn1 O5 119.9(3) . 12_656 ? O2 Zn1 O5 110.6(3) 16_656 12_656 ? O3 P1 O2 113.5(5) . . ? O3 P1 O1 113.1(4) . . ? O2 P1 O1 108.3(4) . . ? O3 P1 C1 106.0(4) . . ? O2 P1 C1 108.5(4) . . ? O1 P1 C1 107.2(4) . . ? P1 O1 Zn1 126.2(3) . . ? P1 O2 Zn1 132.6(5) . 16_655 ? P1 O3 Zn1 159.1(7) . 9_656 ? C7 O5 Zn1 121.0(7) . 11_666 ? C6 C1 C2 118.7(8) . . ? C6 C1 P1 120.8(7) . . ? C2 C1 P1 120.6(7) . . ? C3 C2 C1 120.9(10) . . ? C3 C2 H2A 119.6 . . ? C1 C2 H2A 119.6 . . ? C2 C3 C4 119.7(10) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C5 C4 C3 120.9(10) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 118.4(9) . . ? C4 C5 C7 120.7(9) . . ? C6 C5 C7 120.9(9) . . ? C1 C6 C5 121.4(8) . . ? C1 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? O4 C7 O5 124.1(10) . . ? O4 C7 C5 119.7(9) . . ? O5 C7 C5 116.2(10) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.232 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.207 _database_code_depnum_ccdc_archive 'CCDC 928844' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_f70117as #TrackingRef 'web_deposit_cif_file_1_ZhenxiaChen_1363075380.f70117as.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H10 O11 P2 Zn2.50' _chemical_formula_sum 'C14 H10 O11 P2 Zn2.50' _chemical_formula_weight 579.59 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' 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 Cubic _symmetry_space_group_name_H-M Pn-3n _symmetry_space_group_name_Hall '-P 4a 2bc 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x, y' 'z, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, x, -y+1/2' 'y, z, x' '-y+1/2, z, -x+1/2' 'y, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' 'x, z, -y+1/2' '-x+1/2, z, y' '-x+1/2, -z+1/2, -y+1/2' 'x, -z+1/2, y' 'z, y, -x+1/2' 'z, -y+1/2, x' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-z, -x, -y' '-z, x-1/2, y-1/2' 'z-1/2, x-1/2, -y' 'z-1/2, -x, y-1/2' '-y, -z, -x' 'y-1/2, -z, x-1/2' '-y, z-1/2, x-1/2' 'y-1/2, z-1/2, -x' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' '-x, -z, y-1/2' 'x-1/2, -z, -y' 'x-1/2, z-1/2, y-1/2' '-x, z-1/2, -y' '-z, -y, x-1/2' '-z, y-1/2, -x' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' _cell_length_a 32.652(5) _cell_length_b 32.652(5) _cell_length_c 32.652(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 34811(9) _cell_formula_units_Z 48 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 966 _cell_measurement_theta_min 2.334 _cell_measurement_theta_max 22.381 _exptl_crystal_description cubic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13776 _exptl_absorpt_coefficient_mu 2.205 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7332 _exptl_absorpt_correction_T_max 0.8096 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 122161 _diffrn_reflns_av_R_equivalents 0.1027 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 0.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5138 _reflns_number_gt 3780 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0781P)^2^+51.8819P] 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 5138 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0896 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1473 _refine_ls_wR_factor_gt 0.1345 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.308222(18) 0.637519(19) 0.025702(18) 0.02053(19) Uani 1 1 d . . . Zn2 Zn 0.137926(19) 0.584035(18) -0.016926(18) 0.02090(18) Uani 1 1 d . . . Zn3 Zn 0.2500 0.40039(3) 0.09961(3) 0.1044(7) Uani 1 2 d S . . P1 P 0.20419(4) 0.63841(4) 0.02681(4) 0.0195(3) Uani 1 1 d . . . P2 P 0.13521(4) 0.49524(4) -0.05876(4) 0.0217(3) Uani 1 1 d . . . O1 O 0.08417(12) 0.64483(15) 0.17848(12) 0.0454(12) Uani 1 1 d . . . O2 O 0.06999(11) 0.64344(14) 0.11223(12) 0.0374(11) Uani 1 1 d . . . O3 O 0.24992(11) 0.63893(12) 0.02229(11) 0.0340(10) Uani 1 1 d . . . O4 O 0.18447(11) 0.67393(11) 0.00481(12) 0.0318(10) Uani 1 1 d . . . O5 O 0.18623(11) 0.59745(12) 0.01397(12) 0.0313(10) Uani 1 1 d . . . O6 O 0.20613(19) 0.4146(2) 0.0614(2) 0.092(2) Uani 1 1 d . . . O7 O 0.1725(3) 0.3582(2) 0.0744(2) 0.129(3) Uani 1 1 d . . . O8 O 0.14134(13) 0.52677(12) -0.02519(12) 0.0376(11) Uani 1 1 d . . . O9 O 0.17394(12) 0.49114(13) -0.08365(12) 0.0380(11) Uani 1 1 d . . . O10 O 0.09788(13) 0.50428(12) -0.08485(12) 0.0364(10) Uani 1 1 d . . . O11 O 0.2777(5) 0.3478(5) 0.0602(6) 0.127(6) Uiso 0.50 1 d P . . O11' O 0.2712(7) 0.3452(8) 0.1003(8) 0.195(9) Uiso 0.50 1 d P . . C1 C 0.09407(17) 0.64503(18) 0.14158(18) 0.0303(14) Uani 1 1 d . . . C2 C 0.13882(17) 0.6467(2) 0.13134(17) 0.0396(16) Uani 1 1 d . . . C3 C 0.15123(16) 0.64307(17) 0.09166(17) 0.0279(13) Uani 1 1 d . . . H5A H 0.1315 0.6396 0.0714 0.013(13) Uiso 1 1 calc R . . C4 C 0.19169(17) 0.64440(18) 0.08034(18) 0.0324(14) Uani 1 1 d . . . C5 C 0.2207(2) 0.6514(3) 0.1106(2) 0.075(3) Uani 1 1 d . . . H6A H 0.2483 0.6538 0.1037 0.08(3) Uiso 1 1 calc R . . C6 C 0.2086(2) 0.6549(4) 0.1509(2) 0.125(5) Uani 1 1 d . . . H12A H 0.2282 0.6587 0.1712 0.12(4) Uiso 1 1 calc R . . C7 C 0.1683(2) 0.6527(3) 0.1612(2) 0.089(4) Uani 1 1 d . . . H10A H 0.1605 0.6553 0.1884 0.08(3) Uiso 1 1 calc R . . C8 C 0.1760(3) 0.3911(3) 0.0558(3) 0.072(3) Uani 1 1 d . . . C9 C 0.1470(2) 0.4018(2) 0.0228(2) 0.053(2) Uani 1 1 d . . . C10 C 0.15273(18) 0.43692(19) 0.00036(19) 0.0351(15) Uani 1 1 d . . . H8A H 0.1746 0.4540 0.0067 0.033(16) Uiso 1 1 calc R . . C11 C 0.12643(18) 0.44768(17) -0.03179(17) 0.0292(14) Uani 1 1 d . . . C12 C 0.0938(2) 0.4223(2) -0.0396(2) 0.066(3) Uani 1 1 d . . . H7A H 0.0760 0.4287 -0.0608 0.046(19) Uiso 1 1 calc R . . C13 C 0.0870(3) 0.3882(3) -0.0173(3) 0.105(4) Uani 1 1 d . . . H13A H 0.0648 0.3715 -0.0236 0.14(4) Uiso 1 1 calc R . . C14 C 0.1128(3) 0.3780(3) 0.0149(3) 0.086(3) Uani 1 1 d . . . H14A H 0.1071 0.3552 0.0311 0.07(2) 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 0.0149(3) 0.0262(4) 0.0205(3) 0.0005(3) -0.0015(2) 0.0000(3) Zn2 0.0251(4) 0.0183(3) 0.0193(3) -0.0003(2) -0.0005(3) 0.0004(3) Zn3 0.0727(11) 0.1203(10) 0.1203(10) 0.0770(12) -0.0393(9) -0.0393(9) P1 0.0127(7) 0.0254(8) 0.0203(7) -0.0013(6) 0.0002(5) -0.0012(6) P2 0.0289(8) 0.0189(7) 0.0173(7) -0.0021(6) -0.0014(6) -0.0015(6) O1 0.021(2) 0.091(4) 0.024(2) -0.005(2) 0.0039(18) -0.005(2) O2 0.014(2) 0.072(3) 0.026(2) -0.008(2) -0.0040(17) -0.002(2) O3 0.0150(19) 0.055(3) 0.032(2) -0.0020(19) 0.0015(17) 0.002(2) O4 0.027(2) 0.027(2) 0.042(3) 0.0028(19) -0.0107(19) -0.0010(17) O5 0.026(2) 0.029(2) 0.038(2) 0.0019(18) -0.0102(18) -0.0016(17) O6 0.073(4) 0.097(5) 0.105(5) 0.045(4) -0.055(4) -0.021(4) O7 0.169(8) 0.096(5) 0.122(6) 0.077(5) -0.056(6) -0.036(5) O8 0.068(3) 0.020(2) 0.025(2) -0.0018(16) -0.011(2) 0.001(2) O9 0.034(2) 0.051(3) 0.028(2) -0.005(2) 0.0117(19) -0.013(2) O10 0.046(3) 0.034(2) 0.029(2) -0.0072(19) -0.0088(19) 0.013(2) C1 0.024(3) 0.040(4) 0.027(3) -0.008(3) 0.004(3) -0.008(3) C2 0.021(3) 0.077(5) 0.022(3) -0.007(3) 0.002(3) -0.004(3) C3 0.016(3) 0.041(4) 0.027(3) -0.005(3) -0.006(2) -0.002(2) C4 0.024(3) 0.042(4) 0.031(3) -0.003(3) 0.001(3) -0.006(3) C5 0.018(4) 0.172(10) 0.034(4) -0.017(5) 0.003(3) -0.014(5) C6 0.024(4) 0.315(17) 0.034(5) -0.042(7) -0.009(4) -0.022(7) C7 0.031(4) 0.221(12) 0.015(4) -0.017(5) 0.003(3) -0.023(6) C8 0.076(6) 0.070(6) 0.071(6) 0.039(5) -0.013(5) -0.015(5) C9 0.062(5) 0.038(4) 0.060(5) 0.019(3) -0.015(4) -0.010(4) C10 0.028(3) 0.036(4) 0.041(4) 0.007(3) -0.005(3) -0.005(3) C11 0.037(4) 0.024(3) 0.027(3) 0.002(2) -0.001(3) -0.008(3) C12 0.067(5) 0.067(5) 0.064(5) 0.029(4) -0.032(4) -0.044(4) C13 0.112(8) 0.083(7) 0.119(9) 0.063(6) -0.066(7) -0.072(7) C14 0.104(8) 0.062(6) 0.093(7) 0.049(5) -0.036(6) -0.038(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 O3 1.907(4) . ? Zn1 O4 1.919(4) 39_665 ? Zn1 O9 1.932(4) 19 ? Zn1 O1 1.972(4) 23 ? Zn2 O8 1.893(4) . ? Zn2 O10 1.920(4) 30_565 ? Zn2 O5 1.923(4) . ? Zn2 O2 1.970(4) 36_565 ? Zn3 O11' 1.93(2) . ? Zn3 O11' 1.93(2) 19 ? Zn3 O6 1.954(5) . ? Zn3 O6 1.954(5) 19 ? Zn3 O11 2.329(17) 19 ? Zn3 O11 2.329(17) . ? P1 O3 1.500(4) . ? P1 O4 1.509(4) . ? P1 O5 1.519(4) . ? P1 C4 1.805(6) . ? P2 O9 1.509(4) . ? P2 O10 1.516(4) . ? P2 O8 1.517(4) . ? P2 C11 1.808(6) . ? O1 C1 1.247(7) . ? O1 Zn1 1.972(4) 21 ? O2 C1 1.241(7) . ? O2 Zn2 1.970(4) 30_565 ? O4 Zn1 1.919(4) 40_565 ? O6 C8 1.260(9) . ? O7 C8 1.240(9) . ? O9 Zn1 1.933(4) 19 ? O10 Zn2 1.920(4) 36_565 ? O11 O11' 1.33(2) . ? C1 C2 1.500(8) . ? C2 C3 1.363(8) . ? C2 C7 1.383(8) . ? C3 C4 1.372(8) . ? C3 H5A 0.9300 . ? C4 C5 1.389(9) . ? C5 C6 1.378(10) . ? C5 H6A 0.9300 . ? C6 C7 1.361(10) . ? C6 H12A 0.9300 . ? C7 H10A 0.9300 . ? C8 C9 1.478(10) . ? C9 C10 1.372(8) . ? C9 C14 1.387(11) . ? C10 C11 1.401(8) . ? C10 H8A 0.9300 . ? C11 C12 1.374(8) . ? C12 C13 1.347(10) . ? C12 H7A 0.9300 . ? C13 C14 1.389(11) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O4 104.68(17) . 39_665 ? O3 Zn1 O9 107.82(17) . 19 ? O4 Zn1 O9 119.20(18) 39_665 19 ? O3 Zn1 O1 105.86(16) . 23 ? O4 Zn1 O1 109.81(19) 39_665 23 ? O9 Zn1 O1 108.62(19) 19 23 ? O8 Zn2 O10 109.70(19) . 30_565 ? O8 Zn2 O5 104.57(17) . . ? O10 Zn2 O5 119.85(18) 30_565 . ? O8 Zn2 O2 109.32(16) . 36_565 ? O10 Zn2 O2 106.83(17) 30_565 36_565 ? O5 Zn2 O2 106.25(17) . 36_565 ? O11' Zn3 O11' 96.1(16) . 19 ? O11' Zn3 O6 119.4(8) . . ? O11' Zn3 O6 109.6(8) 19 . ? O11' Zn3 O6 109.6(8) . 19 ? O11' Zn3 O6 119.4(8) 19 19 ? O6 Zn3 O6 103.6(4) . 19 ? O11' Zn3 O11 130.3(10) . 19 ? O11' Zn3 O11 34.8(7) 19 19 ? O6 Zn3 O11 93.1(5) . 19 ? O6 Zn3 O11 96.1(5) 19 19 ? O11' Zn3 O11 34.8(7) . . ? O11' Zn3 O11 130.3(10) 19 . ? O6 Zn3 O11 96.1(5) . . ? O6 Zn3 O11 93.1(5) 19 . ? O11 Zn3 O11 165.0(9) 19 . ? O3 P1 O4 111.7(2) . . ? O3 P1 O5 111.5(2) . . ? O4 P1 O5 112.4(2) . . ? O3 P1 C4 108.6(2) . . ? O4 P1 C4 106.3(3) . . ? O5 P1 C4 106.0(3) . . ? O9 P2 O10 112.9(2) . . ? O9 P2 O8 109.8(2) . . ? O10 P2 O8 112.3(2) . . ? O9 P2 C11 108.6(3) . . ? O10 P2 C11 108.3(3) . . ? O8 P2 C11 104.6(2) . . ? C1 O1 Zn1 117.7(4) . 21 ? C1 O2 Zn2 157.2(4) . 30_565 ? P1 O3 Zn1 170.8(3) . . ? P1 O4 Zn1 145.3(2) . 40_565 ? P1 O5 Zn2 131.5(2) . . ? C8 O6 Zn3 121.4(5) . . ? P2 O8 Zn2 140.0(2) . . ? P2 O9 Zn1 140.2(3) . 19 ? P2 O10 Zn2 128.8(2) . 36_565 ? O11' O11 Zn3 56.0(13) . . ? O11 O11' Zn3 89.1(16) . . ? O2 C1 O1 125.6(5) . . ? O2 C1 C2 116.5(5) . . ? O1 C1 C2 117.9(5) . . ? C3 C2 C7 118.3(6) . . ? C3 C2 C1 119.9(5) . . ? C7 C2 C1 121.8(5) . . ? C2 C3 C4 122.7(5) . . ? C2 C3 H5A 118.7 . . ? C4 C3 H5A 118.7 . . ? C3 C4 C5 118.1(6) . . ? C3 C4 P1 118.4(4) . . ? C5 C4 P1 123.5(5) . . ? C6 C5 C4 119.8(6) . . ? C6 C5 H6A 120.1 . . ? C4 C5 H6A 120.1 . . ? C7 C6 C5 120.5(7) . . ? C7 C6 H12A 119.7 . . ? C5 C6 H12A 119.7 . . ? C6 C7 C2 120.5(6) . . ? C6 C7 H10A 119.7 . . ? C2 C7 H10A 119.7 . . ? O7 C8 O6 121.9(8) . . ? O7 C8 C9 120.2(8) . . ? O6 C8 C9 117.6(7) . . ? C10 C9 C14 118.7(7) . . ? C10 C9 C8 120.0(7) . . ? C14 C9 C8 121.3(7) . . ? C9 C10 C11 121.7(6) . . ? C9 C10 H8A 119.1 . . ? C11 C10 H8A 119.1 . . ? C12 C11 C10 117.5(6) . . ? C12 C11 P2 123.5(5) . . ? C10 C11 P2 118.9(4) . . ? C13 C12 C11 121.8(7) . . ? C13 C12 H7A 119.1 . . ? C11 C12 H7A 119.1 . . ? C12 C13 C14 120.5(8) . . ? C12 C13 H13A 119.7 . . ? C14 C13 H13A 119.7 . . ? C9 C14 C13 119.6(7) . . ? C9 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.242 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.108 # SQUEEZE RESULTS (APPEND TO CIF) 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 0.000 0.000 0.000 130.0 32.9 2 0.223 0.001 0.003 14451.7 2761.3 3 0.500 0.000 0.000 130.0 31.5 4 0.500 0.000 0.500 130.0 31.5 5 0.000 0.000 0.500 130.0 31.3 6 0.000 0.500 0.000 130.0 31.9 7 0.500 0.500 0.000 130.0 31.0 8 0.000 0.500 0.500 130.0 31.0 9 0.500 0.500 0.500 130.0 32.0 _platon_squeeze_details ; The disordered solvents within the void were not crystallographically well defined. The SQUEEZE routine of the program PLATON was used in order to eliminate the contribution of disordered solvents molecules, thereby a final model based only on the ordered part of the crystal structure was obtained. The SQUEEZE routine suggested that a total potential solvent area volume of 15497.6 Ang^3^, and a void electron population of 3014 per cell. The solvent we used in the synthesis is DMF and water. And there might be some dimethylamine decomposed by DMF. So the amount of the disordered solvent was about 62 per cell suggested by electron count. The overall formula should be Zn2.5(3-pbc)2(H2O).(H2N(CH3)2).2(H2O), considering the contribution of solvent. Refinement after the SQUEEZE routine gave significantly improved R values. [R values before SQUEEZE] R1 = 0.1336, wR2 = 0.3245, GooF = S = 1.167 for all data ; _database_code_depnum_ccdc_archive 'CCDC 928845'