# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Anthony Cheetham' 'S. Neeraj' 'C. N. R. Rao' _publ_contact_author_name 'Prof Anthony Cheetham' _publ_contact_author_address ; Materials Research Laboratory University of California # 3004A, Santa Barbara CA 93106-5121 UNITED STATES OF AMERICA ; _publ_contact_author_email CHEETHAM@MRL.UCSB.EDU _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; Open-Framework Zinc and Cobalt Phosphates Synthesized by the Tributylphosphate Route ; data_COMPOUND_I _database_code_depnum_ccdc_archive 'CCDC 220185' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Zinc phosphate' _chemical_melting_point ? _chemical_formula_moiety [C6N2H18][Zn(HPO4)2] _chemical_formula_sum 'C3 H14 N2 O11 P2 Zn' _chemical_formula_weight 381.47 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' 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.0797(18) _cell_length_b 14.555(3) _cell_length_c 28.575(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3360.4(13) _cell_formula_units_Z 8 _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 ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 1.695 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 18685 _diffrn_reflns_av_R_equivalents 0.2649 _diffrn_reflns_av_sigmaI/netI 0.1767 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 28.84 _reflns_number_total 3986 _reflns_number_gt 2036 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1871P)^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 SHELXL _refine_ls_extinction_coef 0.0092(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3986 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1858 _refine_ls_R_factor_gt 0.1024 _refine_ls_wR_factor_ref 0.3310 _refine_ls_wR_factor_gt 0.2678 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.098 _refine_ls_shift/su_mean 0.007 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 0.23085(15) 0.52432(6) 0.01759(4) 0.0317(4) Uani 1 1 d . . . P1 P 0.0266(3) 0.59011(14) -0.07055(8) 0.0318(6) Uani 1 1 d . . . P2 P 0.4273(3) 0.40448(13) -0.05602(9) 0.0320(6) Uani 1 1 d . . . O1 O 0.1016(11) 0.4860(4) 0.0704(2) 0.0432(19) Uani 1 1 d . . . O2 O 0.3092(10) 0.4182(4) -0.0156(2) 0.0395(17) Uani 1 1 d . . . O3 O 0.3955(8) 0.6112(4) 0.0390(2) 0.0354(15) Uani 1 1 d . . . O4 O 0.0987(9) 0.6061(4) -0.0220(2) 0.0400(17) Uani 1 1 d . . . O5 O 0.1625(10) 0.5717(4) -0.1065(2) 0.0466(19) Uani 1 1 d . . . O6 O -0.0631(9) 0.6800(4) -0.0850(2) 0.0419(18) Uani 1 1 d . . . H14 H 0.0023 0.7230 -0.0839 0.063 Uiso 1 1 calc R . . O7 O 0.4260(10) 0.4886(4) -0.0884(3) 0.047(2) Uani 1 1 d . . . H13 H 0.3312 0.5080 -0.0909 0.071 Uiso 1 1 calc R . . O8 O 0.3684(9) 0.3182(4) -0.0826(2) 0.0424(18) Uani 1 1 d . . . N1 N -0.145(3) 0.2441(13) -0.1404(6) 0.162(8) Uani 1 1 d . . . H12 H -0.2094 0.1983 -0.1298 0.194 Uiso 1 1 calc R . . H11 H -0.0716 0.2198 -0.1607 0.194 Uiso 1 1 calc R . . N2 N 0.0857(12) 0.2580(5) -0.0273(3) 0.043(2) Uani 1 1 d . . . H10 H 0.1071 0.2153 -0.0058 0.064 Uiso 1 1 calc R . . H9 H 0.0283 0.3035 -0.0143 0.064 Uiso 1 1 calc R . . H8 H 0.1804 0.2798 -0.0386 0.064 Uiso 1 1 calc R . . C1 C -0.011(2) 0.2173(8) -0.0653(5) 0.071(4) Uani 1 1 d . . . H7 H 0.0526 0.1683 -0.0797 0.086 Uiso 1 1 calc R . . H6 H -0.1114 0.1908 -0.0526 0.086 Uiso 1 1 calc R . . C2 C -0.054(2) 0.2853(8) -0.1007(6) 0.076(4) Uani 1 1 d . . . H5 H 0.0465 0.3140 -0.1123 0.091 Uiso 1 1 calc R . . H4 H -0.1217 0.3328 -0.0866 0.091 Uiso 1 1 calc R . . C3 C -0.255(6) 0.317(2) -0.1664(13) 0.30(3) Uani 1 1 d . . . H3 H -0.3122 0.2885 -0.1918 0.454 Uiso 1 1 calc R . . H2 H -0.1856 0.3657 -0.1783 0.454 Uiso 1 1 calc R . . H1 H -0.3337 0.3428 -0.1448 0.454 Uiso 1 1 calc R . . O100 O 0.674(3) 0.5655(17) -0.1471(9) 0.240(11) Uani 1 1 d . . . O300 O 0.148(3) 0.6334(18) -0.1965(10) 0.263(11) Uiso 1 1 d . . . O200 O 0.320(4) 0.325(2) -0.1810(12) 0.308(15) 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 0.0377(8) 0.0195(5) 0.0380(7) 0.0017(4) -0.0001(5) -0.0003(4) P1 0.0395(15) 0.0212(10) 0.0347(13) 0.0027(9) 0.0011(11) 0.0002(10) P2 0.0371(15) 0.0164(10) 0.0424(13) -0.0018(9) -0.0023(11) -0.0005(9) O1 0.067(6) 0.026(3) 0.037(4) -0.001(3) 0.014(4) -0.012(3) O2 0.047(5) 0.024(3) 0.048(4) -0.002(3) 0.009(3) -0.005(3) O3 0.033(4) 0.019(3) 0.055(4) 0.000(3) -0.004(3) 0.000(3) O4 0.053(5) 0.025(3) 0.041(4) 0.003(3) -0.011(3) 0.005(3) O5 0.048(5) 0.043(4) 0.049(4) 0.012(3) 0.013(4) 0.010(3) O6 0.048(5) 0.023(3) 0.055(4) 0.009(3) -0.014(4) 0.002(3) O7 0.050(5) 0.031(3) 0.061(5) 0.017(3) 0.013(4) 0.007(3) O8 0.043(5) 0.029(3) 0.054(4) -0.012(3) -0.012(3) -0.002(3) N1 0.21(2) 0.171(18) 0.104(13) -0.032(13) -0.013(16) 0.054(17) N2 0.040(6) 0.031(4) 0.057(5) 0.007(4) -0.007(4) -0.003(4) C1 0.100(13) 0.042(6) 0.072(9) 0.001(6) -0.009(8) -0.009(7) C2 0.070(10) 0.051(7) 0.107(11) 0.001(7) -0.024(9) 0.004(7) C3 0.43(6) 0.20(3) 0.28(4) 0.17(3) 0.23(4) 0.15(4) O100 0.20(2) 0.27(2) 0.24(2) -0.10(2) -0.02(2) -0.08(2) _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 O1 1.918(7) . ? Zn1 O2 1.920(6) . ? Zn1 O3 1.934(6) . ? Zn1 O4 1.958(6) . ? P1 O1 1.516(7) 5_565 ? P1 O4 1.524(7) . ? P1 O5 1.528(8) . ? P1 O6 1.552(6) . ? P2 O2 1.511(7) . ? P2 O3 1.529(7) 5_665 ? P2 O7 1.535(6) . ? P2 O8 1.542(6) . ? O1 P1 1.516(7) 5_565 ? O3 P2 1.529(7) 5_665 ? O6 H14 0.8200 . ? O7 H13 0.8200 . ? N1 C2 1.48(2) . ? N1 C3 1.58(3) . ? N1 H12 0.9000 . ? N1 H11 0.9000 . ? N2 C1 1.461(16) . ? N2 H10 0.8900 . ? N2 H9 0.8900 . ? N2 H8 0.8900 . ? C1 C2 1.458(17) . ? C1 H7 0.9700 . ? C1 H6 0.9700 . ? C2 H5 0.9700 . ? C2 H4 0.9700 . ? C3 H3 0.9600 . ? C3 H2 0.9600 . ? C3 H1 0.9600 . ? 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 O1 Zn1 O2 109.5(3) . . ? O1 Zn1 O3 108.4(3) . . ? O2 Zn1 O3 117.1(3) . . ? O1 Zn1 O4 109.5(3) . . ? O2 Zn1 O4 112.6(3) . . ? O3 Zn1 O4 99.2(3) . . ? O1 P1 O4 111.7(4) 5_565 . ? O1 P1 O5 111.4(4) 5_565 . ? O4 P1 O5 111.4(4) . . ? O1 P1 O6 107.3(4) 5_565 . ? O4 P1 O6 107.0(4) . . ? O5 P1 O6 107.7(4) . . ? O2 P2 O3 111.6(4) . 5_665 ? O2 P2 O7 110.6(4) . . ? O3 P2 O7 108.5(4) 5_665 . ? O2 P2 O8 106.8(4) . . ? O3 P2 O8 108.9(4) 5_665 . ? O7 P2 O8 110.5(4) . . ? P1 O1 Zn1 125.9(4) 5_565 . ? P2 O2 Zn1 133.8(4) . . ? P2 O3 Zn1 130.3(3) 5_665 . ? P1 O4 Zn1 129.9(4) . . ? P1 O6 H14 109.5 . . ? P2 O7 H13 109.5 . . ? C2 N1 C3 112(2) . . ? C2 N1 H12 109.3 . . ? C3 N1 H12 109.2 . . ? C2 N1 H11 109.3 . . ? C3 N1 H11 109.4 . . ? H12 N1 H11 108.0 . . ? C1 N2 H10 109.5 . . ? C1 N2 H9 109.4 . . ? H10 N2 H9 109.5 . . ? C1 N2 H8 109.5 . . ? H10 N2 H8 109.5 . . ? H9 N2 H8 109.5 . . ? C2 C1 N2 111.6(10) . . ? C2 C1 H7 109.3 . . ? N2 C1 H7 109.3 . . ? C2 C1 H6 109.3 . . ? N2 C1 H6 109.3 . . ? H7 C1 H6 107.9 . . ? C1 C2 N1 112.1(12) . . ? C1 C2 H5 109.2 . . ? N1 C2 H5 109.2 . . ? C1 C2 H4 109.2 . . ? N1 C2 H4 109.2 . . ? H5 C2 H4 107.9 . . ? N1 C3 H3 109.6 . . ? N1 C3 H2 109.4 . . ? H3 C3 H2 109.5 . . ? N1 C3 H1 109.5 . . ? H3 C3 H1 109.5 . . ? H2 C3 H1 109.5 . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 28.84 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 1.373 _refine_diff_density_min -2.033 _refine_diff_density_rms 0.393 #===END OF COMPOUND I data_COMPOUND_II _database_code_depnum_ccdc_archive 'CCDC 220186' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Zinc Phosphate' _chemical_melting_point ? _chemical_formula_moiety [C4N2H14][Zn5(PO4)4(H2O)] _chemical_formula_sum 'C4 H16 N2 O17 P4 Zn5' _chemical_formula_weight 814.92 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 ? _symmetry_space_group_name_H-M ? 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' _cell_length_a 20.7603(12) _cell_length_b 5.2207(3) _cell_length_c 17.9147(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1941.65(19) _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 ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.788 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 6.507 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 10549 _diffrn_reflns_av_R_equivalents 0.0798 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.26 _reflns_number_total 4153 _reflns_number_gt 3835 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^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 SHELXL _refine_ls_extinction_coef 0.0044(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(12) _refine_ls_number_reflns 4153 _refine_ls_number_parameters 290 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.016 _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 -0.14898(3) 0.28443(12) -0.08111(4) 0.01294(15) Uani 1 1 d . . . Zn2 Zn 0.12851(3) 0.34904(11) -0.09878(4) 0.01282(14) Uani 1 1 d . . . Zn3 Zn -0.00098(3) 0.72530(12) -0.06521(4) 0.01302(15) Uani 1 1 d . . . Zn4 Zn -0.24659(3) 0.77312(11) -0.11234(4) 0.01270(15) Uani 1 1 d . . . Zn5 Zn -0.25015(3) 0.61469(13) 0.12253(4) 0.01414(15) Uani 1 1 d . . . P1 P -0.01200(7) 0.2497(3) -0.16002(9) 0.0116(3) Uani 1 1 d . . . P2 P -0.25733(7) 0.2641(3) -0.20231(9) 0.0110(3) Uani 1 1 d . . . P3 P 0.14084(7) -0.1486(3) -0.00158(8) 0.0111(3) Uani 1 1 d . . . P4 P -0.13937(7) 0.7699(3) 0.01550(8) 0.0103(3) Uani 1 1 d . . . O17 O -0.18115(18) 0.6245(7) -0.0445(2) 0.0147(8) Uani 1 1 d . . . O16 O 0.00355(19) 0.3011(8) -0.2413(3) 0.0170(9) Uani 1 1 d . . . O15 O 0.15804(19) 0.1321(7) -0.0172(2) 0.0170(9) Uani 1 1 d . . . O14 O 0.03680(17) 0.3996(7) -0.1077(2) 0.0172(8) Uani 1 1 d . . . O13 O -0.16271(18) 0.6940(8) 0.0935(2) 0.0157(8) Uani 1 1 d . . . O12 O -0.0076(2) 0.9659(9) -0.1441(3) 0.0287(10) Uani 1 1 d . . . O11 O -0.14941(19) 0.0596(8) 0.0054(2) 0.0171(8) Uani 1 1 d . . . O10 O -0.06980(19) 0.6881(9) 0.0066(2) 0.0192(9) Uani 1 1 d . . . O9 O -0.22011(19) 0.1231(7) -0.1371(2) 0.0132(8) Uani 1 1 d . . . O8 O -0.2684(2) 0.6632(9) 0.2245(2) 0.0211(9) Uani 1 1 d . . . O7 O -0.24279(19) 0.5478(8) -0.1952(2) 0.0192(9) Uani 1 1 d . . . O6 O -0.3274(2) 0.7319(8) 0.0717(2) 0.0183(9) Uani 1 1 d . . . O5 O -0.25134(19) 0.2387(8) 0.0897(3) 0.0217(10) Uani 1 1 d . . . H5A H -0.2768 0.2209 0.0551 0.033 Uiso 1 1 calc R . . O4 O 0.1710(2) 0.2960(8) -0.1934(2) 0.0186(9) Uani 1 1 d . . . O3 O 0.06901(19) 0.8082(9) 0.0037(2) 0.0197(9) Uani 1 1 d . . . O2 O 0.16792(17) 0.6838(8) -0.0669(2) 0.0162(8) Uani 1 1 d . . . O1 O -0.0774(2) 0.3638(9) -0.1410(2) 0.0240(10) Uani 1 1 d . . . N2 N -0.0728(2) 0.3642(10) 0.1791(3) 0.0210(11) Uani 1 1 d . . . H14 H -0.0931 0.4571 0.1439 0.025 Uiso 1 1 calc R . . H13 H -0.0553 0.4734 0.2123 0.025 Uiso 1 1 calc R . . N1 N 0.0804(2) 0.4643(10) 0.1668(3) 0.0221(11) Uani 1 1 d . . . H12 H 0.1091 0.5642 0.1429 0.027 Uiso 1 1 calc R . . H11 H 0.0599 0.5626 0.2005 0.027 Uiso 1 1 calc R . . C2 C -0.0209(3) 0.2106(12) 0.1437(4) 0.0252(14) Uani 1 1 d . . . H10 H -0.0397 0.1058 0.1046 0.030 Uiso 1 1 calc R . . H9 H -0.0027 0.0962 0.1808 0.030 Uiso 1 1 calc R . . C1 C 0.0320(3) 0.3681(14) 0.1109(4) 0.0260(14) Uani 1 1 d . . . H8 H 0.0131 0.5140 0.0855 0.031 Uiso 1 1 calc R . . H7 H 0.0544 0.2662 0.0737 0.031 Uiso 1 1 calc R . . C4 C -0.1205(4) 0.1956(15) 0.2179(4) 0.0311(16) Uani 1 1 d . . . H6 H -0.1534 0.2993 0.2403 0.047 Uiso 1 1 calc R . . H5 H -0.0990 0.0984 0.2560 0.047 Uiso 1 1 calc R . . H4 H -0.1396 0.0808 0.1824 0.047 Uiso 1 1 calc R . . C3 C 0.1158(4) 0.2595(15) 0.2069(5) 0.0316(16) Uani 1 1 d . . . H3 H 0.1455 0.3354 0.2415 0.047 Uiso 1 1 calc R . . H2 H 0.1390 0.1563 0.1716 0.047 Uiso 1 1 calc R . . H1 H 0.0857 0.1542 0.2337 0.047 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 0.0118(3) 0.0089(3) 0.0181(3) 0.0001(3) 0.0002(2) -0.0004(2) Zn2 0.0113(3) 0.0099(3) 0.0172(3) 0.0004(2) -0.0007(2) 0.0003(2) Zn3 0.0114(3) 0.0107(3) 0.0170(4) 0.0008(3) 0.0011(2) 0.0015(2) Zn4 0.0118(3) 0.0085(3) 0.0177(4) 0.0001(3) -0.0005(2) 0.0009(2) Zn5 0.0112(3) 0.0175(3) 0.0137(3) -0.0013(3) -0.0001(2) -0.0001(2) P1 0.0105(6) 0.0094(7) 0.0149(7) 0.0010(5) -0.0005(5) -0.0016(5) P2 0.0127(7) 0.0088(7) 0.0114(7) -0.0002(5) 0.0005(5) 0.0003(5) P3 0.0099(6) 0.0086(7) 0.0148(7) 0.0002(5) -0.0002(5) -0.0004(5) P4 0.0086(6) 0.0092(7) 0.0131(7) -0.0005(5) -0.0005(5) 0.0005(5) O17 0.0125(17) 0.0117(19) 0.020(2) -0.0029(15) -0.0041(15) 0.0008(15) O16 0.018(2) 0.016(2) 0.017(2) 0.0039(17) 0.0002(16) 0.0010(16) O15 0.022(2) 0.008(2) 0.021(2) 0.0028(16) -0.0032(17) -0.0009(15) O14 0.0101(17) 0.0148(19) 0.027(2) -0.0058(17) 0.0006(17) 0.0007(14) O13 0.0091(17) 0.022(2) 0.016(2) 0.0009(16) 0.0000(16) -0.0018(15) O12 0.052(3) 0.015(2) 0.019(2) 0.0003(18) -0.007(2) -0.004(2) O11 0.025(2) 0.0102(19) 0.016(2) 0.0010(16) -0.0005(16) 0.0013(16) O10 0.0122(19) 0.025(2) 0.020(2) 0.0028(16) 0.0012(17) 0.0023(17) O9 0.0165(19) 0.0085(18) 0.0146(19) 0.0028(14) -0.0052(15) -0.0025(15) O8 0.028(2) 0.021(2) 0.015(2) -0.0055(17) -0.0015(18) -0.0027(19) O7 0.033(2) 0.009(2) 0.016(2) -0.0018(17) -0.0007(17) -0.0005(17) O6 0.018(2) 0.018(2) 0.019(2) -0.0013(16) -0.0060(17) 0.0069(17) O5 0.022(2) 0.012(2) 0.031(3) -0.0042(18) -0.0026(18) -0.0025(16) O4 0.014(2) 0.022(2) 0.019(2) -0.0038(17) -0.0004(17) 0.0068(16) O3 0.0124(19) 0.029(2) 0.018(2) -0.0055(16) -0.0015(17) -0.0011(17) O2 0.0133(18) 0.0160(19) 0.019(2) -0.0064(16) 0.0045(16) -0.0042(15) O1 0.014(2) 0.035(3) 0.023(2) 0.0040(19) 0.0073(17) 0.0030(18) N2 0.022(3) 0.019(3) 0.023(3) -0.002(2) -0.006(2) 0.001(2) N1 0.020(2) 0.017(3) 0.029(3) -0.002(2) 0.004(2) -0.001(2) C2 0.022(3) 0.016(3) 0.038(4) -0.005(3) -0.001(3) 0.001(2) C1 0.024(3) 0.036(4) 0.019(3) 0.001(3) -0.001(3) 0.003(3) C4 0.028(4) 0.024(4) 0.041(4) -0.001(3) 0.006(3) -0.004(3) C3 0.022(3) 0.036(5) 0.037(4) -0.002(3) -0.008(3) 0.004(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 O1 1.880(4) . ? Zn1 O11 1.944(4) . ? Zn1 O9 1.973(4) . ? Zn1 O17 2.007(4) . ? Zn2 O14 1.929(4) . ? Zn2 O4 1.931(4) . ? Zn2 O15 1.949(4) . ? Zn2 O2 2.013(4) . ? Zn3 O12 1.896(5) . ? Zn3 O10 1.932(4) . ? Zn3 O3 1.955(4) . ? Zn3 O14 2.022(4) . ? Zn4 O7 1.895(4) . ? Zn4 O9 1.959(4) 1_565 ? Zn4 O2 1.966(4) 3_465 ? Zn4 O17 1.982(4) . ? Zn5 O8 1.882(4) . ? Zn5 O13 1.933(4) . ? Zn5 O6 1.943(4) . ? Zn5 O5 2.050(4) . ? P1 O12 1.511(5) 1_545 ? P1 O16 1.515(5) . ? P1 O1 1.521(4) . ? P1 O14 1.586(4) . ? P2 O8 1.511(5) 4_444 ? P2 O7 1.517(4) . ? P2 O4 1.529(4) 3_455 ? P2 O9 1.583(4) . ? P3 O3 1.511(4) 1_545 ? P3 O6 1.532(4) 3 ? P3 O15 1.534(4) . ? P3 O2 1.565(4) 1_545 ? P4 O10 1.515(4) . ? P4 O13 1.530(4) . ? P4 O11 1.537(4) 1_565 ? P4 O17 1.576(4) . ? O12 P1 1.511(5) 1_565 ? O11 P4 1.537(4) 1_545 ? O9 Zn4 1.959(4) 1_545 ? O8 P2 1.511(5) 4_455 ? O6 P3 1.532(4) 3_455 ? O5 H5A 0.8200 . ? O4 P2 1.529(4) 3 ? O3 P3 1.511(4) 1_565 ? O2 P3 1.565(4) 1_565 ? O2 Zn4 1.966(4) 3_565 ? N2 C2 1.485(8) . ? N2 C4 1.496(9) . ? N2 H14 0.9000 . ? N2 H13 0.9000 . ? N1 C3 1.483(9) . ? N1 C1 1.505(8) . ? N1 H12 0.9000 . ? N1 H11 0.9000 . ? C2 C1 1.493(9) . ? C2 H10 0.9700 . ? C2 H9 0.9700 . ? C1 H8 0.9700 . ? C1 H7 0.9700 . ? C4 H6 0.9600 . ? C4 H5 0.9600 . ? C4 H4 0.9600 . ? C3 H3 0.9600 . ? C3 H2 0.9600 . ? C3 H1 0.9600 . ? 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 O1 Zn1 O11 126.27(18) . . ? O1 Zn1 O9 113.34(18) . . ? O11 Zn1 O9 98.26(16) . . ? O1 Zn1 O17 104.76(18) . . ? O11 Zn1 O17 105.78(17) . . ? O9 Zn1 O17 107.13(15) . . ? O14 Zn2 O4 113.44(18) . . ? O14 Zn2 O15 116.90(18) . . ? O4 Zn2 O15 115.57(18) . . ? O14 Zn2 O2 107.83(16) . . ? O4 Zn2 O2 100.83(17) . . ? O15 Zn2 O2 99.44(17) . . ? O12 Zn3 O10 120.6(2) . . ? O12 Zn3 O3 112.2(2) . . ? O10 Zn3 O3 98.72(19) . . ? O12 Zn3 O14 107.73(19) . . ? O10 Zn3 O14 116.94(18) . . ? O3 Zn3 O14 97.81(17) . . ? O7 Zn4 O9 112.97(17) . 1_565 ? O7 Zn4 O2 115.65(17) . 3_465 ? O9 Zn4 O2 103.91(16) 1_565 3_465 ? O7 Zn4 O17 102.06(17) . . ? O9 Zn4 O17 108.16(16) 1_565 . ? O2 Zn4 O17 114.18(17) 3_465 . ? O8 Zn5 O13 114.94(19) . . ? O8 Zn5 O6 104.27(19) . . ? O13 Zn5 O6 125.51(18) . . ? O8 Zn5 O5 113.9(2) . . ? O13 Zn5 O5 98.00(17) . . ? O6 Zn5 O5 99.03(18) . . ? O12 P1 O16 110.0(3) 1_545 . ? O12 P1 O1 113.3(3) 1_545 . ? O16 P1 O1 109.6(2) . . ? O12 P1 O14 109.5(2) 1_545 . ? O16 P1 O14 110.1(2) . . ? O1 P1 O14 104.1(2) . . ? O8 P2 O7 110.1(2) 4_444 . ? O8 P2 O4 111.3(3) 4_444 3_455 ? O7 P2 O4 112.7(2) . 3_455 ? O8 P2 O9 107.9(2) 4_444 . ? O7 P2 O9 107.1(2) . . ? O4 P2 O9 107.6(2) 3_455 . ? O3 P3 O6 109.2(2) 1_545 3 ? O3 P3 O15 112.6(3) 1_545 . ? O6 P3 O15 109.1(2) 3 . ? O3 P3 O2 108.5(2) 1_545 1_545 ? O6 P3 O2 109.1(2) 3 1_545 ? O15 P3 O2 108.3(2) . 1_545 ? O10 P4 O13 109.0(2) . . ? O10 P4 O11 113.2(2) . 1_565 ? O13 P4 O11 108.6(2) . 1_565 ? O10 P4 O17 108.5(2) . . ? O13 P4 O17 108.9(2) . . ? O11 P4 O17 108.6(2) 1_565 . ? P4 O17 Zn4 127.4(2) . . ? P4 O17 Zn1 117.8(2) . . ? Zn4 O17 Zn1 111.95(18) . . ? P3 O15 Zn2 128.2(3) . . ? P1 O14 Zn2 127.7(2) . . ? P1 O14 Zn3 112.9(2) . . ? Zn2 O14 Zn3 117.82(19) . . ? P4 O13 Zn5 126.8(2) . . ? P1 O12 Zn3 142.6(3) 1_565 . ? P4 O11 Zn1 133.4(2) 1_545 . ? P4 O10 Zn3 138.4(3) . . ? P2 O9 Zn4 117.6(2) . 1_545 ? P2 O9 Zn1 122.8(2) . . ? Zn4 O9 Zn1 119.56(18) 1_545 . ? P2 O8 Zn5 144.9(3) 4_455 . ? P2 O7 Zn4 131.6(3) . . ? P3 O6 Zn5 131.9(3) 3_455 . ? Zn5 O5 H5A 109.5 . . ? P2 O4 Zn2 124.5(3) 3 . ? P3 O3 Zn3 136.6(3) 1_565 . ? P3 O2 Zn4 124.7(2) 1_565 3_565 ? P3 O2 Zn2 123.5(2) 1_565 . ? Zn4 O2 Zn2 110.42(19) 3_565 . ? P1 O1 Zn1 138.4(3) . . ? C2 N2 C4 111.2(5) . . ? C2 N2 H14 109.4 . . ? C4 N2 H14 109.4 . . ? C2 N2 H13 109.4 . . ? C4 N2 H13 109.4 . . ? H14 N2 H13 108.0 . . ? C3 N1 C1 114.4(5) . . ? C3 N1 H12 108.7 . . ? C1 N1 H12 108.7 . . ? C3 N1 H11 108.7 . . ? C1 N1 H11 108.7 . . ? H12 N1 H11 107.6 . . ? N2 C2 C1 113.9(5) . . ? N2 C2 H10 108.8 . . ? C1 C2 H10 108.8 . . ? N2 C2 H9 108.8 . . ? C1 C2 H9 108.8 . . ? H10 C2 H9 107.7 . . ? C2 C1 N1 114.4(5) . . ? C2 C1 H8 108.7 . . ? N1 C1 H8 108.7 . . ? C2 C1 H7 108.7 . . ? N1 C1 H7 108.7 . . ? H8 C1 H7 107.6 . . ? N2 C4 H6 109.5 . . ? N2 C4 H5 109.5 . . ? H6 C4 H5 109.5 . . ? N2 C4 H4 109.5 . . ? H6 C4 H4 109.5 . . ? H5 C4 H4 109.5 . . ? N1 C3 H3 109.5 . . ? N1 C3 H2 109.5 . . ? H3 C3 H2 109.5 . . ? N1 C3 H1 109.5 . . ? H3 C3 H1 109.5 . . ? H2 C3 H1 109.5 . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.998 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.177 #====END OF COMPOUND II data_COMPOUND_III _database_code_depnum_ccdc_archive 'CCDC 220187' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Zinc Phosphate' _chemical_melting_point ? _chemical_formula_moiety [NH4][H3O][Zn4(PO4)3]2.H2O _chemical_formula_sum 'H2 N0.50 O13 P3 Zn4' _chemical_formula_weight 571.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.0400(9) _cell_length_b 9.584(3) _cell_length_c 13.117(2) _cell_angle_alpha 101.094(19) _cell_angle_beta 100.931(19) _cell_angle_gamma 103.598(18) _cell_volume 585.7(2) _cell_formula_units_Z 2 _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 ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 549 _exptl_absorpt_coefficient_mu 8.572 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 3484 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.32 _reflns_number_total 2529 _reflns_number_gt 2327 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+3.9700P] 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 2529 _refine_ls_number_parameters 197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1228 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _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 0.44980(14) 0.02160(7) 0.79790(6) 0.01408(19) Uani 1 1 d . . . Zn2 Zn 0.87434(14) -0.19176(8) 0.84527(6) 0.01430(19) Uani 1 1 d . . . Zn3 Zn 0.05894(15) 0.34251(8) 0.72382(6) 0.01465(19) Uani 1 1 d . . . Zn4 Zn 0.14456(14) -0.15780(8) 0.54017(5) 0.01392(19) Uani 1 1 d . . . P1 P 0.2403(3) -0.32500(16) 0.71453(12) 0.0111(3) Uani 1 1 d . . . P2 P 0.0448(3) 0.16685(16) 0.90468(12) 0.0122(3) Uani 1 1 d . . . P3 P 0.4293(3) 0.17393(16) 0.60406(12) 0.0114(3) Uani 1 1 d . . . O1 O 0.3329(9) 0.1518(5) 0.8962(4) 0.0212(10) Uani 1 1 d . . . O2 O 0.8249(9) 0.0111(5) 0.8623(4) 0.0210(10) Uani 1 1 d . . . O3 O 0.3717(9) 0.0306(5) 0.6458(3) 0.0161(9) Uani 1 1 d . . . O4 O 0.2010(9) -0.1800(4) 0.7819(3) 0.0136(8) Uani 1 1 d . . . O5 O -0.0620(10) 0.2623(5) 0.8349(4) 0.0212(10) Uani 1 1 d . . . O6 O 0.0604(10) 0.5452(5) 0.7430(4) 0.0213(10) Uani 1 1 d . . . O7 O 0.3885(9) 0.3002(5) 0.6830(4) 0.0201(9) Uani 1 1 d . . . O8 O -0.2607(8) 0.2158(5) 0.5949(3) 0.0142(8) Uani 1 1 d . . . O9 O 0.1361(11) -0.3303(5) 0.5964(4) 0.0251(10) Uani 1 1 d . . . O10 O -0.2374(9) -0.1395(6) 0.5062(4) 0.0225(10) Uani 1 1 d . . . O11 O 0.5494(10) -0.3180(6) 0.7385(5) 0.0306(12) Uani 1 1 d . . . O12 O 0.0450(10) 0.2353(5) 1.0185(4) 0.0210(10) Uani 1 1 d . . . N1 N 0.5000 -0.5000 0.5000 0.040(3) Uani 1 2 d S . . O20 O -0.269(6) 0.4517(19) 0.964(3) 0.072(13) Uani 0.51(6) 1 d P . . O20A O 0.582(9) 0.463(2) 0.898(3) 0.074(11) Uani 0.49(6) 1 d P . . 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 0.0140(4) 0.0118(3) 0.0175(4) 0.0045(3) 0.0056(3) 0.0034(3) Zn2 0.0132(3) 0.0152(4) 0.0158(4) 0.0060(3) 0.0055(3) 0.0032(3) Zn3 0.0168(4) 0.0116(3) 0.0195(4) 0.0070(3) 0.0103(3) 0.0042(3) Zn4 0.0127(3) 0.0141(4) 0.0149(4) 0.0046(3) 0.0039(3) 0.0024(3) P1 0.0099(7) 0.0087(7) 0.0153(7) 0.0033(5) 0.0049(5) 0.0016(5) P2 0.0131(7) 0.0111(7) 0.0138(7) 0.0048(5) 0.0060(5) 0.0025(5) P3 0.0088(6) 0.0109(7) 0.0171(7) 0.0074(5) 0.0059(5) 0.0022(5) O1 0.012(2) 0.019(2) 0.030(3) -0.0010(19) 0.0086(18) 0.0027(17) O2 0.012(2) 0.013(2) 0.036(3) 0.0070(19) 0.0048(19) 0.0020(17) O3 0.020(2) 0.0100(19) 0.018(2) 0.0075(16) 0.0065(17) -0.0005(16) O4 0.017(2) 0.0073(18) 0.018(2) 0.0025(15) 0.0101(17) 0.0032(16) O5 0.026(2) 0.024(2) 0.023(2) 0.0154(19) 0.0125(19) 0.012(2) O6 0.025(2) 0.0066(19) 0.038(3) 0.0115(19) 0.018(2) 0.0036(17) O7 0.014(2) 0.013(2) 0.033(3) 0.0033(19) 0.0094(19) 0.0033(17) O8 0.0064(18) 0.018(2) 0.016(2) 0.0025(16) 0.0042(15) -0.0001(16) O9 0.039(3) 0.016(2) 0.021(2) 0.0070(18) 0.008(2) 0.006(2) O10 0.012(2) 0.035(3) 0.024(2) 0.014(2) 0.0038(18) 0.0062(19) O11 0.011(2) 0.031(3) 0.042(3) -0.008(2) 0.003(2) 0.007(2) O12 0.029(3) 0.024(2) 0.016(2) 0.0078(18) 0.0102(19) 0.013(2) N1 0.035(5) 0.018(4) 0.070(7) 0.008(4) 0.032(5) 0.003(4) O20 0.079(16) 0.018(7) 0.11(3) -0.010(9) 0.045(17) 0.005(7) O20A 0.12(3) 0.045(10) 0.08(2) 0.024(10) 0.059(19) 0.032(11) _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 O1 1.893(5) . ? Zn1 O2 1.953(5) . ? Zn1 O3 1.981(4) . ? Zn1 O4 1.988(4) . ? Zn2 O12 1.903(5) 2_657 ? Zn2 O11 1.911(5) . ? Zn2 O4 1.970(4) 1_655 ? Zn2 O2 1.993(5) . ? Zn3 O5 1.907(5) . ? Zn3 O6 1.908(4) . ? Zn3 O7 1.944(4) . ? Zn3 O8 2.046(4) . ? Zn4 O9 1.930(5) . ? Zn4 O10 1.949(5) . ? Zn4 O3 1.989(4) . ? Zn4 O8 1.989(4) 2_556 ? P1 O6 1.512(4) 1_545 ? P1 O11 1.512(5) . ? P1 O9 1.526(5) . ? P1 O4 1.573(4) . ? P2 O12 1.511(5) . ? P2 O1 1.515(5) . ? P2 O5 1.526(5) . ? P2 O2 1.560(5) 1_455 ? P3 O10 1.508(5) 2_556 ? P3 O7 1.515(5) . ? P3 O8 1.553(4) 1_655 ? P3 O3 1.561(4) . ? O2 P2 1.560(5) 1_655 ? O4 Zn2 1.970(4) 1_455 ? O6 P1 1.512(4) 1_565 ? O8 P3 1.553(4) 1_455 ? O8 Zn4 1.989(4) 2_556 ? O10 P3 1.508(5) 2_556 ? O12 Zn2 1.903(5) 2_657 ? O20 O20A 1.07(3) 1_455 ? O20A O20 1.07(3) 1_655 ? 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 O1 Zn1 O2 110.0(2) . . ? O1 Zn1 O3 118.2(2) . . ? O2 Zn1 O3 117.1(2) . . ? O1 Zn1 O4 105.87(19) . . ? O2 Zn1 O4 103.99(19) . . ? O3 Zn1 O4 99.28(18) . . ? O12 Zn2 O11 118.6(2) 2_657 . ? O12 Zn2 O4 110.46(19) 2_657 1_655 ? O11 Zn2 O4 107.6(2) . 1_655 ? O12 Zn2 O2 110.2(2) 2_657 . ? O11 Zn2 O2 105.2(2) . . ? O4 Zn2 O2 103.62(18) 1_655 . ? O5 Zn3 O6 111.5(2) . . ? O5 Zn3 O7 117.7(2) . . ? O6 Zn3 O7 114.3(2) . . ? O5 Zn3 O8 99.9(2) . . ? O6 Zn3 O8 109.3(2) . . ? O7 Zn3 O8 102.26(18) . . ? O9 Zn4 O10 108.3(2) . . ? O9 Zn4 O3 113.2(2) . . ? O10 Zn4 O3 105.3(2) . . ? O9 Zn4 O8 101.6(2) . 2_556 ? O10 Zn4 O8 109.53(19) . 2_556 ? O3 Zn4 O8 118.60(18) . 2_556 ? O6 P1 O11 113.0(3) 1_545 . ? O6 P1 O9 110.3(3) 1_545 . ? O11 P1 O9 109.5(3) . . ? O6 P1 O4 107.2(2) 1_545 . ? O11 P1 O4 109.3(3) . . ? O9 P1 O4 107.3(3) . . ? O12 P2 O1 111.5(3) . . ? O12 P2 O5 107.1(3) . . ? O1 P2 O5 113.1(3) . . ? O12 P2 O2 110.5(3) . 1_455 ? O1 P2 O2 109.2(3) . 1_455 ? O5 P2 O2 105.2(3) . 1_455 ? O10 P3 O7 113.3(3) 2_556 . ? O10 P3 O8 108.6(3) 2_556 1_655 ? O7 P3 O8 108.6(3) . 1_655 ? O10 P3 O3 107.8(3) 2_556 . ? O7 P3 O3 109.6(3) . . ? O8 P3 O3 108.8(3) 1_655 . ? P2 O1 Zn1 132.3(3) . . ? P2 O2 Zn1 112.6(3) 1_655 . ? P2 O2 Zn2 130.9(3) 1_655 . ? Zn1 O2 Zn2 115.9(2) . . ? P3 O3 Zn1 126.2(3) . . ? P3 O3 Zn4 117.4(3) . . ? Zn1 O3 Zn4 115.7(2) . . ? P1 O4 Zn2 119.8(2) . 1_455 ? P1 O4 Zn1 123.3(2) . . ? Zn2 O4 Zn1 116.8(2) 1_455 . ? P2 O5 Zn3 134.1(3) . . ? P1 O6 Zn3 132.6(3) 1_565 . ? P3 O7 Zn3 133.3(3) . . ? P3 O8 Zn4 123.7(2) 1_455 2_556 ? P3 O8 Zn3 121.0(2) 1_455 . ? Zn4 O8 Zn3 115.25(19) 2_556 . ? P1 O9 Zn4 124.4(3) . . ? P3 O10 Zn4 126.5(3) 2_556 . ? P1 O11 Zn2 133.8(3) . . ? P2 O12 Zn2 137.2(3) . 2_657 ? _diffrn_measured_fraction_theta_max 0.867 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.867 _refine_diff_density_max 1.514 _refine_diff_density_min -1.378 _refine_diff_density_rms 0.237 #=====END OF COMPOUNDIII data_COMPOUND_IV _database_code_depnum_ccdc_archive 'CCDC 220188' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cobalt Phosphate' _chemical_melting_point ? _chemical_formula_moiety [C5N2H14][Co(HPO4)2] _chemical_formula_sum 'C3 H9 Co0.50 N O4 P' _chemical_formula_weight 183.55 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 11.939(2) _cell_length_b 13.803(3) _cell_length_c 7.9473(15) _cell_angle_alpha 90.00 _cell_angle_beta 91.514(3) _cell_angle_gamma 90.00 _cell_volume 1309.2(4) _cell_formula_units_Z 8 _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 ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.862 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 1.592 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 3800 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 28.27 _reflns_number_total 1515 _reflns_number_gt 1361 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+1.6713P] 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 1515 _refine_ls_number_parameters 87 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _refine_ls_shift/su_max 0.005 _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 Co1 Co 0.0000 0.46964(3) -0.7500 0.01798(17) Uani 1 2 d S . . P1 P -0.14247(5) 0.37008(5) -0.45136(8) 0.01820(19) Uani 1 1 d . . . O1 O 0.12522(17) 0.54766(14) -0.6730(3) 0.0302(4) Uani 1 1 d . . . O2 O -0.05563(16) 0.37323(14) -0.5900(2) 0.0278(4) Uani 1 1 d . . . O3 O -0.13832(15) 0.27201(13) -0.3660(2) 0.0246(4) Uani 1 1 d . . . O4 O -0.26211(16) 0.38643(14) -0.5327(3) 0.0301(4) Uani 1 1 d . . . H1 H -0.2888 0.3342 -0.5620 0.045 Uiso 1 1 calc R . . N1 N 0.1390(2) 0.28294(19) -0.4744(3) 0.0330(6) Uani 1 1 d . . . H2 H 0.0735 0.3071 -0.5143 0.040 Uiso 1 1 calc R . . H3 H 0.1336 0.2755 -0.3624 0.040 Uiso 1 1 calc R . . C1 C 0.1585(3) 0.1866(3) -0.5529(4) 0.0371(7) Uani 1 1 d . . . H4 H 0.1601 0.1947 -0.6753 0.045 Uiso 1 1 calc R . . C2 C 0.2296(3) 0.3525(2) -0.5087(4) 0.0363(7) Uani 1 1 d . . . H5 H 0.2146 0.4134 -0.4528 0.044 Uiso 1 1 calc R . . H6 H 0.2319 0.3647 -0.6288 0.044 Uiso 1 1 calc R . . C3 C 0.0709(7) 0.1183(6) -0.5136(13) 0.148(4) Uani 1 1 d . . . H7 H 0.0860 0.0573 -0.5663 0.221 Uiso 1 1 calc R . . H8 H 0.0000 0.1427 -0.5546 0.221 Uiso 1 1 calc R . . H9 H 0.0688 0.1097 -0.3939 0.221 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 Co1 0.0199(3) 0.0188(3) 0.0153(3) 0.000 0.00175(17) 0.000 P1 0.0173(3) 0.0201(3) 0.0173(3) 0.0004(2) 0.0015(2) -0.0028(2) O1 0.0310(10) 0.0281(10) 0.0316(11) -0.0081(8) -0.0007(8) -0.0062(8) O2 0.0269(10) 0.0314(10) 0.0257(10) 0.0105(8) 0.0109(8) 0.0036(8) O3 0.0309(10) 0.0251(9) 0.0177(9) 0.0036(7) -0.0005(7) -0.0062(8) O4 0.0215(9) 0.0262(10) 0.0420(12) -0.0015(9) -0.0087(8) -0.0009(7) N1 0.0329(12) 0.0457(15) 0.0204(11) 0.0013(10) 0.0027(9) 0.0181(11) C1 0.0365(15) 0.0472(19) 0.0278(14) -0.0064(13) 0.0025(12) 0.0069(14) C2 0.0462(18) 0.0352(15) 0.0279(15) 0.0019(13) 0.0079(13) 0.0165(14) C3 0.136(8) 0.148(8) 0.160(8) -0.048(7) 0.032(6) -0.007(6) _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 Co1 O1 1.929(2) . ? Co1 O1 1.929(2) 2_553 ? Co1 O2 1.9681(18) . ? Co1 O2 1.9681(18) 2_553 ? P1 O3 1.5144(19) . ? P1 O1 1.516(2) 5_564 ? P1 O2 1.5333(19) . ? P1 O4 1.5686(19) . ? O1 P1 1.516(2) 5_564 ? O4 H1 0.8200 . ? N1 C2 1.477(4) . ? N1 C1 1.489(4) . ? N1 H2 0.9000 . ? N1 H3 0.9000 . ? C1 C3 1.448(9) . ? C1 C2 1.510(4) 7_554 ? C1 H4 0.9800 . ? C2 C1 1.510(4) 7_554 ? C2 H5 0.9700 . ? C2 H6 0.9700 . ? C3 H7 0.9600 . ? C3 H8 0.9600 . ? C3 H9 0.9600 . ? 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 O1 Co1 O1 112.13(13) . 2_553 ? O1 Co1 O2 116.38(9) . . ? O1 Co1 O2 108.10(8) 2_553 . ? O1 Co1 O2 108.10(8) . 2_553 ? O1 Co1 O2 116.38(9) 2_553 2_553 ? O2 Co1 O2 94.92(12) . 2_553 ? O3 P1 O1 112.05(11) . 5_564 ? O3 P1 O2 109.43(11) . . ? O1 P1 O2 111.37(12) 5_564 . ? O3 P1 O4 109.38(11) . . ? O1 P1 O4 105.51(12) 5_564 . ? O2 P1 O4 108.99(12) . . ? P1 O1 Co1 135.72(13) 5_564 . ? P1 O2 Co1 136.85(12) . . ? P1 O4 H1 109.5 . . ? C2 N1 C1 112.3(2) . . ? C2 N1 H2 109.1 . . ? C1 N1 H2 109.1 . . ? C2 N1 H3 109.1 . . ? C1 N1 H3 109.1 . . ? H2 N1 H3 107.9 . . ? C3 C1 N1 111.7(4) . . ? C3 C1 C2 109.5(5) . 7_554 ? N1 C1 C2 109.3(3) . 7_554 ? C3 C1 H4 108.8 . . ? N1 C1 H4 108.8 . . ? C2 C1 H4 108.8 7_554 . ? N1 C2 C1 110.7(3) . 7_554 ? N1 C2 H5 109.5 . . ? C1 C2 H5 109.5 7_554 . ? N1 C2 H6 109.5 . . ? C1 C2 H6 109.5 7_554 . ? H5 C2 H6 108.1 . . ? C1 C3 H7 109.5 . . ? C1 C3 H8 109.5 . . ? H7 C3 H8 109.5 . . ? C1 C3 H9 109.5 . . ? H7 C3 H9 109.5 . . ? H8 C3 H9 109.5 . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 0.503 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.108 #==END OF COMPOUND V data_COMPOUND_VI _database_code_depnum_ccdc_archive 'CCDC 220190' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cobalt Phosphate' _chemical_melting_point ? _chemical_formula_moiety [C4N2H12]3[Co2(OH)(HPO4)3]2 _chemical_formula_sum 'C6 H21 Co2 N3 O13 P3' _chemical_formula_weight 554.03 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 7.2743(18) _cell_length_b 23.030(6) _cell_length_c 9.873(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.131(4) _cell_angle_gamma 90.00 _cell_volume 1651.4(7) _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 ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 2.377 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 10083 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 28.24 _reflns_number_total 3857 _reflns_number_gt 2831 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0894P)^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 3857 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0727 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1464 _refine_ls_wR_factor_gt 0.1348 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 Co1 Co 0.71128(8) 0.07323(3) 0.03494(6) 0.01301(17) Uani 1 1 d . . . Co2 Co 1.20970(8) 0.08465(3) 0.04708(6) 0.01333(17) Uani 1 1 d . . . P1 P 0.97226(16) 0.14967(5) 0.26149(12) 0.0137(3) Uani 1 1 d . . . P2 P 1.43521(16) 0.13788(5) -0.19910(11) 0.0132(3) Uani 1 1 d . . . P3 P 1.02557(15) 0.02619(5) -0.16677(11) 0.0117(2) Uani 1 1 d . . . O1 O 0.6167(4) 0.11595(16) -0.1332(3) 0.0233(8) Uani 1 1 d . . . O2 O 1.4621(10) 0.0643(3) 0.1132(7) 0.0036(19) Uiso 0.50 1 d P . . O2A O 1.4640(10) 0.0765(3) 0.1237(7) 0.0010(18) Uiso 0.50 1 d P . . O3 O 0.7843(4) -0.00531(14) 0.1127(3) 0.0174(7) Uani 1 1 d . . . O4 O 0.7982(4) 0.13335(14) 0.1760(3) 0.0201(7) Uani 1 1 d . . . O5 O 0.9629(4) 0.07158(13) -0.0638(3) 0.0153(7) Uani 1 1 d . . . O6 O 1.1395(4) 0.15133(14) 0.1738(3) 0.0193(7) Uani 1 1 d . . . O7 O 1.2880(4) 0.14636(13) -0.0961(3) 0.0157(7) Uani 1 1 d . . . O8 O 1.1174(4) 0.02106(14) 0.1920(3) 0.0160(7) Uani 1 1 d . . . O9 O 0.9472(5) 0.20496(14) 0.3394(3) 0.0207(7) Uani 1 1 d . . . O10 O 1.0080(5) 0.10130(15) 0.3741(3) 0.0269(8) Uani 1 1 d . . . H1 H 1.0444 0.0715 0.3388 0.040 Uiso 1 1 calc R . . O11 O 1.3675(5) 0.09834(15) -0.3159(3) 0.0212(7) Uani 1 1 d . . . O12 O 1.4745(5) 0.19742(15) -0.2685(3) 0.0235(8) Uani 1 1 d . . . H2 H 1.4573 0.2239 -0.2152 0.035 Uiso 1 1 calc R . . O13 O 1.0467(5) 0.05690(15) -0.3064(3) 0.0197(7) Uani 1 1 d . . . H3 H 1.1509 0.0703 -0.3090 0.030 Uiso 1 1 calc R . . N1 N 0.5273(7) 0.2444(2) 0.1452(5) 0.0375(12) Uani 1 1 d . . . H13 H 0.5076 0.2324 0.0589 0.045 Uiso 1 1 calc R . . H12 H 0.6468 0.2543 0.1574 0.045 Uiso 1 1 calc R . . N2 N 0.3902(7) 0.2664(2) 0.4073(5) 0.0360(12) Uani 1 1 d . . . H15 H 0.2709 0.2563 0.3944 0.043 Uiso 1 1 calc R . . H14 H 0.4093 0.2781 0.4939 0.043 Uiso 1 1 calc R . . N3 N 0.4361(6) -0.00258(18) 0.3599(4) 0.0219(9) Uani 1 1 d . . . H21 H 0.5054 -0.0317 0.3294 0.026 Uiso 1 1 calc R . . H20 H 0.3624 0.0103 0.2901 0.026 Uiso 1 1 calc R . . C1 C 0.4874(6) 0.19643(18) 0.2374(4) 0.0117(8) Uani 1 1 d . . . H4 H 0.5701 0.1644 0.2220 0.014 Uiso 1 1 calc R . . H5 H 0.3624 0.1830 0.2175 0.014 Uiso 1 1 calc R . . C2 C 0.5086(7) 0.2145(2) 0.3831(5) 0.0241(11) Uani 1 1 d . . . H6 H 0.6365 0.2239 0.4062 0.029 Uiso 1 1 calc R . . H7 H 0.4734 0.1827 0.4406 0.029 Uiso 1 1 calc R . . C3 C 0.4310(6) 0.31497(17) 0.3150(4) 0.0126(9) Uani 1 1 d . . . H8 H 0.5560 0.3283 0.3352 0.015 Uiso 1 1 calc R . . H9 H 0.3485 0.3471 0.3308 0.015 Uiso 1 1 calc R . . C4 C 0.4097(7) 0.2972(2) 0.1685(5) 0.0238(11) Uani 1 1 d . . . H10 H 0.4468 0.3289 0.1113 0.029 Uiso 1 1 calc R . . H11 H 0.2816 0.2883 0.1447 0.029 Uiso 1 1 calc R . . C5 C 0.5579(8) 0.0455(2) 0.4114(5) 0.0287(12) Uani 1 1 d . . . H17 H 0.4833 0.0779 0.4391 0.034 Uiso 1 1 calc R . . H16 H 0.6337 0.0588 0.3398 0.034 Uiso 1 1 calc R . . C6 C 0.3211(7) -0.0248(3) 0.4697(5) 0.0287(12) Uani 1 1 d . . . H19 H 0.2446 -0.0565 0.4351 0.034 Uiso 1 1 calc R . . H18 H 0.2409 0.0059 0.4988 0.034 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 Co1 0.0126(3) 0.0166(3) 0.0094(3) 0.0012(2) -0.0032(2) 0.0012(2) Co2 0.0122(3) 0.0181(3) 0.0093(3) -0.0002(2) -0.0040(2) -0.0005(2) P1 0.0151(6) 0.0157(6) 0.0102(5) -0.0019(4) -0.0013(4) 0.0000(4) P2 0.0127(6) 0.0177(6) 0.0090(5) 0.0018(4) -0.0024(4) -0.0002(4) P3 0.0120(5) 0.0153(5) 0.0071(5) 0.0008(4) -0.0041(4) -0.0001(4) O1 0.0136(16) 0.038(2) 0.0183(18) 0.0103(15) -0.0039(13) 0.0024(14) O3 0.0141(16) 0.0198(16) 0.0176(17) 0.0041(13) -0.0057(13) 0.0014(13) O4 0.0146(16) 0.0270(18) 0.0182(17) -0.0094(14) -0.0033(13) 0.0007(13) O5 0.0165(16) 0.0177(15) 0.0116(16) -0.0015(12) -0.0014(12) 0.0009(13) O6 0.0173(17) 0.0241(18) 0.0165(17) -0.0057(13) 0.0018(13) -0.0041(13) O7 0.0140(16) 0.0204(17) 0.0125(16) 0.0010(12) -0.0011(12) 0.0016(12) O8 0.0169(16) 0.0186(16) 0.0121(15) 0.0003(12) -0.0041(12) -0.0022(13) O9 0.0277(19) 0.0194(17) 0.0150(17) -0.0071(13) 0.0011(14) -0.0014(14) O10 0.042(2) 0.0245(19) 0.0145(17) 0.0023(14) -0.0013(16) 0.0053(16) O11 0.0220(18) 0.0274(18) 0.0140(17) -0.0051(13) -0.0021(14) -0.0033(14) O12 0.032(2) 0.0203(17) 0.0184(18) 0.0032(13) 0.0043(15) -0.0022(14) O13 0.0152(16) 0.0326(19) 0.0108(16) 0.0053(13) -0.0027(13) -0.0054(14) N1 0.032(3) 0.055(3) 0.025(3) -0.008(2) 0.001(2) 0.001(2) N2 0.033(3) 0.052(3) 0.024(3) -0.008(2) 0.003(2) -0.003(2) N3 0.028(2) 0.029(2) 0.0072(19) -0.0030(16) -0.0107(16) 0.0043(18) C1 0.010(2) 0.0105(19) 0.014(2) -0.0012(15) 0.0012(16) 0.0051(15) C2 0.027(3) 0.030(3) 0.015(2) 0.001(2) -0.004(2) 0.003(2) C3 0.016(2) 0.0088(19) 0.013(2) -0.0073(15) 0.0010(17) 0.0006(16) C4 0.025(3) 0.030(3) 0.016(2) 0.001(2) -0.004(2) 0.005(2) C5 0.039(3) 0.028(3) 0.018(3) 0.006(2) -0.005(2) -0.006(2) C6 0.026(3) 0.039(3) 0.020(3) -0.004(2) -0.005(2) -0.008(2) _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 Co1 O1 2.018(3) . ? Co1 O2 2.019(7) 1_455 ? Co1 O3 2.024(3) . ? Co1 O4 2.039(3) . ? Co1 O2A 2.045(7) 1_455 ? Co1 O5 2.121(3) . ? Co2 O2A 1.969(7) . ? Co2 O2 1.972(7) . ? Co2 O6 2.062(3) . ? Co2 O5 2.073(3) . ? Co2 O7 2.105(3) . ? Co2 O8 2.179(3) . ? Co2 P3 2.7848(13) . ? P1 O9 1.504(3) . ? P1 O4 1.530(3) . ? P1 O6 1.532(3) . ? P1 O10 1.585(3) . ? P2 O1 1.526(3) 1_655 ? P2 O7 1.529(3) . ? P2 O11 1.529(3) . ? P2 O12 1.566(3) . ? P3 O8 1.517(3) 3_755 ? P3 O3 1.533(3) 3_755 ? P3 O5 1.544(3) . ? P3 O13 1.565(3) . ? O1 P2 1.526(3) 1_455 ? O2 Co1 2.019(7) 1_655 ? O2A Co1 2.045(7) 1_655 ? O3 P3 1.533(3) 3_755 ? O8 P3 1.517(3) 3_755 ? O10 H1 0.8200 . ? O12 H2 0.8200 . ? O13 H3 0.8200 . ? N1 C1 1.471(6) . ? N1 C4 1.511(7) . ? N1 H13 0.9000 . ? N1 H12 0.9000 . ? N2 C3 1.483(6) . ? N2 C2 1.500(7) . ? N2 H15 0.9000 . ? N2 H14 0.9000 . ? N3 C5 1.490(6) . ? N3 C6 1.495(7) . ? N3 H21 0.9000 . ? N3 H20 0.9000 . ? C1 C2 1.497(6) . ? C1 H4 0.9700 . ? C1 H5 0.9700 . ? C2 H6 0.9700 . ? C2 H7 0.9700 . ? C3 C4 1.503(6) . ? C3 H8 0.9700 . ? C3 H9 0.9700 . ? C4 H10 0.9700 . ? C4 H11 0.9700 . ? C5 C6 1.506(7) 3_656 ? C5 H17 0.9700 . ? C5 H16 0.9700 . ? C6 C5 1.506(7) 3_656 ? C6 H19 0.9700 . ? C6 H18 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 O1 Co1 O2 95.3(2) . 1_455 ? O1 Co1 O3 144.88(14) . . ? O2 Co1 O3 89.2(2) 1_455 . ? O1 Co1 O4 108.05(14) . . ? O2 Co1 O4 93.4(2) 1_455 . ? O3 Co1 O4 106.41(13) . . ? O1 Co1 O2A 93.8(2) . 1_455 ? O2 Co1 O2A 8.5(3) 1_455 1_455 ? O3 Co1 O2A 95.1(2) . 1_455 ? O4 Co1 O2A 86.0(2) . 1_455 ? O1 Co1 O5 83.95(13) . . ? O2 Co1 O5 171.6(2) 1_455 . ? O3 Co1 O5 86.73(12) . . ? O4 Co1 O5 94.74(12) . . ? O2A Co1 O5 177.7(2) 1_455 . ? O2A Co2 O2 8.8(3) . . ? O2A Co2 O6 95.5(2) . . ? O2 Co2 O6 103.5(2) . . ? O2A Co2 O5 163.2(2) . . ? O2 Co2 O5 154.7(2) . . ? O6 Co2 O5 101.09(13) . . ? O2A Co2 O7 92.2(2) . . ? O2 Co2 O7 95.8(2) . . ? O6 Co2 O7 89.40(13) . . ? O5 Co2 O7 90.10(12) . . ? O2A Co2 O8 90.0(2) . . ? O2 Co2 O8 86.4(2) . . ? O6 Co2 O8 90.40(13) . . ? O5 Co2 O8 87.72(12) . . ? O7 Co2 O8 177.73(12) . . ? O2A Co2 P3 130.4(2) . . ? O2 Co2 P3 122.5(2) . . ? O6 Co2 P3 134.03(10) . . ? O5 Co2 P3 33.14(9) . . ? O7 Co2 P3 87.36(9) . . ? O8 Co2 P3 91.16(9) . . ? O9 P1 O4 111.8(2) . . ? O9 P1 O6 112.98(19) . . ? O4 P1 O6 110.67(18) . . ? O9 P1 O10 104.8(2) . . ? O4 P1 O10 108.3(2) . . ? O6 P1 O10 108.0(2) . . ? O1 P2 O7 112.33(18) 1_655 . ? O1 P2 O11 111.1(2) 1_655 . ? O7 P2 O11 111.65(18) . . ? O1 P2 O12 107.6(2) 1_655 . ? O7 P2 O12 109.29(19) . . ? O11 P2 O12 104.51(19) . . ? O8 P3 O3 115.47(19) 3_755 3_755 ? O8 P3 O5 111.67(18) 3_755 . ? O3 P3 O5 106.03(18) 3_755 . ? O8 P3 O13 106.22(18) 3_755 . ? O3 P3 O13 108.58(18) 3_755 . ? O5 P3 O13 108.72(18) . . ? O8 P3 Co2 140.22(13) 3_755 . ? O3 P3 Co2 59.99(13) 3_755 . ? O5 P3 Co2 47.21(12) . . ? O13 P3 Co2 112.52(14) . . ? P2 O1 Co1 139.5(2) 1_455 . ? Co2 O2 Co1 133.5(4) . 1_655 ? Co2 O2A Co1 132.0(4) . 1_655 ? P3 O3 Co1 128.73(19) 3_755 . ? P1 O4 Co1 139.5(2) . . ? P3 O5 Co2 99.65(16) . . ? P3 O5 Co1 127.45(18) . . ? Co2 O5 Co1 119.94(15) . . ? P1 O6 Co2 123.70(19) . . ? P2 O7 Co2 125.83(18) . . ? P3 O8 Co2 127.41(18) 3_755 . ? P1 O10 H1 109.5 . . ? P2 O12 H2 109.5 . . ? P3 O13 H3 109.5 . . ? C1 N1 C4 112.2(4) . . ? C1 N1 H13 109.2 . . ? C4 N1 H13 109.2 . . ? C1 N1 H12 109.2 . . ? C4 N1 H12 109.2 . . ? H13 N1 H12 107.9 . . ? C3 N2 C2 111.5(4) . . ? C3 N2 H15 109.3 . . ? C2 N2 H15 109.3 . . ? C3 N2 H14 109.3 . . ? C2 N2 H14 109.3 . . ? H15 N2 H14 108.0 . . ? C5 N3 C6 110.6(4) . . ? C5 N3 H21 109.5 . . ? C6 N3 H21 109.5 . . ? C5 N3 H20 109.5 . . ? C6 N3 H20 109.5 . . ? H21 N3 H20 108.1 . . ? N1 C1 C2 111.9(4) . . ? N1 C1 H4 109.2 . . ? C2 C1 H4 109.2 . . ? N1 C1 H5 109.2 . . ? C2 C1 H5 109.2 . . ? H4 C1 H5 107.9 . . ? C1 C2 N2 110.1(4) . . ? C1 C2 H6 109.6 . . ? N2 C2 H6 109.6 . . ? C1 C2 H7 109.6 . . ? N2 C2 H7 109.6 . . ? H6 C2 H7 108.1 . . ? N2 C3 C4 111.8(4) . . ? N2 C3 H8 109.3 . . ? C4 C3 H8 109.3 . . ? N2 C3 H9 109.3 . . ? C4 C3 H9 109.3 . . ? H8 C3 H9 107.9 . . ? C3 C4 N1 109.6(4) . . ? C3 C4 H10 109.7 . . ? N1 C4 H10 109.7 . . ? C3 C4 H11 109.7 . . ? N1 C4 H11 109.7 . . ? H10 C4 H11 108.2 . . ? N3 C5 C6 110.0(4) . 3_656 ? N3 C5 H17 109.7 . . ? C6 C5 H17 109.7 3_656 . ? N3 C5 H16 109.7 . . ? C6 C5 H16 109.7 3_656 . ? H17 C5 H16 108.2 . . ? N3 C6 C5 110.3(4) . 3_656 ? N3 C6 H19 109.6 . . ? C5 C6 H19 109.6 3_656 . ? N3 C6 H18 109.6 . . ? C5 C6 H18 109.6 3_656 . ? H19 C6 H18 108.1 . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 1.253 _refine_diff_density_min -0.943 _refine_diff_density_rms 0.178