Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Torben R. Jensen' _publ_contact_author_address ; University of Aarhus Department of Chemistry Langelandsgade 140 8000 Aarhus C Denmark ; _publ_contact_author_email trj@chem.au.dk _publ_contact_author_fax '+45 8619 6199' _publ_contact_author_phone '+45 8942 3894' _publ_section_title ; Two new cobalt zinc orthophosphate monohydrates: hydrothermal synthesis, crystal structures and thermal investigation ; loop_ _publ_author_name 'Torben Jensen' 'Anders Bentien' 'Andrew D. Bond' 'Rita G. Hazell' 'Morten B. Sorensen' ################ ## Compound 1 ## ################ data_1 _database_code_depnum_ccdc_archive 'CCDC 246850' _audit_creation_method 'KRYSTAL plus manual editing' _chemical_name_systematic ; Cobalt zinc orthophosphate monohydrate ; _chemical_formula_sum 'Co2.59 H2 O9 P2 Zn0.41' _chemical_formula_moiety 'Co2.59 H2 O9 P2 Zn0.41' _chemical_formula_weight 387.39 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _atom_type_scat_source IntTabIV loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 7.976(1) _cell_length_b 9.878(2) _cell_length_c 9.057(2) _cell_angle_alpha 90.000 _cell_angle_beta 113.856(3) _cell_angle_gamma 90.000 _cell_volume 652.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2186 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 29.71 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.005 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 3.943 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744.9 _exptl_absorpt_coefficient_mu 8.52 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'XPREP, Sheldrick (1995)' _exptl_absorpt_correction_T_min 0.135 _exptl_absorpt_correction_T_max 0.829 _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation scans with narrow frames' _diffrn_standards_decay_% 0 _diffrn_reflns_number 4239 _diffrn_reflns_av_R_equivalents 0.075 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 29.71 _diffrn_reflns_reduction_process 4239 _reflns_number_total 1751 _diffrn_measured_fraction_theta_max 0.890 _diffrn_measured_fraction_theta_full 0.977 _diffrn_reflns_theta_full 26.37 _reflns_number_gt 1318 _reflns_threshold_expression I>3\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Altomare et al., 1997 ), KRYSTAL (REFERENCE) ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _refine_special_details ; The crystal is a twin such that the 0kl reflections have complete overlap, while 1kl has partial overlap and some contribution from the second twin, all other reflections could be resolved. The L.S. program was modified to take this into account. The substitution of Co with Zn was dealt with by means of 10 constraints, forcing them to have identical parameters except for the occupancies, which were forced to add up to 1.00. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w= 1/{[\s~cs~(F^2^)+B+(1+A)F^2^]^1/2^- |F|}^2^ where A = 0.03 and B = 0.0 ; _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method ; Type 1 Lorentzian isotropic (Becker & Coppens, 1974) ; _refine_ls_extinction_coef 12(2) _refine_ls_number_reflns 1318 _refine_ls_number_parameters 131 _refine_ls_number_restraints 0 _refine_ls_number_constraints 10 _refine_ls_R_factor_gt 0.032 _refine_ls_wR_factor_ref 0.043 _refine_ls_goodness_of_fit_ref 1.370 _refine_ls_shift/su_max 0.0060 _refine_ls_shift/su_mean 0.0003 _refine_diff_density_max 1.4(3) _refine_diff_density_min -1.1(3) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy Co1 -0.01755(10) 0.37450(7) 0.72016(9) 0.0048(4) Uij 1.00 Co2 0.38317(10) 0.36629(7) 0.97021(9) 0.0043(4) Uij 1.00 Zn3 -0.13305(9) 0.12019(6) 0.93663(8) 0.0043(4) Uij 0.41(2) Co3 -0.13305 0.12019 0.93663 0.0043 Uij 0.59 P1 0.1093(2) 0.3316(1) 1.1353(2) 0.0048(8) Uij 1.00 P2 0.2928(2) 0.5871(1) 0.6737(2) 0.0042(8) Uij 1.00 O1 0.1328(5) 0.3710(3) 0.9817(5) 0.008(2) Uij 1.00 O2 0.1415(5) 0.4505(3) 1.2562(4) 0.006(2) Uij 1.00 O3 -0.0820(5) 0.2713(4) 1.0897(4) 0.007(2) Uij 1.00 O4 0.2609(5) 0.2301(3) 1.2348(4) 0.007(2) Uij 1.00 O5 0.4211(5) 0.5313(4) 0.5966(4) 0.007(2) Uij 1.00 O6 0.4100(5) 0.6877(4) 0.8050(4) 0.007(2) Uij 1.00 O7 0.1282(5) 0.6585(3) 0.5428(4) 0.006(2) Uij 1.00 O8 0.2301(5) 0.4682(3) 0.7478(5) 0.007(2) Uij 1.00 O9 0.6113(5) 0.4174(4) 0.9289(4) 0.007(2) Uij 1.00 H9a 0.6141 0.3914 0.8437 0.009 Uiso 1.00 H9b 0.7160 0.3950 0.9889 0.009 Uiso 1.00 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co1 0.0052(4) 0.0030(3) 0.0057(4) 0.0002(3) 0.0018(3) 0.0002(2) Co2 0.0041(4) 0.0029(3) 0.0051(4) 0.0001(3) 0.0010(3) 0.0006(2) Zn3 0.0048(4) 0.0029(3) 0.0038(4) 0.0001(2) 0.0002(3) -0.0002(2) Co3 0.0048(4) 0.0029(3) 0.0038(4) 0.0001(2) 0.0002(3) -0.0002(2) P1 0.0052(7) 0.0028(6) 0.0055(7) -0.0002(5) 0.0014(6) -0.0002(5) P2 0.0044(7) 0.0031(6) 0.0042(6) -0.0002(5) 0.0008(6) -0.0002(5) O1 0.008(2) 0.007(2) 0.008(2) 0.001(1) 0.003(2) 0.001(1) O2 0.005(2) 0.004(2) 0.005(2) 0.001(1) -0.001(2) 0.000(1) O3 0.006(2) 0.008(2) 0.005(2) -0.001(1) 0.001(2) -0.003(1) O4 0.008(2) 0.006(2) 0.005(2) 0.001(1) 0.000(2) 0.002(1) O5 0.007(2) 0.007(2) 0.009(2) 0.000(1) 0.004(2) -0.001(1) O6 0.007(2) 0.004(2) 0.007(2) -0.001(1) 0.001(2) 0.001(1) O7 0.008(2) 0.003(2) 0.005(2) 0.001(1) 0.000(2) 0.003(1) O8 0.010(2) 0.004(2) 0.007(2) -0.001(1) 0.003(2) 0.002(1) O9 0.006(2) 0.009(2) 0.006(2) 0.001(1) 0.002(2) 0.000(1) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Co1 O1 2.180(4) . . Co1 O2 2.045(4) . 3_567 Co1 O4 2.097(4) . 4_454 Co1 O6 2.086(4) . 2_546 Co1 O7 2.204(4) . 3_566 Co1 O8 2.103(4) . . Co2 O1 2.042(4) . . Co2 O6 2.105(4) . 3_667 Co2 O7 2.056(4) . 2_546 Co2 O8 2.138(4) . . Co2 O9 2.063(4) . . Co2 O9 2.317(4) . 3_667 Co3 O2 2.004(4) . 4_454 Co3 O3 1.964(4) . . Co3 O4 2.235(4) . 4_454 Co3 O5 2.005(4) . 4_455 Co3 O5 2.032(4) . 2_546 P1 O1 1.528(4) . . P1 O3 1.531(4) . . P1 O4 1.548(4) . . P1 O2 1.555(4) . . P2 O8 1.534(4) . . P2 O7 1.539(4) . . P2 O6 1.541(4) . . P2 O5 1.555(4) . . 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_2 _geom_angle_site_symmetry_3 O6 Co1 O2 175.4(1) 2_546 . 3_567 O4 Co1 O2 87.4(1) 4_454 . 3_567 O8 Co1 O2 94.9(1) . . 3_567 O1 Co1 O2 88.6(1) . . 3_567 O7 Co1 O2 103.8(1) 3_566 . 3_567 O4 Co1 O6 88.0(1) 4_454 . 2_546 O8 Co1 O6 89.7(1) . . 2_546 O1 Co1 O6 92.0(1) . . 2_546 O7 Co1 O6 75.7(1) 3_566 . 2_546 O8 Co1 O4 169.9(2) . . 4_454 O1 Co1 O4 91.8(1) . . 4_454 O7 Co1 O4 90.9(1) 3_566 . 4_454 O1 Co1 O8 78.5(1) . . . O7 Co1 O8 98.1(1) 3_566 . . O7 Co1 O1 167.4(1) 3_566 . . O7 Co2 O1 90.3(2) 2_546 . . O9 Co2 O1 163.0(1) . . . O6 Co2 O1 110.9(2) 3_667 . . O8 Co2 O1 80.8(1) . . . O9 Co2 O1 79.7(1) 3_667 . . O9 Co2 O7 104.8(1) . . 2_546 O6 Co2 O7 78.6(1) 3_667 . 2_546 O8 Co2 O7 114.9(1) . . 2_546 O9 Co2 O7 159.5(1) 3_667 . 2_546 O6 Co2 O9 80.4(1) 3_667 . . O8 Co2 O9 85.6(1) . . . O9 Co2 O9 88.2(1) 3_667 . . O8 Co2 O6 162.9(1) . . 3_667 O9 Co2 O6 88.3(1) 3_667 . 3_667 O9 Co2 O8 81.4(1) 3_667 . . O5 Co3 O3 97.8(2) 4_455 . . O2 Co3 O3 134.6(2) 4_454 . . O5 Co3 O3 119.0(2) 2_546 . . O4 Co3 O3 88.6(1) 4_454 . . O2 Co3 O5 100.9(2) 4_454 . 4_455 O5 Co3 O5 80.5(2) 2_546 . 4_455 O4 Co3 O5 170.0(2) 4_454 . 4_455 O5 Co3 O2 104.8(2) 2_546 . 4_454 O4 Co3 O2 69.2(1) 4_454 . 4_454 O4 Co3 O5 103.1(1) 4_454 . 2_546 O3 P1 O1 109.2(2) . . . O4 P1 O1 109.9(2) . . . O2 P1 O1 113.7(2) . . . O4 P1 O3 111.3(2) . . . O2 P1 O3 110.3(2) . . . O2 P1 O4 102.2(2) . . . O7 P2 O8 111.1(2) . . . O6 P2 O8 111.0(2) . . . O5 P2 O8 108.4(2) . . . O6 P2 O7 111.2(2) . . . O5 P2 O7 109.1(2) . . . O5 P2 O6 105.7(2) . . . Co2 O1 P1 121.6(2) . . . Co1 O1 P1 141.0(2) . . . Co1 O1 Co2 93.7(2) . . . Co1 O2 P1 139.8(2) 3_567 . . Co1 O2 Co3 121.4(2) 3_567 . 4_555 Co3 O3 P1 112.7(2) . . . Co3 O3 H9b 104.6(2) . . 1_455 Co1 O4 P1 139.6(2) 4_555 . . Co3 O4 P1 89.8(2) 4_555 . . Co3 O4 Co1 109.1(2) 4_555 . 4_555 Co3 O4 H9a 95.1(1) 4_555 . 4_455 Co3 O5 P2 126.9(2) 4_554 . . Co3 O5 P2 130.7(2) 2_556 . . Co3 O5 Co3 99.5(2) 2_556 . 4_554 Co1 O6 P2 129.3(2) 2_556 . . Co2 O6 P2 125.2(2) 3_667 . . Co2 O6 Co1 97.7(2) 3_667 . 2_556 Co2 O7 P2 120.4(2) 2_556 . . Co1 O7 P2 127.5(2) 3_566 . . Co1 O7 Co2 95.5(1) 3_566 . 2_556 Co1 O8 P2 137.9(2) . . . Co2 O8 P2 127.6(2) . . . Co2 O8 Co1 93.2(1) . . . Co2 O9 Co2 91.8(1) 3_667 . . H9a O9 H9b 97.5 . . . Co2 O9 H9b 123.3 . . . Co2 O9 H9b 97.8 3_667 . . Co2 O9 H9a 117.0 . . . Co2 O9 H9a 130.9 3_667 . . loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A O9 H9a O4 0.823 2.172 2.887(5) 145.4 4_455 O9 H9b O3 0.821 1.932 2.703(5) 156.0 1_655 _chemical_name_common 'Cobalt zinc orthophosphate monohydrate' #===END ################ ## Compound 2 ## ################ data_2 _database_code_depnum_ccdc_archive 'CCDC 246851' _audit_creation_method 'SHELXL-97 plus manual editing' _chemical_name_systematic ; Cobalt zinc orthophosphate monohydrate ; _chemical_name_common 'Cobalt zinc orthophosphate monohydrate' _chemical_melting_point ? _chemical_formula_moiety 'Co0.72 H2 O9 P2 Zn2.28' _chemical_formula_sum 'Co0.72 H2 O9 P2 Zn2.28' _chemical_formula_weight 399.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.7021(6) _cell_length_b 4.8662(3) _cell_length_c 16.6722(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.388(3) _cell_angle_gamma 90.00 _cell_volume 702.88(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5159 _cell_measurement_theta_min 3.24 _cell_measurement_theta_max 30.52 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 767 _exptl_absorpt_coefficient_mu 9.880 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.378 _exptl_absorpt_correction_T_max 0.693 _exptl_absorpt_process_details ; SADABS v.2.10 (Sheldrick, 2003) Ratio of minimum to maximum apparent transmission: 0.544812 ; _exptl_special_details ; Metal site occupancies refined as free variables with all other parameters constrained to be equivalent (EXYZ, EADP). Occupancy Zn(1) = 0.86(1) : Co(1) = 0.14(1) Occupancy Zn(2) = 0.87(1) : Co(2) = 0.13(1) Occupancy Zn(3) = 0.55(1) : Co(3) = 0.45(1) H atoms located in difference Fourier map and refined with the two O---H distances restrained to a common value and the H...H distance restrained to be 1.6 times this value. ; _diffrn_ambient_temperature 100(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 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 6269 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 30.51 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.996 _reflns_number_total 2132 _reflns_number_gt 2042 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-8 (Bruker-Nonius, 2003)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a (Bruker, 2003)' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL v.6.10 (Sheldrick, 2000)' _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^)+(0.0255P)^2^+0.4179P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2132 _refine_ls_number_parameters 139 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0202 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0518 _refine_ls_wR_factor_gt 0.0513 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.718 _refine_diff_density_min -0.892 _refine_diff_density_rms 0.189 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 0.93428(2) 0.20182(4) 0.654218(12) 0.00456(8) Uani 0.860(13) 1 d P . . Zn2 Zn 0.82844(2) 0.20206(4) 0.443570(12) 0.00449(8) Uani 0.871(14) 1 d P . . Zn3 Zn 0.57567(3) 0.49776(4) 0.678855(13) 0.00563(8) Uani 0.546(13) 1 d P . . Co1 Co 0.93428(2) 0.20182(4) 0.654218(12) 0.00456(8) Uani 0.140(13) 1 d P . . Co2 Co 0.82844(2) 0.20206(4) 0.443570(12) 0.00449(8) Uani 0.129(14) 1 d P . . Co3 Co 0.57567(3) 0.49776(4) 0.678855(13) 0.00563(8) Uani 0.454(13) 1 d P . . P1 P 0.81794(5) 0.70658(9) 0.55528(3) 0.00452(11) Uani 1 1 d . . . P2 P 0.73598(5) 0.48933(8) 0.28166(3) 0.00477(11) Uani 1 1 d . . . O1 O 0.68511(15) 0.7455(3) 0.60597(8) 0.0071(2) Uani 1 1 d . . . O2 O 0.59363(15) 0.6704(3) 0.25694(8) 0.0065(2) Uani 1 1 d . . . O3 O 0.86252(15) 0.3979(3) 0.54833(7) 0.0060(2) Uani 1 1 d . . . O4 O 0.75636(15) 0.2646(3) 0.21649(8) 0.0064(2) Uani 1 1 d . . . O5 O 0.78287(15) 0.8245(3) 0.47065(8) 0.0067(2) Uani 1 1 d . . . O6 O 0.96434(14) 0.8518(3) 0.59747(7) 0.0063(2) Uani 1 1 d . . . O7 O 0.88441(15) 0.6527(3) 0.29067(8) 0.0086(2) Uani 1 1 d . . . O8 O 0.69198(15) 0.3443(3) 0.35852(7) 0.0067(2) Uani 1 1 d . . . O9 O 0.52683(16) 0.2328(3) 0.58253(8) 0.0084(2) Uani 1 1 d D . . H1 H 0.438(3) 0.210(6) 0.567(2) 0.034(9) Uiso 1 1 d D . . H2 H 0.568(3) 0.085(5) 0.584(2) 0.037(9) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.00368(11) 0.00498(12) 0.00511(11) -0.00056(6) 0.00090(7) -0.00033(6) Zn2 0.00435(11) 0.00467(12) 0.00454(11) 0.00035(6) 0.00092(7) 0.00011(6) Zn3 0.00613(12) 0.00509(12) 0.00615(12) -0.00063(7) 0.00306(8) -0.00108(7) Co1 0.00368(11) 0.00498(12) 0.00511(11) -0.00056(6) 0.00090(7) -0.00033(6) Co2 0.00435(11) 0.00467(12) 0.00454(11) 0.00035(6) 0.00092(7) 0.00011(6) Co3 0.00613(12) 0.00509(12) 0.00615(12) -0.00063(7) 0.00306(8) -0.00108(7) P1 0.0041(2) 0.0046(2) 0.00506(19) -0.00010(14) 0.00133(15) -0.00017(13) P2 0.0036(2) 0.0054(2) 0.0053(2) 0.00002(14) 0.00095(14) -0.00001(14) O1 0.0063(6) 0.0071(5) 0.0085(6) 0.0005(5) 0.0034(4) 0.0004(4) O2 0.0050(6) 0.0067(5) 0.0081(5) 0.0011(4) 0.0020(4) 0.0010(4) O3 0.0062(5) 0.0053(6) 0.0065(5) -0.0006(4) 0.0012(4) 0.0004(4) O4 0.0054(6) 0.0070(5) 0.0072(5) -0.0011(4) 0.0024(4) -0.0005(4) O5 0.0075(6) 0.0065(5) 0.0060(5) 0.0013(4) 0.0004(4) -0.0003(4) O6 0.0050(5) 0.0061(5) 0.0079(5) -0.0021(4) 0.0014(4) -0.0002(4) O7 0.0061(6) 0.0102(5) 0.0094(6) -0.0006(5) 0.0003(5) -0.0026(4) O8 0.0066(6) 0.0076(5) 0.0059(5) 0.0013(4) 0.0010(4) 0.0004(4) O9 0.0063(6) 0.0085(6) 0.0102(6) -0.0010(5) -0.0004(5) 0.0008(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 O7 1.8874(13) 3_766 ? Zn1 O4 1.9503(13) 4_566 ? Zn1 O6 1.9778(13) 1_545 ? Zn1 O3 2.0518(12) . ? Zn2 O8 1.8930(13) . ? Zn2 O5 1.9419(13) 1_545 ? Zn2 O3 1.9872(12) . ? Zn2 O6 2.0049(13) 3_766 ? Zn3 O1 2.0136(13) . ? Zn3 O2 2.0693(13) 3_666 ? Zn3 O2 2.0710(13) 4_576 ? Zn3 O9 2.0723(14) . ? Zn3 O4 2.0763(13) 4_566 ? Zn3 O8 2.4762(13) 3_666 ? Zn3 P2 2.8509(5) 3_666 ? P1 O1 1.5066(13) . ? P1 O5 1.5272(13) . ? P1 O3 1.5585(13) . ? P1 O6 1.5648(13) . ? P2 O7 1.5122(14) . ? P2 O8 1.5424(13) . ? P2 O2 1.5442(13) . ? P2 O4 1.5633(13) . ? O9 H1 0.80(2) . ? O9 H2 0.80(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Zn1 O4 112.25(6) 3_766 4_566 ? O7 Zn1 O6 114.44(6) 3_766 1_545 ? O4 Zn1 O6 118.30(5) 4_566 1_545 ? O7 Zn1 O3 114.68(5) 3_766 . ? O4 Zn1 O3 103.09(5) 4_566 . ? O6 Zn1 O3 91.84(5) 1_545 . ? O8 Zn2 O5 113.12(6) . 1_545 ? O8 Zn2 O3 120.96(5) . . ? O5 Zn2 O3 105.44(5) 1_545 . ? O8 Zn2 O6 108.25(5) . 3_766 ? O5 Zn2 O6 99.53(5) 1_545 3_766 ? O3 Zn2 O6 107.33(5) . 3_766 ? O1 Zn3 O2 161.62(5) . 3_666 ? O1 Zn3 O2 84.28(5) . 4_576 ? O2 Zn3 O2 89.91(3) 3_666 4_576 ? O1 Zn3 O9 88.80(5) . . ? O2 Zn3 O9 92.90(5) 3_666 . ? O2 Zn3 O9 166.00(5) 4_576 . ? O1 Zn3 O4 99.38(5) . 4_566 ? O2 Zn3 O4 98.99(5) 3_666 4_566 ? O2 Zn3 O4 106.21(5) 4_576 4_566 ? O9 Zn3 O4 86.90(5) . 4_566 ? O1 Zn3 O8 98.58(5) . 3_666 ? O2 Zn3 O8 63.54(5) 3_666 3_666 ? O2 Zn3 O8 85.97(5) 4_576 3_666 ? O9 Zn3 O8 83.03(5) . 3_666 ? O4 Zn3 O8 159.18(5) 4_566 3_666 ? O1 Zn3 P2 129.81(4) . 3_666 ? O2 Zn3 P2 31.82(4) 3_666 3_666 ? O2 Zn3 P2 81.66(4) 4_576 3_666 ? O9 Zn3 P2 93.57(4) . 3_666 ? O4 Zn3 P2 130.81(4) 4_566 3_666 ? O8 Zn3 P2 32.71(3) 3_666 3_666 ? O1 P1 O5 111.94(8) . . ? O1 P1 O3 111.87(7) . . ? O5 P1 O3 108.84(7) . . ? O1 P1 O6 109.04(7) . . ? O5 P1 O6 109.23(7) . . ? O3 P1 O6 105.72(7) . . ? O7 P2 O8 115.75(7) . . ? O7 P2 O2 112.51(7) . . ? O8 P2 O2 103.14(7) . . ? O7 P2 O4 106.57(7) . . ? O8 P2 O4 108.09(7) . . ? O2 P2 O4 110.74(7) . . ? O7 P2 Zn3 141.97(6) . 3_666 ? O4 P2 Zn3 110.39(5) . 3_666 ? P1 O1 Zn3 133.98(8) . . ? P2 O2 Zn3 103.21(6) . 3_666 ? P2 O2 Zn3 128.61(7) . 4_575 ? Co3 O2 Zn3 128.18(6) 3_666 4_575 ? Zn3 O2 Zn3 128.18(6) 3_666 4_575 ? P1 O3 Zn2 120.66(7) . . ? P1 O3 Zn1 116.23(7) . . ? Zn2 O3 Zn1 122.79(6) . . ? P2 O4 Zn1 117.32(7) . 4_565 ? P2 O4 Zn3 120.54(7) . 4_565 ? Zn1 O4 Zn3 120.47(6) 4_565 4_565 ? P1 O5 Zn2 122.87(8) . 1_565 ? P1 O6 Zn1 117.73(7) . 1_565 ? P1 O6 Zn2 120.53(7) . 3_766 ? Zn1 O6 Zn2 116.07(6) 1_565 3_766 ? P2 O7 Zn1 155.88(9) . 3_766 ? P2 O8 Zn2 127.04(8) . . ? P2 O8 Zn3 87.13(6) . 3_666 ? Zn2 O8 Zn3 144.20(6) . 3_666 ? Zn3 O9 H1 117(2) . . ? Zn3 O9 H2 119(2) . . ? H1 O9 H2 107.4(17) . . ? 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 O5 P1 O1 Zn3 133.35(10) . . . . ? O3 P1 O1 Zn3 10.89(14) . . . . ? O6 P1 O1 Zn3 -105.68(11) . . . . ? O2 Zn3 O1 P1 -153.15(13) 3_666 . . . ? O2 Zn3 O1 P1 134.66(12) 4_576 . . . ? O9 Zn3 O1 P1 -57.53(11) . . . . ? O4 Zn3 O1 P1 29.13(12) 4_566 . . . ? O8 Zn3 O1 P1 -140.30(11) 3_666 . . . ? P2 Zn3 O1 P1 -151.19(8) 3_666 . . . ? O7 P2 O2 Zn3 -142.34(7) . . . 3_666 ? O8 P2 O2 Zn3 -16.91(8) . . . 3_666 ? O4 P2 O2 Zn3 98.51(7) . . . 3_666 ? O7 P2 O2 Zn3 37.45(12) . . . 4_575 ? O8 P2 O2 Zn3 162.88(9) . . . 4_575 ? O4 P2 O2 Zn3 -81.70(10) . . . 4_575 ? Zn3 P2 O2 Zn3 179.79(13) 3_666 . . 4_575 ? O1 P1 O3 Zn2 112.41(9) . . . . ? O5 P1 O3 Zn2 -11.81(10) . . . . ? O6 P1 O3 Zn2 -129.03(8) . . . . ? O1 P1 O3 Zn1 -61.19(10) . . . . ? O5 P1 O3 Zn1 174.59(7) . . . . ? O6 P1 O3 Zn1 57.37(9) . . . . ? O8 Zn2 O3 P1 -17.91(11) . . . . ? O5 Zn2 O3 P1 -147.75(8) 1_545 . . . ? O6 Zn2 O3 P1 106.82(9) 3_766 . . . ? O8 Zn2 O3 Zn1 155.26(7) . . . . ? O5 Zn2 O3 Zn1 25.42(8) 1_545 . . . ? O6 Zn2 O3 Zn1 -80.01(8) 3_766 . . . ? O7 Zn1 O3 P1 -62.24(9) 3_766 . . . ? O4 Zn1 O3 P1 60.07(9) 4_566 . . . ? O6 Zn1 O3 P1 179.70(8) 1_545 . . . ? O7 Zn1 O3 Zn2 124.30(8) 3_766 . . . ? O4 Zn1 O3 Zn2 -113.39(8) 4_566 . . . ? O6 Zn1 O3 Zn2 6.25(8) 1_545 . . . ? O7 P2 O4 Zn1 -11.16(10) . . . 4_565 ? O8 P2 O4 Zn1 -136.19(8) . . . 4_565 ? O2 P2 O4 Zn1 111.51(8) . . . 4_565 ? Zn3 P2 O4 Zn1 159.72(5) 3_666 . . 4_565 ? O7 P2 O4 Zn3 -176.49(8) . . . 4_565 ? O8 P2 O4 Zn3 58.47(10) . . . 4_565 ? O2 P2 O4 Zn3 -53.82(10) . . . 4_565 ? Zn3 P2 O4 Zn3 -5.62(9) 3_666 . . 4_565 ? O1 P1 O5 Zn2 89.47(10) . . . 1_565 ? O3 P1 O5 Zn2 -146.36(8) . . . 1_565 ? O6 P1 O5 Zn2 -31.40(11) . . . 1_565 ? O1 P1 O6 Zn1 -36.64(10) . . . 1_565 ? O5 P1 O6 Zn1 85.98(9) . . . 1_565 ? O3 P1 O6 Zn1 -157.06(7) . . . 1_565 ? O1 P1 O6 Zn2 170.96(8) . . . 3_766 ? O5 P1 O6 Zn2 -66.42(10) . . . 3_766 ? O3 P1 O6 Zn2 50.53(9) . . . 3_766 ? O8 P2 O7 Zn1 0.2(3) . . . 3_766 ? O2 P2 O7 Zn1 118.4(2) . . . 3_766 ? O4 P2 O7 Zn1 -120.0(2) . . . 3_766 ? Zn3 P2 O7 Zn1 73.9(3) 3_666 . . 3_766 ? O7 P2 O8 Zn2 -31.37(12) . . . . ? O2 P2 O8 Zn2 -154.68(9) . . . . ? O4 P2 O8 Zn2 88.02(10) . . . . ? Zn3 P2 O8 Zn2 -168.38(11) 3_666 . . . ? O7 P2 O8 Zn3 137.01(7) . . . 3_666 ? O2 P2 O8 Zn3 13.71(6) . . . 3_666 ? O4 P2 O8 Zn3 -103.60(6) . . . 3_666 ? O5 Zn2 O8 P2 -128.98(9) 1_545 . . . ? O3 Zn2 O8 P2 104.61(10) . . . . ? O6 Zn2 O8 P2 -19.69(11) 3_766 . . . ? O5 Zn2 O8 Zn3 71.13(12) 1_545 . . 3_666 ? O3 Zn2 O8 Zn3 -55.28(13) . . . 3_666 ? O6 Zn2 O8 Zn3 -179.58(10) 3_766 . . 3_666 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H1 O5 0.80(3) 1.97(3) 2.771(2) 177(3) 3_666 O9 H2 O1 0.80(2) 1.96(3) 2.7514(18) 169(3) 1_545 #===END