data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Co1.50 F2 H5 N O4 P' _chemical_formula_weight 240.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'N' 'N' 0.0061 0.0033 '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' 'Co' 'Co' 0.3494 0.9721 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c 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 10.050(2) _cell_length_b 7.4652(15) _cell_length_c 7.4871(15) _cell_angle_alpha 90.00 _cell_angle_beta 105.83(3) _cell_angle_gamma 90.00 _cell_volume 540.43(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 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.955 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 470 _exptl_absorpt_coefficient_mu 4.945 _exptl_absorpt_correction_type none _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 6188 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 27.98 _reflns_number_total 1285 _reflns_number_gt 1123 _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^)+(0.0539P)^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 1285 _refine_ls_number_parameters 108 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.039 _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 0.81814(3) 0.22763(5) 0.57239(4) 0.00964(13) Uani 1 1 d . . . Co2 Co 1.0000 0.5000 0.5000 0.00952(14) Uani 1 2 d S . . P1 P 1.15688(6) 0.11680(8) 0.68499(8) 0.00876(15) Uani 1 1 d . . . O1 O 0.87796(19) 0.4867(2) 0.6782(3) 0.0135(4) Uani 1 1 d . . . O2 O 1.03225(19) 0.2308(3) 0.5894(3) 0.0142(4) Uani 1 1 d . . . O3 O 0.77820(19) -0.0233(2) 0.4515(2) 0.0134(4) Uani 1 1 d . . . O4 O 1.2756(2) 0.2456(3) 0.7978(3) 0.0154(4) Uani 1 1 d D . . H5 H 1.253(4) 0.315(5) 0.878(5) 0.048(13) Uiso 1 1 d D . . F1 F 0.82752(14) 0.1253(2) 0.83003(18) 0.0124(3) Uani 1 1 d . . . F2 F 0.61566(17) 0.2647(2) 0.5396(2) 0.0198(4) Uani 1 1 d . . . N1 N 0.5298(3) 0.0188(4) 0.7486(4) 0.0225(5) Uani 1 1 d D . . H4 H 0.4448(19) -0.024(5) 0.709(6) 0.064(16) Uiso 1 1 d D . . H3 H 0.543(4) 0.093(4) 0.662(3) 0.041(12) Uiso 1 1 d D . . H2 H 0.547(3) 0.080(3) 0.855(2) 0.018(8) Uiso 1 1 d D . . H1 H 0.588(3) -0.073(3) 0.768(4) 0.025(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 Co1 0.01203(19) 0.0091(2) 0.00809(19) 0.00009(11) 0.00333(13) -0.00064(12) Co2 0.0120(2) 0.0085(3) 0.0088(2) -0.00018(15) 0.00402(18) -0.00100(16) P1 0.0106(3) 0.0082(3) 0.0081(3) 0.0007(2) 0.0037(2) 0.0002(2) O1 0.0194(9) 0.0119(10) 0.0118(8) -0.0045(6) 0.0087(7) -0.0032(7) O2 0.0134(9) 0.0135(10) 0.0152(9) 0.0052(6) 0.0030(7) 0.0016(7) O3 0.0175(9) 0.0119(9) 0.0126(8) -0.0011(7) 0.0073(7) 0.0000(7) O4 0.0135(9) 0.0162(10) 0.0169(9) -0.0068(7) 0.0047(7) -0.0040(7) F1 0.0160(7) 0.0141(8) 0.0071(6) 0.0010(5) 0.0030(5) 0.0011(5) F2 0.0143(7) 0.0235(10) 0.0219(8) 0.0062(6) 0.0054(6) 0.0020(6) N1 0.0198(12) 0.0224(14) 0.0264(13) -0.0059(10) 0.0082(10) -0.0027(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 F2 2.0014(17) . ? Co1 F1 2.0528(14) . ? Co1 O3 2.0716(19) . ? Co1 O1 2.1140(18) . ? Co1 O2 2.121(2) . ? Co1 F1 2.1448(15) 4_565 ? Co1 Co2 2.8825(5) . ? Co2 O1 2.0461(19) . ? Co2 O1 2.0461(19) 3_766 ? Co2 F1 2.0726(15) 4_565 ? Co2 F1 2.0726(15) 2_756 ? Co2 O2 2.1152(19) . ? Co2 O2 2.1152(19) 3_766 ? Co2 Co1 2.8825(5) 3_766 ? P1 O1 1.5203(19) 2_746 ? P1 O2 1.5218(19) . ? P1 O3 1.5234(19) 3_756 ? P1 O4 1.585(2) . ? O1 P1 1.5203(19) 2_756 ? O3 P1 1.5234(19) 3_756 ? F1 Co2 2.0726(15) 2_746 ? F1 Co1 2.1448(15) 4_566 ? 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 F2 Co1 F1 87.22(7) . . ? F2 Co1 O3 90.12(7) . . ? F1 Co1 O3 91.60(7) . . ? F2 Co1 O1 95.46(8) . . ? F1 Co1 O1 93.03(7) . . ? O3 Co1 O1 172.91(7) . . ? F2 Co1 O2 170.71(7) . . ? F1 Co1 O2 99.32(7) . . ? O3 Co1 O2 96.24(7) . . ? O1 Co1 O2 77.72(7) . . ? F2 Co1 F1 95.92(7) . 4_565 ? F1 Co1 F1 169.77(5) . 4_565 ? O3 Co1 F1 98.11(7) . 4_565 ? O1 Co1 F1 77.00(7) . 4_565 ? O2 Co1 F1 76.53(7) . 4_565 ? F2 Co1 Co2 123.70(5) . . ? F1 Co1 Co2 124.77(5) . . ? O3 Co1 Co2 127.80(5) . . ? O1 Co1 Co2 45.17(5) . . ? O2 Co1 Co2 47.04(5) . . ? F1 Co1 Co2 45.85(4) 4_565 . ? O1 Co2 O1 180.0 . 3_766 ? O1 Co2 F1 80.13(7) . 4_565 ? O1 Co2 F1 99.87(7) 3_766 4_565 ? O1 Co2 F1 99.87(7) . 2_756 ? O1 Co2 F1 80.13(7) 3_766 2_756 ? F1 Co2 F1 180.0 4_565 2_756 ? O1 Co2 O2 79.34(8) . . ? O1 Co2 O2 100.66(8) 3_766 . ? F1 Co2 O2 78.21(7) 4_565 . ? F1 Co2 O2 101.79(7) 2_756 . ? O1 Co2 O2 100.66(8) . 3_766 ? O1 Co2 O2 79.34(8) 3_766 3_766 ? F1 Co2 O2 101.79(7) 4_565 3_766 ? F1 Co2 O2 78.21(7) 2_756 3_766 ? O2 Co2 O2 180.000(1) . 3_766 ? O1 Co2 Co1 47.12(5) . . ? O1 Co2 Co1 132.88(5) 3_766 . ? F1 Co2 Co1 47.94(4) 4_565 . ? F1 Co2 Co1 132.06(4) 2_756 . ? O2 Co2 Co1 47.20(5) . . ? O2 Co2 Co1 132.80(5) 3_766 . ? O1 Co2 Co1 132.88(5) . 3_766 ? O1 Co2 Co1 47.12(5) 3_766 3_766 ? F1 Co2 Co1 132.06(4) 4_565 3_766 ? F1 Co2 Co1 47.94(4) 2_756 3_766 ? O2 Co2 Co1 132.80(5) . 3_766 ? O2 Co2 Co1 47.20(5) 3_766 3_766 ? Co1 Co2 Co1 180.000(10) . 3_766 ? O1 P1 O2 111.27(11) 2_746 . ? O1 P1 O3 112.26(11) 2_746 3_756 ? O2 P1 O3 112.88(11) . 3_756 ? O1 P1 O4 107.86(11) 2_746 . ? O2 P1 O4 108.36(11) . . ? O3 P1 O4 103.73(11) 3_756 . ? P1 O1 Co2 134.23(11) 2_756 . ? P1 O1 Co1 137.96(12) 2_756 . ? Co2 O1 Co1 87.70(7) . . ? P1 O2 Co2 135.68(12) . . ? P1 O2 Co1 135.52(12) . . ? Co2 O2 Co1 85.76(7) . . ? P1 O3 Co1 129.79(11) 3_756 . ? Co1 F1 Co2 124.14(7) . 2_746 ? Co1 F1 Co1 127.10(8) . 4_566 ? Co2 F1 Co1 86.22(5) 2_746 4_566 ? 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 O4 H5 O3 0.874(19) 1.84(2) 2.711(3) 174(5) 2_756 N1 H4 O3 0.883(13) 2.26(2) 3.049(3) 148(3) 3_656 N1 H4 F2 0.883(13) 2.54(4) 3.091(3) 121(4) 3_656 N1 H3 F2 0.891(13) 1.838(16) 2.702(3) 163(3) . N1 H2 F2 0.894(13) 1.791(16) 2.660(3) 163(3) 4_566 N1 H1 O4 0.885(13) 2.081(18) 2.911(3) 156(3) 2_746 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.549 _refine_diff_density_min -0.982 _refine_diff_density_rms 0.151 # and data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Co12 F8 H32 N4 O48 P12' _chemical_formula_weight 2087.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.917(4) _cell_length_b 7.5116(15) _cell_length_c 7.5942(15) _cell_angle_alpha 90.00 _cell_angle_beta 102.76(3) _cell_angle_gamma 90.00 _cell_volume 1108.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 4.973 _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 5077 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 28.06 _reflns_number_total 1324 _reflns_number_gt 1009 _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^)+(0.0543P)^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 1324 _refine_ls_number_parameters 98 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0826 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.952 _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 -0.2500 0.2500 -0.5000 0.01016(19) Uani 1 2 d S . . Co2 Co -0.16005(3) 0.52008(7) -0.30539(7) 0.01073(16) Uani 1 1 d . . . P1 P -0.17405(5) 0.14008(13) -0.07935(12) 0.0089(2) Uani 1 1 d . . . P2 P 0.0000 0.37975(18) -0.2500 0.0109(3) Uani 1 2 d S . . F1 F -0.16327(12) 0.3718(3) -0.5549(3) 0.0133(5) Uani 1 1 d . . . O1 O -0.18963(15) 0.2619(4) -0.2425(4) 0.0154(6) Uani 1 1 d . . . O2 O -0.14540(15) 0.2358(4) 0.0949(4) 0.0162(6) Uani 1 1 d . . . O3 O -0.05779(15) 0.4851(4) -0.2070(4) 0.0203(7) Uani 1 1 d . . . O4 O 0.02987(16) 0.2448(4) -0.0947(4) 0.0223(7) Uani 1 1 d . . . H4 H 0.0734 0.2675 -0.0368 0.033 Uiso 1 1 d R . . O5 O -0.23359(15) 0.0170(4) -0.0727(4) 0.0155(6) Uani 1 1 d . . . O6 O -0.11336(14) 0.0177(4) -0.1051(4) 0.0134(6) Uani 1 1 d . . . H6 H -0.1282 -0.0775 -0.1872 0.020 Uiso 1 1 d R . . N1 N 0.0000 0.1430(7) -0.7500 0.0211(11) Uani 1 2 d SD . . H1N H -0.0220 0.2050 -0.8591 0.025 Uiso 1 1 d RD . . H2N H 0.0322 0.0656 -0.7799 0.025 Uiso 1 1 d RD . . 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 0.0112(4) 0.0101(4) 0.0087(3) -0.0006(3) 0.0012(3) -0.0015(3) Co2 0.0103(3) 0.0113(3) 0.0104(3) 0.0001(2) 0.0018(2) -0.0001(2) P1 0.0089(5) 0.0086(4) 0.0088(4) 0.0009(3) 0.0009(4) 0.0002(4) P2 0.0090(7) 0.0107(6) 0.0125(6) 0.000 0.0013(5) 0.000 F1 0.0149(12) 0.0152(11) 0.0103(10) 0.0002(9) 0.0038(9) -0.0020(9) O1 0.0206(15) 0.0133(14) 0.0101(12) 0.0038(11) -0.0014(11) -0.0048(11) O2 0.0211(15) 0.0134(14) 0.0108(12) -0.0031(11) -0.0039(12) 0.0025(12) O3 0.0100(14) 0.0243(16) 0.0254(16) -0.0066(13) 0.0016(12) 0.0017(12) O4 0.0237(17) 0.0209(16) 0.0192(15) 0.0091(12) -0.0019(13) -0.0014(13) O5 0.0133(14) 0.0128(14) 0.0195(14) 0.0027(11) 0.0015(12) -0.0029(11) O6 0.0094(13) 0.0118(13) 0.0205(14) -0.0031(11) 0.0069(11) 0.0057(11) N1 0.024(3) 0.024(3) 0.018(2) 0.000 0.008(2) 0.000 _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 2.059(3) . ? Co1 O1 2.059(3) 7_454 ? Co1 F1 2.077(2) . ? Co1 F1 2.077(2) 7_454 ? Co1 O5 2.125(3) 6 ? Co1 O5 2.125(3) 4_454 ? Co1 Co2 2.8879(8) . ? Co1 Co2 2.8879(8) 7_454 ? Co2 O3 2.026(3) . ? Co2 O2 2.029(3) 6_565 ? Co2 F1 2.082(2) 6_566 ? Co2 O1 2.112(3) . ? Co2 O5 2.116(3) 4_454 ? Co2 F1 2.187(2) . ? P1 O2 1.504(3) . ? P1 O5 1.513(3) . ? P1 O1 1.517(3) . ? P1 O6 1.565(3) . ? P2 O3 1.491(3) 2_554 ? P2 O3 1.491(3) . ? P2 O4 1.569(3) 2_554 ? P2 O4 1.569(3) . ? F1 Co2 2.082(2) 6_565 ? O2 Co2 2.029(3) 6_566 ? O4 H4 0.8976 . ? O5 Co2 2.116(3) 4_444 ? O5 Co1 2.125(3) 4_444 ? O6 H6 0.9519 . ? N1 H1N 0.9672 . ? N1 H2N 0.9307 . ? 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 180.00(18) . 7_454 ? O1 Co1 F1 80.46(10) . . ? O1 Co1 F1 99.54(10) 7_454 . ? O1 Co1 F1 99.54(10) . 7_454 ? O1 Co1 F1 80.46(10) 7_454 7_454 ? F1 Co1 F1 180.00(6) . 7_454 ? O1 Co1 O5 101.36(11) . 6 ? O1 Co1 O5 78.64(11) 7_454 6 ? F1 Co1 O5 100.43(10) . 6 ? F1 Co1 O5 79.57(10) 7_454 6 ? O1 Co1 O5 78.64(11) . 4_454 ? O1 Co1 O5 101.36(11) 7_454 4_454 ? F1 Co1 O5 79.57(10) . 4_454 ? F1 Co1 O5 100.43(10) 7_454 4_454 ? O5 Co1 O5 180.0 6 4_454 ? O1 Co1 Co2 46.93(8) . . ? O1 Co1 Co2 133.07(8) 7_454 . ? F1 Co1 Co2 48.99(6) . . ? F1 Co1 Co2 131.01(6) 7_454 . ? O5 Co1 Co2 133.04(8) 6 . ? O5 Co1 Co2 46.96(8) 4_454 . ? O1 Co1 Co2 133.07(8) . 7_454 ? O1 Co1 Co2 46.93(8) 7_454 7_454 ? F1 Co1 Co2 131.01(6) . 7_454 ? F1 Co1 Co2 48.99(6) 7_454 7_454 ? O5 Co1 Co2 46.96(8) 6 7_454 ? O5 Co1 Co2 133.04(8) 4_454 7_454 ? Co2 Co1 Co2 180.000(18) . 7_454 ? O3 Co2 O2 92.24(12) . 6_565 ? O3 Co2 F1 86.86(11) . 6_566 ? O2 Co2 F1 91.39(10) 6_565 6_566 ? O3 Co2 O1 96.05(12) . . ? O2 Co2 O1 169.85(10) 6_565 . ? F1 Co2 O1 94.90(10) 6_566 . ? O3 Co2 O5 170.99(11) . 4_454 ? O2 Co2 O5 93.40(11) 6_565 4_454 ? F1 Co2 O5 100.02(11) 6_566 4_454 ? O1 Co2 O5 77.68(11) . 4_454 ? O3 Co2 F1 95.05(11) . . ? O2 Co2 F1 96.67(10) 6_565 . ? F1 Co2 F1 171.63(8) 6_566 . ? O1 Co2 F1 76.81(10) . . ? O5 Co2 F1 77.32(10) 4_454 . ? O3 Co2 Co1 123.85(9) . . ? O2 Co2 Co1 124.61(8) 6_565 . ? F1 Co2 Co1 126.92(7) 6_566 . ? O1 Co2 Co1 45.42(7) . . ? O5 Co2 Co1 47.20(8) 4_454 . ? F1 Co2 Co1 45.78(6) . . ? O2 P1 O5 114.25(17) . . ? O2 P1 O1 113.58(17) . . ? O5 P1 O1 112.05(16) . . ? O2 P1 O6 103.75(16) . . ? O5 P1 O6 106.13(16) . . ? O1 P1 O6 106.06(17) . . ? O3 P2 O3 115.9(3) 2_554 . ? O3 P2 O4 111.17(17) 2_554 2_554 ? O3 P2 O4 108.93(16) . 2_554 ? O3 P2 O4 108.93(16) 2_554 . ? O3 P2 O4 111.17(17) . . ? O4 P2 O4 99.5(2) 2_554 . ? Co1 F1 Co2 123.38(11) . 6_565 ? Co1 F1 Co2 85.23(9) . . ? Co2 F1 Co2 126.29(11) 6_565 . ? P1 O1 Co1 136.13(17) . . ? P1 O1 Co2 136.22(17) . . ? Co1 O1 Co2 87.65(10) . . ? P1 O2 Co2 134.64(17) . 6_566 ? P2 O3 Co2 138.60(19) . . ? P2 O4 H4 114.2 . . ? P1 O5 Co2 134.02(17) . 4_444 ? P1 O5 Co1 138.76(18) . 4_444 ? Co2 O5 Co1 85.84(10) 4_444 4_444 ? P1 O6 H6 112.8 . . ? H1N N1 H2N 107.4 . . ? 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 O4 H4 F1 0.90 1.94 2.816(4) 165.7 2_554 O6 H6 O2 0.95 2.00 2.929(4) 163.3 6 O6 H6 F1 0.95 2.59 3.140(4) 117.3 6_556 N1 H1N O4 0.97 2.28 2.912(3) 122.5 1_554 N1 H1N O2 0.97 2.42 2.959(3) 115.1 1_554 N1 H2N O6 0.93 2.09 2.977(3) 157.7 5_554 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.508 _refine_diff_density_min -1.094 _refine_diff_density_rms 0.174 # and data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Co1.50 F H2 K0.50 O6 P1.50' _chemical_formula_weight 271.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'F' 'F' 0.0171 0.0103 '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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.773(4) _cell_length_b 7.4649(15) _cell_length_c 7.5566(15) _cell_angle_alpha 90.00 _cell_angle_beta 102.51(3) _cell_angle_gamma 90.00 _cell_volume 1088.9(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 0.156 _exptl_crystal_size_mid 0.143 _exptl_crystal_size_min 0.138 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 5.439 _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 5040 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.97 _reflns_number_total 1294 _reflns_number_gt 1205 _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^)+(0.0573P)^2^+3.6510P] 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 1294 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0980 _refine_ls_wR_factor_gt 0.0966 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _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 0.34008(2) 1.02080(6) 0.69319(5) 0.00778(17) Uani 1 1 d . . . Co2 Co 0.2500 0.7500 0.5000 0.00725(19) Uani 1 2 d S . . K1 K 0.5000 0.6518(2) 0.2500 0.0274(3) Uani 1 2 d S . . P1 P 0.17279(4) 1.14101(11) 0.57920(10) 0.0061(2) Uani 1 1 d . . . P2 P 0.5000 0.87315(16) 0.7500 0.0093(3) Uani 1 2 d S . . O1 O 0.23266(14) 1.0168(3) 0.5701(4) 0.0136(5) Uani 1 1 d . . . O2 O 0.31047(14) 0.7635(3) 0.7569(3) 0.0131(5) Uani 1 1 d . . . O3 O 0.11232(13) 1.0170(3) 0.6092(4) 0.0123(5) Uani 1 1 d . . . H3 H 0.1245 0.9628 0.7052 0.019 Uiso 1 1 calc R . . O4 O 0.35753(14) 1.2626(3) 0.5946(3) 0.0141(5) Uani 1 1 d . . . O5 O 0.44215(14) 0.9794(4) 0.7947(4) 0.0197(6) Uani 1 1 d . . . O6 O 0.52966(16) 0.7371(4) 0.9064(4) 0.0214(6) Uani 1 1 d . . . H6 H 0.4978 0.6778 0.9300 0.032 Uiso 1 1 calc R . . F1 F 0.33680(10) 1.1289(3) 0.9439(2) 0.0109(4) Uani 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 Co1 0.0092(3) 0.0090(3) 0.0057(3) 0.00022(14) 0.00274(17) 0.00010(15) Co2 0.0100(3) 0.0082(3) 0.0041(3) -0.0004(2) 0.0027(2) -0.0013(2) K1 0.0289(7) 0.0316(7) 0.0240(6) 0.000 0.0103(5) 0.000 P1 0.0078(4) 0.0064(4) 0.0046(4) -0.0009(3) 0.0022(3) -0.0001(3) P2 0.0092(5) 0.0096(6) 0.0100(5) 0.000 0.0038(4) 0.000 O1 0.0148(12) 0.0108(12) 0.0149(12) -0.0050(9) 0.0029(10) 0.0041(9) O2 0.0215(13) 0.0112(12) 0.0052(10) 0.0017(8) -0.0001(9) -0.0058(9) O3 0.0097(11) 0.0131(12) 0.0157(12) 0.0039(9) 0.0060(9) -0.0061(9) O4 0.0216(13) 0.0120(12) 0.0072(10) 0.0015(8) -0.0005(9) -0.0010(10) O5 0.0097(12) 0.0272(15) 0.0211(13) -0.0063(11) 0.0010(10) 0.0046(10) O6 0.0285(15) 0.0177(14) 0.0176(12) 0.0105(10) 0.0039(11) 0.0002(11) F1 0.0145(10) 0.0141(11) 0.0059(8) -0.0003(7) 0.0059(7) 0.0029(7) _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 O4 2.011(3) . ? Co1 O5 2.021(3) . ? Co1 F1 2.0731(19) . ? Co1 O2 2.094(3) . ? Co1 O1 2.126(3) . ? Co1 F1 2.179(2) 6_575 ? Co1 Co2 2.8747(7) . ? Co1 K1 3.9455(12) 5_676 ? Co2 O2 2.050(2) . ? Co2 O2 2.050(2) 7_566 ? Co2 F1 2.0634(19) 6_575 ? Co2 F1 2.0634(19) 4_546 ? Co2 O1 2.108(3) . ? Co2 O1 2.108(3) 7_566 ? Co2 Co1 2.8747(7) 7_566 ? K1 O6 2.855(3) 2_656 ? K1 O6 2.855(3) 1_554 ? K1 O4 2.879(3) 5_676 ? K1 O4 2.879(3) 6_575 ? K1 O3 2.946(2) 8_565 ? K1 O3 2.946(2) 7_566 ? K1 O5 3.028(3) 5_676 ? K1 O5 3.028(3) 6_575 ? K1 O6 3.141(3) 5_666 ? K1 O6 3.141(3) 6_565 ? K1 O3 3.271(3) 4_545 ? K1 O3 3.271(3) 3_545 ? P1 O4 1.503(3) 7_576 ? P1 O1 1.517(3) . ? P1 O2 1.517(2) 4_556 ? P1 O3 1.567(2) . ? P1 K1 3.7664(15) 3_455 ? P2 O5 1.490(3) 2_656 ? P2 O5 1.490(3) . ? P2 O6 1.572(3) 2_656 ? P2 O6 1.572(3) . ? P2 K1 3.546(2) 5_676 ? O2 P1 1.517(2) 4_546 ? O3 K1 2.946(2) 7_566 ? O3 K1 3.271(3) 3_455 ? O3 H3 0.8200 . ? O4 P1 1.503(3) 7_576 ? O4 K1 2.879(3) 5_676 ? O5 K1 3.028(3) 5_676 ? O6 K1 2.855(3) 1_556 ? O6 K1 3.141(3) 5_666 ? O6 H6 0.8200 . ? F1 Co2 2.0634(19) 4_556 ? F1 Co1 2.1791(19) 6_576 ? 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 O4 Co1 O5 92.32(12) . . ? O4 Co1 F1 91.78(9) . . ? O5 Co1 F1 86.51(10) . . ? O4 Co1 O2 170.89(9) . . ? O5 Co1 O2 94.50(12) . . ? F1 Co1 O2 94.66(9) . . ? O4 Co1 O1 94.92(11) . . ? O5 Co1 O1 169.86(10) . . ? F1 Co1 O1 100.32(9) . . ? O2 Co1 O1 77.59(10) . . ? O4 Co1 F1 96.63(9) . 6_575 ? O5 Co1 F1 95.16(10) . 6_575 ? F1 Co1 F1 171.35(6) . 6_575 ? O2 Co1 F1 76.76(9) . 6_575 ? O1 Co1 F1 76.98(9) . 6_575 ? O4 Co1 Co2 125.47(7) . . ? O5 Co1 Co2 122.89(9) . . ? F1 Co1 Co2 126.81(6) . . ? O2 Co1 Co2 45.45(7) . . ? O1 Co1 Co2 46.97(7) . . ? F1 Co1 Co2 45.67(5) 6_575 . ? O4 Co1 K1 44.49(8) . 5_676 ? O5 Co1 K1 48.90(9) . 5_676 ? F1 Co1 K1 80.94(6) . 5_676 ? O2 Co1 K1 143.17(8) . 5_676 ? O1 Co1 K1 139.23(8) . 5_676 ? F1 Co1 K1 106.55(6) 6_575 5_676 ? Co2 Co1 K1 152.206(17) . 5_676 ? O2 Co2 O2 180.000(1) . 7_566 ? O2 Co2 F1 80.36(9) . 6_575 ? O2 Co2 F1 99.64(9) 7_566 6_575 ? O2 Co2 F1 99.64(9) . 4_546 ? O2 Co2 F1 80.36(9) 7_566 4_546 ? F1 Co2 F1 180.00(11) 6_575 4_546 ? O2 Co2 O1 78.98(10) . . ? O2 Co2 O1 101.02(10) 7_566 . ? F1 Co2 O1 79.95(9) 6_575 . ? F1 Co2 O1 100.05(9) 4_546 . ? O2 Co2 O1 101.02(10) . 7_566 ? O2 Co2 O1 78.98(10) 7_566 7_566 ? F1 Co2 O1 100.05(9) 6_575 7_566 ? F1 Co2 O1 79.95(9) 4_546 7_566 ? O1 Co2 O1 180.0 . 7_566 ? O2 Co2 Co1 46.72(7) . . ? O2 Co2 Co1 133.28(7) 7_566 . ? F1 Co2 Co1 49.06(5) 6_575 . ? F1 Co2 Co1 130.94(5) 4_546 . ? O1 Co2 Co1 47.51(7) . . ? O1 Co2 Co1 132.49(7) 7_566 . ? O2 Co2 Co1 133.28(7) . 7_566 ? O2 Co2 Co1 46.72(7) 7_566 7_566 ? F1 Co2 Co1 130.94(5) 6_575 7_566 ? F1 Co2 Co1 49.06(5) 4_546 7_566 ? O1 Co2 Co1 132.49(7) . 7_566 ? O1 Co2 Co1 47.51(7) 7_566 7_566 ? Co1 Co2 Co1 180.0 . 7_566 ? O6 K1 O6 154.24(13) 2_656 1_554 ? O6 K1 O4 87.43(8) 2_656 5_676 ? O6 K1 O4 86.90(8) 1_554 5_676 ? O6 K1 O4 86.90(8) 2_656 6_575 ? O6 K1 O4 87.43(8) 1_554 6_575 ? O4 K1 O4 154.38(12) 5_676 6_575 ? O6 K1 O3 138.02(8) 2_656 8_565 ? O6 K1 O3 56.46(8) 1_554 8_565 ? O4 K1 O3 59.64(7) 5_676 8_565 ? O4 K1 O3 134.04(7) 6_575 8_565 ? O6 K1 O3 56.46(8) 2_656 7_566 ? O6 K1 O3 138.02(8) 1_554 7_566 ? O4 K1 O3 134.04(7) 5_676 7_566 ? O4 K1 O3 59.64(7) 6_575 7_566 ? O3 K1 O3 129.33(12) 8_565 7_566 ? O6 K1 O5 93.19(9) 2_656 5_676 ? O6 K1 O5 62.54(8) 1_554 5_676 ? O4 K1 O5 58.93(7) 5_676 5_676 ? O4 K1 O5 96.48(8) 6_575 5_676 ? O3 K1 O5 90.93(7) 8_565 5_676 ? O3 K1 O5 139.63(8) 7_566 5_676 ? O6 K1 O5 62.54(8) 2_656 6_575 ? O6 K1 O5 93.19(9) 1_554 6_575 ? O4 K1 O5 96.48(8) 5_676 6_575 ? O4 K1 O5 58.93(7) 6_575 6_575 ? O3 K1 O5 139.63(8) 8_565 6_575 ? O3 K1 O5 90.93(7) 7_566 6_575 ? O5 K1 O5 49.22(10) 5_676 6_575 ? O6 K1 O6 119.33(9) 2_656 5_666 ? O6 K1 O6 85.54(8) 1_554 5_666 ? O4 K1 O6 116.41(8) 5_676 5_666 ? O4 K1 O6 88.00(8) 6_575 5_666 ? O3 K1 O6 64.06(8) 8_565 5_666 ? O3 K1 O6 69.30(8) 7_566 5_666 ? O5 K1 O6 147.40(7) 5_676 5_666 ? O5 K1 O6 146.92(8) 6_575 5_666 ? O6 K1 O6 85.54(8) 2_656 6_565 ? O6 K1 O6 119.33(9) 1_554 6_565 ? O4 K1 O6 88.00(8) 5_676 6_565 ? O4 K1 O6 116.41(8) 6_575 6_565 ? O3 K1 O6 69.30(8) 8_565 6_565 ? O3 K1 O6 64.06(8) 7_566 6_565 ? O5 K1 O6 146.92(8) 5_676 6_565 ? O5 K1 O6 147.40(7) 6_575 6_565 ? O6 K1 O6 44.92(10) 5_666 6_565 ? O6 K1 O3 125.94(8) 2_656 4_545 ? O6 K1 O3 63.27(8) 1_554 4_545 ? O4 K1 O3 146.63(6) 5_676 4_545 ? O4 K1 O3 45.68(6) 6_575 4_545 ? O3 K1 O3 89.90(7) 8_565 4_545 ? O3 K1 O3 74.85(6) 7_566 4_545 ? O5 K1 O3 113.09(8) 5_676 4_545 ? O5 K1 O3 99.62(7) 6_575 4_545 ? O6 K1 O3 50.63(7) 5_666 4_545 ? O6 K1 O3 93.77(8) 6_565 4_545 ? O6 K1 O3 63.27(8) 2_656 3_545 ? O6 K1 O3 125.94(8) 1_554 3_545 ? O4 K1 O3 45.68(6) 5_676 3_545 ? O4 K1 O3 146.63(6) 6_575 3_545 ? O3 K1 O3 74.85(5) 8_565 3_545 ? O3 K1 O3 89.90(7) 7_566 3_545 ? O5 K1 O3 99.62(7) 5_676 3_545 ? O5 K1 O3 113.09(8) 6_575 3_545 ? O6 K1 O3 93.77(8) 5_666 3_545 ? O6 K1 O3 50.63(7) 6_565 3_545 ? O3 K1 O3 144.18(10) 4_545 3_545 ? O4 P1 O1 114.85(15) 7_576 . ? O4 P1 O2 113.58(15) 7_576 4_556 ? O1 P1 O2 111.78(15) . 4_556 ? O4 P1 O3 103.68(15) 7_576 . ? O1 P1 O3 105.84(15) . . ? O2 P1 O3 106.03(14) 4_556 . ? O4 P1 K1 43.93(11) 7_576 3_455 ? O1 P1 K1 126.03(11) . 3_455 ? O2 P1 K1 122.18(11) 4_556 3_455 ? O3 P1 K1 59.78(10) . 3_455 ? O5 P2 O5 115.7(2) 2_656 . ? O5 P2 O6 110.69(16) 2_656 2_656 ? O5 P2 O6 109.55(16) . 2_656 ? O5 P2 O6 109.55(16) 2_656 . ? O5 P2 O6 110.69(16) . . ? O6 P2 O6 99.5(2) 2_656 . ? O5 P2 K1 57.83(12) 2_656 5_676 ? O5 P2 K1 57.83(12) . 5_676 ? O6 P2 K1 130.24(12) 2_656 5_676 ? O6 P2 K1 130.24(12) . 5_676 ? P1 O1 Co2 139.46(17) . . ? P1 O1 Co1 133.38(16) . . ? Co2 O1 Co1 85.51(9) . . ? P1 O2 Co2 136.28(16) 4_546 . ? P1 O2 Co1 135.88(15) 4_546 . ? Co2 O2 Co1 87.83(9) . . ? P1 O3 K1 164.52(15) . 7_566 ? P1 O3 K1 95.77(11) . 3_455 ? K1 O3 K1 90.10(7) 7_566 3_455 ? P1 O3 H3 109.5 . . ? K1 O3 H3 64.4 7_566 . ? K1 O3 H3 154.4 3_455 . ? P1 O4 Co1 133.24(16) 7_576 . ? P1 O4 K1 114.84(14) 7_576 5_676 ? Co1 O4 K1 106.21(10) . 5_676 ? P2 O5 Co1 138.42(18) . . ? P2 O5 K1 97.57(14) . 5_676 ? Co1 O5 K1 100.89(11) . 5_676 ? P2 O6 K1 135.32(16) . 1_556 ? P2 O6 K1 107.78(14) . 5_666 ? K1 O6 K1 94.46(8) 1_556 5_666 ? P2 O6 H6 109.5 . . ? K1 O6 H6 50.5 1_556 . ? K1 O6 H6 59.5 5_666 . ? Co2 F1 Co1 123.39(10) 4_556 . ? Co2 F1 Co1 85.26(7) 4_556 6_576 ? Co1 F1 Co1 126.12(10) . 6_576 ? 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 O3 H3 O4 0.82 2.10 2.897(4) 163.7 4_546 O6 H6 O3 0.82 2.45 3.233(4) 160.6 4_546 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.080 _refine_diff_density_min -1.577 _refine_diff_density_rms 0.212 # and data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'F Fe1.50 H2 K0.50 O6 P1.50' _chemical_formula_weight 266.80 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.003(4) _cell_length_b 7.4692(15) _cell_length_c 7.6879(15) _cell_angle_alpha 90.00 _cell_angle_beta 102.72(3) _cell_angle_gamma 90.00 _cell_volume 1120.4(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 0.160 _exptl_crystal_size_mid 0.154 _exptl_crystal_size_min 0.142 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.163 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 4.729 _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 6519 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 28.06 _reflns_number_total 1307 _reflns_number_gt 1047 _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^)+(0.0354P)^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 1307 _refine_ls_number_parameters 106 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0615 _refine_ls_wR_factor_gt 0.0601 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 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 Fe1 Fe 0.34159(2) 0.02446(6) 0.69574(6) 0.00959(12) Uani 1 1 d . . . Fe2 Fe 0.2500 -0.2500 0.5000 0.00960(15) Uani 1 2 d S . . P1 P 0.17303(3) 0.14021(10) 0.58151(11) 0.00880(17) Uani 1 1 d . . . P2 P 0.5000 -0.12978(15) 0.7500 0.0125(2) Uani 1 2 d S . . F1 F 0.33797(8) 0.1320(2) 0.9450(2) 0.0147(4) Uani 1 1 d . . . O1 O 0.23309(10) 0.0210(3) 0.5702(3) 0.0155(5) Uani 1 1 d . . . O2 O 0.31000(11) -0.2356(3) 0.7593(3) 0.0156(5) Uani 1 1 d . . . O3 O 0.11439(10) 0.0138(3) 0.6147(3) 0.0144(5) Uani 1 1 d D . . O4 O 0.35827(11) 0.2655(3) 0.5894(3) 0.0172(5) Uani 1 1 d . . . O5 O 0.44314(11) -0.0218(3) 0.7938(3) 0.0222(5) Uani 1 1 d . . . O6 O 0.52958(12) -0.2649(3) 0.9043(3) 0.0246(6) Uani 1 1 d D . . H6 H 0.5763(13) -0.245(8) 0.960(7) 0.09(2) Uiso 1 1 d D . . K1 K 0.0000 0.15065(16) 0.2500 0.0309(3) Uani 1 2 d S . . H3 H 0.126(4) -0.071(8) 0.701(8) 0.12(3) 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 Fe1 0.0093(2) 0.0094(2) 0.0096(2) 0.00034(17) 0.00107(15) -0.00005(15) Fe2 0.0111(3) 0.0091(3) 0.0082(3) -0.0014(2) 0.0013(2) -0.0019(2) P1 0.0092(3) 0.0080(3) 0.0089(4) -0.0008(3) 0.0012(3) -0.0004(3) P2 0.0094(5) 0.0127(5) 0.0150(7) 0.000 0.0015(4) 0.000 F1 0.0172(8) 0.0167(9) 0.0116(11) 0.0010(7) 0.0058(7) 0.0036(7) O1 0.0131(10) 0.0115(10) 0.0213(14) -0.0047(9) 0.0028(9) 0.0032(8) O2 0.0216(11) 0.0115(10) 0.0108(13) 0.0041(8) -0.0026(9) -0.0055(8) O3 0.0102(9) 0.0136(11) 0.0203(13) 0.0018(9) 0.0055(9) -0.0061(8) O4 0.0208(11) 0.0154(11) 0.0124(13) 0.0044(9) -0.0031(9) -0.0022(9) O5 0.0109(10) 0.0266(13) 0.0280(16) -0.0033(11) 0.0018(9) 0.0041(9) O6 0.0238(13) 0.0219(12) 0.0248(16) 0.0112(10) -0.0020(10) 0.0007(10) K1 0.0303(6) 0.0313(6) 0.0322(8) 0.000 0.0093(5) 0.000 _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 Fe1 O5 2.034(2) . ? Fe1 O4 2.035(2) . ? Fe1 F1 2.0938(19) . ? Fe1 O2 2.132(2) . ? Fe1 O1 2.173(2) . ? Fe1 F1 2.2419(18) 6 ? Fe1 Fe2 2.9343(7) . ? Fe1 K1 3.9396(11) 7_556 ? Fe2 O2 2.091(2) . ? Fe2 O2 2.091(2) 7_546 ? Fe2 F1 2.0927(16) 4_546 ? Fe2 F1 2.0927(16) 6 ? Fe2 O1 2.141(2) 7_546 ? Fe2 O1 2.141(2) . ? Fe2 Fe1 2.9343(7) 7_546 ? P1 O4 1.501(2) 7_556 ? P1 O1 1.513(2) . ? P1 O2 1.513(2) 4_556 ? P1 O3 1.570(2) . ? P1 K1 3.8206(15) . ? P2 O5 1.492(2) . ? P2 O5 1.492(2) 2_656 ? P2 O6 1.571(2) 2_656 ? P2 O6 1.571(2) . ? P2 K1 3.5787(18) 7_556 ? F1 Fe2 2.0927(16) 4_556 ? F1 Fe1 2.2419(18) 6_556 ? O2 P1 1.513(2) 4_546 ? O3 K1 2.979(2) 5_556 ? O3 K1 3.364(3) . ? O4 P1 1.501(2) 7_556 ? O4 K1 2.900(2) 7_556 ? O5 K1 3.043(3) 7_556 ? O6 K1 2.916(3) 3_546 ? O6 K1 3.123(3) 7_546 ? K1 O4 2.900(2) 7_556 ? K1 O4 2.900(2) 8_455 ? K1 O6 2.916(3) 4_556 ? K1 O6 2.916(3) 3_454 ? K1 O3 2.979(2) 6 ? K1 O3 2.979(2) 5_556 ? K1 O5 3.043(3) 7_556 ? K1 O5 3.043(3) 8_455 ? K1 O6 3.123(3) 7_546 ? K1 O6 3.123(3) 8_445 ? K1 O3 3.364(3) 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 O5 Fe1 O4 93.47(9) . . ? O5 Fe1 F1 87.66(9) . . ? O4 Fe1 F1 94.00(8) . . ? O5 Fe1 O2 94.73(9) . . ? O4 Fe1 O2 168.83(9) . . ? F1 Fe1 O2 93.90(8) . . ? O5 Fe1 O1 168.73(9) . . ? O4 Fe1 O1 93.91(8) . . ? F1 Fe1 O1 100.30(8) . . ? O2 Fe1 O1 76.91(8) . . ? O5 Fe1 F1 94.05(9) . 6 ? O4 Fe1 F1 95.34(8) . 6 ? F1 Fe1 F1 170.38(5) . 6 ? O2 Fe1 F1 76.53(8) . 6 ? O1 Fe1 F1 76.80(8) . 6 ? O5 Fe1 Fe2 122.07(7) . . ? O4 Fe1 Fe2 123.45(7) . . ? F1 Fe1 Fe2 126.44(5) . . ? O2 Fe1 Fe2 45.42(6) . . ? O1 Fe1 Fe2 46.68(6) . . ? F1 Fe1 Fe2 45.28(4) 6 . ? O5 Fe1 K1 49.56(7) . 7_556 ? O4 Fe1 K1 45.44(6) . 7_556 ? F1 Fe1 K1 81.71(5) . 7_556 ? O2 Fe1 K1 143.98(6) . 7_556 ? O1 Fe1 K1 139.10(6) . 7_556 ? F1 Fe1 K1 106.57(5) 6 7_556 ? Fe2 Fe1 K1 151.821(18) . 7_556 ? O2 Fe2 O2 180.00(11) . 7_546 ? O2 Fe2 F1 99.24(8) . 4_546 ? O2 Fe2 F1 80.76(8) 7_546 4_546 ? O2 Fe2 F1 80.76(8) . 6 ? O2 Fe2 F1 99.24(8) 7_546 6 ? F1 Fe2 F1 180.00(4) 4_546 6 ? O2 Fe2 O1 101.51(8) . 7_546 ? O2 Fe2 O1 78.49(8) 7_546 7_546 ? F1 Fe2 O1 80.76(7) 4_546 7_546 ? F1 Fe2 O1 99.24(7) 6 7_546 ? O2 Fe2 O1 78.49(8) . . ? O2 Fe2 O1 101.51(8) 7_546 . ? F1 Fe2 O1 99.24(7) 4_546 . ? F1 Fe2 O1 80.76(7) 6 . ? O1 Fe2 O1 180.00(14) 7_546 . ? O2 Fe2 Fe1 133.42(6) . 7_546 ? O2 Fe2 Fe1 46.58(6) 7_546 7_546 ? F1 Fe2 Fe1 49.58(5) 4_546 7_546 ? F1 Fe2 Fe1 130.42(5) 6 7_546 ? O1 Fe2 Fe1 47.60(6) 7_546 7_546 ? O1 Fe2 Fe1 132.40(6) . 7_546 ? O2 Fe2 Fe1 46.58(6) . . ? O2 Fe2 Fe1 133.42(6) 7_546 . ? F1 Fe2 Fe1 130.42(5) 4_546 . ? F1 Fe2 Fe1 49.58(5) 6 . ? O1 Fe2 Fe1 132.40(6) 7_546 . ? O1 Fe2 Fe1 47.60(6) . . ? Fe1 Fe2 Fe1 180.00(2) 7_546 . ? O4 P1 O1 114.15(13) 7_556 . ? O4 P1 O2 113.35(13) 7_556 4_556 ? O1 P1 O2 111.58(13) . 4_556 ? O4 P1 O3 103.99(13) 7_556 . ? O1 P1 O3 106.65(12) . . ? O2 P1 O3 106.26(13) 4_556 . ? O4 P1 K1 42.64(9) 7_556 . ? O1 P1 K1 125.99(9) . . ? O2 P1 K1 122.40(9) 4_556 . ? O3 P1 K1 61.38(9) . . ? O5 P2 O5 114.6(2) . 2_656 ? O5 P2 O6 109.78(13) . 2_656 ? O5 P2 O6 110.85(14) 2_656 2_656 ? O5 P2 O6 110.85(14) . . ? O5 P2 O6 109.78(13) 2_656 . ? O6 P2 O6 100.1(2) 2_656 . ? O5 P2 K1 57.28(10) . 7_556 ? O5 P2 K1 57.28(10) 2_656 7_556 ? O6 P2 K1 129.97(10) 2_656 7_556 ? O6 P2 K1 129.97(10) . 7_556 ? Fe2 F1 Fe1 123.14(9) 4_556 . ? Fe2 F1 Fe1 85.14(6) 4_556 6_556 ? Fe1 F1 Fe1 125.86(8) . 6_556 ? P1 O1 Fe2 137.94(13) . . ? P1 O1 Fe1 134.06(13) . . ? Fe2 O1 Fe1 85.73(7) . . ? P1 O2 Fe2 135.95(13) 4_546 . ? P1 O2 Fe1 135.95(13) 4_546 . ? Fe2 O2 Fe1 88.00(8) . . ? P1 O3 K1 164.49(13) . 5_556 ? P1 O3 K1 94.44(10) . . ? K1 O3 K1 89.00(6) 5_556 . ? P1 O4 Fe1 133.88(14) 7_556 . ? P1 O4 K1 116.85(11) 7_556 7_556 ? Fe1 O4 K1 104.56(9) . 7_556 ? P2 O5 Fe1 139.19(16) . . ? P2 O5 K1 98.36(11) . 7_556 ? Fe1 O5 K1 99.86(9) . 7_556 ? P2 O6 K1 135.17(13) . 3_546 ? P2 O6 K1 107.30(13) . 7_546 ? K1 O6 K1 94.99(7) 3_546 7_546 ? O4 K1 O4 155.06(10) 7_556 8_455 ? O4 K1 O6 86.61(7) 7_556 4_556 ? O4 K1 O6 88.03(7) 8_455 4_556 ? O4 K1 O6 88.03(7) 7_556 3_454 ? O4 K1 O6 86.61(7) 8_455 3_454 ? O6 K1 O6 155.00(11) 4_556 3_454 ? O4 K1 O3 58.92(7) 7_556 6 ? O4 K1 O3 133.97(7) 8_455 6 ? O6 K1 O3 137.14(7) 4_556 6 ? O6 K1 O3 56.32(7) 3_454 6 ? O4 K1 O3 133.97(7) 7_556 5_556 ? O4 K1 O3 58.92(7) 8_455 5_556 ? O6 K1 O3 56.32(7) 4_556 5_556 ? O6 K1 O3 137.14(7) 3_454 5_556 ? O3 K1 O3 131.30(9) 6 5_556 ? O4 K1 O5 59.75(6) 7_556 7_556 ? O4 K1 O5 96.34(7) 8_455 7_556 ? O6 K1 O5 93.40(7) 4_556 7_556 ? O6 K1 O5 63.02(7) 3_454 7_556 ? O3 K1 O5 90.14(6) 6 7_556 ? O3 K1 O5 138.48(7) 5_556 7_556 ? O4 K1 O5 96.34(7) 7_556 8_455 ? O4 K1 O5 59.75(6) 8_455 8_455 ? O6 K1 O5 63.02(7) 4_556 8_455 ? O6 K1 O5 93.40(7) 3_454 8_455 ? O3 K1 O5 138.48(7) 6 8_455 ? O3 K1 O5 90.14(6) 5_556 8_455 ? O5 K1 O5 48.72(8) 7_556 8_455 ? O4 K1 O6 116.53(7) 7_556 7_546 ? O4 K1 O6 87.24(6) 8_455 7_546 ? O6 K1 O6 119.11(8) 4_556 7_546 ? O6 K1 O6 85.01(7) 3_454 7_546 ? O3 K1 O6 65.33(6) 6 7_546 ? O3 K1 O6 69.90(7) 5_556 7_546 ? O5 K1 O6 147.43(7) 7_556 7_546 ? O5 K1 O6 146.98(6) 8_455 7_546 ? O4 K1 O6 87.24(6) 7_556 8_445 ? O4 K1 O6 116.53(7) 8_455 8_445 ? O6 K1 O6 85.01(7) 4_556 8_445 ? O6 K1 O6 119.11(8) 3_454 8_445 ? O3 K1 O6 69.90(7) 6 8_445 ? O3 K1 O6 65.33(6) 5_556 8_445 ? O5 K1 O6 146.98(6) 7_556 8_445 ? O5 K1 O6 147.43(7) 8_455 8_445 ? O6 K1 O6 45.34(9) 7_546 8_445 ? O4 K1 O3 147.36(6) 7_556 2 ? O4 K1 O3 44.69(6) 8_455 2 ? O6 K1 O3 126.02(6) 4_556 2 ? O6 K1 O3 62.84(6) 3_454 2 ? O3 K1 O3 91.00(6) 6 2 ? O3 K1 O3 74.45(5) 5_556 2 ? O5 K1 O3 112.76(6) 7_556 2 ? O5 K1 O3 99.60(6) 8_455 2 ? O6 K1 O3 50.64(6) 7_546 2 ? O6 K1 O3 94.21(7) 8_445 2 ? O4 K1 O3 44.69(6) 7_556 . ? O4 K1 O3 147.36(6) 8_455 . ? O6 K1 O3 62.84(6) 4_556 . ? O6 K1 O3 126.02(6) 3_454 . ? O3 K1 O3 74.45(5) 6 . ? O3 K1 O3 91.00(6) 5_556 . ? O5 K1 O3 99.60(6) 7_556 . ? O5 K1 O3 112.76(6) 8_455 . ? O6 K1 O3 94.21(7) 7_546 . ? O6 K1 O3 50.64(6) 8_445 . ? O3 K1 O3 144.62(8) 2 . ? 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 O6 H6 F1 0.95(2) 1.91(3) 2.827(3) 162(5) 5_657 O3 H3 O4 0.91(2) 1.99(2) 2.892(3) 170(7) 4_546 _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.539 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.134