data_m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H8 Co2 N2 O8 P2' _chemical_formula_weight 343.88 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' _cell_length_a 10.7207(5) _cell_length_b 10.7207(5) _cell_length_c 8.7241(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 868.36(10) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 4914 _cell_measurement_theta_min 3.20 _cell_measurement_theta_max 28.31 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 4.212 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.2272 _exptl_absorpt_correction_T_max 0.3370 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5195 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 27.49 _reflns_number_total 1204 _reflns_number_gt 1199 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.4795P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 1204 _refine_ls_number_parameters 107 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0225 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0611 _refine_ls_wR_factor_gt 0.0608 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.128 _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 Co1 Co 0.82234(3) 0.14802(4) 0.48138(5) 0.01069(12) Uani 1 1 d . . . Co2 Co 0.6667 0.3333 0.85445(8) 0.01034(15) Uani 1 3 d S . . P1 P 1.14684(8) 0.32684(7) 0.36093(12) 0.0148(2) Uani 1 1 d . . . P2 P 0.6667 0.3333 0.4657(2) 0.0173(3) Uani 1 3 d S . . O1 O 1.1913(3) 0.4762(2) 0.4286(3) 0.0234(5) Uani 1 1 d . . . O2 O 1.0251(2) 0.2098(2) 0.4588(3) 0.0219(5) Uani 1 1 d . . . O3 O 0.7748(2) 0.0935(2) 0.6959(3) 0.0232(5) Uani 1 1 d . . . O4 O 0.6992(3) -0.0254(2) 0.3613(3) 0.0255(5) Uani 1 1 d . . . O5 O 0.6667 0.3333 0.6409(8) 0.0533(16) Uani 1 3 d S . . O6 O 0.7716(3) 0.2867(3) 0.4039(3) 0.0245(5) Uani 1 1 d . . . N1 N 0.0509(3) 0.5152(3) 0.6771(5) 0.0247(6) Uani 1 1 d D . . N2 N 1.0000 0.0000 0.6842(6) 0.0241(10) Uani 1 3 d SD . . H1 H 0.012(3) 0.434(3) 0.740(4) 0.030(11) Uiso 1 1 d D . . H2 H -0.026(3) 0.528(3) 0.640(4) 0.024(10) Uiso 1 1 d D . . H3 H 0.096(4) 0.507(4) 0.589(3) 0.047(13) Uiso 1 1 d D . . H4 H 0.117(4) 0.600(3) 0.730(4) 0.044(13) Uiso 1 1 d D . . H5 H 1.0000 0.0000 0.792(2) 0.20(7) Uiso 1 3 d SD . . H6 H 0.95(2) 0.04(2) 0.646(6) 0.31(10) 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 0.01100(17) 0.01170(17) 0.0096(2) -0.0001(2) 0.00017(17) 0.00586(12) Co2 0.01149(18) 0.01149(18) 0.0081(4) 0.000 0.000 0.00574(9) P1 0.0160(4) 0.0158(4) 0.0134(5) 0.0011(3) 0.0014(4) 0.0086(3) P2 0.0177(4) 0.0177(4) 0.0164(8) 0.000 0.000 0.00886(19) O1 0.0279(12) 0.0180(10) 0.0194(12) -0.0007(8) 0.0062(9) 0.0079(9) O2 0.0194(10) 0.0223(10) 0.0227(13) 0.0054(10) 0.0039(9) 0.0095(8) O3 0.0252(10) 0.0298(11) 0.0134(14) -0.0006(10) -0.0012(9) 0.0128(9) O4 0.0330(11) 0.0183(10) 0.0278(13) -0.0042(10) -0.0106(11) 0.0149(9) O5 0.066(2) 0.066(2) 0.027(4) 0.000 0.000 0.0331(11) O6 0.0221(11) 0.0249(11) 0.0309(14) 0.0056(10) 0.0046(9) 0.0151(9) N1 0.0289(13) 0.0275(12) 0.0218(15) 0.0000(13) 0.0024(16) 0.0173(10) N2 0.0246(13) 0.0246(13) 0.023(3) 0.000 0.000 0.0123(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 O2 1.940(2) . ? Co1 O6 1.943(2) . ? Co1 O3 1.950(2) . ? Co1 O4 1.960(2) . ? Co2 O5 1.863(7) . ? Co2 O1 1.948(2) 6_545 ? Co2 O1 1.948(2) 5_565 ? Co2 O1 1.948(2) 4_765 ? P1 O3 1.536(3) 5_664 ? P1 O4 1.537(2) 3_765 ? P1 O2 1.539(2) . ? P1 O1 1.542(2) . ? P2 O5 1.529(7) . ? P2 O6 1.539(2) 3_665 ? P2 O6 1.539(2) . ? P2 O6 1.539(2) 2_655 ? O1 Co2 1.948(2) 4_764 ? O3 P1 1.536(3) 6_545 ? O4 P1 1.537(2) 2_645 ? N1 H1 0.934(16) . ? N1 H2 0.954(16) . ? N1 H3 0.938(17) . ? N1 H4 0.946(17) . ? N2 H5 0.94(2) . ? N2 H6 0.94(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 O2 Co1 O6 113.46(10) . . ? O2 Co1 O3 106.26(10) . . ? O6 Co1 O3 115.60(10) . . ? O2 Co1 O4 112.22(10) . . ? O6 Co1 O4 103.06(10) . . ? O3 Co1 O4 106.12(11) . . ? O5 Co2 O1 109.38(8) . 6_545 ? O5 Co2 O1 109.38(8) . 5_565 ? O1 Co2 O1 109.56(8) 6_545 5_565 ? O5 Co2 O1 109.38(8) . 4_765 ? O1 Co2 O1 109.56(8) 6_545 4_765 ? O1 Co2 O1 109.56(8) 5_565 4_765 ? O3 P1 O4 109.48(15) 5_664 3_765 ? O3 P1 O2 109.51(13) 5_664 . ? O4 P1 O2 108.86(13) 3_765 . ? O3 P1 O1 109.32(13) 5_664 . ? O4 P1 O1 110.38(14) 3_765 . ? O2 P1 O1 109.27(14) . . ? O5 P2 O6 110.53(12) . 3_665 ? O5 P2 O6 110.53(12) . . ? O6 P2 O6 108.40(12) 3_665 . ? O5 P2 O6 110.53(12) . 2_655 ? O6 P2 O6 108.40(12) 3_665 2_655 ? O6 P2 O6 108.40(12) . 2_655 ? P1 O1 Co2 129.42(15) . 4_764 ? P1 O2 Co1 133.13(14) . . ? P1 O3 Co1 143.30(15) 6_545 . ? P1 O4 Co1 134.14(15) 2_645 . ? P2 O5 Co2 180.0 . . ? P2 O6 Co1 131.03(17) . . ? H1 N1 H2 109(2) . . ? H1 N1 H3 114(2) . . ? H2 N1 H3 105(3) . . ? H1 N1 H4 112(3) . . ? H2 N1 H4 108(2) . . ? H3 N1 H4 108(3) . . ? H5 N2 H6 111(4) . . ? 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 O3 P1 O1 Co2 -57.8(2) 5_664 . . 4_764 ? O4 P1 O1 Co2 62.6(2) 3_765 . . 4_764 ? O2 P1 O1 Co2 -177.67(17) . . . 4_764 ? O3 P1 O2 Co1 -46.4(2) 5_664 . . . ? O4 P1 O2 Co1 -166.11(19) 3_765 . . . ? O1 P1 O2 Co1 73.3(2) . . . . ? O6 Co1 O2 P1 -16.7(3) . . . . ? O3 Co1 O2 P1 -144.8(2) . . . . ? O4 Co1 O2 P1 99.6(2) . . . . ? O2 Co1 O3 P1 52.8(2) . . . 6_545 ? O6 Co1 O3 P1 -74.1(2) . . . 6_545 ? O4 Co1 O3 P1 172.4(2) . . . 6_545 ? O2 Co1 O4 P1 60.5(3) . . . 2_645 ? O6 Co1 O4 P1 -177.1(2) . . . 2_645 ? O3 Co1 O4 P1 -55.2(2) . . . 2_645 ? O6 P2 O5 Co2 -56(100) 3_665 . . . ? O6 P2 O5 Co2 -176(100) . . . . ? O6 P2 O5 Co2 64(100) 2_655 . . . ? O1 Co2 O5 P2 147(100) 6_545 . . . ? O1 Co2 O5 P2 27(100) 5_565 . . . ? O1 Co2 O5 P2 -93(100) 4_765 . . . ? O5 P2 O6 Co1 35.0(2) . . . . ? O6 P2 O6 Co1 -86.2(3) 3_665 . . . ? O6 P2 O6 Co1 156.32(19) 2_655 . . . ? O2 Co1 O6 P2 -141.23(19) . . . . ? O3 Co1 O6 P2 -18.1(2) . . . . ? O4 Co1 O6 P2 97.2(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 N2 H6 O2 0.94(2) 2.28(15) 2.897(4) 123(13) . N2 H6 O3 0.94(2) 2.22(6) 3.044(2) 146(8) . N2 H5 O2 0.94(2) 2.578(12) 3.204(5) 124.4(4) 4_755 N2 H5 O2 0.94(2) 2.578(12) 3.204(5) 124.4(4) 5_665 N2 H5 O2 0.94(2) 2.578(12) 3.204(5) 124.4(4) 6_545 N1 H4 O6 0.946(17) 1.94(2) 2.829(4) 156(3) 4_665 N1 H3 O1 0.938(17) 1.855(18) 2.787(4) 173(4) 1_455 N1 H2 O3 0.954(16) 2.16(3) 2.889(3) 132(3) 2 N1 H1 O4 0.934(16) 1.865(18) 2.785(4) 168(3) 5_565 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.307 _refine_diff_density_min -1.151 _refine_diff_density_rms 0.113