# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2032 data_COMPOUNDI _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C5 H16 Co N2 O8 P2' _chemical_formula_weight 353.07 _chemical_melting_point ? _chemical_compound_source ? 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 8.6140(2) _cell_length_b 13.4561(4) _cell_length_c 10.8168(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.488(2) _cell_angle_gamma 90.00 _cell_volume 1248.04(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 1.879 _exptl_crystal_density_method ? _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 1.666 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5019 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 23.29 _reflns_number_total 1788 _reflns_number_observed 1468 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+0.3930P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0030(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1788 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_obs 0.0384 _refine_ls_wR_factor_all 0.1112 _refine_ls_wR_factor_obs 0.1062 _refine_ls_goodness_of_fit_all 1.057 _refine_ls_goodness_of_fit_obs 1.125 _refine_ls_restrained_S_all 1.057 _refine_ls_restrained_S_obs 1.125 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.23734(7) 0.47199(5) 0.46961(6) 0.0214(3) Uani 1 d . . P1 P 0.03917(14) 0.41828(9) 0.68889(11) 0.0222(3) Uani 1 d . . P2 P 0.54850(13) 0.41175(9) 0.35818(12) 0.0217(4) Uani 1 d . . O1 O 0.3893(3) 0.3876(2) 0.3995(3) 0.0287(8) Uani 1 d . . O2 O 0.1144(4) 0.3884(2) 0.5724(3) 0.0274(8) Uani 1 d . . O3 O 0.3198(4) 0.5998(2) 0.5364(3) 0.0285(8) Uani 1 d . . O4 O 0.0711(4) 0.4936(2) 0.3333(3) 0.0327(9) Uani 1 d . . O5 O -0.0451(4) 0.3317(2) 0.7419(3) 0.0362(9) Uani 1 d . . O6 O 0.1742(4) 0.4531(3) 0.7882(3) 0.0352(9) Uani 1 d . . H30 H 0.2351(4) 0.4071(3) 0.8040(3) 0.053 Uiso 1 calc R . O7 O 0.5601(4) 0.5153(2) 0.3028(3) 0.0325(9) Uani 1 d . . O8 O 0.5844(4) 0.3354(3) 0.2551(3) 0.0345(9) Uani 1 d . . H20 H 0.5842(4) 0.2789(3) 0.2835(3) 0.052 Uiso 1 calc R . N1 N 0.9714(6) 0.2066(5) 0.4173(6) 0.082(2) Uani 1 d . . H1 H 0.9040(6) 0.1574(5) 0.3943(6) 0.098 Uiso 1 calc R . H2 H 0.9685(6) 0.2169(5) 0.4993(6) 0.098 Uiso 1 calc R . C1 C 0.9231(5) 0.2964(4) 0.3505(6) 0.0337(14) Uani 1 d . . H3 H 0.8170(5) 0.3124(4) 0.3664(6) 0.040 Uiso 1 calc R . H4 H 0.9895(5) 0.3510(4) 0.3815(6) 0.040 Uiso 1 calc R . C2 C 0.9304(6) 0.2873(5) 0.2199(7) 0.060(2) Uani 1 d . . H5 H 0.8981(6) 0.3494(5) 0.1799(7) 0.072 Uiso 1 calc R . H6 H 0.8584(6) 0.2360(5) 0.1877(7) 0.072 Uiso 1 calc R . N2 N 1.0969(6) 0.2609(4) 0.1878(6) 0.071(2) Uani 1 d . . H7 H 1.0973(6) 0.2511(4) 0.1055(6) 0.085 Uiso 1 calc R . H8 H 1.1633(6) 0.3107(4) 0.2105(6) 0.085 Uiso 1 calc R . C3 C 1.1451(6) 0.1684(4) 0.2568(6) 0.0181(13) Uani 1 d . . H9 H 1.1043(59) 0.1356(42) 0.2368(52) 0.022 Uiso 1 d . . H10 H 1.1921(65) 0.1652(52) 0.2460(65) 0.022 Uiso 1 d . . C4 C 1.1366(6) 0.1747(4) 0.3924(5) 0.0360(13) Uani 1 d . . H11 H 1.2092(6) 0.2265(4) 0.4251(5) 0.043 Uiso 1 calc R . C5 C 1.1867(8) 0.0784(5) 0.4534(6) 0.067(2) Uani 1 d . . H12 H 1.1806(8) 0.0836(5) 0.5413(6) 0.101 Uiso 1 calc R . H13 H 1.2922(8) 0.0641(5) 0.4376(6) 0.101 Uiso 1 calc R . H14 H 1.1195(8) 0.0260(5) 0.4203(6) 0.101 Uiso 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 0.0158(4) 0.0194(4) 0.0296(4) 0.0004(3) 0.0054(3) 0.0005(3) P1 0.0173(7) 0.0215(7) 0.0281(7) 0.0052(6) 0.0035(5) 0.0007(5) P2 0.0140(6) 0.0188(7) 0.0326(7) -0.0053(6) 0.0043(5) -0.0006(5) O1 0.018(2) 0.025(2) 0.044(2) -0.007(2) 0.010(2) -0.0008(15) O2 0.026(2) 0.027(2) 0.031(2) -0.002(2) 0.0085(15) -0.010(2) O3 0.020(2) 0.026(2) 0.039(2) 0.001(2) -0.0023(15) -0.0006(15) O4 0.030(2) 0.025(2) 0.041(2) -0.001(2) -0.008(2) 0.006(2) O5 0.024(2) 0.030(2) 0.057(2) 0.018(2) 0.018(2) 0.002(2) O6 0.023(2) 0.050(2) 0.031(2) 0.005(2) -0.003(2) 0.006(2) O7 0.024(2) 0.023(2) 0.050(2) 0.007(2) 0.006(2) 0.002(2) O8 0.032(2) 0.030(2) 0.045(2) -0.013(2) 0.019(2) -0.008(2) N1 0.056(4) 0.120(6) 0.073(4) -0.049(4) 0.029(3) -0.036(4) C1 0.009(2) 0.016(3) 0.076(4) -0.024(3) 0.007(3) 0.002(2) C2 0.023(3) 0.032(4) 0.120(7) 0.012(4) -0.018(4) 0.003(3) N2 0.066(4) 0.054(4) 0.093(5) -0.004(3) 0.012(3) -0.006(3) C3 0.008(3) 0.012(3) 0.035(3) -0.009(2) 0.005(3) 0.002(2) C4 0.018(3) 0.043(4) 0.045(3) -0.010(3) -0.003(2) -0.002(2) C5 0.068(5) 0.074(5) 0.058(4) 0.007(4) -0.004(4) -0.002(4) _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 1.941(3) . ? Co1 O2 1.962(3) . ? Co1 O3 1.972(3) . ? Co1 O4 1.976(3) . ? P1 O5 1.514(3) . ? P1 O4 1.524(3) 3_566 ? P1 O2 1.525(3) . ? P1 O6 1.577(3) . ? P2 O1 1.517(3) . ? P2 O7 1.523(3) . ? P2 O3 1.538(3) 3_666 ? P2 O8 1.569(3) . ? O3 P2 1.538(3) 3_666 ? O4 P1 1.524(3) 3_566 ? O6 H30 0.82 . ? O8 H20 0.82 . ? N1 C1 1.449(8) . ? N1 C4 1.534(7) . ? N1 H1 0.90 . ? N1 H2 0.90 . ? C1 C2 1.426(9) . ? C1 H3 0.97 . ? C1 H4 0.97 . ? C2 N2 1.549(8) . ? C2 H5 0.97 . ? C2 H6 0.97 . ? N2 C3 1.489(9) . ? N2 H7 0.90 . ? N2 H8 0.90 . ? C3 C4 1.478(9) . ? C3 H9 0.59(5) . ? C3 H10 0.43(5) . ? C4 C5 1.498(8) . ? C4 H11 0.98 . ? C5 H12 0.96 . ? C5 H13 0.96 . ? C5 H14 0.96 . ? 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 107.87(14) . . ? O1 Co1 O3 114.88(13) . . ? O2 Co1 O3 119.18(13) . . ? O1 Co1 O4 105.20(14) . . ? O2 Co1 O4 96.62(14) . . ? O3 Co1 O4 110.80(13) . . ? O5 P1 O4 110.1(2) . 3_566 ? O5 P1 O2 111.5(2) . . ? O4 P1 O2 112.5(2) 3_566 . ? O5 P1 O6 108.6(2) . . ? O4 P1 O6 106.5(2) 3_566 . ? O2 P1 O6 107.3(2) . . ? O1 P2 O7 114.0(2) . . ? O1 P2 O3 112.6(2) . 3_666 ? O7 P2 O3 108.2(2) . 3_666 ? O1 P2 O8 108.3(2) . . ? O7 P2 O8 107.1(2) . . ? O3 P2 O8 106.2(2) 3_666 . ? P2 O1 Co1 130.7(2) . . ? P1 O2 Co1 127.7(2) . . ? P2 O3 Co1 113.4(2) 3_666 . ? P1 O4 Co1 128.9(2) 3_566 . ? P1 O6 H30 109.47(14) . . ? P2 O8 H20 109.47(14) . . ? C1 N1 C4 111.9(5) . . ? C1 N1 H1 109.2(3) . . ? C4 N1 H1 109.2(3) . . ? C1 N1 H2 109.2(3) . . ? C4 N1 H2 109.2(3) . . ? H1 N1 H2 107.9 . . ? C2 C1 N1 112.6(5) . . ? C2 C1 H3 109.1(3) . . ? N1 C1 H3 109.1(3) . . ? C2 C1 H4 109.1(3) . . ? N1 C1 H4 109.1(3) . . ? H3 C1 H4 107.8 . . ? C1 C2 N2 111.8(5) . . ? C1 C2 H5 109.3(3) . . ? N2 C2 H5 109.3(3) . . ? C1 C2 H6 109.3(3) . . ? N2 C2 H6 109.3(3) . . ? H5 C2 H6 107.9 . . ? C3 N2 C2 107.4(5) . . ? C3 N2 H7 110.2(3) . . ? C2 N2 H7 110.2(4) . . ? C3 N2 H8 110.2(3) . . ? C2 N2 H8 110.2(3) . . ? H7 N2 H8 108.5 . . ? C4 C3 N2 114.3(5) . . ? C4 C3 H9 108.7(57) . . ? N2 C3 H9 108.2(59) . . ? C4 C3 H10 114.1(100) . . ? N2 C3 H10 99.9(100) . . ? H9 C3 H10 111.3(100) . . ? C3 C4 C5 110.4(5) . . ? C3 C4 N1 109.0(4) . . ? C5 C4 N1 113.5(5) . . ? C3 C4 H11 108.0(3) . . ? C5 C4 H11 108.0(3) . . ? N1 C4 H11 108.0(3) . . ? C4 C5 H12 109.5(3) . . ? C4 C5 H13 109.5(3) . . ? H12 C5 H13 109.5 . . ? C4 C5 H14 109.5(3) . . ? H12 C5 H14 109.5 . . ? H13 C5 H14 109.5 . . ? _refine_diff_density_max 0.645 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.237 data_COMPOUNDII _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C6 H18 Co N2 O8 P2' _chemical_formula_weight 367.09 _chemical_melting_point ? _chemical_compound_source ? 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' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 11.8793(11) _cell_length_b 13.5078(12) _cell_length_c 8.1681(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1310.7(2) _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 1.860 _exptl_crystal_density_method ? _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 1.590 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4929 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 23.30 _reflns_number_total 938 _reflns_number_observed 758 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+0.9501P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0031(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 938 _refine_ls_number_parameters 88 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_obs 0.0261 _refine_ls_wR_factor_all 0.0695 _refine_ls_wR_factor_obs 0.0650 _refine_ls_goodness_of_fit_all 1.037 _refine_ls_goodness_of_fit_obs 1.092 _refine_ls_restrained_S_all 1.037 _refine_ls_restrained_S_obs 1.092 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.2500 0.2500 -0.67531(7) 0.0198(2) Uani 1 d S . P1 P 0.39601(7) 0.37954(6) -0.42390(11) 0.0203(3) Uani 1 d . . O1 O 0.3812(2) 0.1964(2) -0.7893(3) 0.0295(6) Uani 1 d . . O2 O 0.3132(2) 0.3650(2) -0.5636(3) 0.0302(6) Uani 1 d . . O3 O 0.3885(2) 0.4858(2) -0.3618(3) 0.0228(5) Uani 1 d . . O4 O 0.5206(2) 0.3624(2) -0.4870(3) 0.0325(6) Uani 1 d . . H10 H 0.5345(2) 0.4016(2) -0.5610(3) 0.049 Uiso 1 calc R . N1 N 0.9112(2) 0.4396(2) -0.4344(3) 0.0301(7) Uani 1 d . . H4 H 0.8952(2) 0.4778(2) -0.3457(3) 0.036 Uiso 1 calc R . C1 C 0.8338(4) 0.3528(3) -0.4319(6) 0.0651(14) Uani 1 d . . H3 H 0.7574(4) 0.3753(3) -0.4399(6) 0.098 Uiso 1 calc R . H2 H 0.8437(4) 0.3169(3) -0.3315(6) 0.098 Uiso 1 calc R . H1 H 0.8506(4) 0.3102(3) -0.5228(6) 0.098 Uiso 1 calc R . C2 C 1.0305(3) 0.4092(3) -0.4225(4) 0.0356(9) Uani 1 d . . H5 H 1.0502(3) 0.3689(3) -0.5164(4) 0.043 Uiso 1 calc R . H6 H 1.0414(3) 0.3698(3) -0.3245(4) 0.043 Uiso 1 calc R . C3 C 0.8947(3) 0.5016(3) -0.5836(5) 0.0363(9) Uani 1 d . . H8 H 0.8167(3) 0.5224(3) -0.5905(5) 0.044 Uiso 1 calc R . H7 H 0.9120(3) 0.4628(3) -0.6804(5) 0.044 Uiso 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 0.0244(4) 0.0195(4) 0.0153(4) 0.000 0.000 0.0003(3) P1 0.0225(5) 0.0197(5) 0.0187(5) -0.0007(4) 0.0025(4) -0.0019(4) O1 0.0316(14) 0.0274(14) 0.0295(14) -0.0085(11) 0.0072(11) 0.0009(11) O2 0.0363(14) 0.0283(13) 0.0259(14) -0.0068(11) -0.0089(11) -0.0014(11) O3 0.0275(13) 0.0213(13) 0.0198(13) -0.0023(10) 0.0011(10) -0.0042(10) O4 0.0305(14) 0.0295(14) 0.038(2) 0.0095(11) 0.0121(12) 0.0026(10) N1 0.035(2) 0.031(2) 0.024(2) -0.0091(14) 0.0067(14) -0.0014(14) C1 0.074(3) 0.054(3) 0.068(3) -0.021(3) 0.021(3) -0.031(2) C2 0.044(2) 0.037(2) 0.026(2) 0.004(2) 0.005(2) 0.021(2) C3 0.026(2) 0.058(3) 0.025(2) -0.004(2) -0.004(2) 0.013(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 O2 1.952(2) . ? Co1 O2 1.952(2) 2 ? Co1 O1 1.955(2) . ? Co1 O1 1.955(2) 2 ? P1 O1 1.514(2) 7_566 ? P1 O2 1.519(2) . ? P1 O3 1.525(2) . ? P1 O4 1.584(2) . ? O1 P1 1.514(2) 7_565 ? O4 H10 0.82 . ? N1 C2 1.478(4) . ? N1 C1 1.491(5) . ? N1 C3 1.491(4) . ? N1 H4 0.91 . ? C1 H3 0.96 . ? C1 H2 0.96 . ? C1 H1 0.96 . ? C2 C3 1.498(5) 5_764 ? C2 H5 0.97 . ? C2 H6 0.97 . ? C3 C2 1.498(5) 5_764 ? C3 H8 0.97 . ? C3 H7 0.97 . ? 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 O2 124.25(13) . 2 ? O2 Co1 O1 102.15(9) . . ? O2 Co1 O1 103.59(9) 2 . ? O2 Co1 O1 103.59(9) . 2 ? O2 Co1 O1 102.15(9) 2 2 ? O1 Co1 O1 123.12(14) . 2 ? O1 P1 O2 112.51(13) 7_566 . ? O1 P1 O3 112.92(13) 7_566 . ? O2 P1 O3 109.49(13) . . ? O1 P1 O4 104.21(13) 7_566 . ? O2 P1 O4 109.98(14) . . ? O3 P1 O4 107.49(12) . . ? P1 O1 Co1 133.56(14) 7_565 . ? P1 O2 Co1 134.67(14) . . ? P1 O4 H10 109.47(9) . . ? C2 N1 C1 111.8(3) . . ? C2 N1 C3 109.6(3) . . ? C1 N1 C3 111.8(3) . . ? C2 N1 H4 107.8(2) . . ? C1 N1 H4 107.8(2) . . ? C3 N1 H4 107.8(2) . . ? N1 C1 H3 109.5(2) . . ? N1 C1 H2 109.5(2) . . ? H3 C1 H2 109.5 . . ? N1 C1 H1 109.5(2) . . ? H3 C1 H1 109.5 . . ? H2 C1 H1 109.5 . . ? N1 C2 C3 110.3(3) . 5_764 ? N1 C2 H5 109.6(2) . . ? C3 C2 H5 109.6(2) 5_764 . ? N1 C2 H6 109.6(2) . . ? C3 C2 H6 109.6(2) 5_764 . ? H5 C2 H6 108.1 . . ? N1 C3 C2 110.3(3) . 5_764 ? N1 C3 H8 109.6(2) . . ? C2 C3 H8 109.6(2) 5_764 . ? N1 C3 H7 109.6(2) . . ? C2 C3 H7 109.6(2) 5_764 . ? H8 C3 H7 108.1 . . ? _refine_diff_density_max 0.373 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.162