Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Gary Hix' 'Paul-Alain Jaffres' 'Elizabeth J. MacLean' 'Vickie McKee' 'A. Turner' 'D. Villemin' _publ_contact_author_name 'Dr Gary Hix' _publ_contact_author_address ; Molecular Sciences De Montfort University The Gateway Leicester Leics LE1 9BH UNITED KINGDOM ; _publ_contact_author_email GHIX@DMU.AC.UK _publ_section_title ; Hydrothermal synthesis and crystal structure of two Co phosphonates containing trifunctional phosphonate anions: Co3(O3PCH2NH2CH2PO3)2 and Co3(O3PCH2-NC4H7-CO2)2.5H2O ; data_ksrgbh11 _database_code_CSD 199769 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tricobalt amino bis(methylenephosphonate) ; _chemical_name_common ? _chemical_melting_point decomposes _chemical_formula_moiety ? _chemical_formula_sum 'C2 H6 Co1.50 N O6 P2' _chemical_formula_weight 290.41 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 10.733(3) _cell_length_b 13.387(4) _cell_length_c 5.3953(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 775.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 574 _exptl_absorpt_coefficient_mu 3.651 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.784113 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 6689 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 28.74 _reflns_number_total 1840 _reflns_number_gt 1585 _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^)+(0.0320P)^2^+3.8497P] 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 0.49(4) _refine_ls_number_reflns 1840 _refine_ls_number_parameters 121 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 0.31937(6) 0.12312(5) 0.50009(16) 0.01393(17) Uani 1 1 d . . . Co2 Co 0.0000 0.0000 0.3214(2) 0.0119(3) Uani 0.84 2 d SP . 1 P2 P 0.04523(17) 0.21800(14) 0.5542(4) 0.0105(3) Uani 0.84 1 d P . 1 Co2A Co 0.0000 0.0000 0.6941(16) 0.0289(18) Uiso 0.16 2 d SP . 2 P2A P 0.0463(11) 0.2172(9) 0.429(3) 0.019(2) Uiso 0.16 1 d P . 2 P1 P 0.23067(11) 0.50315(10) 0.9860(3) 0.0163(3) Uani 1 1 d . . . O5 O 0.1806(3) 0.2161(3) 0.4757(8) 0.0185(8) Uani 1 1 d . . . N1 N 0.0736(4) 0.3426(3) 0.9784(12) 0.0190(10) Uani 1 1 d . . . H1A H 0.0221 0.3874 0.8997 0.023 Uiso 1 1 calc R . . H1B H 0.0579 0.3468 1.1458 0.023 Uiso 1 1 calc R . . O3 O 0.1994(5) 0.5193(3) 1.2517(9) 0.0356(12) Uani 1 1 d . . . O6 O -0.0190(4) 0.3083(3) 0.4454(9) 0.0235(10) Uani 1 1 d . . . O2 O 0.1409(4) 0.5602(3) 0.8191(9) 0.0292(11) Uani 1 1 d . . . O4 O -0.0248(3) 0.1213(3) 0.5109(8) 0.0209(8) Uani 1 1 d . . . O1 O 0.3642(4) 0.5224(3) 0.9172(9) 0.0265(11) Uani 1 1 d . . . C1 C 0.0413(5) 0.2387(4) 0.8915(11) 0.0189(12) Uani 1 1 d . . . H2A H -0.0433 0.2223 0.9519 0.023 Uiso 1 1 calc R . 1 H2B H 0.0999 0.1912 0.9702 0.023 Uiso 1 1 calc R . 1 C2 C 0.2059(5) 0.3721(4) 0.9323(13) 0.0238(14) Uani 1 1 d . . . H3A H 0.2282 0.3560 0.7588 0.029 Uiso 1 1 calc R . . H3B H 0.2612 0.3331 1.0426 0.029 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0096(3) 0.0119(3) 0.0203(4) 0.0008(4) 0.0000(4) -0.0001(3) Co2 0.0098(6) 0.0071(5) 0.0187(7) 0.000 0.000 -0.0005(5) P2 0.0105(7) 0.0088(8) 0.0122(10) -0.0005(6) 0.0006(6) 0.0001(6) P1 0.0110(5) 0.0100(6) 0.0278(7) 0.0011(9) -0.0001(7) 0.0003(5) O5 0.0120(16) 0.0156(17) 0.028(2) -0.0001(19) 0.002(2) 0.0003(15) N1 0.014(2) 0.010(2) 0.033(3) -0.003(2) -0.002(3) 0.0009(16) O3 0.045(3) 0.023(3) 0.039(3) -0.007(2) -0.002(2) 0.004(2) O6 0.0122(19) 0.0175(19) 0.041(3) 0.0025(18) 0.0006(19) 0.0032(15) O2 0.023(2) 0.028(3) 0.037(3) 0.016(2) 0.001(2) 0.0064(19) O4 0.0193(18) 0.0129(17) 0.030(2) -0.003(2) 0.000(2) -0.0031(14) O1 0.0102(19) 0.018(2) 0.051(3) -0.0038(19) 0.0023(18) -0.0009(16) C1 0.020(3) 0.015(3) 0.022(3) 0.000(2) 0.000(2) -0.002(2) C2 0.010(3) 0.016(3) 0.046(4) -0.003(3) 0.001(2) 0.000(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 O3 1.940(5) 3_547 ? Co1 O5 1.945(4) . ? Co1 O2 1.964(5) 3_546 ? Co1 O6 1.985(4) 4_556 ? Co2 O4 1.937(4) . ? Co2 O4 1.937(4) 2 ? Co2 O1 1.967(4) 4_456 ? Co2 O1 1.967(4) 3_546 ? P2 O6 1.510(4) . ? P2 O5 1.514(4) . ? P2 O4 1.516(4) . ? P2 C1 1.841(6) . ? Co2A O4 1.919(6) 2 ? Co2A O4 1.919(6) . ? P2A O6 1.410(12) . ? P2A O5 1.464(12) . ? P2A O4 1.558(13) . ? P1 O3 1.488(5) . ? P1 O1 1.503(4) . ? P1 O2 1.524(4) . ? P1 C2 1.797(6) . ? N1 C2 1.495(7) . ? N1 C1 1.508(7) . ? O3 Co1 1.940(5) 3_557 ? O6 Co1 1.985(4) 4_456 ? O2 Co1 1.964(5) 3_556 ? O1 Co2 1.967(4) 3_556 ? 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 O3 Co1 O5 115.2(2) 3_547 . ? O3 Co1 O2 108.7(2) 3_547 3_546 ? O5 Co1 O2 112.42(19) . 3_546 ? O3 Co1 O6 108.7(2) 3_547 4_556 ? O5 Co1 O6 112.52(16) . 4_556 ? O2 Co1 O6 97.96(18) 3_546 4_556 ? O4 Co2 O4 116.3(3) . 2 ? O4 Co2 O1 111.78(16) . 4_456 ? O4 Co2 O1 108.64(17) 2 4_456 ? O4 Co2 O1 108.64(17) . 3_546 ? O4 Co2 O1 111.78(16) 2 3_546 ? O1 Co2 O1 98.3(3) 4_456 3_546 ? O6 P2 O5 110.1(2) . . ? O6 P2 O4 113.4(2) . . ? O5 P2 O4 114.8(2) . . ? O6 P2 C1 104.7(3) . . ? O5 P2 C1 107.5(3) . . ? O4 P2 C1 105.6(3) . . ? O4 Co2A O4 118.0(5) 2 . ? O6 P2A O5 119.2(9) . . ? O6 P2A O4 116.8(8) . . ? O5 P2A O4 115.2(8) . . ? O3 P1 O1 115.3(3) . . ? O3 P1 O2 110.7(3) . . ? O1 P1 O2 111.8(3) . . ? O3 P1 C2 105.3(3) . . ? O1 P1 C2 105.6(3) . . ? O2 P1 C2 107.5(3) . . ? P2A O5 P2 26.2(5) . . ? P2A O5 Co1 140.5(5) . . ? P2 O5 Co1 136.6(2) . . ? C2 N1 C1 114.2(5) . . ? P1 O3 Co1 142.4(3) . 3_557 ? P2A O6 P2 26.5(5) . . ? P2A O6 Co1 147.6(6) . 4_456 ? P2 O6 Co1 135.4(3) . 4_456 ? P1 O2 Co1 126.6(3) . 3_556 ? P2 O4 P2A 25.4(5) . . ? P2 O4 Co2A 125.1(3) . . ? P2A O4 Co2A 140.8(5) . . ? P2 O4 Co2 136.8(3) . . ? P2A O4 Co2 118.2(6) . . ? Co2A O4 Co2 62.9(2) . . ? P1 O1 Co2 147.4(3) . 3_556 ? N1 C1 P2 116.2(4) . . ? N1 C2 P1 111.9(4) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.101 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.157 data_ejm48 _database_code_CSD 199770 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point decomposes _chemical_formula_moiety ? _chemical_formula_sum 'C12 H28 Co3 N2 O15 P2' _chemical_formula_weight 679.02 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' Co Co 0.3494 0.9721 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.985(2) _cell_length_b 10.378(3) _cell_length_c 11.942(3) _cell_angle_alpha 90.238(5) _cell_angle_beta 106.810(5) _cell_angle_gamma 111.346(4) _cell_volume 1095.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.060 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 690 _exptl_absorpt_coefficient_mu 2.472 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7902 _exptl_absorpt_correction_T_max 0.7902 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 0(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 8099 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.1207 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 24.77 _reflns_number_total 3736 _reflns_number_gt 2475 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0638P)^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 3736 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1384 _refine_ls_wR_factor_gt 0.1222 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _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 0.02839(10) 0.58569(9) 0.88900(8) 0.0134(3) Uani 1 1 d . . . Co2 Co 0.47778(11) 0.93956(10) 1.12339(9) 0.0171(3) Uani 1 1 d . . . Co3 Co -0.10927(11) 0.84039(10) 0.98060(9) 0.0158(3) Uani 1 1 d . . . P1 P -0.1435(2) 0.25761(18) 0.83656(17) 0.0142(4) Uani 1 1 d . . . P2 P 0.1906(2) 0.92822(18) 0.88715(16) 0.0132(4) Uani 1 1 d . . . O15 O 0.0846(5) 0.9631(5) 0.9421(4) 0.0171(11) Uani 1 1 d . . . O7 O -0.1506(5) 0.6441(5) 0.8834(5) 0.0190(11) Uani 1 1 d . . . O1 O 0.4364(6) 0.7455(6) 1.0314(6) 0.0442(17) Uani 1 1 d . . . O9 O 0.3558(5) 0.9909(5) 0.9674(4) 0.0199(12) Uani 1 1 d . . . O5 O -0.1031(5) 0.3813(5) 0.9289(4) 0.0166(11) Uani 1 1 d . . . O6 O 0.2009(6) 0.5131(6) 0.8879(5) 0.0260(13) Uani 1 1 d . . . O2 O -0.5271(6) 0.8689(6) 0.7895(5) 0.0300(13) Uani 1 1 d . . . N2 N 0.3241(7) 1.0467(6) 0.7218(5) 0.0207(14) Uani 1 1 d . . . N1 N -0.1176(6) 0.4868(6) 0.7139(5) 0.0151(13) Uani 1 1 d . . . O14 O 0.1411(5) 0.7746(5) 0.8472(4) 0.0172(11) Uani 1 1 d . . . O11 O 0.0310(6) 0.8125(5) 1.1336(4) 0.0232(12) Uani 1 1 d . . . O12 O -0.3060(6) 0.1570(5) 0.8093(4) 0.0236(12) Uani 1 1 d . . . O8 O -0.3991(6) 0.5252(6) 0.8310(6) 0.0414(16) Uani 1 1 d . . . C6 C -0.1214(9) 0.3407(7) 0.7042(6) 0.0168(16) Uani 1 1 d . . . H6A H -0.0264 0.3433 0.6923 0.020 Uiso 1 1 calc R . . H6B H -0.2066 0.2845 0.6346 0.020 Uiso 1 1 calc R . . C1 C -0.2746(8) 0.5560(8) 0.8140(7) 0.0226(18) Uani 1 1 d . . . C3 C -0.0685(9) 0.5604(8) 0.6173(7) 0.0228(17) Uani 1 1 d . . . H3A H -0.0997 0.4943 0.5460 0.027 Uiso 1 1 calc R . . H3B H 0.0427 0.6112 0.6422 0.027 Uiso 1 1 calc R . . C2 C -0.2707(8) 0.4880(8) 0.7027(7) 0.0237(18) Uani 1 1 d . . . H2 H -0.3479 0.3903 0.6833 0.028 Uiso 1 1 calc R . . C12 C -0.6204(10) 0.8353(9) 0.6845(8) 0.035(2) Uani 1 1 d . . . O13 O -0.6486(9) 0.7304(7) 0.6175(6) 0.060(2) Uani 1 1 d . . . C11 C 0.3539(10) 1.1717(9) 0.6554(8) 0.031(2) Uani 1 1 d . . . H11A H 0.2594 1.1869 0.6178 0.037 Uiso 1 1 calc R . . H11B H 0.4287 1.2568 0.7084 0.037 Uiso 1 1 calc R . . C7 C 0.1942(8) 1.0293(8) 0.7646(6) 0.0189(16) Uani 1 1 d . . . H7A H 0.0990 0.9828 0.6991 0.023 Uiso 1 1 calc R . . H7B H 0.1985 1.1224 0.7890 0.023 Uiso 1 1 calc R . . C4 C -0.1501(10) 0.6614(9) 0.5949(8) 0.037(2) Uani 1 1 d . . . H4A H -0.0997 0.7429 0.6565 0.044 Uiso 1 1 calc R . . H4B H -0.1550 0.6943 0.5167 0.044 Uiso 1 1 calc R . . C5 C -0.3063(10) 0.5723(10) 0.6002(8) 0.037(2) Uani 1 1 d . . . H5A H -0.3690 0.5103 0.5255 0.044 Uiso 1 1 calc R . . H5B H -0.3592 0.6306 0.6171 0.044 Uiso 1 1 calc R . . C10 C 0.4143(12) 1.1356(10) 0.5659(9) 0.049(3) Uani 1 1 d . . . H10A H 0.5201 1.1435 0.6013 0.059 Uiso 1 1 calc R . . H10B H 0.4093 1.1954 0.5016 0.059 Uiso 1 1 calc R . . C8 C 0.2880(10) 0.9246(9) 0.6364(7) 0.032(2) Uani 1 1 d . . . H8 H 0.1786 0.8646 0.6200 0.038 Uiso 1 1 calc R . . C9 C 0.3073(14) 0.9848(11) 0.5220(8) 0.058(3) Uani 1 1 d . . . H9A H 0.3522 0.9353 0.4822 0.069 Uiso 1 1 calc R . . H9B H 0.2092 0.9792 0.4670 0.069 Uiso 1 1 calc R . . O16 O -0.2320(6) 0.8858(5) 0.8188(5) 0.0252(12) Uani 1 1 d . . . O17 O -0.3096(6) 0.7152(6) 1.0141(5) 0.0325(14) Uani 1 1 d . . . O18 O 0.3036(7) 0.4902(7) 0.7123(6) 0.0435(16) 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 0.0160(5) 0.0089(5) 0.0160(5) 0.0028(4) 0.0056(4) 0.0049(4) Co2 0.0158(5) 0.0175(6) 0.0199(6) 0.0042(4) 0.0084(4) 0.0065(4) Co3 0.0143(5) 0.0093(5) 0.0267(6) 0.0045(4) 0.0096(4) 0.0053(4) P1 0.0158(10) 0.0103(9) 0.0175(10) 0.0030(8) 0.0082(8) 0.0040(8) P2 0.0119(9) 0.0103(9) 0.0188(10) 0.0044(8) 0.0063(8) 0.0046(7) O15 0.012(2) 0.013(3) 0.029(3) 0.004(2) 0.010(2) 0.005(2) O7 0.009(2) 0.011(3) 0.036(3) -0.004(2) 0.005(2) 0.004(2) O1 0.023(3) 0.028(3) 0.079(5) -0.016(3) 0.014(3) 0.007(3) O9 0.011(3) 0.020(3) 0.026(3) 0.003(2) 0.005(2) 0.004(2) O5 0.017(3) 0.014(3) 0.017(3) 0.002(2) 0.007(2) 0.004(2) O6 0.017(3) 0.029(3) 0.033(3) 0.003(3) 0.002(2) 0.014(2) O2 0.023(3) 0.025(3) 0.036(4) -0.006(3) 0.000(3) 0.009(3) N2 0.028(4) 0.012(3) 0.025(4) 0.007(3) 0.013(3) 0.006(3) N1 0.019(3) 0.010(3) 0.016(3) 0.006(2) 0.007(3) 0.003(2) O14 0.026(3) 0.007(2) 0.021(3) 0.003(2) 0.011(2) 0.006(2) O11 0.027(3) 0.027(3) 0.025(3) 0.003(2) 0.011(2) 0.019(2) O12 0.028(3) 0.018(3) 0.022(3) 0.001(2) 0.009(2) 0.003(2) O8 0.020(3) 0.044(4) 0.056(4) -0.012(3) 0.015(3) 0.005(3) C6 0.027(4) 0.008(4) 0.016(4) 0.003(3) 0.006(3) 0.008(3) C1 0.018(4) 0.012(4) 0.038(5) 0.005(3) 0.007(4) 0.008(3) C3 0.028(4) 0.016(4) 0.021(4) 0.008(3) 0.010(4) 0.002(3) C2 0.023(4) 0.012(4) 0.034(5) 0.003(3) 0.007(4) 0.005(3) C12 0.035(5) 0.020(5) 0.049(6) -0.002(4) 0.006(5) 0.014(4) O13 0.085(5) 0.030(4) 0.055(5) -0.017(3) 0.000(4) 0.028(4) C11 0.030(5) 0.032(5) 0.038(5) 0.022(4) 0.016(4) 0.014(4) C7 0.021(4) 0.018(4) 0.022(4) 0.010(3) 0.009(3) 0.011(3) C4 0.040(5) 0.027(5) 0.034(5) 0.010(4) 0.003(4) 0.009(4) C5 0.034(5) 0.045(6) 0.030(5) 0.009(4) -0.002(4) 0.022(4) C10 0.066(7) 0.041(6) 0.043(6) 0.008(5) 0.022(5) 0.018(5) C8 0.044(5) 0.028(5) 0.022(5) -0.001(4) 0.008(4) 0.016(4) C9 0.092(9) 0.056(7) 0.026(5) 0.002(5) 0.020(6) 0.028(7) O16 0.029(3) 0.019(3) 0.029(3) 0.003(2) 0.002(3) 0.017(2) O17 0.027(3) 0.026(3) 0.047(4) 0.005(3) 0.021(3) 0.007(3) O18 0.039(4) 0.046(4) 0.044(4) -0.006(3) 0.012(3) 0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O14 2.021(5) . ? Co1 O5 2.067(5) 2_567 ? Co1 O7 2.070(5) . ? Co1 O6 2.119(5) . ? Co1 N1 2.163(6) . ? Co1 O5 2.189(5) . ? Co2 O12 2.036(5) 2_567 ? Co2 O2 2.062(5) 2_577 ? Co2 O9 2.099(5) . ? Co2 O1 2.133(6) . ? Co2 O9 2.152(5) 2_677 ? Co2 N2 2.243(6) 2_677 ? Co3 O11 2.050(5) . ? Co3 O15 2.075(5) . ? Co3 O17 2.103(5) . ? Co3 O16 2.125(5) . ? Co3 O15 2.135(5) 2_577 ? Co3 O7 2.182(5) . ? P1 O11 1.511(5) 2_567 ? P1 O12 1.512(5) . ? P1 O5 1.543(5) . ? P1 C6 1.834(7) . ? P2 O14 1.516(5) . ? P2 O15 1.536(5) . ? P2 O9 1.537(5) . ? P2 C7 1.805(7) . ? O15 Co3 2.135(5) 2_577 ? O7 C1 1.278(9) . ? O9 Co2 2.152(5) 2_677 ? O5 Co1 2.067(5) 2_567 ? O2 C12 1.283(10) . ? O2 Co2 2.062(5) 2_577 ? N2 C7 1.480(9) . ? N2 C8 1.491(10) . ? N2 C11 1.505(9) . ? N2 Co2 2.243(6) 2_677 ? N1 C3 1.489(9) . ? N1 C2 1.500(9) . ? N1 C6 1.506(8) . ? O11 P1 1.511(5) 2_567 ? O12 Co2 2.036(5) 2_567 ? O8 C1 1.244(9) . ? C1 C2 1.519(11) . ? C3 C4 1.527(11) . ? C2 C5 1.541(11) . ? C12 O13 1.242(10) . ? C12 C8 1.531(12) 1_455 ? C11 C10 1.477(12) . ? C4 C5 1.517(12) . ? C10 C9 1.522(14) . ? C8 C12 1.531(12) 1_655 ? C8 C9 1.538(12) . ? 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 O14 Co1 O5 101.94(19) . 2_567 ? O14 Co1 O7 89.98(19) . . ? O5 Co1 O7 91.06(19) 2_567 . ? O14 Co1 O6 92.7(2) . . ? O5 Co1 O6 91.1(2) 2_567 . ? O7 Co1 O6 176.1(2) . . ? O14 Co1 N1 98.7(2) . . ? O5 Co1 N1 158.0(2) 2_567 . ? O7 Co1 N1 81.3(2) . . ? O6 Co1 N1 95.5(2) . . ? O14 Co1 O5 177.46(19) . . ? O5 Co1 O5 79.7(2) 2_567 . ? O7 Co1 O5 88.00(18) . . ? O6 Co1 O5 89.27(19) . . ? N1 Co1 O5 79.43(19) . . ? O12 Co2 O2 92.5(2) 2_567 2_577 ? O12 Co2 O9 99.5(2) 2_567 . ? O2 Co2 O9 90.6(2) 2_577 . ? O12 Co2 O1 90.1(2) 2_567 . ? O2 Co2 O1 177.3(2) 2_577 . ? O9 Co2 O1 89.5(2) . . ? O12 Co2 O9 170.3(2) 2_567 2_677 ? O2 Co2 O9 97.1(2) 2_577 2_677 ? O9 Co2 O9 78.53(19) . 2_677 ? O1 Co2 O9 80.3(2) . 2_677 ? O12 Co2 N2 99.8(2) 2_567 2_677 ? O2 Co2 N2 79.4(2) 2_577 2_677 ? O9 Co2 N2 158.6(2) . 2_677 ? O1 Co2 N2 99.6(2) . 2_677 ? O9 Co2 N2 84.0(2) 2_677 2_677 ? O11 Co3 O15 87.1(2) . . ? O11 Co3 O17 94.5(2) . . ? O15 Co3 O17 178.2(2) . . ? O11 Co3 O16 173.5(2) . . ? O15 Co3 O16 86.4(2) . . ? O17 Co3 O16 92.0(2) . . ? O11 Co3 O15 91.22(19) . 2_577 ? O15 Co3 O15 82.04(19) . 2_577 ? O17 Co3 O15 98.5(2) . 2_577 ? O16 Co3 O15 87.16(19) . 2_577 ? O11 Co3 O7 95.3(2) . . ? O15 Co3 O7 98.08(18) . . ? O17 Co3 O7 81.2(2) . . ? O16 Co3 O7 86.37(19) . . ? O15 Co3 O7 173.51(19) 2_577 . ? O11 P1 O12 113.4(3) 2_567 . ? O11 P1 O5 112.8(3) 2_567 . ? O12 P1 O5 112.2(3) . . ? O11 P1 C6 105.8(3) 2_567 . ? O12 P1 C6 108.4(3) . . ? O5 P1 C6 103.4(3) . . ? O14 P2 O15 114.4(3) . . ? O14 P2 O9 111.7(3) . . ? O15 P2 O9 111.6(3) . . ? O14 P2 C7 111.3(3) . . ? O15 P2 C7 104.1(3) . . ? O9 P2 C7 102.7(3) . . ? P2 O15 Co3 132.8(3) . . ? P2 O15 Co3 129.0(3) . 2_577 ? Co3 O15 Co3 97.96(18) . 2_577 ? C1 O7 Co1 110.9(4) . . ? C1 O7 Co3 129.0(4) . . ? Co1 O7 Co3 120.0(2) . . ? P2 O9 Co2 134.2(3) . . ? P2 O9 Co2 115.1(3) . 2_677 ? Co2 O9 Co2 101.47(19) . 2_677 ? P1 O5 Co1 134.5(3) . 2_567 ? P1 O5 Co1 115.1(3) . . ? Co1 O5 Co1 100.34(19) 2_567 . ? C12 O2 Co2 118.2(5) . 2_577 ? C7 N2 C8 110.6(6) . . ? C7 N2 C11 109.4(6) . . ? C8 N2 C11 106.3(6) . . ? C7 N2 Co2 108.4(4) . 2_677 ? C8 N2 Co2 108.5(5) . 2_677 ? C11 N2 Co2 113.7(5) . 2_677 ? C3 N1 C2 107.0(6) . . ? C3 N1 C6 110.0(5) . . ? C2 N1 C6 111.9(5) . . ? C3 N1 Co1 114.1(4) . . ? C2 N1 Co1 107.0(4) . . ? C6 N1 Co1 106.9(4) . . ? P2 O14 Co1 140.2(3) . . ? P1 O11 Co3 135.1(3) 2_567 . ? P1 O12 Co2 145.6(3) . 2_567 ? N1 C6 P1 111.6(5) . . ? O8 C1 O7 123.6(7) . . ? O8 C1 C2 118.1(7) . . ? O7 C1 C2 118.3(6) . . ? N1 C3 C4 103.2(6) . . ? N1 C2 C1 112.4(6) . . ? N1 C2 C5 106.4(6) . . ? C1 C2 C5 109.2(6) . . ? O13 C12 O2 125.1(8) . . ? O13 C12 C8 115.4(8) . 1_455 ? O2 C12 C8 119.4(7) . 1_455 ? C10 C11 N2 103.8(7) . . ? N2 C7 P2 113.0(5) . . ? C5 C4 C3 102.4(7) . . ? C4 C5 C2 102.5(6) . . ? C11 C10 C9 101.6(8) . . ? N2 C8 C12 113.0(7) . 1_655 ? N2 C8 C9 105.5(7) . . ? C12 C8 C9 115.4(8) 1_655 . ? C10 C9 C8 102.7(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.77 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.820 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.146