# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _journal_volume ? _journal_year ? _journal_page_first ? loop_ _publ_author_name 'Xintao Wu' 'Rui-Biao Fu' 'Zhi-Youg Fu' 'Sheng-Min Hu' 'Xin-Tao Wu' 'Jian-Jun Zhang' _publ_contact_author_name 'Prof Xintao Wu' _publ_contact_author_address ; Prof Xintao Wu Dept. of Chemistry Fujian Ins. Res. Struct.Matter of Chinese Academy of Sciences Yangqiao road 155 Xihe Fuzhou Fujian 350002 CHINA ; _publ_contact_author_email WXT@MS.FJIRSM.AC.CN _publ_section_title ; Hydrothermal synthesis and crystal structure of two hetero-transition metal polymers: [Co(1,10-phen)2(V2O4) (O3PCH2CH2CH2PO3)]n and [{Co(1,10-phen)2}2(V4O10) (O3PCH2CH2CH2CH2PO3)(2H2O)]n ; data_f1 _database_code_CSD 194197 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H22 Co N4 O10 P2 V2' _chemical_formula_weight 785.24 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' V V 0.3005 0.5294 '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 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 16.553(2) _cell_length_b 10.5323(15) _cell_length_c 17.341(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.430(3) _cell_angle_gamma 90.00 _cell_volume 2927.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 69 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 25.09 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'salmon pink' _exptl_crystal_size_max .64 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1580 _exptl_absorpt_coefficient_mu 1.360 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .7480 _exptl_absorpt_correction_T_max 1.0000 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 4896 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.09 _reflns_number_total 2582 _reflns_number_gt 1773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _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^)+(0.0577P)^2^+19.0522P] 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 2582 _refine_ls_number_parameters 213 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1525 _refine_ls_wR_factor_gt 0.1306 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 0.0000 0.19436(11) 0.2500 0.0335(3) Uani 1 2 d S . . V1 V 0.13044(7) 0.54102(11) 0.53162(6) 0.0430(3) Uani 1 1 d . . . P1 P 0.01099(9) 0.44026(15) 0.37141(9) 0.0330(4) Uani 1 1 d . . . N1 N -0.1190(3) 0.1795(5) 0.2753(3) 0.0375(12) Uani 1 1 d . . . N2 N 0.0198(3) 0.0445(4) 0.3375(3) 0.0363(12) Uani 1 1 d . . . O1 O 0.1681(4) 0.4117(6) 0.5716(3) 0.0840(18) Uani 1 1 d . . . O2 O 0.2045(3) 0.6412(6) 0.5407(3) 0.0773(17) Uani 1 1 d . . . O3 O 0.0815(3) 0.5225(4) 0.4235(2) 0.0436(11) Uani 1 1 d . . . O4 O 0.0455(2) 0.3305(4) 0.3358(2) 0.0385(10) Uani 1 1 d . . . O5 O -0.0485(3) 0.3970(4) 0.4217(2) 0.0443(11) Uani 1 1 d . . . C1 C -0.1870(4) 0.2474(6) 0.2457(4) 0.0451(16) Uani 1 1 d . . . H1A H -0.1862 0.3064 0.2060 0.054 Uiso 1 1 calc R . . C2 C -0.2599(4) 0.2338(7) 0.2719(4) 0.0500(17) Uani 1 1 d . . . H2A H -0.3054 0.2865 0.2518 0.060 Uiso 1 1 calc R . . C3 C -0.2642(4) 0.1445(7) 0.3260(4) 0.0517(18) Uani 1 1 d . . . H3A H -0.3126 0.1352 0.3434 0.062 Uiso 1 1 calc R . . C4 C -0.1956(4) 0.0655(6) 0.3562(4) 0.0439(16) Uani 1 1 d . . . C5 C -0.1958(5) -0.0357(7) 0.4110(4) 0.0522(18) Uani 1 1 d . . . H5A H -0.2436 -0.0515 0.4284 0.063 Uiso 1 1 calc R . . C6 C -0.1287(5) -0.1073(7) 0.4373(4) 0.0561(19) Uani 1 1 d . . . H6A H -0.1311 -0.1740 0.4718 0.067 Uiso 1 1 calc R . . C7 C -0.0526(4) -0.0851(6) 0.4142(4) 0.0437(16) Uani 1 1 d . . . C8 C 0.0215(5) -0.1547(6) 0.4426(4) 0.0525(18) Uani 1 1 d . . . H8A H 0.0226 -0.2219 0.4777 0.063 Uiso 1 1 calc R . . C9 C 0.0910(4) -0.1238(6) 0.4190(4) 0.0518(17) Uani 1 1 d . . . H9A H 0.1399 -0.1700 0.4372 0.062 Uiso 1 1 calc R . . C10 C 0.0882(4) -0.0227(6) 0.3674(4) 0.0462(16) Uani 1 1 d . . . H10A H 0.1369 -0.0008 0.3530 0.055 Uiso 1 1 calc R . . C11 C -0.0495(4) 0.0144(6) 0.3611(3) 0.0364(14) Uani 1 1 d . . . C12 C -0.1238(4) 0.0897(5) 0.3298(4) 0.0365(14) Uani 1 1 d . . . C13 C -0.0489(4) 0.5456(6) 0.2979(3) 0.0380(14) Uani 1 1 d . . . H13A H -0.0908 0.4960 0.2611 0.046 Uiso 1 1 calc R . . H13B H -0.0781 0.6047 0.3244 0.046 Uiso 1 1 calc R . . C14 C 0.0000 0.6219(9) 0.2500 0.041(2) Uani 1 2 d S . . H14 H 0.038(3) 0.673(5) 0.287(3) 0.036(16) Uiso 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 0.0320(6) 0.0329(6) 0.0373(7) 0.000 0.0119(5) 0.000 V1 0.0428(6) 0.0483(7) 0.0392(6) -0.0007(5) 0.0125(5) 0.0025(5) P1 0.0360(8) 0.0344(9) 0.0294(8) -0.0016(7) 0.0100(6) 0.0032(7) N1 0.039(3) 0.035(3) 0.040(3) 0.003(2) 0.011(2) 0.001(2) N2 0.040(3) 0.033(3) 0.037(3) -0.002(2) 0.012(2) 0.002(2) O1 0.112(4) 0.075(4) 0.070(4) 0.024(3) 0.032(3) 0.049(4) O2 0.055(3) 0.102(4) 0.077(4) -0.024(3) 0.020(3) -0.032(3) O3 0.049(2) 0.046(3) 0.035(2) -0.006(2) 0.0096(19) -0.002(2) O4 0.040(2) 0.040(2) 0.035(2) -0.0047(19) 0.0085(18) 0.0066(19) O5 0.056(3) 0.040(2) 0.042(2) 0.007(2) 0.022(2) 0.008(2) C1 0.037(3) 0.044(4) 0.052(4) 0.006(3) 0.005(3) -0.001(3) C2 0.027(3) 0.056(4) 0.064(5) -0.006(4) 0.007(3) 0.005(3) C3 0.040(4) 0.067(5) 0.052(4) -0.013(4) 0.019(3) -0.014(3) C4 0.045(4) 0.049(4) 0.041(4) -0.013(3) 0.017(3) -0.018(3) C5 0.056(4) 0.055(5) 0.051(4) -0.005(4) 0.024(3) -0.021(4) C6 0.080(5) 0.042(4) 0.051(4) 0.001(3) 0.027(4) -0.019(4) C7 0.062(4) 0.031(3) 0.040(4) -0.007(3) 0.015(3) -0.006(3) C8 0.079(5) 0.036(4) 0.041(4) 0.003(3) 0.012(4) 0.004(4) C9 0.057(4) 0.041(4) 0.052(4) -0.001(3) 0.005(3) 0.012(3) C10 0.046(4) 0.039(4) 0.052(4) 0.001(3) 0.009(3) 0.006(3) C11 0.047(3) 0.033(3) 0.030(3) -0.003(3) 0.011(3) -0.005(3) C12 0.043(3) 0.030(3) 0.040(3) -0.005(3) 0.016(3) -0.004(3) C13 0.044(3) 0.037(3) 0.035(3) 0.004(3) 0.013(3) 0.005(3) C14 0.048(5) 0.035(5) 0.039(5) 0.000 0.008(4) 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 O4 2.069(4) . ? Co1 O4 2.069(4) 2 ? Co1 N1 2.128(5) . ? Co1 N1 2.128(5) 2 ? Co1 N2 2.156(5) 2 ? Co1 N2 2.156(5) . ? V1 O1 1.584(5) . ? V1 O2 1.595(5) . ? V1 O3 1.857(4) . ? V1 O5 1.863(4) 5_566 ? P1 O4 1.490(4) . ? P1 O5 1.538(4) . ? P1 O3 1.551(4) . ? P1 C13 1.791(6) . ? N1 C1 1.324(7) . ? N1 C12 1.352(7) . ? N2 C10 1.327(8) . ? N2 C11 1.348(7) . ? O5 V1 1.863(4) 5_566 ? C1 C2 1.399(8) . ? C2 C3 1.343(10) . ? C3 C4 1.399(9) . ? C4 C12 1.400(8) . ? C4 C5 1.428(9) . ? C5 C6 1.326(10) . ? C6 C7 1.434(9) . ? C7 C11 1.404(8) . ? C7 C8 1.408(9) . ? C8 C9 1.353(9) . ? C9 C10 1.384(9) . ? C11 C12 1.450(8) . ? C13 C14 1.526(7) . ? C14 C13 1.526(7) 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 O4 Co1 O4 92.3(2) . 2 ? O4 Co1 N1 95.31(17) . . ? O4 Co1 N1 90.54(17) 2 . ? O4 Co1 N1 90.54(17) . 2 ? O4 Co1 N1 95.31(17) 2 2 ? N1 Co1 N1 171.6(3) . 2 ? O4 Co1 N2 167.79(16) . 2 ? O4 Co1 N2 92.12(17) 2 2 ? N1 Co1 N2 96.04(18) . 2 ? N1 Co1 N2 77.70(18) 2 2 ? O4 Co1 N2 92.12(17) . . ? O4 Co1 N2 167.79(16) 2 . ? N1 Co1 N2 77.70(18) . . ? N1 Co1 N2 96.04(18) 2 . ? N2 Co1 N2 85.9(3) 2 . ? O1 V1 O2 108.5(3) . . ? O1 V1 O3 112.1(3) . . ? O2 V1 O3 107.5(2) . . ? O1 V1 O5 111.2(2) . 5_566 ? O2 V1 O5 110.5(3) . 5_566 ? O3 V1 O5 107.07(19) . 5_566 ? O4 P1 O5 111.8(2) . . ? O4 P1 O3 111.3(2) . . ? O5 P1 O3 109.3(2) . . ? O4 P1 C13 112.8(3) . . ? O5 P1 C13 105.5(2) . . ? O3 P1 C13 105.8(3) . . ? C1 N1 C12 117.2(5) . . ? C1 N1 Co1 128.4(4) . . ? C12 N1 Co1 114.4(4) . . ? C10 N2 C11 117.6(5) . . ? C10 N2 Co1 129.1(4) . . ? C11 N2 Co1 113.2(4) . . ? P1 O3 V1 136.3(3) . . ? P1 O4 Co1 136.6(2) . . ? P1 O5 V1 141.3(3) . 5_566 ? N1 C1 C2 122.5(6) . . ? C3 C2 C1 119.9(6) . . ? C2 C3 C4 119.9(6) . . ? C3 C4 C12 116.4(6) . . ? C3 C4 C5 123.8(6) . . ? C12 C4 C5 119.7(6) . . ? C6 C5 C4 120.9(6) . . ? C5 C6 C7 122.0(7) . . ? C11 C7 C8 116.6(6) . . ? C11 C7 C6 118.9(6) . . ? C8 C7 C6 124.5(6) . . ? C9 C8 C7 120.0(6) . . ? C8 C9 C10 119.1(6) . . ? N2 C10 C9 123.5(6) . . ? N2 C11 C7 123.2(6) . . ? N2 C11 C12 117.6(5) . . ? C7 C11 C12 119.2(5) . . ? N1 C12 C4 123.9(6) . . ? N1 C12 C11 116.9(5) . . ? C4 C12 C11 119.2(6) . . ? C14 C13 P1 116.0(4) . . ? C13 C14 C13 116.4(7) . 2 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.496 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.106 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ; data_f1_2 _database_code_CSD 194198 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H44 Co2 N8 O18 P2 V4' _chemical_formula_weight 1452.51 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' V V 0.3005 0.5294 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2132(3) _cell_length_b 11.7055(5) _cell_length_c 12.3666(5) _cell_angle_alpha 75.594(2) _cell_angle_beta 82.445(2) _cell_angle_gamma 86.071(2) _cell_volume 1418.53(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 56 _cell_measurement_theta_min 1.71 _cell_measurement_theta_max 25.03 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max .36 _exptl_crystal_size_mid .28 _exptl_crystal_size_min .18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 1.340 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .7302 _exptl_absorpt_correction_T_max 1.0000 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 7439 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4961 _reflns_number_gt 3742 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _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^)+(0.0103P)^2^+5.5896P] 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 4961 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0872 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 0.19370(7) 0.74479(6) 0.72724(6) 0.03123(19) Uani 1 1 d . . . V1 V 0.39718(8) 0.68161(8) 0.50951(7) 0.0305(2) Uani 1 1 d . . . V2 V 0.34552(9) 0.26513(8) 0.70391(7) 0.0341(2) Uani 1 1 d . . . P1 P 0.40101(14) 0.51303(12) 0.74551(11) 0.0329(3) Uani 1 1 d . . . N1 N 0.0734(4) 0.9020(4) 0.6830(4) 0.0326(10) Uani 1 1 d . . . N2 N 0.0381(4) 0.6846(4) 0.6599(4) 0.0334(10) Uani 1 1 d . . . N3 N 0.0960(4) 0.7153(4) 0.8960(4) 0.0387(11) Uani 1 1 d . . . N4 N 0.3289(4) 0.8147(4) 0.8116(4) 0.0354(10) Uani 1 1 d . . . O1 O 0.2699(3) 0.5729(3) 0.7712(3) 0.0365(9) Uani 1 1 d . . . O2 O 0.4593(4) 0.5577(3) 0.6210(3) 0.0432(10) Uani 1 1 d . . . O3 O 0.3924(4) 0.3775(3) 0.7734(3) 0.0440(10) Uani 1 1 d . . . O4 O 0.3250(3) 0.7777(3) 0.5785(3) 0.0374(9) Uani 1 1 d . . . O5 O 0.2888(4) 0.6378(4) 0.4468(3) 0.0480(10) Uani 1 1 d . . . O6 O 0.5315(4) 0.7448(4) 0.4131(3) 0.0469(10) Uani 1 1 d . . . O7 O 0.2041(4) 0.3060(4) 0.6593(3) 0.0552(12) Uani 1 1 d . . . O8 O 0.3320(5) 0.1412(4) 0.7963(4) 0.0645(13) Uani 1 1 d . . . O9 O 0.1434(14) 0.0479(11) 0.9957(13) 0.299(8) Uani 1 1 d . . . C1 C 0.5149(5) 0.5352(5) 0.8356(4) 0.0371(13) Uani 1 1 d . . . H1A H 0.5978 0.4925 0.8219 0.045 Uiso 1 1 calc R . . H1B H 0.5326 0.6185 0.8203 0.045 Uiso 1 1 calc R . . C2 C 0.4550(6) 0.4906(5) 0.9590(5) 0.0445(14) Uani 1 1 d . . . H2A H 0.3707 0.5318 0.9710 0.053 Uiso 1 1 calc R . . H2B H 0.4389 0.4071 0.9736 0.053 Uiso 1 1 calc R . . C3 C 0.0949(5) 1.0094(5) 0.6898(5) 0.0400(14) Uani 1 1 d . . . H3 H 0.1725 1.0223 0.7160 0.048 Uiso 1 1 calc R . . C4 C 0.0059(6) 1.1052(5) 0.6593(5) 0.0477(15) Uani 1 1 d . . . H4 H 0.0255 1.1802 0.6639 0.057 Uiso 1 1 calc R . . C5 C -0.1091(6) 1.0874(5) 0.6230(5) 0.0446(14) Uani 1 1 d . . . H5 H -0.1695 1.1500 0.6033 0.053 Uiso 1 1 calc R . . C6 C -0.1367(5) 0.9733(5) 0.6154(4) 0.0358(12) Uani 1 1 d . . . C7 C -0.2538(5) 0.9466(5) 0.5760(5) 0.0426(14) Uani 1 1 d . . . H7 H -0.3168 1.0064 0.5543 0.051 Uiso 1 1 calc R . . C8 C -0.2740(5) 0.8365(5) 0.5699(5) 0.0431(14) Uani 1 1 d . . . H8 H -0.3520 0.8211 0.5457 0.052 Uiso 1 1 calc R . . C9 C -0.1792(5) 0.7424(5) 0.5994(4) 0.0356(13) Uani 1 1 d . . . C10 C -0.1930(5) 0.6259(5) 0.5913(4) 0.0389(13) Uani 1 1 d . . . H10 H -0.2706 0.6045 0.5710 0.047 Uiso 1 1 calc R . . C11 C -0.0918(6) 0.5449(5) 0.6136(5) 0.0423(14) Uani 1 1 d . . . H11 H -0.0990 0.4682 0.6069 0.051 Uiso 1 1 calc R . . C12 C 0.0235(5) 0.5777(5) 0.6466(5) 0.0396(13) Uani 1 1 d . . . H12 H 0.0926 0.5220 0.6596 0.048 Uiso 1 1 calc R . . C13 C -0.0610(5) 0.7670(5) 0.6352(4) 0.0306(11) Uani 1 1 d . . . C14 C -0.0412(5) 0.8830(4) 0.6456(4) 0.0298(11) Uani 1 1 d . . . C15 C -0.0200(6) 0.6685(6) 0.9368(5) 0.0533(17) Uani 1 1 d . . . H15 H -0.0724 0.6511 0.8874 0.064 Uiso 1 1 calc R . . C16 C -0.0674(7) 0.6442(7) 1.0520(6) 0.069(2) Uani 1 1 d . . . H16 H -0.1490 0.6106 1.0781 0.082 Uiso 1 1 calc R . . C17 C 0.0083(8) 0.6706(6) 1.1241(6) 0.067(2) Uani 1 1 d . . . H17 H -0.0233 0.6576 1.2000 0.080 Uiso 1 1 calc R . . C18 C 0.1319(7) 0.7167(5) 1.0861(5) 0.0489(16) Uani 1 1 d . . . C19 C 0.2200(8) 0.7429(6) 1.1576(5) 0.064(2) Uani 1 1 d . . . H19 H 0.1949 0.7267 1.2347 0.077 Uiso 1 1 calc R . . C20 C 0.3361(8) 0.7898(7) 1.1160(6) 0.063(2) Uani 1 1 d . . . H20 H 0.3910 0.8049 1.1648 0.076 Uiso 1 1 calc R . . C21 C 0.3790(6) 0.8175(5) 0.9977(5) 0.0453(15) Uani 1 1 d . . . C22 C 0.4996(6) 0.8681(6) 0.9486(6) 0.0589(19) Uani 1 1 d . . . H22 H 0.5583 0.8844 0.9938 0.071 Uiso 1 1 calc R . . C23 C 0.5316(6) 0.8935(6) 0.8350(6) 0.0603(19) Uani 1 1 d . . . H23 H 0.6106 0.9288 0.8018 0.072 Uiso 1 1 calc R . . C24 C 0.4427(6) 0.8653(5) 0.7696(5) 0.0470(15) Uani 1 1 d . . . H24 H 0.4649 0.8831 0.6920 0.056 Uiso 1 1 calc R . . C25 C 0.2958(5) 0.7921(5) 0.9249(5) 0.0370(13) Uani 1 1 d . . . C26 C 0.1718(6) 0.7402(5) 0.9695(4) 0.0379(13) 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 0.0236(4) 0.0397(4) 0.0328(4) -0.0142(3) -0.0012(3) -0.0026(3) V1 0.0247(5) 0.0400(5) 0.0287(5) -0.0117(4) -0.0030(4) -0.0022(4) V2 0.0319(5) 0.0409(5) 0.0316(5) -0.0132(4) 0.0008(4) -0.0078(4) P1 0.0331(8) 0.0373(8) 0.0304(7) -0.0108(6) -0.0078(6) 0.0021(6) N1 0.027(2) 0.036(3) 0.038(3) -0.015(2) -0.0016(19) -0.0047(19) N2 0.031(2) 0.036(3) 0.035(3) -0.011(2) -0.0009(19) -0.005(2) N3 0.033(3) 0.044(3) 0.040(3) -0.016(2) 0.003(2) -0.002(2) N4 0.027(2) 0.042(3) 0.041(3) -0.017(2) -0.003(2) 0.000(2) O1 0.031(2) 0.041(2) 0.037(2) -0.0089(17) -0.0037(16) 0.0014(16) O2 0.041(2) 0.055(2) 0.029(2) -0.0069(18) -0.0024(17) 0.0141(19) O3 0.049(2) 0.045(2) 0.043(2) -0.0155(19) -0.0156(19) 0.0001(19) O4 0.035(2) 0.044(2) 0.033(2) -0.0151(17) 0.0042(16) 0.0013(17) O5 0.036(2) 0.060(3) 0.056(3) -0.023(2) -0.0136(19) -0.0065(19) O6 0.035(2) 0.056(3) 0.054(3) -0.027(2) 0.0129(18) -0.0157(19) O7 0.033(2) 0.088(3) 0.052(3) -0.029(2) -0.0076(19) -0.005(2) O8 0.089(4) 0.046(3) 0.055(3) -0.007(2) 0.000(3) -0.014(2) O9 0.274(15) 0.196(12) 0.328(17) 0.040(11) 0.093(13) 0.040(11) C1 0.037(3) 0.043(3) 0.036(3) -0.014(3) -0.011(2) -0.001(3) C2 0.052(4) 0.048(4) 0.037(3) -0.010(3) -0.019(3) -0.003(3) C3 0.032(3) 0.049(4) 0.048(3) -0.027(3) -0.004(3) -0.009(3) C4 0.046(4) 0.038(3) 0.065(4) -0.024(3) -0.004(3) -0.006(3) C5 0.041(3) 0.038(3) 0.055(4) -0.014(3) -0.006(3) 0.005(3) C6 0.029(3) 0.043(3) 0.036(3) -0.012(3) -0.004(2) 0.002(2) C7 0.033(3) 0.051(4) 0.044(3) -0.011(3) -0.010(3) 0.008(3) C8 0.027(3) 0.056(4) 0.050(4) -0.017(3) -0.010(3) -0.003(3) C9 0.031(3) 0.048(3) 0.029(3) -0.012(3) 0.001(2) -0.008(2) C10 0.034(3) 0.050(4) 0.037(3) -0.013(3) -0.009(2) -0.010(3) C11 0.049(4) 0.039(3) 0.043(3) -0.015(3) -0.007(3) -0.011(3) C12 0.036(3) 0.038(3) 0.049(4) -0.015(3) -0.008(3) -0.007(2) C13 0.025(3) 0.038(3) 0.030(3) -0.012(2) 0.000(2) -0.004(2) C14 0.021(3) 0.037(3) 0.031(3) -0.011(2) 0.003(2) -0.005(2) C15 0.044(4) 0.066(4) 0.050(4) -0.018(3) 0.008(3) -0.019(3) C16 0.059(5) 0.074(5) 0.062(5) -0.009(4) 0.020(4) -0.012(4) C17 0.074(5) 0.074(5) 0.041(4) -0.010(4) 0.019(4) 0.007(4) C18 0.059(4) 0.050(4) 0.035(3) -0.010(3) -0.004(3) 0.014(3) C19 0.086(6) 0.073(5) 0.034(4) -0.017(3) -0.013(4) 0.021(4) C20 0.076(5) 0.081(5) 0.044(4) -0.031(4) -0.030(4) 0.025(4) C21 0.046(4) 0.053(4) 0.044(4) -0.024(3) -0.017(3) 0.013(3) C22 0.045(4) 0.071(5) 0.077(5) -0.040(4) -0.028(4) 0.004(3) C23 0.038(4) 0.075(5) 0.079(5) -0.034(4) -0.012(3) -0.015(3) C24 0.034(3) 0.058(4) 0.054(4) -0.024(3) -0.003(3) -0.007(3) C25 0.034(3) 0.044(3) 0.038(3) -0.019(3) -0.009(2) 0.008(3) C26 0.043(3) 0.040(3) 0.032(3) -0.012(3) -0.005(3) 0.008(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 O1 2.075(4) . ? Co1 O4 2.098(3) . ? Co1 N2 2.124(4) . ? Co1 N1 2.136(4) . ? Co1 N3 2.147(4) . ? Co1 N4 2.150(4) . ? V1 O5 1.609(4) . ? V1 O4 1.654(3) . ? V1 O6 1.766(4) . ? V1 O2 1.875(4) . ? V2 O8 1.609(4) . ? V2 O7 1.613(4) . ? V2 O6 1.809(4) 2_666 ? V2 O3 1.859(4) . ? P1 O1 1.501(4) . ? P1 O3 1.544(4) . ? P1 O2 1.549(4) . ? P1 C1 1.786(5) . ? N1 C3 1.316(6) . ? N1 C14 1.364(6) . ? N2 C12 1.322(6) . ? N2 C13 1.360(6) . ? N3 C15 1.324(7) . ? N3 C26 1.363(7) . ? N4 C24 1.324(7) . ? N4 C25 1.361(7) . ? O6 V2 1.809(4) 2_666 ? C1 C2 1.542(8) . ? C2 C2 1.518(10) 2_667 ? C3 C4 1.402(8) . ? C4 C5 1.359(8) . ? C5 C6 1.412(8) . ? C6 C14 1.402(7) . ? C6 C7 1.430(7) . ? C7 C8 1.341(8) . ? C8 C9 1.424(8) . ? C9 C13 1.410(7) . ? C9 C10 1.411(7) . ? C10 C11 1.362(8) . ? C11 C12 1.402(7) . ? C13 C14 1.426(7) . ? C15 C16 1.407(9) . ? C16 C17 1.356(10) . ? C17 C18 1.385(9) . ? C18 C26 1.409(8) . ? C18 C19 1.437(9) . ? C19 C20 1.327(10) . ? C20 C21 1.433(9) . ? C21 C22 1.401(9) . ? C21 C25 1.410(7) . ? C22 C23 1.361(9) . ? C23 C24 1.398(8) . ? C25 C26 1.425(8) . ? 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 O4 90.19(14) . . ? O1 Co1 N2 89.56(15) . . ? O4 Co1 N2 96.42(15) . . ? O1 Co1 N1 166.64(15) . . ? O4 Co1 N1 96.26(15) . . ? N2 Co1 N1 78.12(16) . . ? O1 Co1 N3 87.15(16) . . ? O4 Co1 N3 167.67(16) . . ? N2 Co1 N3 95.60(17) . . ? N1 Co1 N3 88.89(17) . . ? O1 Co1 N4 94.62(15) . . ? O4 Co1 N4 90.81(15) . . ? N2 Co1 N4 171.65(16) . . ? N1 Co1 N4 96.97(16) . . ? N3 Co1 N4 77.43(17) . . ? O5 V1 O4 108.8(2) . . ? O5 V1 O6 111.3(2) . . ? O4 V1 O6 110.75(18) . . ? O5 V1 O2 111.4(2) . . ? O4 V1 O2 104.67(17) . . ? O6 V1 O2 109.73(19) . . ? O8 V2 O7 109.3(2) . . ? O8 V2 O6 111.7(2) . 2_666 ? O7 V2 O6 109.9(2) . 2_666 ? O8 V2 O3 108.2(2) . . ? O7 V2 O3 108.0(2) . . ? O6 V2 O3 109.69(18) 2_666 . ? O1 P1 O3 112.1(2) . . ? O1 P1 O2 111.9(2) . . ? O3 P1 O2 109.1(2) . . ? O1 P1 C1 110.1(2) . . ? O3 P1 C1 103.3(2) . . ? O2 P1 C1 109.8(2) . . ? C3 N1 C14 118.5(5) . . ? C3 N1 Co1 128.7(4) . . ? C14 N1 Co1 112.8(3) . . ? C12 N2 C13 118.0(4) . . ? C12 N2 Co1 128.3(4) . . ? C13 N2 Co1 113.6(3) . . ? C15 N3 C26 118.0(5) . . ? C15 N3 Co1 128.5(4) . . ? C26 N3 Co1 113.2(3) . . ? C24 N4 C25 117.6(5) . . ? C24 N4 Co1 128.8(4) . . ? C25 N4 Co1 113.3(3) . . ? P1 O1 Co1 134.5(2) . . ? P1 O2 V1 129.0(2) . . ? P1 O3 V2 137.3(2) . . ? V1 O4 Co1 128.2(2) . . ? V1 O6 V2 148.6(2) . 2_666 ? C2 C1 P1 109.0(4) . . ? C2 C2 C1 112.2(6) 2_667 . ? N1 C3 C4 122.9(5) . . ? C5 C4 C3 119.3(5) . . ? C4 C5 C6 119.7(5) . . ? C14 C6 C5 117.3(5) . . ? C14 C6 C7 119.1(5) . . ? C5 C6 C7 123.6(5) . . ? C8 C7 C6 120.8(5) . . ? C7 C8 C9 121.8(5) . . ? C13 C9 C10 117.0(5) . . ? C13 C9 C8 118.6(5) . . ? C10 C9 C8 124.3(5) . . ? C11 C10 C9 119.5(5) . . ? C10 C11 C12 119.6(5) . . ? N2 C12 C11 122.8(5) . . ? N2 C13 C9 123.0(5) . . ? N2 C13 C14 117.2(4) . . ? C9 C13 C14 119.8(5) . . ? N1 C14 C6 122.4(5) . . ? N1 C14 C13 117.8(5) . . ? C6 C14 C13 119.8(5) . . ? N3 C15 C16 122.7(6) . . ? C17 C16 C15 118.7(7) . . ? C16 C17 C18 120.9(6) . . ? C17 C18 C26 117.1(6) . . ? C17 C18 C19 124.3(6) . . ? C26 C18 C19 118.7(6) . . ? C20 C19 C18 121.6(6) . . ? C19 C20 C21 121.5(6) . . ? C22 C21 C25 117.2(6) . . ? C22 C21 C20 124.2(6) . . ? C25 C21 C20 118.6(6) . . ? C23 C22 C21 120.4(6) . . ? C22 C23 C24 118.4(6) . . ? N4 C24 C23 123.9(6) . . ? N4 C25 C21 122.6(5) . . ? N4 C25 C26 117.4(5) . . ? C21 C25 C26 120.0(5) . . ? N3 C26 C18 122.5(5) . . ? N3 C26 C25 117.8(5) . . ? C18 C26 C25 119.6(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.417 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.090 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ;