data_ic14157 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H16 Co2 N2 O6' _chemical_formula_weight 462.18 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' '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 P2(1)/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 14.2780(7) _cell_length_b 11.1546(6) _cell_length_c 11.3505(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.082(3) _cell_angle_gamma 90.00 _cell_volume 1753.42(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10397 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.930 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.787 _exptl_absorpt_correction_T_max 0.982 _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10397 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4031 _reflns_number_gt 3049 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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^)+(0.0617P)^2^+0.5667P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4031 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 0.16141(3) 0.42156(4) 0.28339(4) 0.01384(13) Uani 1 1 d . . . Co2 Co 0.01011(3) 0.56653(4) 0.37625(4) 0.01449(13) Uani 1 1 d . . . O1 O -0.05557(14) 0.73230(19) 0.33208(18) 0.0166(4) Uani 1 1 d . . . O2 O -0.04528(15) 0.59782(18) 0.52752(18) 0.0150(4) Uani 1 1 d . . . O3 O 0.15418(14) 0.6208(2) 0.47001(18) 0.0193(5) Uani 1 1 d . . . O4 O 0.25828(15) 0.53958(19) 0.37238(19) 0.0191(5) Uani 1 1 d . . . O5 O 0.04937(14) 0.52030(19) 0.22938(18) 0.0177(5) Uani 1 1 d . . . O6 O -0.13070(15) 0.4812(2) 0.30825(19) 0.0213(5) Uani 1 1 d . . . H6A H -0.1417 0.4356 0.3604 0.032 Uiso 1 1 d R . . N1 N -0.18067(17) 0.8396(2) 0.3666(2) 0.0134(5) Uani 1 1 d . . . N2 N -0.17268(16) 0.6946(2) 0.5743(2) 0.0139(5) Uani 1 1 d . . . C1 C -0.1155(2) 0.7530(3) 0.3962(3) 0.0150(6) Uani 1 1 d . . . C2 C -0.1117(2) 0.6786(3) 0.5053(3) 0.0125(6) Uani 1 1 d . . . C3 C -0.24286(19) 0.8605(3) 0.4418(3) 0.0138(6) Uani 1 1 d . . . C4 C -0.3079(2) 0.9566(3) 0.4165(3) 0.0195(7) Uani 1 1 d . . . H4 H -0.3100 1.0056 0.3474 0.023 Uiso 1 1 calc R . . C5 C -0.3686(2) 0.9805(3) 0.4908(3) 0.0245(7) Uani 1 1 d . . . H5 H -0.4119 1.0464 0.4736 0.029 Uiso 1 1 calc R . . C6 C -0.3666(2) 0.9079(3) 0.5914(3) 0.0249(8) Uani 1 1 d . . . H6 H -0.4089 0.9244 0.6424 0.030 Uiso 1 1 calc R . . C7 C -0.3038(2) 0.8124(3) 0.6173(3) 0.0217(7) Uani 1 1 d . . . H7 H -0.3040 0.7625 0.6850 0.026 Uiso 1 1 calc R . . C8 C -0.2396(2) 0.7884(3) 0.5444(3) 0.0147(6) Uani 1 1 d . . . C9 C 0.3226(2) 0.6392(3) 0.5582(3) 0.0176(6) Uani 1 1 d . . . C10 C 0.3109(2) 0.7242(3) 0.6423(3) 0.0215(7) Uani 1 1 d . . . H10 H 0.2495 0.7606 0.6347 0.026 Uiso 1 1 calc R . . C11 C 0.3874(2) 0.7569(3) 0.7372(3) 0.0260(8) Uani 1 1 d . . . H11 H 0.3787 0.8156 0.7943 0.031 Uiso 1 1 calc R . . C12 C 0.4765(2) 0.7038(3) 0.7485(3) 0.0312(8) Uani 1 1 d . . . H12 H 0.5291 0.7254 0.8139 0.037 Uiso 1 1 calc R . . C13 C 0.4893(3) 0.6190(4) 0.6644(4) 0.0418(10) Uani 1 1 d . . . H13 H 0.5508 0.5828 0.6719 0.050 Uiso 1 1 calc R . . C14 C 0.4124(2) 0.5870(3) 0.5693(3) 0.0322(9) Uani 1 1 d . . . H14 H 0.4213 0.5291 0.5116 0.039 Uiso 1 1 calc R . . C15 C 0.2383(2) 0.5982(3) 0.4588(3) 0.0166(6) Uani 1 1 d . . . C16 C 0.0472(3) 0.6018(4) 0.1344(3) 0.0376(10) Uani 1 1 d . . . H16A H 0.0724 0.6794 0.1683 0.056 Uiso 1 1 calc R . . H16B H -0.0195 0.6116 0.0867 0.056 Uiso 1 1 calc R . . H16C H 0.0871 0.5712 0.0820 0.056 Uiso 1 1 calc R . . C17 C -0.1510(3) 0.4137(3) 0.1967(3) 0.0267(8) Uani 1 1 d . . . H17A H -0.1491 0.4672 0.1289 0.040 Uiso 1 1 calc R . . H17B H -0.2153 0.3775 0.1832 0.040 Uiso 1 1 calc R . . H17C H -0.1025 0.3504 0.2021 0.040 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 0.0188(2) 0.0132(2) 0.0105(2) 0.00014(16) 0.00536(17) 0.00138(16) Co2 0.0181(2) 0.0152(2) 0.0111(2) 0.00093(16) 0.00550(17) 0.00293(16) O1 0.0216(10) 0.0158(11) 0.0155(10) 0.0030(9) 0.0110(9) 0.0044(8) O2 0.0214(11) 0.0144(11) 0.0109(10) 0.0014(9) 0.0071(9) 0.0042(8) O3 0.0200(11) 0.0226(12) 0.0160(11) -0.0022(10) 0.0059(9) -0.0009(9) O4 0.0231(11) 0.0170(12) 0.0177(11) -0.0040(9) 0.0061(9) -0.0032(9) O5 0.0245(11) 0.0160(12) 0.0136(11) 0.0016(9) 0.0067(9) 0.0034(9) O6 0.0238(11) 0.0255(13) 0.0146(11) 0.0024(10) 0.0047(9) -0.0013(10) N1 0.0174(12) 0.0120(13) 0.0107(12) 0.0010(10) 0.0034(10) -0.0009(9) N2 0.0157(12) 0.0147(13) 0.0111(12) 0.0009(10) 0.0031(10) 0.0013(10) C1 0.0175(14) 0.0150(16) 0.0124(14) -0.0006(12) 0.0033(12) -0.0024(12) C2 0.0136(14) 0.0131(15) 0.0101(13) -0.0033(12) 0.0015(11) -0.0012(11) C3 0.0142(14) 0.0180(16) 0.0088(14) -0.0026(12) 0.0023(11) 0.0002(11) C4 0.0220(16) 0.0208(17) 0.0148(15) 0.0038(13) 0.0030(13) 0.0025(12) C5 0.0246(17) 0.0269(19) 0.0226(18) 0.0027(15) 0.0069(14) 0.0111(14) C6 0.0227(17) 0.034(2) 0.0192(17) 0.0059(15) 0.0085(14) 0.0107(14) C7 0.0233(17) 0.0285(19) 0.0158(15) 0.0043(14) 0.0098(13) 0.0041(13) C8 0.0152(14) 0.0156(16) 0.0127(14) -0.0006(12) 0.0021(12) 0.0025(11) C9 0.0190(15) 0.0167(16) 0.0172(15) 0.0018(13) 0.0046(13) -0.0040(12) C10 0.0231(16) 0.0199(17) 0.0210(16) -0.0023(14) 0.0043(13) 0.0013(13) C11 0.0326(18) 0.0215(18) 0.0232(18) -0.0065(14) 0.0054(15) -0.0015(14) C12 0.0281(18) 0.037(2) 0.0242(19) -0.0055(16) -0.0010(15) -0.0038(16) C13 0.0234(19) 0.060(3) 0.038(2) -0.017(2) -0.0008(17) 0.0142(18) C14 0.0249(18) 0.042(2) 0.0272(19) -0.0145(17) 0.0021(16) 0.0052(15) C15 0.0220(16) 0.0125(15) 0.0168(15) 0.0017(12) 0.0073(13) -0.0022(12) C16 0.058(3) 0.034(2) 0.028(2) 0.0162(17) 0.0241(19) 0.0225(19) C17 0.0319(18) 0.030(2) 0.0183(17) -0.0058(15) 0.0065(15) -0.0051(14) _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 O5 1.916(2) . ? Co1 O4 1.997(2) . ? Co1 N1 2.009(2) 2_545 ? Co1 N2 2.046(2) 3_566 ? Co2 O5 1.953(2) . ? Co2 O1 2.079(2) . ? Co2 O2 2.087(2) . ? Co2 O2 2.131(2) 3_566 ? Co2 O3 2.160(2) . ? Co2 O6 2.188(2) . ? O1 C1 1.272(3) . ? O2 C2 1.287(3) . ? O2 Co2 2.131(2) 3_566 ? O3 C15 1.264(3) . ? O4 C15 1.267(4) . ? O5 C16 1.405(4) . ? O6 C17 1.441(4) . ? N1 C1 1.327(4) . ? N1 C3 1.393(3) . ? N1 Co1 2.009(2) 2 ? N2 C2 1.318(4) . ? N2 C8 1.402(4) . ? N2 Co1 2.046(2) 3_566 ? C1 C2 1.481(4) . ? C3 C4 1.401(4) . ? C3 C8 1.406(4) . ? C4 C5 1.375(4) . ? C5 C6 1.394(5) . ? C6 C7 1.377(4) . ? C7 C8 1.403(4) . ? C9 C10 1.384(4) . ? C9 C14 1.386(4) . ? C9 C15 1.506(4) . ? C10 C11 1.384(4) . ? C11 C12 1.380(5) . ? C12 C13 1.388(5) . ? C13 C14 1.386(5) . ? 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 Co1 O4 101.80(9) . . ? O5 Co1 N1 105.44(9) . 2_545 ? O4 Co1 N1 120.52(9) . 2_545 ? O5 Co1 N2 121.05(9) . 3_566 ? O4 Co1 N2 96.11(9) . 3_566 ? N1 Co1 N2 112.33(10) 2_545 3_566 ? O5 Co2 O1 103.61(8) . . ? O5 Co2 O2 172.44(9) . . ? O1 Co2 O2 79.08(8) . . ? O5 Co2 O2 97.45(8) . 3_566 ? O1 Co2 O2 157.71(8) . 3_566 ? O2 Co2 O2 79.13(8) . 3_566 ? O5 Co2 O3 93.32(8) . . ? O1 Co2 O3 100.92(8) . . ? O2 Co2 O3 93.09(8) . . ? O2 Co2 O3 84.89(8) 3_566 . ? O5 Co2 O6 90.80(8) . . ? O1 Co2 O6 88.84(8) . . ? O2 Co2 O6 82.15(8) . . ? O2 Co2 O6 83.59(8) 3_566 . ? O3 Co2 O6 168.18(8) . . ? C1 O1 Co2 110.49(18) . . ? C2 O2 Co2 111.36(17) . . ? C2 O2 Co2 140.62(19) . 3_566 ? Co2 O2 Co2 100.87(8) . 3_566 ? C15 O3 Co2 135.2(2) . . ? C15 O4 Co1 118.24(19) . . ? C16 O5 Co1 118.6(2) . . ? C16 O5 Co2 121.8(2) . . ? Co1 O5 Co2 105.63(9) . . ? C17 O6 Co2 120.58(19) . . ? C1 N1 C3 118.6(2) . . ? C1 N1 Co1 108.28(19) . 2 ? C3 N1 Co1 133.0(2) . 2 ? C2 N2 C8 117.9(2) . . ? C2 N2 Co1 116.54(19) . 3_566 ? C8 N2 Co1 125.59(19) . 3_566 ? O1 C1 N1 121.0(3) . . ? O1 C1 C2 118.9(3) . . ? N1 C1 C2 120.1(3) . . ? O2 C2 N2 122.7(3) . . ? O2 C2 C1 115.6(2) . . ? N2 C2 C1 121.7(3) . . ? N1 C3 C4 119.4(3) . . ? N1 C3 C8 120.9(3) . . ? C4 C3 C8 119.6(3) . . ? C5 C4 C3 120.5(3) . . ? C4 C5 C6 120.0(3) . . ? C7 C6 C5 120.4(3) . . ? C6 C7 C8 120.5(3) . . ? N2 C8 C7 120.3(3) . . ? N2 C8 C3 120.7(2) . . ? C7 C8 C3 119.0(3) . . ? C10 C9 C14 119.3(3) . . ? C10 C9 C15 121.1(3) . . ? C14 C9 C15 119.6(3) . . ? C9 C10 C11 120.8(3) . . ? C12 C11 C10 119.6(3) . . ? C11 C12 C13 120.2(3) . . ? C14 C13 C12 119.9(3) . . ? C13 C14 C9 120.2(3) . . ? O3 C15 O4 125.4(3) . . ? O3 C15 C9 118.0(3) . . ? O4 C15 C9 116.6(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.993 _refine_diff_density_min -0.937 _refine_diff_density_rms 0.115