data_1100144 loop_ _publ_author_name 'Esther R. Acuna-Cueva' 'Rene Faure' 'Nuria A. Illan-Cabeza' 'Sonia B. Jimenez-Pulido' 'Miguel N. Moreno-Carretero' 'Miguel Quiros' _journal_name_full 'Inorganica Chimica Acta' _journal_volume 342 _journal_page_first 209 _journal_page_last 218 _journal_year 2003 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Co N10 O12' _chemical_formula_weight 631.40 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 'P 21/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 13.2319(9) _cell_length_b 8.1677(7) _cell_length_c 12.9061(9) _cell_angle_alpha 90.00 _cell_angle_beta 109.305(5) _cell_angle_gamma 90.00 _cell_volume 1316.39(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 37 _cell_measurement_theta_min 4.99 _cell_measurement_theta_max 12.06 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 650 _exptl_absorpt_coefficient_mu 0.732 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 5.91 _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4853 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 30.00 _reflns_number_total 3844 _reflns_number_gt 2016 _reflns_threshold_expression >2sigma(I) _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^)+(0.0700P)^2^+0.0500P] 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 3844 _refine_ls_number_parameters 196 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1266 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1540 _refine_ls_wR_factor_gt 0.1248 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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 Co Co 0.5000 0.5000 0.5000 0.03881(19) Uani 1 2 d S . . N1 N 0.0826(2) 0.5954(4) 0.3632(2) 0.0497(7) Uani 1 1 d . . . C1 C -0.0273(3) 0.6165(6) 0.2878(4) 0.0749(13) Uani 1 1 d . . . H11 H -0.0255 0.6577 0.2187 0.090 Uiso 1 1 d R . . H12 H -0.0646 0.6927 0.3187 0.090 Uiso 1 1 d R . . H13 H -0.0635 0.5129 0.2766 0.090 Uiso 1 1 d R . . C1A C 0.1631(2) 0.5482(4) 0.3232(3) 0.0415(7) Uani 1 1 d . . . C2 C 0.1022(3) 0.6263(5) 0.4739(3) 0.0518(9) Uani 1 1 d . . . O2 O 0.0351(2) 0.6752(4) 0.5109(2) 0.0684(8) Uani 1 1 d . . . N3 N 0.2072(2) 0.5977(4) 0.5420(2) 0.0504(7) Uani 1 1 d . . . H3 H 0.2197 0.6079 0.6114 0.060 Uiso 1 1 d R . . C4 C 0.2916(2) 0.5569(4) 0.5100(3) 0.0427(7) Uani 1 1 d . . . O4 O 0.38286(16) 0.5391(3) 0.57649(18) 0.0546(7) Uani 1 1 d . . . C4A C 0.2676(2) 0.5351(3) 0.3942(3) 0.0380(7) Uani 1 1 d . . . N5 N 0.35001(18) 0.5036(3) 0.35665(19) 0.0395(5) Uani 1 1 d . . . C6 C 0.3275(2) 0.4799(4) 0.2503(2) 0.0430(7) Uani 1 1 d . . . C61 C 0.4154(3) 0.4500(6) 0.2058(3) 0.0700(13) Uani 1 1 d . . . H61 H 0.4829 0.4583 0.2639 0.084 Uiso 1 1 d R . . H62 H 0.4124 0.5299 0.1503 0.084 Uiso 1 1 d R . . H63 H 0.4082 0.3423 0.1743 0.084 Uiso 1 1 d R . . C7 C 0.2181(3) 0.4819(4) 0.1798(3) 0.0459(8) Uani 1 1 d . . . C71 C 0.1883(3) 0.4381(5) 0.0607(3) 0.0649(11) Uani 1 1 d . . . H71 H 0.1122 0.4476 0.0259 0.078 Uiso 1 1 d R . . H72 H 0.2100 0.3275 0.0541 0.078 Uiso 1 1 d R . . H73 H 0.2240 0.5109 0.0257 0.078 Uiso 1 1 d R . . N8 N 0.1380(2) 0.5175(4) 0.2160(2) 0.0470(7) Uani 1 1 d . . . O1W O 0.4852(2) 0.2546(3) 0.5092(2) 0.0611(7) Uani 1 1 d D . . H11W H 0.542(2) 0.199(4) 0.539(3) 0.073 Uiso 1 1 d D . . H12W H 0.430(2) 0.210(5) 0.463(3) 0.073 Uiso 1 1 d D . . N1N N 0.6950(2) 0.0089(4) 0.6779(2) 0.0526(7) Uani 1 1 d . . . O1N O 0.6361(2) 0.0190(4) 0.5813(2) 0.0891(11) Uani 1 1 d . . . O2N O 0.7147(3) -0.1238(4) 0.7226(3) 0.1006(12) Uani 1 1 d . . . O3N O 0.7348(2) 0.1348(3) 0.7288(2) 0.0680(8) 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 Co 0.0335(3) 0.0450(3) 0.0386(3) 0.0032(3) 0.0128(2) 0.0020(3) N1 0.0337(13) 0.0582(19) 0.0556(17) 0.0015(15) 0.0127(12) 0.0063(13) C1 0.0376(18) 0.100(4) 0.078(3) -0.003(3) 0.0065(18) 0.016(2) C1A 0.0383(15) 0.0383(17) 0.0471(17) 0.0054(13) 0.0129(13) 0.0000(12) C2 0.0441(18) 0.053(2) 0.058(2) -0.0010(18) 0.0163(16) 0.0042(16) O2 0.0478(13) 0.086(2) 0.0766(19) -0.0091(16) 0.0273(14) 0.0149(14) N3 0.0429(14) 0.069(2) 0.0415(14) 0.0001(14) 0.0175(12) 0.0067(14) C4 0.0390(15) 0.0480(18) 0.0424(16) 0.0026(14) 0.0152(13) 0.0007(14) O4 0.0369(11) 0.086(2) 0.0403(11) 0.0000(12) 0.0127(9) 0.0085(11) C4A 0.0368(14) 0.0349(18) 0.0423(15) 0.0038(12) 0.0130(12) -0.0004(11) N5 0.0376(11) 0.0413(13) 0.0404(12) 0.0012(14) 0.0141(10) 0.0015(13) C6 0.0475(16) 0.0435(19) 0.0382(15) 0.0013(15) 0.0144(13) 0.0023(15) C61 0.057(2) 0.113(4) 0.0428(18) -0.003(2) 0.0199(16) 0.013(2) C7 0.0499(16) 0.045(2) 0.0405(15) 0.0022(16) 0.0117(13) -0.0046(16) C71 0.065(2) 0.080(3) 0.046(2) -0.0115(19) 0.0134(17) -0.012(2) N8 0.0445(13) 0.0484(17) 0.0437(14) 0.0031(14) 0.0084(11) -0.0027(13) O1W 0.0586(17) 0.0473(15) 0.0661(18) 0.0074(14) 0.0055(13) -0.0012(12) N1N 0.0403(14) 0.0566(19) 0.0568(16) -0.0054(18) 0.0105(12) 0.0043(16) O1N 0.0774(19) 0.112(3) 0.0566(16) -0.0201(18) -0.0059(14) 0.0281(19) O2N 0.095(2) 0.0460(18) 0.146(3) 0.020(2) 0.020(2) -0.0046(17) O3N 0.094(2) 0.0476(16) 0.0537(15) -0.0010(13) 0.0132(14) -0.0185(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 Co O1W 2.021(3) . ? Co O4 2.119(2) . ? Co N5 2.221(2) . ? N1 C1A 1.384(4) . ? N1 C2 1.389(4) . ? N1 C1 1.468(4) . ? C1A N8 1.336(4) . ? C1A C4A 1.388(4) . ? C2 O2 1.206(4) . ? C2 N3 1.397(4) . ? N3 C4 1.354(4) . ? C4 O4 1.237(4) . ? C4 C4A 1.433(4) . ? C4A N5 1.356(4) . ? N5 C6 1.318(4) . ? C6 C7 1.433(4) . ? C6 C61 1.480(5) . ? C7 N8 1.323(4) . ? C7 C71 1.499(5) . ? N1N O2N 1.215(4) . ? N1N O1N 1.235(4) . ? N1N O3N 1.239(4) . ? 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 O1W Co O4 91.26(11) . . ? O1W Co N5 89.13(10) . . ? O4 Co N5 78.25(8) . . ? C1A N1 C2 122.0(3) . . ? C1A N1 C1 120.1(3) . . ? C2 N1 C1 117.9(3) . . ? N8 C1A N1 118.8(3) . . ? N8 C1A C4A 121.4(3) . . ? N1 C1A C4A 119.8(3) . . ? O2 C2 N1 123.8(3) . . ? O2 C2 N3 121.1(3) . . ? N1 C2 N3 115.2(3) . . ? C4 N3 C2 126.8(3) . . ? O4 C4 N3 122.1(3) . . ? O4 C4 C4A 122.5(3) . . ? N3 C4 C4A 115.4(3) . . ? C4 O4 Co 113.0(2) . . ? N5 C4A C1A 121.5(3) . . ? N5 C4A C4 118.0(3) . . ? C1A C4A C4 120.5(3) . . ? C6 N5 C4A 117.9(2) . . ? C6 N5 Co 134.2(2) . . ? C4A N5 Co 107.90(18) . . ? N5 C6 C7 119.6(3) . . ? N5 C6 C61 119.5(3) . . ? C7 C6 C61 120.9(3) . . ? N8 C7 C6 122.4(3) . . ? N8 C7 C71 116.4(3) . . ? C6 C7 C71 121.1(3) . . ? C7 N8 C1A 117.0(3) . . ? O2N N1N O1N 120.2(4) . . ? O2N N1N O3N 120.1(3) . . ? O1N N1N O3N 119.7(4) . . ? 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 O1W H11W O1N 0.857(10) 1.885(18) 2.707(4) 160(4) . O1W H12W O1N 0.855(10) 2.07(3) 2.774(4) 140(4) 3_656 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.359 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.063