Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Galindo, Agustin' 'Grirrane, Abdessamad' 'Ienco, Andrea' 'Mealli, Carlo' 'Pastor, Antonio' _publ_contact_author_name 'Prof Agustin Galindo' _publ_contact_author_address ; Quimica Inorganica Universidad de Sevilla Aptdo 553 Sevilla 41071 SPAIN ; _publ_contact_author_email 'GALINDO@US.ES' _publ_section_title ; Synthesis and molecular structure of oxydiacetate complexes of nickel(II) and cobalt(II). Theoretical analysis of the planar and non planar conformations of oxydiacetate ligand and oxydiacetic acid ; data_nickel _database_code_CSD 180037 _audit_creation_date 2002-02-12T16:29:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Ni(oda)(bipy)(H2O).1.5H2O' _chemical_formula_sum 'C14 H19 N2 Ni O8.50' _chemical_formula_weight 410.02 _chemical_formula_moiety 'C28 H38 N4 Ni2 O17' _chemical_formula_structural 'C28 H38 N6 O17 NI2' _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d 2' _symmetry_space_group_name_Hall 'F 2 -2d' _symmetry_Int_Tables_number 43 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' _cell_length_a 13.560(5) _cell_length_b 47.533(5) _cell_length_c 10.781(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 6949(4) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 20 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3408 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.165 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Nonius Cad4' _diffrn_measurement_method omega-2theta _diffrn_standards_interval_time 2h _diffrn_standards_decay_% 3 _diffrn_reflns_number 3100 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_unetI/netI 0.0226 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 56 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 2862 _reflns_number_gt 2684 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Nonious CAD4 programs' _computing_cell_refinement 'Nonious CAD4 programs' _computing_data_reduction 'local routines' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'shelxl-97 (sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0446P)^2^+8.4850P] 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_number_reflns 2862 _refine_ls_number_parameters 233 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0802 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.002 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(15) _refine_diff_density_max 0.199 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.059 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ni1 Ni -0.03854(3) 0.192796(8) 0.06472(4) 0.03187(12) Uani 1 1 d . . . N1 N -0.1560(2) 0.16647(5) 0.0912(2) 0.0343(6) Uani 1 1 d . . . N2 N 0.0259(2) 0.15426(6) 0.0284(3) 0.0378(7) Uani 1 1 d . . . O1 O -0.0440(2) 0.20420(5) -0.1190(2) 0.0458(6) Uani 1 1 d . . . O2 O 0.01585(18) 0.19296(5) 0.2425(2) 0.0402(6) Uani 1 1 d . . . O3 O 0.08963(19) 0.21485(5) 0.0440(3) 0.0470(6) Uani 1 1 d . . . O4 O 0.0250(2) 0.23097(6) -0.2621(3) 0.0598(8) Uani 1 1 d . . . O5 O 0.1309(2) 0.21040(6) 0.3655(3) 0.0584(7) Uani 1 1 d . . . O6 O -0.1195(2) 0.22733(5) 0.1181(3) 0.0501(7) Uani 1 1 d D . . O7 O -0.25 0.25 -0.0401(3) 0.0445(8) Uani 1 2 d SD . . O8 O -0.1865(3) 0.19226(11) 0.4076(4) 0.1094(17) Uani 1 1 d . . . O9 O -0.0152(2) 0.19408(7) 0.5476(4) 0.0718(10) Uani 1 1 d . . . C1 C 0.0193(3) 0.22148(7) -0.1553(3) 0.0427(8) Uani 1 1 d . . . C2 C 0.0962(3) 0.23182(8) -0.0632(4) 0.0483(9) Uani 1 1 d . . . H21 H 0.1616 0.2304 -0.099 0.064(7) Uiso 1 1 calc R . . H22 H 0.0838 0.2513 -0.0421 0.064(7) Uiso 1 1 calc R . . C3 C 0.1379(3) 0.22314(8) 0.1544(4) 0.0447(9) Uani 1 1 d . . . H31 H 0.1317 0.2433 0.1658 0.064(7) Uiso 1 1 calc R . . H32 H 0.2075 0.2185 0.1495 0.064(7) Uiso 1 1 calc R . . C4 C 0.0909(3) 0.20777(7) 0.2623(3) 0.0402(8) Uani 1 1 d . . . C5 C 0.1178(3) 0.14988(9) -0.0101(4) 0.0511(9) Uani 1 1 d . . . H51 H 0.1575 0.1653 -0.0285 0.062(4) Uiso 1 1 calc R . . C6 C 0.1560(3) 0.12304(10) -0.0236(5) 0.0628(12) Uani 1 1 d . . . H61 H 0.2201 0.1204 -0.052 0.062(4) Uiso 1 1 calc R . . C7 C 0.0988(4) 0.10063(10) 0.0050(5) 0.0637(12) Uani 1 1 d . . . H71 H 0.1237 0.0825 -0.0019 0.062(4) Uiso 1 1 calc R . . C8 C 0.0035(3) 0.10490(7) 0.0444(4) 0.0510(9) Uani 1 1 d . . . H81 H -0.0368 0.0897 0.0639 0.062(4) Uiso 1 1 calc R . . C9 C -0.0315(3) 0.13214(6) 0.0544(4) 0.0363(7) Uani 1 1 d . . . C10 C -0.1337(3) 0.13898(6) 0.0893(3) 0.0350(7) Uani 1 1 d . . . C11 C -0.2046(3) 0.11878(8) 0.1179(4) 0.0469(9) Uani 1 1 d . . . H111 H -0.1881 0.0998 0.1175 0.062(4) Uiso 1 1 calc R . . C12 C -0.2985(3) 0.12697(9) 0.1465(4) 0.0567(11) Uani 1 1 d . . . H121 H -0.3462 0.1137 0.1666 0.062(4) Uiso 1 1 calc R . . C13 C -0.3214(3) 0.15494(10) 0.1453(5) 0.0604(12) Uani 1 1 d . . . H131 H -0.3852 0.161 0.1622 0.062(4) Uiso 1 1 calc R . . C14 C -0.2483(3) 0.17403(8) 0.1185(4) 0.0454(8) Uani 1 1 d . . . H141 H -0.2639 0.1931 0.1194 0.062(4) Uiso 1 1 calc R . . H7A H -0.2147 0.2631 -0.0836 0.062 Uiso 1 1 d D . . H6A H -0.1597 0.236 0.0669 0.062 Uiso 1 1 d D . . H6B H -0.0908 0.2402 0.1629 0.062 Uiso 1 1 d D . . H9A H -0.0135 0.2092 0.6028 0.062 Uiso 1 1 d . . . H9B H 0.0269 0.1969 0.4843 0.062 Uiso 1 1 d . . . H8A H -0.1375 0.1906 0.466 0.062 Uiso 1 1 d . . . H8B H -0.1495 0.1918 0.3431 0.062 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 Ni1 0.03414(19) 0.02745(19) 0.0340(2) 0.00258(16) -0.00151(19) -0.00683(17) N1 0.0327(14) 0.0336(13) 0.0367(16) 0.0019(11) -0.0042(11) -0.0050(10) N2 0.0392(15) 0.0371(14) 0.0370(17) -0.0009(11) 0.0022(12) 0.0003(12) O1 0.0583(16) 0.0426(14) 0.0366(14) 0.0059(11) -0.0036(12) -0.0145(12) O2 0.0425(13) 0.0383(14) 0.0399(14) 0.0040(10) -0.0038(11) -0.0068(10) O3 0.0515(15) 0.0490(14) 0.0404(14) 0.0090(11) -0.0060(12) -0.0226(11) O4 0.089(2) 0.0506(17) 0.0394(16) 0.0114(12) 0.0035(15) -0.0185(14) O5 0.0611(18) 0.0671(18) 0.0471(16) 0.0024(14) -0.0151(14) -0.0135(14) O6 0.0571(16) 0.0311(12) 0.0620(17) -0.0086(11) -0.0216(13) 0.0032(11) O7 0.0375(18) 0.054(2) 0.042(2) 0 0 -0.0015(15) O8 0.055(2) 0.178(5) 0.095(3) -0.022(3) 0.010(2) -0.022(2) O9 0.074(2) 0.073(2) 0.068(3) -0.0131(17) 0.006(2) -0.0090(16) C1 0.059(2) 0.0307(17) 0.038(2) 0.0024(14) 0.0060(16) -0.0055(15) C2 0.054(2) 0.043(2) 0.047(2) 0.0094(17) 0.0055(19) -0.0163(17) C3 0.0384(19) 0.047(2) 0.049(2) -0.0053(16) -0.0055(17) -0.0109(15) C4 0.040(2) 0.0367(19) 0.044(2) -0.0035(15) -0.0084(16) -0.0003(15) C5 0.042(2) 0.056(2) 0.055(2) -0.0010(18) 0.0051(19) 0.0073(17) C6 0.057(3) 0.072(3) 0.060(3) -0.004(2) 0.005(2) 0.023(2) C7 0.077(3) 0.051(3) 0.063(3) -0.006(2) -0.004(2) 0.028(2) C8 0.071(2) 0.0314(17) 0.051(2) -0.0004(15) -0.005(2) 0.0053(16) C9 0.0479(18) 0.0299(15) 0.0312(16) -0.0014(15) -0.0047(15) -0.0009(13) C10 0.0454(19) 0.0313(15) 0.0284(18) 0.0000(12) -0.0039(13) -0.0100(13) C11 0.058(2) 0.0369(18) 0.046(2) 0.0014(16) -0.0021(18) -0.0152(16) C12 0.052(2) 0.057(3) 0.061(3) 0.011(2) -0.002(2) -0.0253(19) C13 0.0341(19) 0.074(3) 0.073(3) 0.007(2) 0.000(2) -0.0109(19) C14 0.0350(18) 0.0454(19) 0.056(2) 0.0035(17) -0.0027(17) 0.0000(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Ni1 O3 2.042(2) . ? Ni1 N1 2.046(3) . ? Ni1 O2 2.054(3) . ? Ni1 O1 2.055(3) . ? Ni1 N2 2.067(3) . ? Ni1 O6 2.057(3) . ? N1 C14 1.335(5) . ? N1 C10 1.342(4) . ? N2 C5 1.329(5) . ? N2 C9 1.338(4) . ? O1 C1 1.251(4) . ? O2 C4 1.256(4) . ? O3 C3 1.415(5) . ? O3 C2 1.412(4) . ? O4 C1 1.239(4) . ? O5 C4 1.245(4) . ? C1 C2 1.521(5) . ? C3 C4 1.514(5) . ? C5 C6 1.385(6) . ? C6 C7 1.353(7) . ? C7 C8 1.374(6) . ? C8 C9 1.384(5) . ? C9 C10 1.472(5) . ? C10 C11 1.394(5) . ? C11 C12 1.367(6) . ? C12 C13 1.365(7) . ? C13 C14 1.374(6) . ? 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 Ni1 N1 172.79(11) . . ? O3 Ni1 O2 78.14(10) . . ? N1 Ni1 O2 98.73(10) . . ? O3 Ni1 O1 77.85(11) . . ? N1 Ni1 O1 105.55(10) . . ? O2 Ni1 O1 155.70(9) . . ? O3 Ni1 N2 94.26(11) . . ? N1 Ni1 N2 79.26(11) . . ? O2 Ni1 N2 91.63(10) . . ? O1 Ni1 N2 93.80(11) . . ? O3 Ni1 O6 94.32(11) . . ? N1 Ni1 O6 91.92(11) . . ? O2 Ni1 O6 85.86(11) . . ? O1 Ni1 O6 92.29(11) . . ? N2 Ni1 O6 170.37(12) . . ? C14 N1 C10 118.5(3) . . ? C14 N1 Ni1 126.6(2) . . ? C10 N1 Ni1 114.7(2) . . ? C5 N2 C9 119.2(3) . . ? C5 N2 Ni1 126.4(3) . . ? C9 N2 Ni1 114.2(2) . . ? C1 O1 Ni1 116.7(2) . . ? C4 O2 Ni1 116.9(2) . . ? C3 O3 C2 120.0(3) . . ? C3 O3 Ni1 116.4(2) . . ? C2 O3 Ni1 115.9(2) . . ? O4 C1 O1 124.9(4) . . ? O4 C1 C2 116.5(3) . . ? O1 C1 C2 118.6(3) . . ? O3 C2 C1 107.9(3) . . ? O3 C3 C4 108.5(3) . . ? O5 C4 O2 124.2(3) . . ? O5 C4 C3 117.1(3) . . ? O2 C4 C3 118.8(3) . . ? N2 C5 C6 121.8(4) . . ? C7 C6 C5 119.1(4) . . ? C6 C7 C8 119.5(4) . . ? C7 C8 C9 119.0(4) . . ? N2 C9 C8 121.3(3) . . ? N2 C9 C10 115.3(3) . . ? C8 C9 C10 123.3(3) . . ? N1 C10 C11 120.8(3) . . ? N1 C10 C9 115.6(3) . . ? C11 C10 C9 123.7(3) . . ? C12 C11 C10 119.8(4) . . ? C13 C12 C11 119.1(4) . . ? C12 C13 C14 118.8(4) . . ? N1 C14 C13 123.0(4) . . ? data_cobalt _database_code_CSD 180038 _audit_creation_date 2002-02-20T10:56:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Co(oda)(bipy)(H2O).1.5H2O' _chemical_formula_moiety 'C14 H19 Co1 N2 O8' _chemical_formula_structural 'C14 H19 N2 O8.5 CO1' _chemical_formula_sum 'C14 H19 Co N2 O8.50' _chemical_formula_weight 410.24 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d 2' _symmetry_space_group_name_Hall 'F 2 -2d' _symmetry_Int_Tables_number 43 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+3/4, -y+5/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+5/4, -y+3/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+5/4, -y+5/4, z+1/4' _cell_length_a 13.646(6) _cell_length_b 47.908(9) _cell_length_c 10.752(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7029(4) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 20 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour marron _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3392 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.024 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type mok\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Nonius Cad4' _diffrn_measurement_method omega-2theta _diffrn_standards_interval_time 2h _diffrn_standards_decay_% 2 _diffrn_reflns_number 1627 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.0137 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 56 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 24.91 _diffrn_reflns_theta_full 24.91 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 1627 _reflns_number_gt 1571 _reflns_threshold_expression >2sigma(i) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Nonius Cad4' _computing_cell_refinement 'Nonious CAD4 programs' _computing_data_reduction 'local routines' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0591P)^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_number_reflns 1627 _refine_ls_number_parameters 262 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0732 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 1.15 _refine_ls_restrained_S_all 1.15 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0 _refine_diff_density_max 0.263 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.102 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.20609(3) 0.056817(8) 0.29101(4) 0.03477(15) Uani 1 1 d . . . O1 O 0.21148(19) 0.04618(6) 0.1065(3) 0.0504(6) Uani 1 1 d . . . O2 O 0.2705(2) 0.05670(5) 0.4680(3) 0.0446(6) Uani 1 1 d . . . O3 O 0.3349(2) 0.03258(7) 0.2735(3) 0.0645(8) Uani 1 1 d . . . O4 O 0.2787(2) 0.01939(6) -0.0382(3) 0.0617(8) Uani 1 1 d . . . O5 O 0.3825(2) 0.03872(7) 0.5923(3) 0.0663(8) Uani 1 1 d . . . O6 O 0.1239(2) 0.02263(5) 0.3529(3) 0.0543(7) Uani 1 1 d . . . O7 O -0.25 0.25 0.9396(4) 0.0484(8) Uani 1 2 d S . . O8 O -0.0171(4) 0.19425(9) 0.5208(5) 0.0791(12) Uani 1 1 d . . . O9 O -0.1890(3) 0.19204(15) 0.3864(6) 0.1128(18) Uani 1 1 d . . . N1 N 0.08815(19) 0.08417(5) 0.3193(3) 0.0374(6) Uani 1 1 d . . . N2 N 0.2692(2) 0.09641(6) 0.2571(3) 0.0418(6) Uani 1 1 d . . . C1 C 0.2726(3) 0.02848(7) 0.0701(3) 0.0444(8) Uani 1 1 d . . . C2 C 0.3470(3) 0.01758(8) 0.1629(4) 0.0493(9) Uani 1 1 d . . . H8 H 0.3366 -0.0022 0.1776 0.073(9) Uiso 1 1 calc R . . H9 H 0.4129 0.0201 0.131 0.071(14) Uiso 1 1 calc R . . C3 C 0.3878(3) 0.02541(8) 0.3801(4) 0.0493(9) Uani 1 1 d . . . H10 H 0.4562 0.0304 0.3701 0.073(9) Uiso 1 1 calc R . . H11 H 0.3838 0.0055 0.3948 0.073(9) Uiso 1 1 calc R . . C4 C 0.3434(3) 0.04123(7) 0.4879(4) 0.0437(8) Uani 1 1 d . . . C5 C -0.0038(2) 0.07639(8) 0.3463(4) 0.0494(8) Uani 1 1 d . . . H12 H -0.0193 0.0575 0.346 0.074(5) Uiso 1 1 calc R . . C6 C -0.0766(3) 0.09548(9) 0.3745(5) 0.0610(11) Uani 1 1 d . . . H13 H -0.1397 0.0896 0.3935 0.074(5) Uiso 1 1 calc R . . C7 C -0.0533(3) 0.12332(9) 0.3738(5) 0.0586(11) Uani 1 1 d . . . H14 H -0.1008 0.1366 0.3928 0.074(5) Uiso 1 1 calc R . . C8 C 0.0397(3) 0.13159(8) 0.3451(4) 0.0502(9) Uani 1 1 d . . . H15 H 0.0558 0.1505 0.3441 0.074(5) Uiso 1 1 calc R . . C9 C 0.1106(2) 0.11148(6) 0.3173(3) 0.0374(7) Uani 1 1 d . . . C10 C 0.2114(2) 0.11835(6) 0.2823(4) 0.0384(7) Uani 1 1 d . . . C11 C 0.2459(3) 0.14571(8) 0.2722(4) 0.0535(9) Uani 1 1 d . . . H16 H 0.2053 0.1607 0.2906 0.074(5) Uiso 1 1 calc R . . C12 C 0.3413(3) 0.15007(9) 0.2344(5) 0.0654(12) Uani 1 1 d . . . H17 H 0.3661 0.1681 0.2279 0.074(5) Uiso 1 1 calc R . . C13 C 0.3987(3) 0.12771(11) 0.2066(5) 0.0653(12) Uani 1 1 d . . . H18 H 0.4625 0.1304 0.1786 0.074(5) Uiso 1 1 calc R . . C14 C 0.3618(3) 0.10105(9) 0.2202(4) 0.0539(9) Uani 1 1 d . . . H19 H 0.4022 0.0859 0.2033 0.074(5) Uiso 1 1 calc R . . H1 H 0.150(3) 0.0110(9) 0.391(4) 0.045(11) Uiso 1 1 d . . . H2 H 0.084(3) 0.0137(9) 0.296(5) 0.057(11) Uiso 1 1 d . . . H3 H -0.280(3) 0.2381(9) 0.895(5) 0.048(12) Uiso 1 1 d . . . H4 H -0.018(5) 0.2016(14) 0.586(7) 0.09(2) Uiso 1 1 d . . . H5 H 0.023(4) 0.1981(12) 0.477(6) 0.063(18) Uiso 1 1 d . . . H6 H -0.202(5) 0.1713(18) 0.393(8) 0.11(3) Uiso 1 1 d . . . H7 H -0.155(8) 0.207(3) 0.420(14) 0.24(6) 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 0.0368(2) 0.0312(2) 0.0364(2) -0.00262(16) -0.00128(19) 0.00831(16) O1 0.0612(16) 0.0479(14) 0.0420(14) -0.0052(12) -0.0039(12) 0.0187(11) O2 0.0500(13) 0.0423(14) 0.0415(13) -0.0043(10) -0.0060(12) 0.0088(10) O3 0.0675(17) 0.0814(19) 0.0446(15) -0.0126(14) -0.0107(15) 0.0431(15) O4 0.091(2) 0.0516(16) 0.0423(15) -0.0118(12) 0.0037(15) 0.0166(13) O5 0.0729(19) 0.0759(19) 0.0501(16) -0.0014(15) -0.0218(15) 0.0164(15) O6 0.0582(14) 0.0358(12) 0.0690(18) 0.0108(13) -0.0210(15) -0.0023(11) O7 0.0396(18) 0.059(2) 0.047(2) 0 0 -0.0033(16) O8 0.078(2) 0.087(3) 0.073(3) -0.015(2) 0.004(2) -0.0113(19) O9 0.070(2) 0.156(5) 0.112(4) -0.027(4) 0.008(3) -0.022(3) N1 0.0342(13) 0.0361(12) 0.0420(16) -0.0004(11) -0.0017(11) 0.0050(10) N2 0.0429(14) 0.0424(14) 0.0400(16) 0.0016(12) 0.0015(12) 0.0025(11) C1 0.0586(19) 0.0355(16) 0.039(2) -0.0048(14) 0.0057(16) 0.0017(14) C2 0.053(2) 0.045(2) 0.049(2) -0.0110(17) 0.0052(18) 0.0157(16) C3 0.0414(18) 0.052(2) 0.055(2) 0.0050(17) -0.0076(17) 0.0112(15) C4 0.0455(19) 0.0415(18) 0.0441(19) 0.0018(15) -0.0100(16) -0.0024(15) C5 0.0340(16) 0.0472(17) 0.067(2) -0.0017(19) -0.0010(17) 0.0003(14) C6 0.0353(17) 0.071(3) 0.076(3) -0.004(2) 0.0018(19) 0.0114(17) C7 0.050(2) 0.062(2) 0.064(3) -0.014(2) -0.0006(19) 0.0278(18) C8 0.064(2) 0.0391(17) 0.048(2) -0.0031(16) -0.0011(17) 0.0181(15) C9 0.0458(16) 0.0333(14) 0.0333(17) -0.0016(12) -0.0052(13) 0.0101(13) C10 0.0509(17) 0.0308(14) 0.0335(16) 0.0007(15) -0.0064(14) -0.0003(12) C11 0.070(2) 0.0379(16) 0.053(2) 0.0020(16) -0.009(2) -0.0068(16) C12 0.077(3) 0.057(2) 0.063(3) 0.005(2) -0.007(2) -0.023(2) C13 0.054(2) 0.076(3) 0.066(3) 0.006(2) 0.004(2) -0.023(2) C14 0.0406(17) 0.063(2) 0.058(2) -0.0006(19) 0.0062(18) -0.0025(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 2.050(3) . ? Co1 O6 2.094(3) . ? Co1 O2 2.096(3) . ? Co1 N1 2.098(3) . ? Co1 O3 2.114(3) . ? Co1 N2 2.115(3) . ? O1 C1 1.251(4) . ? O2 C4 1.258(5) . ? O3 C3 1.398(5) . ? O3 C2 1.400(5) . ? O4 C1 1.246(5) . ? O5 C4 1.249(5) . ? N1 C5 1.341(5) . ? N1 C9 1.344(4) . ? N2 C10 1.342(4) . ? N2 C14 1.343(5) . ? C1 C2 1.516(5) . ? C3 C4 1.512(6) . ? C5 C6 1.384(6) . ? C6 C7 1.371(7) . ? C7 C8 1.364(6) . ? C8 C9 1.398(5) . ? C9 C10 1.463(5) . ? C10 C11 1.398(5) . ? C11 C12 1.380(7) . ? C12 C13 1.360(7) . ? C13 C14 1.381(6) . ? 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 O6 97.60(12) . . ? O1 Co1 O2 149.64(10) . . ? O6 Co1 O2 86.23(12) . . ? O1 Co1 N1 108.85(10) . . ? O6 Co1 N1 91.81(11) . . ? O2 Co1 N1 101.07(10) . . ? O1 Co1 O3 75.38(11) . . ? O6 Co1 O3 92.52(13) . . ? O2 Co1 O3 74.37(10) . . ? N1 Co1 O3 173.48(12) . . ? O1 Co1 N2 92.38(12) . . ? O6 Co1 N2 167.06(12) . . ? O2 Co1 N2 89.32(11) . . ? N1 Co1 N2 77.12(10) . . ? O3 Co1 N2 97.97(13) . . ? C1 O1 Co1 119.6(2) . . ? C4 O2 Co1 119.2(2) . . ? C3 O3 C2 120.6(3) . . ? C3 O3 Co1 119.5(2) . . ? C2 O3 Co1 117.1(2) . . ? C5 N1 C9 119.2(3) . . ? C5 N1 Co1 125.1(2) . . ? C9 N1 Co1 115.5(2) . . ? C10 N2 C14 118.9(3) . . ? C10 N2 Co1 115.3(2) . . ? C14 N2 Co1 125.6(3) . . ? O4 C1 O1 125.0(4) . . ? O4 C1 C2 116.7(3) . . ? O1 C1 C2 118.3(3) . . ? O3 C2 C1 107.6(3) . . ? O3 C3 C4 107.3(3) . . ? O5 C4 O2 123.2(4) . . ? O5 C4 C3 118.0(3) . . ? O2 C4 C3 118.8(3) . . ? N1 C5 C6 122.3(4) . . ? C7 C6 C5 118.4(4) . . ? C8 C7 C6 119.9(3) . . ? C7 C8 C9 119.5(4) . . ? N1 C9 C8 120.7(3) . . ? N1 C9 C10 115.9(3) . . ? C8 C9 C10 123.4(3) . . ? N2 C10 C11 121.3(3) . . ? N2 C10 C9 115.4(3) . . ? C11 C10 C9 123.3(3) . . ? C12 C11 C10 118.9(4) . . ? C13 C12 C11 119.3(4) . . ? C12 C13 C14 119.7(4) . . ? N2 C14 C13 121.8(4) . . ?