#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2216683.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2216683 loop_ _publ_author_name 'Visser, Hendrik G.' 'Purcell, Walter' 'Muller, Alfred' 'Janse van Rensburg, J. Marthinus' 'Molosia, Phillip' _publ_section_title ;\ Racemic dipotassium di-\m~2~-hydroxido-bis{[N,N-bis(carboxylatomethyl)leucinato-\ \k^4^N,O,O',O'']cobaltate(III)} tetrahydrate ; _journal_coeditor_code NG2364 _journal_issue 12 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m2998 _journal_page_last m2999 _journal_volume 63 _journal_year 2007 _chemical_formula_iupac 'K2 [Co2 (C10 H13 N O6)2 (O H)2]' _chemical_formula_moiety '2(K +), C20 H28 N2 O14 Co 2-, 4(H2 O)' _chemical_formula_sum 'C20 H36 Co2 K2 N2 O18' _chemical_formula_weight 788.56 _chemical_name_systematic ; dipotassium di-\m~2~-hydroxido-bis{[N,N- bis(carboxylatomethyl)leucinato- \k^4^N,O,O',O'']cobaltate(III)} tetrahydrate ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-C 2bc 2' _symmetry_space_group_name_H-M 'C m c a' _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.968(5) _cell_length_b 25.868(5) _cell_length_c 9.240(5) _cell_measurement_reflns_used 1747 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.13 _cell_measurement_theta_min 2.71 _cell_volume 3100(2) _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 512 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type ; Bruker Kappa APEXII ; _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 8534 _diffrn_reflns_theta_full 28.4 _diffrn_reflns_theta_max 28.4 _diffrn_reflns_theta_min 2.82 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.419 _exptl_absorpt_correction_T_max 0.9694 _exptl_absorpt_correction_T_min 0.7216 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2004) ; _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.69 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1624 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.626 _refine_diff_density_min -0.658 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.238 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 134 _refine_ls_number_reflns 2015 _refine_ls_number_restraints 33 _refine_ls_restrained_S_all 1.233 _refine_ls_R_factor_gt 0.0542 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+25.1765P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.1334 _reflns_number_gt 1700 _reflns_number_total 2015 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ng2364.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x, -y, -z' '-x+1/2, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x, y, z' 'x-1/2, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' '-x+1/2, y+1/2, z' 'x, -y+1/2, z-1/2' 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' K K 0.2009 0.2494 '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_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy Co Co 0 0.03898(3) 0.61246(8) 0.00824(19) Uani d S 1 C C1 0 0.0787(2) 0.8831(6) 0.0122(10) Uani d S 1 C C2 0 0.1258(2) 0.7900(6) 0.0165(11) Uani d S 1 H H2A -0.0604 0.1464 0.8123 0.02 Uiso calc PR 0.5 H H2B 0.0604 0.1464 0.8123 0.02 Uiso calc PR 0.5 C C3 -0.1807(3) 0.09039(14) 0.5868(4) 0.0129(8) Uani d . 1 C C4 -0.0971(3) 0.13099(14) 0.5611(5) 0.0174(8) Uani d U 1 H H4 -0.0817 0.1271 0.4579 0.021 Uiso calc R 1 C C5 -0.1206(6) 0.1870(3) 0.5748(10) 0.0187(14) Uani d PU 0.5 H H5A -0.0584 0.2047 0.6058 0.022 Uiso calc PR 0.5 H H5B -0.1717 0.1914 0.6505 0.022 Uiso calc PR 0.5 C C6 -0.1607(8) 0.2135(4) 0.4365(12) 0.0320(18) Uani d PU 0.5 H H6 -0.2166 0.1927 0.395 0.038 Uiso calc PR 0.5 C C7 -0.0754(10) 0.2203(4) 0.3234(14) 0.047(3) Uani d PU 0.5 H H7A -0.0226 0.2425 0.3615 0.07 Uiso calc PR 0.5 H H7B -0.1039 0.2355 0.2375 0.07 Uiso calc PR 0.5 H H7C -0.0461 0.1872 0.3004 0.07 Uiso calc PR 0.5 C C8 -0.2027(10) 0.2676(4) 0.4777(17) 0.054(3) Uani d PU 0.5 H H8A -0.2632 0.2638 0.5365 0.081 Uiso calc PR 0.5 H H8B -0.2198 0.2863 0.3913 0.081 Uiso calc PR 0.5 H H8C -0.151 0.2862 0.5307 0.081 Uiso calc PR 0.5 N N 0 0.11323(16) 0.6325(5) 0.0097(9) Uani d S 1 O O1 0 0.03494(14) 0.8175(4) 0.0113(8) Uani d S 1 O O2 -0.1472(2) 0.04429(10) 0.6132(3) 0.0124(5) Uani d . 1 O O3 0 0.08247(15) 1.0160(4) 0.0156(8) Uani d S 1 O O4 -0.2731(2) 0.10165(11) 0.5758(3) 0.0187(6) Uani d . 1 O O5 0 0.03447(14) 0.4072(4) 0.0129(8) Uani d SD 1 O O6 -0.3530(2) -0.08192(14) 0.7397(4) 0.0329(8) Uani d . 1 K K -0.33220(9) 0 0.5 0.0170(3) Uani d S 1 H H5 -0.057(4) 0.043(4) 0.373(10) 0.02 Uiso d PD 0.5 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co 0.0076(4) 0.0083(3) 0.0088(4) 0 0 0.0003(3) C1 0.005(2) 0.017(2) 0.015(3) 0 0 -0.002(2) C2 0.023(3) 0.013(3) 0.013(3) 0 0 -0.002(2) C3 0.0126(19) 0.0149(17) 0.0113(18) -0.0007(14) -0.0036(15) -0.0022(13) C4 0.014(2) 0.0114(16) 0.027(2) 0.0023(13) -0.0090(17) 0.0012(15) C5 0.011(3) 0.014(2) 0.031(3) 0.005(2) -0.006(3) -0.004(3) C6 0.025(4) 0.024(3) 0.048(4) 0.010(3) -0.008(3) 0.013(3) C7 0.055(7) 0.031(5) 0.054(6) 0.006(5) 0.008(5) 0.025(5) C8 0.053(7) 0.025(4) 0.083(9) 0.021(4) 0.001(6) 0.019(5) N 0.007(2) 0.0090(19) 0.013(2) 0 0 0.0007(16) O1 0.0124(19) 0.0118(17) 0.0096(19) 0 0 0.0002(14) O2 0.0092(13) 0.0119(12) 0.0160(14) -0.0005(9) -0.0022(11) -0.0003(11) O3 0.013(2) 0.023(2) 0.0110(19) 0 0 -0.0016(16) O4 0.0105(14) 0.0187(14) 0.0268(17) 0.0053(10) -0.0044(13) -0.0020(12) O5 0.015(2) 0.0105(17) 0.013(2) 0 0 0.0004(14) O6 0.0193(17) 0.055(2) 0.0243(18) 0.0144(15) -0.0040(14) -0.0127(16) K 0.0101(6) 0.0144(5) 0.0265(7) 0 0 -0.0036(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co O1 . 1.897(4) y Co O5 . 1.900(4) y Co O5 9_556 1.909(4) y Co O2 . 1.913(3) y Co O2 11 1.913(3) y Co N . 1.930(4) y Co Co 9_556 2.8959(16) y C1 O3 . 1.232(7) ? C1 O1 . 1.283(6) ? C1 C2 . 1.491(8) ? C2 N . 1.491(7) ? C2 H2A . 0.97 ? C2 H2B . 0.97 ? C3 O4 . 1.237(5) ? C3 O2 . 1.293(4) ? C3 C4 . 1.528(5) ? C4 C5 . 1.485(8) ? C4 N . 1.494(4) ? C4 H4 . 0.98 ? C5 C6 . 1.540(13) ? C5 H5A . 0.97 ? C5 H5B . 0.97 ? C6 C7 . 1.532(16) ? C6 C8 . 1.550(14) ? C6 H6 . 0.98 ? C7 H7A . 0.96 ? C7 H7B . 0.96 ? C7 H7C . 0.96 ? C8 H8A . 0.96 ? C8 H8B . 0.96 ? C8 H8C . 0.96 ? N C4 11 1.494(4) ? O5 Co 9_556 1.909(4) ? O5 H5 . 0.83(2) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Co O5 . . 173.32(16) y O1 Co O5 . 9_556 92.31(17) y O5 Co O5 . 9_556 81.01(18) y O1 Co O2 . . 90.02(9) y O5 Co O2 . . 90.46(9) y O5 Co O2 9_556 . 94.12(8) y O1 Co O2 . 11 90.02(9) y O5 Co O2 . 11 90.46(9) y O5 Co O2 9_556 11 94.12(8) y O2 Co O2 . 11 171.76(16) y O1 Co N . . 87.65(18) y O5 Co N . . 99.03(18) y O5 Co N 9_556 . 179.96(19) y O2 Co N . . 85.88(8) y O2 Co N 11 . 85.88(8) y O1 Co Co . 9_556 132.70(12) ? O5 Co Co . 9_556 40.62(11) ? O5 Co Co 9_556 9_556 40.39(12) ? O2 Co Co . 9_556 93.01(8) ? O2 Co Co 11 9_556 93.01(8) ? N Co Co . 9_556 139.65(14) ? O3 C1 O1 . . 122.8(5) ? O3 C1 C2 . . 120.6(5) ? O1 C1 C2 . . 116.6(5) ? N C2 C1 . . 112.7(4) ? N C2 H2A . . 109.1 ? C1 C2 H2A . . 109.1 ? N C2 H2B . . 109.1 ? C1 C2 H2B . . 109.1 ? H2A C2 H2B . . 107.8 ? O4 C3 O2 . . 124.0(4) ? O4 C3 C4 . . 120.8(3) ? O2 C3 C4 . . 115.1(3) ? C5 C4 N . . 115.8(5) ? C5 C4 C3 . . 120.8(5) ? N C4 C3 . . 108.6(3) ? C5 C4 H4 . . 103 ? N C4 H4 . . 103 ? C3 C4 H4 . . 103 ? C4 C5 C6 . . 115.6(7) ? C4 C5 H5A . . 108.4 ? C6 C5 H5A . . 108.4 ? C4 C5 H5B . . 108.4 ? C6 C5 H5B . . 108.4 ? H5A C5 H5B . . 107.4 ? C7 C6 C5 . . 111.9(8) ? C7 C6 C8 . . 108.5(9) ? C5 C6 C8 . . 108.5(9) ? C7 C6 H6 . . 109.3 ? C5 C6 H6 . . 109.3 ? C8 C6 H6 . . 109.3 ? C6 C7 H7A . . 109.5 ? C6 C7 H7B . . 109.5 ? H7A C7 H7B . . 109.5 ? C6 C7 H7C . . 109.5 ? H7A C7 H7C . . 109.5 ? H7B C7 H7C . . 109.5 ? C6 C8 H8A . . 109.5 ? C6 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? C6 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? C2 N C4 . . 111.3(3) ? C2 N C4 . 11 111.3(3) ? C4 N C4 . 11 114.9(5) ? C2 N Co . . 108.1(3) ? C4 N Co . . 105.3(2) ? C4 N Co 11 . 105.3(2) ? C1 O1 Co . . 115.0(3) ? C3 O2 Co . . 113.7(2) ? Co O5 Co . 9_556 98.99(18) ? Co O5 H5 . . 111(7) ? Co O5 H5 9_556 . 103(7) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion O3 C1 C2 N . . 180.000(2) O1 C1 C2 N . . 0.000(2) O4 C3 C4 C5 . . 22.2(7) O2 C3 C4 C5 . . -160.9(5) O4 C3 C4 N . . 159.4(4) O2 C3 C4 N . . -23.7(5) N C4 C5 C6 . . 137.6(7) C3 C4 C5 C6 . . -88.1(8) C4 C5 C6 C7 . . -72.3(10) C4 C5 C6 C8 . . 168.1(8) C1 C2 N C4 . . 115.2(3) C1 C2 N C4 . 11 -115.2(3) C1 C2 N Co . . 0.0000(10) C5 C4 N C2 . . 57.3(6) C3 C4 N C2 . . -82.3(4) C5 C4 N C4 . 11 -70.5(7) C3 C4 N C4 . 11 149.9(3) C5 C4 N Co . . 174.2(5) C3 C4 N Co . . 34.5(4) O1 Co N C2 . . 0 O5 Co N C2 . . 180 O2 Co N C2 . . 90.19(9) O2 Co N C2 11 . -90.19(9) Co Co N C2 9_556 . 180.0000(10) O1 Co N C4 . . -119.1(3) O5 Co N C4 . . 60.9(3) O2 Co N C4 . . -28.9(3) O2 Co N C4 11 . 150.7(3) Co Co N C4 9_556 . 60.9(3) O1 Co N C4 . 11 119.1(3) O5 Co N C4 . 11 -60.9(3) O2 Co N C4 . 11 -150.7(3) O2 Co N C4 11 11 28.9(3) Co Co N C4 9_556 11 -60.9(3) O3 C1 O1 Co . . 180.0000(10) C2 C1 O1 Co . . 0.0000(10) O2 Co O1 C1 . . -85.88(8) O2 Co O1 C1 11 . 85.88(8) N Co O1 C1 . . 0.0000(10) Co Co O1 C1 9_556 . 180.0000(10) O4 C3 O2 Co . . 176.6(3) C4 C3 O2 Co . . -0.2(4) O1 Co O2 C3 . . 105.1(3) O5 Co O2 C3 . . -81.5(3) O5 Co O2 C3 9_556 . -162.5(3) N Co O2 C3 . . 17.5(3) Co Co O2 C3 9_556 . -122.1(3) O5 Co O5 Co 9_556 9_556 0 O2 Co O5 Co . 9_556 -94.10(8) O2 Co O5 Co 11 9_556 94.10(8) N Co O5 Co . 9_556 180 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O5 H5 O6 6_444 0.83(2) 1.98(5) 2.745(4) 153(9) no C4 H4 O6 6_444 0.98 2.48 3.294(6) 140.4 no _cod_database_code 2216683