#------------------------------------------------------------------------------
#$Date: 2019-06-20 12:58:06 +0300 (Thu, 20 Jun 2019) $
#$Revision: 216218 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/16/1551607.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1551607
loop_
_publ_author_name
'MITSUHASHI, Ryoji'
'MIKURIYA, Masahiro'
_publ_section_title
;
 Synthesis and Crystal Structure of Potassium
 Ethylenediaminetetraacetato-cobaltate(III)
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              5
_journal_paper_doi               10.2116/xraystruct.32.5
_journal_volume                  32
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C10 H12 Co N2 O8, K, 2(H2 O)'
_chemical_formula_sum            'C10 H16 Co K N2 O10'
_chemical_formula_weight         422.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90.000(9)
_cell_angle_beta                 90.000(9)
_cell_angle_gamma                90.000(9)
_cell_formula_units_Z            4
_cell_length_a                   6.432(3)
_cell_length_b                   10.098(5)
_cell_length_c                   22.740(11)
_cell_measurement_temperature    293(2)
_cell_volume                     1477.0(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            9049
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.377
_diffrn_reflns_theta_min         2.698
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.503
_exptl_absorpt_correction_T_max  0.678
_exptl_absorpt_correction_T_min  0.637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_description       platelet
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.280
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0429P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.723
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                3174
_reflns_number_total             3416
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            32_5_1.txt
_cod_data_source_block           K_Co_edta_2H2O
_cod_database_code               1551607
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.637
_shelx_estimated_absorpt_t_max   0.678
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Co1 Co 0.48945(6) 0.60722(4) 0.34110(2) 0.02016(11) Uani 1 1 d . .
N1 N 0.3500(4) 0.7034(3) 0.40301(11) 0.0239(6) Uani 1 1 d . .
C1 C 0.1346(5) 0.7284(4) 0.37979(14) 0.0281(7) Uani 1 1 d . .
H1 H 0.0686 0.7992 0.4017 0.034 Uiso 1 1 calc R U
H1A H 0.0502 0.6492 0.3835 0.034 Uiso 1 1 calc R U
C2 C 0.1564(5) 0.7666(3) 0.31581(14) 0.0262(7) Uani 1 1 d . .
H2 H 0.0205 0.7766 0.2978 0.031 Uiso 1 1 calc R U
H2A H 0.2307 0.8498 0.3122 0.031 Uiso 1 1 calc R U
N2 N 0.2753(4) 0.6574(3) 0.28644(11) 0.0209(5) Uani 1 1 d . .
C3 C 0.3651(5) 0.6168(4) 0.45555(14) 0.0304(7) Uani 1 1 d . .
H3 H 0.2583 0.5490 0.4543 0.036 Uiso 1 1 calc R U
H3A H 0.3465 0.6686 0.4911 0.036 Uiso 1 1 calc R U
C4 C 0.5794(5) 0.5537(4) 0.45489(15) 0.0288(7) Uani 1 1 d . .
O1 O 0.6715(4) 0.5519(3) 0.40467(10) 0.0295(5) Uani 1 1 d . .
O2 O 0.6526(5) 0.5075(3) 0.50050(11) 0.0435(7) Uani 1 1 d . .
C5 C 0.4650(5) 0.8308(3) 0.41316(14) 0.0289(7) Uani 1 1 d . .
H5 H 0.3685 0.9043 0.4100 0.035 Uiso 1 1 calc R U
H5A H 0.5216 0.8310 0.4527 0.035 Uiso 1 1 calc R U
C6 C 0.6385(5) 0.8499(3) 0.36985(14) 0.0260(7) Uani 1 1 d . .
O3 O 0.6506(3) 0.7621(2) 0.32871(10) 0.0266(5) Uani 1 1 d . .
O4 O 0.7575(4) 0.9448(3) 0.37468(12) 0.0380(6) Uani 1 1 d . .
C7 C 0.1416(5) 0.5384(3) 0.27467(15) 0.0276(7) Uani 1 1 d . .
H7 H 0.1703 0.5052 0.2355 0.033 Uiso 1 1 calc R U
H7A H -0.0036 0.5641 0.2762 0.033 Uiso 1 1 calc R U
C8 C 0.1805(5) 0.4296(3) 0.31901(15) 0.0271(7) Uani 1 1 d . .
O5 O 0.3375(4) 0.4500(2) 0.35436(10) 0.0273(5) Uani 1 1 d . .
O6 O 0.0732(4) 0.3299(3) 0.31944(12) 0.0414(7) Uani 1 1 d . .
C9 C 0.3874(5) 0.6957(3) 0.23200(14) 0.0244(7) Uani 1 1 d . .
H9 H 0.4404 0.7854 0.2353 0.029 Uiso 1 1 calc R U
H9A H 0.2951 0.6913 0.1983 0.029 Uiso 1 1 calc R U
C10 C 0.5672(5) 0.5972(3) 0.22495(14) 0.0247(7) Uani 1 1 d . .
O7 O 0.6213(3) 0.5343(2) 0.27246(10) 0.0265(5) Uani 1 1 d . .
O8 O 0.6490(4) 0.5785(3) 0.17649(10) 0.0327(6) Uani 1 1 d . .
K1 K 0.01216(16) 0.15090(8) 0.40461(3) 0.0406(2) Uani 1 1 d . .
O9 O 0.0350(5) 0.3642(3) 0.47765(12) 0.0509(7) Uani 1 1 d . .
O10 O -0.4305(5) 0.2277(3) 0.40767(12) 0.0531(9) Uani 1 1 d . .
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'
Co Co 0.3494 0.9721 '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'
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'
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
O5 Co1 O3 177.99(10) . .
O5 Co1 O7 92.07(10) . .
O3 Co1 O7 87.36(10) . .
O5 Co1 N2 87.37(11) . .
O3 Co1 N2 94.48(11) . .
O7 Co1 N2 83.81(11) . .
O5 Co1 N1 93.78(11) . .
O3 Co1 N1 86.99(11) . .
O7 Co1 N1 171.53(11) . .
N2 Co1 N1 90.34(11) . .
O5 Co1 O1 87.21(10) . .
O3 Co1 O1 91.05(10) . .
O7 Co1 O1 103.18(10) . .
N2 Co1 O1 171.30(10) . .
N1 Co1 O1 83.24(12) . .
C3 N1 C5 110.4(3) . .
C3 N1 C1 116.2(3) . .
C5 N1 C1 111.3(3) . .
C3 N1 Co1 105.1(2) . .
C5 N1 Co1 108.30(19) . .
C1 N1 Co1 104.85(19) . .
N1 C1 C2 107.2(3) . .
N2 C2 C1 106.7(3) . .
C9 N2 C2 115.3(3) . .
C9 N2 C7 109.8(2) . .
C2 N2 C7 112.1(2) . .
C9 N2 Co1 105.05(19) . .
C2 N2 Co1 105.75(18) . .
C7 N2 Co1 108.34(19) . .
N1 C3 C4 107.4(3) . .
O2 C4 O1 124.5(3) . .
O2 C4 C3 119.9(3) . .
O1 C4 C3 115.7(3) . .
C4 O1 Co1 112.2(2) . .
C4 O2 K1 137.2(3) . 3_556
C6 C5 N1 112.1(3) . .
O4 C6 O3 124.2(3) . .
O4 C6 C5 120.3(3) . .
O3 C6 C5 115.6(3) . .
C6 O3 Co1 115.2(2) . .
C6 O4 K1 170.7(2) . 1_665
N2 C7 C8 111.6(3) . .
O6 C8 O5 124.2(3) . .
O6 C8 C7 120.7(3) . .
O5 C8 C7 115.1(3) . .
C8 O5 Co1 115.7(2) . .
C8 O6 K1 130.2(2) . .
N2 C9 C10 106.5(2) . .
O8 C10 O7 123.5(3) . .
O8 C10 C9 120.9(3) . .
O7 C10 C9 115.6(3) . .
C10 O7 Co1 111.7(2) . .
C10 O8 K1 146.6(2) . 4_655
O6 K1 O9 84.23(10) . .
O6 K1 O4 114.92(9) . 1_445
O9 K1 O4 141.81(9) . 1_445
O6 K1 O2 152.23(9) . 3_456
O9 K1 O2 87.99(10) . 3_456
O4 K1 O2 87.19(9) 1_445 3_456
O6 K1 O8 66.82(8) . 4_645
O9 K1 O8 122.53(9) . 4_645
O4 K1 O8 95.65(8) 1_445 4_645
O2 K1 O8 95.77(8) 3_456 4_645
O6 K1 O10 88.93(9) . .
O9 K1 O10 80.22(9) . .
O4 K1 O10 68.15(9) 1_445 .
O2 K1 O10 115.96(9) 3_456 .
O8 K1 O10 142.49(8) 4_645 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O5 1.889(2) .
Co1 O3 1.897(2) .
Co1 O7 1.923(2) .
Co1 N2 1.923(3) .
Co1 N1 1.931(3) .
Co1 O1 1.942(2) .
N1 C3 1.484(4) .
N1 C5 1.502(4) .
N1 C1 1.504(4) .
C1 C2 1.512(5) .
C2 N2 1.499(4) .
N2 C9 1.484(4) .
N2 C7 1.502(4) .
C3 C4 1.519(5) .
C4 O2 1.231(4) .
C4 O1 1.287(4) .
O2 K1 2.834(3) 3_556
C5 C6 1.501(5) .
C6 O4 1.231(4) .
C6 O3 1.291(4) .
O4 K1 2.734(3) 1_665
C7 C8 1.512(5) .
C8 O6 1.221(4) .
C8 O5 1.307(4) .
O6 K1 2.678(3) .
C9 C10 1.534(4) .
C10 O8 1.236(4) .
C10 O7 1.300(4) .
O8 K1 2.947(3) 4_655
K1 O9 2.724(3) .
K1 O4 2.734(3) 1_445
K1 O2 2.834(3) 3_456
K1 O8 2.947(3) 4_645
K1 O10 2.952(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
C1 H1 O4 0.97 2.56 3.267(4) 130.0 1_455
C2 H2 O3 0.97 2.49 3.267(4) 137.5 1_455
C2 H2A O8 0.97 2.45 3.393(5) 164.5 4_655
C3 H3 O9 0.97 2.41 3.356(5) 163.8 .
C5 H5 O2 0.97 2.62 3.249(4) 122.8 3_466
C5 H5 O8 0.97 2.64 3.309(4) 126.3 4_655
C7 H7 O4 0.97 2.62 3.584(5) 173.2 4_645
C7 H7A O7 0.97 2.43 3.347(4) 157.0 1_455
C9 H9 O7 0.97 2.55 3.421(4) 149.3 4_655
C9 H9A O10 0.97 2.59 3.204(4) 121.5 4
C1 H1 O4 0.97 2.56 3.267(4) 130.0 1_455
C2 H2 O3 0.97 2.49 3.267(4) 137.5 1_455
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
_geom_torsion_site_symmetry_4
C3 N1 C1 C2 -157.0(3) .
C5 N1 C1 C2 75.4(3) .
Co1 N1 C1 C2 -41.5(3) .
N1 C1 C2 N2 55.2(3) .
C1 C2 N2 C9 -156.1(3) .
C1 C2 N2 C7 77.4(3) .
C1 C2 N2 Co1 -40.5(3) .
C5 N1 C3 C4 -77.7(3) .
C1 N1 C3 C4 154.2(3) .
Co1 N1 C3 C4 38.9(3) .
N1 C3 C4 O2 160.1(3) .
N1 C3 C4 O1 -20.6(4) .
O2 C4 O1 Co1 170.4(3) .
C3 C4 O1 Co1 -8.8(4) .
O1 C4 O2 K1 -135.4(3) 3_556
C3 C4 O2 K1 43.8(5) 3_556
C3 N1 C5 C6 119.3(3) .
C1 N1 C5 C6 -110.1(3) .
Co1 N1 C5 C6 4.7(3) .
N1 C5 C6 O4 -174.8(3) .
N1 C5 C6 O3 5.5(4) .
O4 C6 O3 Co1 166.8(3) .
C5 C6 O3 Co1 -13.6(3) .
O7 Co1 O3 C6 -172.9(2) .
N2 Co1 O3 C6 103.5(2) .
N1 Co1 O3 C6 13.4(2) .
O1 Co1 O3 C6 -69.8(2) .
C9 N2 C7 C8 128.2(3) .
C2 N2 C7 C8 -102.3(3) .
Co1 N2 C7 C8 14.0(3) .
N2 C7 C8 O6 173.6(3) .
N2 C7 C8 O5 -8.2(4) .
O6 C8 O5 Co1 175.9(3) .
C7 C8 O5 Co1 -2.2(4) .
O7 Co1 O5 C8 -74.9(2) .
N2 Co1 O5 C8 8.8(2) .
N1 Co1 O5 C8 98.9(2) .
O1 Co1 O5 C8 -178.0(2) .
O5 C8 O6 K1 21.6(5) .
C7 C8 O6 K1 -160.4(2) .
C2 N2 C9 C10 155.2(2) .
C7 N2 C9 C10 -77.1(3) .
Co1 N2 C9 C10 39.2(3) .
N2 C9 C10 O8 158.4(3) .
N2 C9 C10 O7 -20.0(4) .
O8 C10 O7 Co1 171.5(3) .
C9 C10 O7 Co1 -10.1(3) .
O7 C10 O8 K1 -87.7(5) 4_655
C9 C10 O8 K1 94.1(4) 4_655
