#------------------------------------------------------------------------------
#$Date: 2022-02-09 12:13:31 +0200 (Wed, 09 Feb 2022) $
#$Revision: 272874 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/45/8104554.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_8104554
loop_
_publ_author_name
'Du, Xigang'
_publ_section_title
;
 Crystal structure of
 trans-tetraaqua-bis{2-carboxy-4-((5-carboxypyridin-3-yl)oxy)benzoato-κ1
 N}cobalt(II) dihydrate C28H28O20N2Co
;
_journal_issue                   6
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              1157
_journal_page_last               1159
_journal_paper_doi               10.1515/ncrs-2021-0257
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C28 H24 Co N2 O18, 2(H2 O)'
_chemical_formula_sum            'C28 H28 Co N2 O20'
_chemical_formula_weight         771.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                93.345(3)
_cell_angle_beta                 105.499(4)
_cell_angle_gamma                104.913(4)
_cell_formula_units_Z            1
_cell_length_a                   7.7951(3)
_cell_length_b                   9.3511(4)
_cell_length_c                   11.3352(4)
_cell_measurement_reflns_used    6101
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.1340
_cell_measurement_theta_min      4.0030
_cell_volume                     762.19(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -18.00  25.00   1.00   10.00    --  -13.64 -99.00 -30.00   43
  2  ω    -17.00  25.00   1.00   10.00    --  -13.64 -99.00  30.00   42
  3  ω    -68.00  -7.00   1.00   10.00    --  -13.64 126.00 -16.13   61
  4  ω    -47.00  84.00   1.00   10.00    --   15.05   0.00  90.00  131
  5  ω      3.00  80.00   1.00   10.00    --   15.05  57.00 -60.00   77
  6  ω     -4.00  83.00   1.00   10.00    --   15.05  38.00-120.00   87
  7  ω     35.00  69.00   1.00   10.00    --   15.05 178.00-180.00   34
  8  ω     -4.00  83.00   1.00   10.00    --   15.05  38.00 150.00   87
  9  ω    -20.00  54.00   1.00   10.00    --   15.05 -99.00 -60.00   74
 10  ω     28.00  67.00   1.00   10.00    --   15.05-122.00-156.96   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0847084000
_diffrn_orient_matrix_UB_12      -0.0352659000
_diffrn_orient_matrix_UB_13      0.0118244000
_diffrn_orient_matrix_UB_21      0.0113075000
_diffrn_orient_matrix_UB_22      -0.0709549000
_diffrn_orient_matrix_UB_23      -0.0153495000
_diffrn_orient_matrix_UB_31      0.0489259000
_diffrn_orient_matrix_UB_32      0.0005899000
_diffrn_orient_matrix_UB_33      0.0626212000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10420
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         3.335
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       block
_exptl_crystal_F_000             397
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         2842
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0278P)²+0.6146P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0798
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2567
_reflns_number_total             2842
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0257_suppl.cif
_cod_data_source_block           dus
_cod_database_code               8104554
_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_max   0.831
_shelx_estimated_absorpt_t_min   0.797
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 Co1-H8A \\sim Co1-H8B
 with sigma of 0.02
3.a Free rotating group:
 O8(H8A,H8B), O10(H10A,H10B)
3.b Rotating group:
 O7(H7A,H7B)
3.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C5(H5), C3(H3A), C1(H1), C8(H8), C9(H9)
3.d Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.854
_oxdiff_exptl_absorpt_empirical_full_min 0.491
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3262(3) 0.7465(2) 0.63020(19) 0.0254(5) Uani 1 1 d . . . . .
H1 H 0.3471 0.8277 0.6889 0.031 Uiso 1 1 calc R . . . .
C2 C 0.2413(3) 0.6054(2) 0.65125(18) 0.0220(4) Uani 1 1 d . . . . .
C3 C 0.2094(3) 0.4835(2) 0.56603(18) 0.0237(4) Uani 1 1 d . . . . .
H3A H 0.1517 0.3879 0.5787 0.028 Uiso 1 1 calc R . . . .
C4 C 0.2652(3) 0.5068(2) 0.46082(18) 0.0217(4) Uani 1 1 d . . . . .
C5 C 0.3488(3) 0.6514(2) 0.44464(18) 0.0242(5) Uani 1 1 d . . . . .
H5 H 0.3850 0.6665 0.3735 0.029 Uiso 1 1 calc R . . . .
C6 C 0.2345(3) 0.3734(2) 0.37034(18) 0.0232(4) Uani 1 1 d . . . . .
C7 C 0.2025(3) 0.4783(2) 0.82234(17) 0.0218(4) Uani 1 1 d . . . . .
C8 C 0.0676(3) 0.4248(2) 0.87936(19) 0.0270(5) Uani 1 1 d . . . . .
H8 H -0.0342 0.4624 0.8681 0.032 Uiso 1 1 calc R . . . .
C9 C 0.0868(3) 0.3141(2) 0.9537(2) 0.0273(5) Uani 1 1 d . . . . .
H9 H -0.0020 0.2793 0.9940 0.033 Uiso 1 1 calc R . . . .
C10 C 0.2347(3) 0.2540(2) 0.96931(17) 0.0204(4) Uani 1 1 d . . . . .
C11 C 0.2349(3) 0.1250(2) 1.04346(18) 0.0216(4) Uani 1 1 d . . . . .
C12 C 0.3685(3) 0.3075(2) 0.90871(17) 0.0202(4) Uani 1 1 d . . . . .
C13 C 0.3520(3) 0.4218(2) 0.83614(18) 0.0225(4) Uani 1 1 d . . . . .
H13 H 0.4419 0.4595 0.7973 0.027 Uiso 1 1 calc R . . . .
C14 C 0.5278(3) 0.2461(2) 0.91323(18) 0.0242(5) Uani 1 1 d . . . . .
Co1 Co 0.5000 1.0000 0.5000 0.02458(13) Uani 1 2 d DS T P . .
N1 N 0.3795(3) 0.77070(19) 0.52806(15) 0.0247(4) Uani 1 1 d . . . . .
O1 O 0.2541(2) 0.15340(17) 1.15780(13) 0.0334(4) Uani 1 1 d . . . . .
O2 O 0.2086(2) -0.00127(16) 0.98920(13) 0.0271(3) Uani 1 1 d . . . . .
O3 O 0.5723(2) 0.17569(19) 1.00879(14) 0.0333(4) Uani 1 1 d . . . . .
H3 H 0.6406 0.1263 0.9971 0.050 Uiso 1 1 calc GR . . . .
O4 O 0.6086(2) 0.2603(2) 0.83498(15) 0.0403(4) Uani 1 1 d . . . . .
O5 O 0.1661(2) 0.24835(16) 0.39192(14) 0.0346(4) Uani 1 1 d . . . . .
O6 O 0.2861(2) 0.39998(18) 0.27250(14) 0.0324(4) Uani 1 1 d . . . . .
H6 H 0.264(5) 0.308(4) 0.220(3) 0.095(13) Uiso 1 1 d . . . . .
O7 O 0.6730(2) 1.04588(18) 0.68233(14) 0.0361(4) Uani 1 1 d . . . . .
H7A H 0.6677 0.9648 0.7132 0.054 Uiso 1 1 d GR . . . .
H7B H 0.6300 1.0962 0.7261 0.054 Uiso 1 1 d GR . . . .
O8 O 0.3075(3) 1.0771(2) 0.56010(16) 0.0384(4) Uani 1 1 d . . . . .
H8A H 0.2525 1.0465 0.6132 0.058 Uiso 1 1 d DG . . . .
H8B H 0.2419 1.1271 0.5185 0.058 Uiso 1 1 d DG . . . .
O9 O 0.1820(2) 0.59623(16) 0.75530(13) 0.0282(4) Uani 1 1 d . . . . .
O10 O 0.1419(3) 0.9888(2) 0.73233(16) 0.0518(5) Uani 1 1 d . . . . .
H10A H 0.0442 0.9166 0.7021 0.078 Uiso 1 1 d G . . . .
H10B H 0.1606 0.9937 0.8100 0.078 Uiso 1 1 d G . . . .
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'
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
O7 Co1 O7 180.00(10) 2_676 .
O7 Co1 N1 89.67(6) . 2_676
O7 Co1 N1 89.67(6) 2_676 .
O7 Co1 N1 90.33(6) 2_676 2_676
O7 Co1 N1 90.33(6) . .
O8 Co1 O7 88.82(7) . .
O8 Co1 O7 91.18(7) . 2_676
O8 Co1 O7 88.82(7) 2_676 2_676
O8 Co1 O7 91.18(7) 2_676 .
O8 Co1 O8 180.0 . 2_676
O8 Co1 N1 92.57(7) . .
O8 Co1 N1 87.43(7) . 2_676
O8 Co1 N1 87.43(7) 2_676 .
O8 Co1 N1 92.57(7) 2_676 2_676
N1 Co1 N1 180.0 . 2_676
C2 O9 C7 118.42(16) . .
C14 O3 H3 109.5 . .
C6 O6 H6 111(2) . .
Co1 O7 H7A 109.4 . .
Co1 O7 H7B 109.2 . .
H7A O7 H7B 104.5 . .
Co1 O8 H8A 129.6 . .
Co1 O8 H8B 123.2 . .
H8A O8 H8B 104.5 . .
C5 N1 Co1 122.88(13) . .
C1 N1 Co1 119.23(14) . .
C1 N1 C5 117.83(18) . .
H10A O10 H10B 104.5 . .
O9 C2 C1 116.86(18) . .
C3 C2 O9 123.14(18) . .
C3 C2 C1 119.87(18) . .
C13 C12 C10 119.63(19) . .
C13 C12 C14 116.65(18) . .
C10 C12 C14 123.69(18) . .
C12 C13 H13 120.1 . .
C7 C13 C12 119.79(19) . .
C7 C13 H13 120.1 . .
C12 C10 C11 123.32(18) . .
C9 C10 C12 118.89(18) . .
C9 C10 C11 117.61(18) . .
C5 C4 C6 122.96(18) . .
C3 C4 C5 119.08(19) . .
C3 C4 C6 117.95(18) . .
O2 C11 O1 124.35(18) . .
O2 C11 C10 118.90(17) . .
O1 C11 C10 116.67(18) . .
C13 C7 O9 122.51(18) . .
C13 C7 C8 121.32(18) . .
C8 C7 O9 116.11(18) . .
N1 C5 C4 122.52(18) . .
N1 C5 H5 118.7 . .
C4 C5 H5 118.7 . .
O5 C6 O6 124.05(19) . .
O5 C6 C4 119.89(18) . .
O6 C6 C4 116.06(18) . .
C2 C3 C4 118.31(19) . .
C2 C3 H3A 120.8 . .
C4 C3 H3A 120.8 . .
N1 C1 C2 122.39(19) . .
N1 C1 H1 118.8 . .
C2 C1 H1 118.8 . .
O3 C14 C12 114.15(18) . .
O4 C14 O3 123.4(2) . .
O4 C14 C12 122.43(19) . .
C7 C8 H8 120.6 . .
C7 C8 C9 118.7(2) . .
C9 C8 H8 120.6 . .
C10 C9 C8 121.6(2) . .
C10 C9 H9 119.2 . .
C8 C9 H9 119.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O7 2.0935(15) .
Co1 O7 2.0935(15) 2_676
Co1 O8 2.0693(16) .
Co1 O8 2.0693(16) 2_676
Co1 N1 2.1872(17) .
Co1 N1 2.1872(17) 2_676
O9 C2 1.376(2) .
O9 C7 1.394(2) .
O2 C11 1.240(2) .
O5 C6 1.222(2) .
O3 H3 0.8200 .
O3 C14 1.314(2) .
O6 C6 1.293(2) .
O6 H6 0.96(4) .
O1 C11 1.268(2) .
O7 H7A 0.8499 .
O7 H7B 0.8502 .
O8 H8A 0.8502 .
O8 H8B 0.8502 .
O4 C14 1.212(3) .
N1 C5 1.347(3) .
N1 C1 1.343(3) .
O10 H10A 0.8500 .
O10 H10B 0.8501 .
C2 C3 1.375(3) .
C2 C1 1.381(3) .
C12 C13 1.397(3) .
C12 C10 1.402(3) .
C12 C14 1.487(3) .
C13 H13 0.9300 .
C13 C7 1.375(3) .
C10 C11 1.510(3) .
C10 C9 1.383(3) .
C4 C5 1.388(3) .
C4 C6 1.494(3) .
C4 C3 1.385(3) .
C7 C8 1.380(3) .
C5 H5 0.9300 .
C3 H3A 0.9300 .
C1 H1 0.9300 .
C8 H8 0.9300 .
C8 C9 1.385(3) .
C9 H9 0.9300 .
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_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
Co1 N1 C5 C4 -177.25(15) . . . .
Co1 N1 C1 C2 176.95(16) . . . .
O9 C2 C3 C4 176.11(19) . . . .
O9 C2 C1 N1 -175.80(19) . . . .
O9 C7 C8 C9 -175.98(19) . . . .
C2 O9 C7 C13 35.7(3) . . . .
C2 O9 C7 C8 -147.11(19) . . . .
C12 C13 C7 O9 177.37(18) . . . .
C12 C13 C7 C8 0.3(3) . . . .
C12 C10 C11 O2 -65.5(3) . . . .
C12 C10 C11 O1 117.6(2) . . . .
C12 C10 C9 C8 0.3(3) . . . .
C13 C12 C10 C11 176.29(18) . . . .
C13 C12 C10 C9 1.3(3) . . . .
C13 C12 C14 O3 159.80(18) . . . .
C13 C12 C14 O4 -20.3(3) . . . .
C13 C7 C8 C9 1.3(3) . . . .
C10 C12 C13 C7 -1.6(3) . . . .
C10 C12 C14 O3 -22.2(3) . . . .
C10 C12 C14 O4 157.7(2) . . . .
C11 C10 C9 C8 -175.0(2) . . . .
C7 O9 C2 C3 42.7(3) . . . .
C7 O9 C2 C1 -141.5(2) . . . .
C7 C8 C9 C10 -1.6(3) . . . .
C5 N1 C1 C2 -0.4(3) . . . .
C5 C4 C6 O5 177.4(2) . . . .
C5 C4 C6 O6 -1.8(3) . . . .
C5 C4 C3 C2 -0.7(3) . . . .
C6 C4 C5 N1 -178.53(19) . . . .
C6 C4 C3 C2 178.42(18) . . . .
C3 C2 C1 N1 0.2(3) . . . .
C3 C4 C5 N1 0.6(3) . . . .
C3 C4 C6 O5 -1.7(3) . . . .
C3 C4 C6 O6 179.04(19) . . . .
C1 N1 C5 C4 0.0(3) . . . .
C1 C2 C3 C4 0.4(3) . . . .
C14 C12 C13 C7 176.50(18) . . . .
C14 C12 C10 C11 -1.6(3) . . . .
C14 C12 C10 C9 -176.67(19) . . . .
C9 C10 C11 O2 109.6(2) . . . .
C9 C10 C11 O1 -67.3(3) . . . .
