Crystal structure of trans-tetraaqua-bis{2-carboxy-4-((5-carboxypyridin-3-yl)oxy)benzoato-κ1 N}cobalt(II) dihydrate C28H28O20N2Co
Du, Xigang; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 1157–1159; doi:10.1515/ncrs-2021-0257

data_8104554
_publ_section_title
;
 Crystal structure of
 trans-tetraaqua-bis{2-carboxy-4-((5-carboxypyridin-3-yl)oxy)benzoato-\k1
 N}cobalt(II) dihydrate C28H28O20N2Co
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur 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  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -18.00  25.00   1.00   10.00    --  -13.64 -99.00 -30.00   43
  2  \w    -17.00  25.00   1.00   10.00    --  -13.64 -99.00  30.00   42
  3  \w    -68.00  -7.00   1.00   10.00    --  -13.64 126.00 -16.13   61
  4  \w    -47.00  84.00   1.00   10.00    --   15.05   0.00  90.00  131
  5  \w      3.00  80.00   1.00   10.00    --   15.05  57.00 -60.00   77
  6  \w     -4.00  83.00   1.00   10.00    --   15.05  38.00-120.00   87
  7  \w     35.00  69.00   1.00   10.00    --   15.05 178.00-180.00   34
  8  \w     -4.00  83.00   1.00   10.00    --   15.05  38.00 150.00   87
  9  \w    -20.00  54.00   1.00   10.00    --   15.05 -99.00 -60.00   74
 10  \w     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       '\w 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/[\s^2^(Fo^2^)+(0.0278P)^2^+0.6146P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0257_suppl.cif
_cod_data_source_block           dus
_cod_database_code               8104554
_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