Crystal structure of (μ 2-1-(4,4′-bipyridine-κ 2N:N′)-bis[diaqua-(4-iodopyridine-2,6-dicarboxylato-κ 3O,N,O′)–cobalt(II)], C24H20Co2I2N4O12
Hong, Dong-Feng; Ye, Jia-Qi; Guo, Wen-Bo; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 845–847; doi:10.1515/ncrs-2023-0229

data_8107579
_publ_section_title
;
 Crystal structure of (\m 2-1-(4,4&#x2032;-bipyridine-\k
 2N:N&#x2032;)-bis[diaqua-(4-iodopyridine-2,6-dicarboxylato-\k
 3O,N,O&#x2032;)--cobalt(II)], C24H20Co2I2N4O12
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              845
_journal_page_last               847
_journal_paper_doi               10.1515/ncrs-2023-0229
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C24 H20 Co2 I2 N4 O12'
_chemical_formula_sum            'C24 H20 Co2 I2 N4 O12'
_chemical_formula_weight         928.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 92.388(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.5649(3)
_cell_length_b                   18.6071(6)
_cell_length_c                   7.4403(2)
_cell_measurement_reflns_used    7166
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6240
_cell_measurement_theta_min      3.9390
_cell_volume                     1461.36(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (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 0.886
_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    -37.00  -3.00   1.00   15.00    --  -15.84 -77.00 -90.00   34
  2  \w    -83.00   1.00   1.00   15.00    --  -15.84 -57.00  60.00   84
  3  \w    -75.00 -18.00   1.00   15.00    --  -15.84 134.00-120.70   57
  4  \w    -33.00   9.00   1.00   15.00    --  -15.84 -77.00 -30.00   42
  5  \w    -42.00 -16.00   1.00   15.00    --  -15.84  77.00-150.00   26
  6  \w     -4.00  42.00   1.00   15.00    --  -15.84  77.00-150.00   46
  7  \w     -1.00  85.00   1.00   15.00    --   17.09  38.00 -90.00   86
  8  \w    -49.00  26.00   1.00   15.00    --   17.09   0.00  60.00   75
;
_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      0.0646554000
_diffrn_orient_matrix_UB_12      -0.0045650000
_diffrn_orient_matrix_UB_13      -0.0194098000
_diffrn_orient_matrix_UB_21      -0.0006330000
_diffrn_orient_matrix_UB_22      0.0336558000
_diffrn_orient_matrix_UB_23      -0.0448612000
_diffrn_orient_matrix_UB_31      0.0182253000
_diffrn_orient_matrix_UB_32      0.0173426000
_diffrn_orient_matrix_UB_33      0.0819278000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14552
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.317
_diffrn_reflns_theta_min         3.463
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.317
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
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    2.109
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.667
_refine_diff_density_min         -1.149
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+2.0382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0781
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3082
_reflns_number_total             3553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0229_suppl_001.cif
_cod_data_source_block           1
_cod_database_code               8107579
_shelx_estimated_absorpt_t_max   0.426
_shelx_estimated_absorpt_t_min   0.365
_reflns_odcompleteness_completeness 99.26
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C8(H8), C9(H9), C11(H11), C12(H12)
;
_shelx_res_checksum              8311
_shelx_hkl_checksum              46153
_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 1.381
_oxdiff_exptl_absorpt_empirical_full_min 0.740