Hydrothermal synthesis and crystal structure of catena-poly[diaqua-bis(μ2-4-((pyridin-4-ylmethyl)amino)benzoato-κ2 N:O)cobalt(II)] – 4,4′-bipyridine – water (1/2/2)
Liu, Guang-Zhen; Wang, Xin; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 1031–1033; doi:10.1515/ncrs-2023-0148

data_8107652
_publ_section_title
;
 Hydrothermal synthesis and crystal structure of
 catena-poly[diaqua-bis(\m2-4-((pyridin-4-ylmethyl)amino)benzoato-\k2
 N:O)cobalt(II)] -- 4,4&#x2032;-bipyridine -- water (1/2/2)
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1031
_journal_page_last               1033
_journal_paper_doi               10.1515/ncrs-2023-0148
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C13 H13 Co0.5 N2 O3, C10 H8 N2, H2 O'
_chemical_formula_sum            'C23 H23 Co0.5 N4 O4'
_chemical_formula_weight         448.92
_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                86.664(4)
_cell_angle_beta                 69.399(5)
_cell_angle_gamma                79.429(4)
_cell_formula_units_Z            2
_cell_length_a                   9.6428(5)
_cell_length_b                   10.3191(5)
_cell_length_c                   11.8710(6)
_cell_measurement_reflns_used    4871
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.9860
_cell_measurement_theta_min      3.6760
_cell_volume                     1086.90(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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    -85.00 -34.00   1.00   15.00    --  -12.53 178.00   0.00   51
  2  \w    -85.00 -34.00   1.00   15.00    --  -12.53 178.00 -30.00   51
  3  \w    -20.00  26.00   1.00   15.00    --  -12.53 -99.00 120.00   46
  4  \w    -85.00 -35.00   1.00   15.00    --  -12.53-178.00  60.00   50
  5  \w    -56.00  83.00   1.00   15.00    --   13.55   0.00 -30.00  139
  6  \w    -20.00  53.00   1.00   15.00    --   13.55 -99.00 -90.00   73
  7  \w     -5.00  83.00   1.00   15.00    --   13.55  38.00  30.00   88
  8  \w    -82.00 -57.00   1.00   15.00    --  -12.53 -38.00  60.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0313686000
_diffrn_orient_matrix_UB_12      -0.0603849000
_diffrn_orient_matrix_UB_13      -0.0322028000
_diffrn_orient_matrix_UB_21      -0.0392899000
_diffrn_orient_matrix_UB_22      -0.0345509000
_diffrn_orient_matrix_UB_23      0.0512707000
_diffrn_orient_matrix_UB_31      -0.0619807000
_diffrn_orient_matrix_UB_32      0.0070446000
_diffrn_orient_matrix_UB_33      -0.0202263000
_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  0.0298
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11718
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         3.359
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.459
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
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    1.372
_exptl_crystal_description       block
_exptl_crystal_F_000             469
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0432
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1454
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3510
_reflns_number_total             3987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0148_suppl_001.cif
_cod_data_source_block           lgz-9
_cod_original_formula_sum        'C23 H23 Co0.50 N4 O4'
_cod_database_code               8107652
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O1W(H1WA,H1WB)
2.b Free rotating group:
 O2W(H2WA,H2WB)
2.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
2.d Aromatic/amide H refined with riding coordinates:
 N4(H4), C3(H3), C4(H4A), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22),
  C23(H23)
;
_olex2_date_sample_data_collection 2016-11-11
_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 1.316
_oxdiff_exptl_absorpt_empirical_full_min 0.754