Crystal structure of catena-poly[(μ2-isophthalato-k3 O,O′:O″)(4-(4-pyridyl)-2,5-dipyrazylpyridine-k3 N,N′,N″)cobalt(II)] trihydrate C26H22N6O7Co1
He, Chao-Jun; Wang, Zhou-Qin; Wang, Yu-Fang; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 659–661; doi:10.1515/ncrs-2023-0138

data_8107523
_publ_section_title
;
 Crystal structure of catena-poly[(\m2-isophthalato-k3
 O,O&#x2032;:O&#x2033;)(4-(4-pyridyl)-2,5-dipyrazylpyridine-k3
 N,N&#x2032;,N&#x2033;)cobalt(II)] trihydrate C26H22N6O7Co1
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              659
_journal_page_last               661
_journal_paper_doi               10.1515/ncrs-2023-0138
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C26 H16 Co N6 O4, 3(H2 O)'
_chemical_formula_sum            'C26 H22 Co N6 O7'
_chemical_formula_weight         589.42
_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                96.164(4)
_cell_angle_beta                 100.835(4)
_cell_angle_gamma                113.867(5)
_cell_formula_units_Z            2
_cell_length_a                   9.0033(4)
_cell_length_b                   10.1338(5)
_cell_length_c                   15.5122(8)
_cell_measurement_reflns_used    7781
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.7730
_cell_measurement_theta_min      3.8360
_cell_volume                     1244.40(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 0.884
_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    -20.00  25.00   1.00    8.65    --  -13.80 -99.00  60.00   45
  2  \w    -20.00  25.00   1.00    8.65    --  -13.80 -99.00 -90.00   45
  3  \w    -31.00  53.00   1.00    8.65    --  -13.80  57.00  30.00   84
  4  \w     -2.00  82.00   1.00    8.65    --   14.82  57.00  90.00   84
  5  \w    -53.00  42.00   1.00    8.65    --   14.82 -77.00 150.00   95
  6  \w    -12.00  82.00   1.00    8.65    --   14.82  77.00 -90.00   94
  7  \w    -86.00 -34.00   1.00    8.65    --  -13.80 178.00-180.00   52
  8  \w    -20.00  54.00   1.00    8.65    --   14.82 -99.00 -60.00   74
  9  \w     -4.00  84.00   1.00    8.65    --   14.82  38.00  60.00   88
 10  \w    -20.00  54.00   1.00    8.65    --   14.82 -99.00  60.00   74
 11  \w     -4.00  84.00   1.00    8.65    --   14.82  38.00-180.00   88
 12  \w    -86.00 -35.00   1.00    8.65    --  -13.80-178.00 120.00   51
 13  \w    -20.00  21.00   1.00    8.65    --   14.82 -99.00-150.00   41
;
_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      0.0378958000
_diffrn_orient_matrix_UB_12      0.0590482000
_diffrn_orient_matrix_UB_13      0.0378419000
_diffrn_orient_matrix_UB_21      0.0783003000
_diffrn_orient_matrix_UB_22      -0.0024369000
_diffrn_orient_matrix_UB_23      0.0024970000
_diffrn_orient_matrix_UB_31      0.0192065000
_diffrn_orient_matrix_UB_32      0.0511909000
_diffrn_orient_matrix_UB_33      -0.0286964000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23992
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.430
_diffrn_reflns_theta_min         3.606
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       block
_exptl_crystal_F_000             606
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0280P)^2^+0.5819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1023
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4418
_reflns_number_total             5532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0138_suppl_001.cif
_cod_data_source_block           w110
_cod_original_cell_volume        1244.40(11)
_cod_database_code               8107523
_shelx_estimated_absorpt_t_max   0.877
_shelx_estimated_absorpt_t_min   0.864
_reflns_odcompleteness_completeness 99.72
_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,H) groups
2.a Free rotating group:
 O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C8(H8), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C25(H25)
;
_olex2_date_sample_data_collection 2018-11-02
_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 4.588
_oxdiff_exptl_absorpt_empirical_full_min 0.253