Hydrothermal synthesis and crystal structure of catena-poly[diaqua-bis(μ2-4-[(4-pyridinylmethyl)amino]benzoato-κ2 N:O)cobalt(II)]–1,2bi(4-pyridyl)ethene–water (1/1/1), C50H50N8O8Co
Guang-Zhen, Liu; Li, Ya-Di; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 719–721; doi:10.1515/ncrs-2022-0127

data_8107198
_publ_section_title
;
 Hydrothermal synthesis and crystal structure of
 catena-poly[diaqua-bis(\m2-4-[(4-pyridinylmethyl)amino]benzoato-\k2
 N:O)cobalt(II)]--1,2bi(4-pyridyl)ethene--water (1/1/1), C50H50N8O8Co
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              719
_journal_page_last               721
_journal_paper_doi               10.1515/ncrs-2022-0127
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C13 H13 Co0.5 N2 O3, C12 H10 N2, H2 O'
_chemical_formula_sum            'C25 H25 Co0.5 N4 O4'
_chemical_formula_weight         474.95
_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                96.478(3)
_cell_angle_beta                 104.766(3)
_cell_angle_gamma                103.901(4)
_cell_formula_units_Z            2
_cell_length_a                   9.2920(4)
_cell_length_b                   11.3648(5)
_cell_length_c                   11.9954(4)
_cell_measurement_reflns_used    6304
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4660
_cell_measurement_theta_min      4.0820
_cell_volume                     1168.41(9)
_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 (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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -86.00 -35.00   1.00    6.60    --  -13.48-178.00 150.00   51
  2  \w    -20.00  25.00   1.00    6.60    --  -13.48 -99.00-150.00   45
  3  \w    -40.00  54.00   1.00    6.60    --  -13.48  77.00 120.00   94
  4  \w    -83.00   5.00   1.00    6.60    --  -13.48 -38.00-180.00   88
  5  \w    -20.00  25.00   1.00    6.60    --  -13.48 -99.00-120.00   45
  6  \w    -85.00  16.00   1.00    6.60    --  -13.48 -19.00  30.00  101
  7  \w    -81.00  13.00   1.00    6.60    --  -13.48 -77.00   0.00   94
  8  \w     35.00  60.00   1.00    6.60    --   14.49 178.00 120.00   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      -0.0338263000
_diffrn_orient_matrix_UB_12      -0.0603964000
_diffrn_orient_matrix_UB_13      0.0075669000
_diffrn_orient_matrix_UB_21      -0.0694286000
_diffrn_orient_matrix_UB_22      0.0157213000
_diffrn_orient_matrix_UB_23      -0.0001131000
_diffrn_orient_matrix_UB_31      -0.0282376000
_diffrn_orient_matrix_UB_32      -0.0196511000
_diffrn_orient_matrix_UB_33      -0.0617680000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_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       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13006
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.499
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         3.323
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76528
_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            'clear pinkish pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       block
_exptl_crystal_F_000             497
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0393
_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          0.1379
_refine_ls_wR_factor_ref         0.1431
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3900
_reflns_number_total             4330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0127_suppl.cif
_cod_data_source_block           lgz-5
_cod_original_cell_volume        1168.40(8)
_cod_original_formula_sum        'C25 H25 Co0.50 N4 O4'
_cod_database_code               8107198
_chemical_oxdiff_usercomment     'c h n o ZN'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.13
_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 Free rotating group:
 O2W(H2WA,H2WB)
2.b Rotating group:
 O1W(H1WA,H1WB)
2.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
2.d Aromatic/amide H refined with riding coordinates:
 N3(H3), C3(H3A), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
  C23(H23), C24(H24), C25(H25)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-10-21
_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 1.280
_oxdiff_exptl_absorpt_empirical_full_min 0.529