Crystal structure of catena-poly[diaqua-bis(3,4,5,6-tetrabromo-carboxybenzoato-κ1O)-(μ2-4,4′-bipyridine-κ2N:N′)cobalt(II)], C26H14Br8CoN2O10
Li, Yong-Shuang; Luo, Jia-Yang; He, Man-Qiu; Han, Min-Le; Zeitschrift für Kristallographie - New Crystal Structures 235 (2019) 113–115; doi:10.1515/ncrs-2019-0527

data_8105033
_publ_section_title
;
 Crystal structure of
 catena-poly[diaqua-bis(3,4,5,6-tetrabromo-carboxybenzoato-\k1O)-(\m2-4,4&#x2032;-bipyridine-\k2N:N&#x2032;)cobalt(II)],
 C26H14Br8CoN2O10
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              113
_journal_page_last               115
_journal_paper_doi               10.1515/ncrs-2019-0527
_journal_volume                  235
_journal_year                    2019
_chemical_formula_moiety         'C26 H14 Br8 Co N2 O10'
_chemical_formula_sum            'C26 H14 Br8 Co N2 O10'
_chemical_formula_weight         1212.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.3935(3)
_cell_length_b                   11.45050(10)
_cell_length_c                   11.70040(10)
_cell_measurement_reflns_used    5990
_cell_measurement_temperature    293
_cell_measurement_theta_max      73.8390
_cell_measurement_theta_min      4.2550
_cell_volume                     3268.13(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9f (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
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     -4.00  29.00   0.50    0.50    --    0.00 -77.00-180.00   66
  2  \w    -16.00  21.00   0.50    0.50    --    0.00 -82.00 -90.00   74
  3  \w    -31.00  -5.00   0.50    0.50    --    0.00 -82.00   0.00   52
  4  \w    -46.00 -17.00   0.50    0.50    --    0.00 -77.00-180.00   58
  5  \w      6.00 107.00   0.50    0.87    --   95.80 -15.00 120.00  202
  6  \w     58.00 112.00   0.50    0.87    --   95.80 -30.00  30.00  108
  7  \w     73.00 127.00   0.50    0.87    --   95.80 -82.00  60.00  108
  8  \w     40.00 113.00   0.50    0.87    --   95.80 -82.00  30.00  146
  9  \w     37.00  63.00   0.50    0.87    --   95.80 -82.00  60.00   52
 10  \w    128.00 154.00   0.50    0.87    --   95.80  82.00 -90.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0340216000
_diffrn_orient_matrix_UB_12      0.0024295000
_diffrn_orient_matrix_UB_13      0.1109256000
_diffrn_orient_matrix_UB_21      -0.0530363000
_diffrn_orient_matrix_UB_22      -0.0124247000
_diffrn_orient_matrix_UB_23      -0.0704472000
_diffrn_orient_matrix_UB_31      0.0043157000
_diffrn_orient_matrix_UB_32      -0.1339216000
_diffrn_orient_matrix_UB_33      0.0085505000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9804
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.591
_diffrn_reflns_theta_max         66.591
_diffrn_reflns_theta_min         3.624
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.099
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.464
_exptl_crystal_description       block
_exptl_crystal_F_000             2284
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.120
_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     217
_refine_ls_number_reflns         2887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+3.6045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2688
_reflns_number_total             2887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0527_suppl.cif
_cod_data_source_block           9-co
_cod_database_code               8105033
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Rotating group:
 O5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C14(H14), C13(H13)
2.c Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;