Crystal structure of catena-poly[diaqua-(μ2-4,4′-bipyridine-κ2 N:N′)-bis(2,3,4,5-tetrabromo-6-carboxybenzoato-κ1 O)-nickel(II)], C26H14Br8NiN2O10
Li, Yong-Shuang; Han, Min-Le; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 539–540; doi:10.1515/ncrs-2019-0766

data_8105164
_publ_section_title
;
 Crystal structure of catena-poly[diaqua-(\m2-4,4&#x2032;-bipyridine-\k2
 N:N&#x2032;)-bis(2,3,4,5-tetrabromo-6-carboxybenzoato-\k1 O)-nickel(II)],
 C26H14Br8NiN2O10
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              539
_journal_page_last               540
_journal_paper_doi               10.1515/ncrs-2019-0766
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C26 H14 Br8 N2 Ni O10'
_chemical_formula_sum            'C26 H14 Br8 N2 Ni O10'
_chemical_formula_weight         1212.38
_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                   24.1740(4)
_cell_length_b                   11.3727(2)
_cell_length_c                   11.7918(2)
_cell_measurement_reflns_used    6692
_cell_measurement_temperature    293
_cell_measurement_theta_max      73.7770
_cell_measurement_theta_min      4.2950
_cell_volume                     3241.84(10)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -29.00   1.00   0.50    0.50    --    0.00 -82.00 150.00   60
  2  \w     -7.00  26.00   0.50    0.50    --    0.00 -82.00  30.00   66
  3  \w    -17.00  31.00   0.50    0.50    --    0.00 -82.00-180.00   96
  4  \w     30.00 121.00   0.50    0.87    --   95.80 -77.00  60.00  182
  5  \w     57.00 115.00   0.50    0.87    --   95.80 -30.00 -60.00  116
  6  \w     55.00 122.00   0.50    0.87    --   95.80 -82.00  30.00  134
  7  \w      6.00 120.00   0.50    0.87    --   95.80 -15.00 120.00  228
;
_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      -0.0176408000
_diffrn_orient_matrix_UB_12      0.0418654000
_diffrn_orient_matrix_UB_13      -0.1189173000
_diffrn_orient_matrix_UB_21      -0.0594615000
_diffrn_orient_matrix_UB_22      0.0190285000
_diffrn_orient_matrix_UB_23      0.0433214000
_diffrn_orient_matrix_UB_31      0.0146276000
_diffrn_orient_matrix_UB_32      0.1273734000
_diffrn_orient_matrix_UB_33      0.0326020000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9567
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.595
_diffrn_reflns_theta_max         66.595
_diffrn_reflns_theta_min         4.296
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.942
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73036
_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 green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.484
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0390P)^2^+4.3255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0804
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2660
_reflns_number_total             2863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0766_suppl.cif
_cod_data_source_block           10-9-5
_cod_database_code               8105164
_shelx_estimated_absorpt_t_max   0.182
_shelx_estimated_absorpt_t_min   0.112
_reflns_odcompleteness_completeness 99.91
_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), C13(H13), C14(H14)
2.c Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.297
_oxdiff_exptl_absorpt_empirical_full_min 0.824