Crystal structure of diaqua-bis(3-carboxy-5-bromoisophthalato-κO)-bis(1-(3-(1H-benzo[d]imidazol-1-yl)propyl)-1H-benzo[d]imidazol-3-ium-κN)nickel(II) bis(3-carboxy-5-bromoisophthalate), C66H54Br4N8NiO18
Han, Min-Le; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 655–657; doi:10.1515/ncrs-2019-0006

data_8105810
_publ_section_title
;
 Crystal structure of
 diaqua-bis(3-carboxy-5-bromoisophthalato-\kO)-bis(1-(3-(1H-benzo[d]imidazol-1-yl)propyl)-1H-benzo[d]imidazol-3-ium-\kN)nickel(II)
 bis(3-carboxy-5-bromoisophthalate), C66H54Br4N8NiO18
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              655
_journal_page_last               657
_journal_paper_doi               10.1515/ncrs-2019-0006
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C50 H46 Br2 N8 Ni O10, 2(C8 H4 Br O4)'
_chemical_formula_sum            'C66 H54 Br4 N8 Ni O18'
_chemical_formula_weight         1625.52
_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                119.6080(10)
_cell_angle_beta                 95.3650(10)
_cell_angle_gamma                99.2490(10)
_cell_formula_units_Z            1
_cell_length_a                   8.821(2)
_cell_length_b                   14.6587(14)
_cell_length_c                   14.8211(14)
_cell_measurement_reflns_used    4142
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.347
_cell_measurement_theta_min      2.389
_cell_volume                     1610.8(4)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12096
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         2.388
_exptl_absorpt_coefficient_mu    2.862
_exptl_absorpt_correction_T_max  0.6574
_exptl_absorpt_correction_T_min  0.5466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_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    1.676
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             818
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.973
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         5952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0327P)^2^+1.3576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4696
_reflns_number_total             5952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncrs-2019-0006_suppl.cif
_cod_data_source_block           a
_cod_original_cell_volume        1610.8(5)
_cod_database_code               8105810
_shelx_estimated_absorpt_t_max   0.657
_shelx_estimated_absorpt_t_min   0.547
_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) groups, All O(H,H) groups
2.a Fixed occupancy and ADP/Uiso:
 H9A, H9B
2.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B)
2.c Aromatic/amide H refined with riding coordinates:
 N4(H4), C3(H3A), C5(H5), C7(H7), C11(H11), C13(H13), C15(H15), C19(H19),
 C20(H20), C21(H21), C22(H22), C24(H24), C28(H28), C31(H31), C32(H32), C33(H33),
  C34(H34)
2.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O7(H7A)
;
_olex2_submission_special_instructions 'No special instructions were received'