The crystal structure of 3,3′-((carbonylbis(azanediyl))bis(ethane-2,1-diyl)) bis(1-methyl-1H-benzo[d]imidazol-3-ium) tetrafluoroborate monohydrate, C21H28N6O3B2F8
Dong, Zhi-Yun; Xi, Fu-Gui; Xu, Xing-Yu; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 553–555; doi:10.1515/ncrs-2020-0646

data_8104765
_publ_section_title
;
 The crystal structure of
 3,3&#x2032;-((carbonylbis(azanediyl))bis(ethane-2,1-diyl))
 bis(1-methyl-1H-benzo[d]imidazol-3-ium) tetrafluoroborate monohydrate,
 C21H28N6O3B2F8
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              553
_journal_page_last               555
_journal_paper_doi               10.1515/ncrs-2020-0646
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C21 H26 N6 O, 2(B F4), 0.5(H4 O2)'
_chemical_formula_sum            'C21 H28 B2 F8 N6 O2'
_chemical_formula_weight         570.11
_chemical_name_systematic
;
3,3'-((carbonylbis(azanediyl))bis(ethane-2,1-diyl))bis(1-
methyl-1H-benzo[d]imidazol-3-ium) 
tetrafluoroborate monohydrate 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c 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                   17.7949(19)
_cell_length_b                   9.3979(10)
_cell_length_c                   15.3455(16)
_cell_measurement_reflns_used    5046
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.671
_cell_measurement_theta_min      2.289
_cell_volume                     2566.3(5)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0533
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32623
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.090
_diffrn_reflns_theta_min         2.289
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  0.9906
_exptl_absorpt_correction_T_min  0.778432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.0646 before and 0.0270 after correction.
The Ratio of minimum to maximum transmission is 0.7784.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3127
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      10.655
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0794P)^2^+1.2701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1846
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1897
_reflns_number_total             3127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0646_suppl.cif
_cod_data_source_block           z
_cod_database_code               8104765
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.967
_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 C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O2-H2A
 0.85 with sigma of 0.0001
3. Others
 Fixed Sof: O2(0.5) H2A(0.5) H2B(0.5)
4.a Rotating group:
 O2(H2A,H2B)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B)
4.c Me refined with riding coordinates:
 C11(H11A,H11B,H11C)
4.d Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C2(H2), C3(H3A), C4(H4), C7(H7)
;