Unexpected hydrolytic transformation of new type hybrid bromobismuthates with methylpyrazinium dications.
Kotov, Vitalii Yu; Ilyukhin, Andrey B.; Buikin, Petr A.; Simonenko, Nikolay P.; Korlyukov, Alexander A.; Smol'yakov, Alexander F.; Yorov, Khursand E.; Gavrikov, Andrey V.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 7602–7611; doi:10.1039/c9dt01019j

data_7049906
_publ_section_title
;
 Unexpected hydrolytic transformation of new type hybrid bromobismuthates
 with methylpyrazinium dications.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7602
_journal_page_last               7611
_journal_paper_doi               10.1039/c9dt01019j
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Bi2 I9, 3(C5 H7 N2)'
_chemical_formula_sum            'C15 H21 Bi2 I9 N6'
_chemical_formula_weight         1845.44
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2017-11-08T23:14:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-04-03 deposited with the CCDC.    2019-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.8902(5)
_cell_length_b                   9.5425(2)
_cell_length_c                   13.4798(2)
_cell_measurement_reflns_used    12084
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.367
_cell_measurement_theta_min      1.954
_cell_volume                     3716.18(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.78
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0159765
_diffrn_orient_matrix_UB_12      0.0178681
_diffrn_orient_matrix_UB_13      -0.0343022
_diffrn_orient_matrix_UB_21      -0.0170305
_diffrn_orient_matrix_UB_22      0.0123734
_diffrn_orient_matrix_UB_23      -0.033164
_diffrn_orient_matrix_UB_31      -0.0010829
_diffrn_orient_matrix_UB_32      0.0673447
_diffrn_orient_matrix_UB_33      0.0152068
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.67522
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0991
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.78
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34170
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.777
_diffrn_reflns_theta_full        23.899
_diffrn_reflns_theta_max         32.68
_diffrn_reflns_theta_min         1.963
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    14.693
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.61732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.298
_exptl_crystal_description       block
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.331
_refine_diff_density_min         -2.338
_refine_diff_density_rms         0.265
_refine_ls_abs_structure_details
;
 Flack x determined using 4389 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         12387
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0901
_reflns_Friedel_coverage         0.926
_reflns_Friedel_fraction_full    0.972
_reflns_Friedel_fraction_max     0.775
_reflns_number_gt                10718
_reflns_number_total             12387
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01019j2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 7049900--7049908.cif.'
_cod_original_cell_volume        3716.17(12)
_cod_database_code               7049906
_shelx_res_checksum              87161