Heterogeneous bromination of alkenes using Bi(III) polybromide complexes as {Br2} source
Adonin, Sergey A.; Perekalin, Dmitry S.; Gorokh, Igor D.; Samsonenko, Denis G.; Sokolov, Maksim Nailyevich; Fedin, Vladimir P.; RSC Adv.  (2016) –; doi:10.1039/C6RA10109G

data_7225653
_publ_section_title
;
 Heterogeneous bromination of alkenes using Bi(III) polybromide complexes
 as {Br2} source
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA10109G
_journal_year                    2016
_chemical_formula_sum            'C15 H18 Bi2 Br11 N3'
_chemical_formula_weight         1537.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-04-18 deposited with the CCDC.
2016-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.370(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8459(2)
_cell_length_b                   23.3803(4)
_cell_length_c                   9.4868(2)
_cell_measurement_reflns_used    4300
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.96
_cell_measurement_theta_min      3.78
_cell_volume                     1631.43(7)
_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    'ShelXle (H\"ubschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.834
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.834
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8267
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.834
_diffrn_reflns_theta_full        26.500
_diffrn_reflns_theta_max         29.535
_diffrn_reflns_theta_min         3.272
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    24.254
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36677
_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            orange
_exptl_crystal_density_diffrn    3.129
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.274
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.179
_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     145
_refine_ls_number_reflns         3879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0237P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0556
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3420
_reflns_number_total             3879
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c6ra10109g2.cif
_cod_data_source_block           sa1160
_cod_database_code               7225653
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.112
_shelx_estimated_absorpt_t_max   0.530
_shelx_res_checksum              708