From a volatile molecular precursor to twin-free single crystals of bismuth
Wei, Zheng; Dubceac, Cristina; Petrukhina, Marina A.; Dikarev, Evgeny V.; Chemical Communications  (2019) –; doi:10.1039/C9CC02820J

data_7123351
_publ_section_title
;
 From a volatile molecular precursor to twin-free single crystals of
 bismuth
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02820J
_journal_year                    2019
_chemical_formula_moiety         Bi
_chemical_formula_sum            Bi
_chemical_formula_weight         208.98
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m'
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-09-13 deposited with the CCDC.    2019-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   4.5392(4)
_cell_length_b                   4.5392(4)
_cell_length_c                   11.8347(11)
_cell_measurement_reflns_used    3387
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.06
_cell_measurement_theta_min      5.17
_cell_volume                     211.18(3)
_computing_cell_refinement       'SAINT V.8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'APEX3 v.2017.3-0 (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V.8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'Xshell v.6.3.1 (Bruker AXS Inc., 2016)'
_computing_publication_material  'APEX3 v.2017.3-0 (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3525
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.055
_diffrn_reflns_theta_min         5.168
_exptl_absorpt_coefficient_mu    124.445
_exptl_absorpt_correction_T_max  0.0417
_exptl_absorpt_correction_T_min  0.0039
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker, 2016/2) was 
used for absorption correction. 
Krause, L., Herbst-Irmer, R., 
Sheldrick G.M. & Stalke D.,
J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            'metallic silver'
_exptl_crystal_density_diffrn    9.860
_exptl_crystal_description       block
_exptl_crystal_F_000             498
_exptl_crystal_size_max          0.115
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.232
_refine_diff_density_min         -1.849
_refine_diff_density_rms         0.290
_refine_ls_extinction_coef       0.0060(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     5
_refine_ls_number_reflns         118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.227
_refine_ls_R_factor_all          0.0104
_refine_ls_R_factor_gt           0.0104
_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^)+(0.0092P)^2^+4.5262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0258
_refine_ls_wR_factor_ref         0.0258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                118
_reflns_number_total             118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02820j2.cif
_cod_data_source_block           100K
_cod_original_cell_volume        211.18(4)
_cod_database_code               7123351
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.025
_shelx_estimated_absorpt_t_max   0.049
_shelx_res_checksum              77052