Bulk crystal growth and characterization of semi-organic nonlinear optical crystal tri-diethylammonium hexachlorobismuthate (TDCB)
Liu, Guangfeng; Liu, Jie; Zheng, Xiaoxin; Liu, Yang; Yuan, Dongsheng; Zhang, Xixia; Gao, Zeliang; Tao, Xutang; CrystEngComm 17 (2015) 2569–; doi:10.1039/C4CE02182G

data_7219621
_publ_section_title
;
 Bulk crystal growth and characterization of semi-organic nonlinear
 optical crystal tri-diethylammonium hexachlorobismuthate (TDCB)
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              2569
_journal_paper_doi               10.1039/C4CE02182G
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'Bi Cl6, 3(C4 H12 N)'
_chemical_formula_sum            'C12 H36 Bi Cl6 N3'
_chemical_formula_weight         644.12
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-10-26 deposited with the CCDC.
2015-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   14.699(4)
_cell_length_b                   14.699(4)
_cell_length_c                   19.102(5)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.67
_cell_volume                     3574.3(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12907
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    8.072
_exptl_absorpt_correction_T_max  0.1956
_exptl_absorpt_correction_T_min  0.1406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 Software Suite (Bruker,2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bulk
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(6)
_refine_ls_extinction_coef       0.00115(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1816
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0109
_refine_ls_R_factor_gt           0.0109
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0295
_refine_ls_wR_factor_ref         0.0295
_reflns_number_gt                1807
_reflns_number_total             1816
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02182g2.cif
_cod_data_source_block           TDCB
_cod_depositor_comments          'Adding full bibliography for 7219621.cif.'
_cod_original_cell_volume        3574.2(17)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               7219621