Synthesis and Crystal Structure of Bis(N,N,N′,N′-tetramethyl-ethylenediammonium)decachlorodibismuthate(III) trihydrate
MASMOUDI, W.; KAMOUN, S.; AYEDI, HF.; DRISS, A.; X-ray Structure Analysis Online 26 (2010) 7–; doi:10.2116/xraystruct.26.7

data_1551748
_publ_section_title
;
 Synthesis and Crystal Structure of
 Bis(N,N,N&#x2032;,N&#x2032;-tetramethyl-ethylenediammonium)decachlorodibismuthate(III)
 trihydrate
;
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              7
_journal_paper_doi               10.2116/xraystruct.26.7
_journal_volume                  26
_journal_year                    2010
_chemical_formula_moiety         'C6 H18 N2, Bi Cl4, Cl, 1.5(H2 O)'
_chemical_formula_sum            'C6 H21 Bi Cl5 N2 O1.5'
_chemical_formula_weight         531.48
_chemical_melting_point          400
_chemical_name_systematic
;
bis(N,N,N',N'- tetramethyl-ethylenediammonium) 
decachlorodibismuthate (III) trihydrate 

;
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 121.54(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.535(4)
_cell_length_b                   14.893(5)
_cell_length_c                   10.158(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      14.74
_cell_measurement_theta_min      11.74
_cell_volume                     1745.1(12)
_computing_cell_refinement       'CAD4 Express (Enarf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enarf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for windows (Farrugia, 1999)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Enarf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta 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  0.0830
_diffrn_reflns_av_sigmaI/netI    0.0826
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3371
_diffrn_reflns_theta_full        26.96
_diffrn_reflns_theta_max         26.96
_diffrn_reflns_theta_min         2.23
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    10.855
_exptl_absorpt_correction_T_max  0.4099
_exptl_absorpt_correction_T_min  0.4099
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T.,phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 
Number of psi-scan sets used was  5 
Theta correction was applied.
Averaged transmission function was used.
no Fourrier smoothing was applied.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_density_meas      2.06
_exptl_crystal_density_method    pycnometric
_exptl_crystal_description       prism
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.263
_refine_diff_density_min         -1.848
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.15(3)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1921
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0771
_reflns_number_gt                1715
_reflns_number_total             1921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            26_7_1.cif
_cod_data_source_block           publication_text
_cod_depositor_comments
;

2022-09-26
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C12 H42 Bi2 Cl10 N4 O3'
_cod_original_formula_weight         1062.96
_cod_original_formula_moiety         'C12 H42 Bi2 Cl10 N4 O3'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        1745.1(10)
_cod_original_sg_symbol_H-M      C2
_cod_database_code               1551748