Redetermination of bis[μ~3~-1,3,5-triamino-1,3,5-trideoxy-<i>cis</i>-inositolato(3‒)]tribismuth(III) trichloride hexahydrate
Hegetschweiler, Kaspar; Stucky, Stefan; Morgenstern, Bernd; Neis, Christian; Weyhermüller, Thomas; Acta Crystallographica Section C 65 (2009) m1–m3; doi:10.1107/S0108270108039772

data_2016928
_publ_section_title
;Redetermination of
 bis[\m~3~-1,3,5-triamino-1,3,5-trideoxy-<i>cis</i>-inositolato(3--)]tribismuth(III)
 trichloride hexahydrate
;
_journal_coeditor_code           LN3118
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m1
_journal_page_last               m3
_journal_paper_doi               10.1107/S0108270108039772
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Bi3 (C6 H12 N3 O3)2] Cl3, 6H2 O'
_chemical_formula_moiety         'C12 H24 Bi3 N6 O6 3+, 3(Cl -), 6(H2 O)'
_chemical_formula_sum            'C12 H36 Bi3 Cl3 N6 O12'
_chemical_formula_weight         1189.76
_chemical_name_systematic
;bis[\m~3~-1,3,5-triamino-trideoxy-<i>cis</i>-inositolato(3-)]-tri-bismuth(III)
trichloride
 hexahydrate
;
_space_group_IT_number           155
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   8.0903(11)
_cell_length_b                   8.0903(11)
_cell_length_c                   35.612(7)
_cell_measurement_reflns_used    57564
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.32
_cell_measurement_theta_min      2.91
_cell_volume                     2018.6(6)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'SAINT (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'Diamond (Brandenburg, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method
'3292 images at 0.5 deg. stepwise rotation in omega and phi, 20 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            24418
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         2.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.930
_exptl_absorpt_correction_T_max  0.1863
_exptl_absorpt_correction_T_min  0.0483
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(XPREP; Bruker, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.936
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             1638
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.690
_refine_diff_density_min         -2.192
_refine_ls_abs_structure_details 'Flack (1983), 824 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.009(8)
_refine_ls_extinction_coef       0.00122(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         1983
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0208
_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^)+(0.0234P)^2^+11.6700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0487
_refine_ls_wR_factor_ref         0.0487
_reflns_number_gt                1981
_reflns_number_total             1983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ln3118.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'R 32'
_cod_database_code               2016928
_cod_database_fobs_code          2016928