Preparation and Characterization of Novel Inorganic-Organic Hybrid Materials Containing Rare, Mixed-Halide Anions of Bismuth(III)
Goforth, Andrea M.; Smith, Mark D.; Peterson, Jr, LeRoy; zur Loye, Hans-Conrad; Inorganic Chemistry 43 (2004) 7042–7049; doi:10.1021/ic049212d

data_4311918
_publ_section_title
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 Preparation and Characterization of Novel Inorganic-Organic Hybrid
 Materials Containing Rare, Mixed-Halide Anions of Bismuth(III)
;
_journal_issue                   22
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7042
_journal_page_last               7049
_journal_paper_doi               10.1021/ic049212d
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         '2(C13 H28 N2), Bi2 I9, Bi Cl2 I2'
_chemical_formula_sum            'C26 H56 Bi3 Cl2 I11 N4'
_chemical_formula_weight         2518.49
_chemical_name_systematic        ?
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 118.7010(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.8586(11)
_cell_length_b                   15.5878(7)
_cell_length_c                   17.6793(9)
_cell_measurement_reflns_used    8279
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      26.370
_cell_measurement_theta_min      2.397
_cell_volume                     5525.4(5)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.625 (Bruker, 2000)'
_computing_data_reduction        'SAINT+ NT V6.02a'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega 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  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0839
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21304
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    15.796
_exptl_absorpt_correction_T_max  0.4131
_exptl_absorpt_correction_T_min  0.1891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.027
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4424
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.776
_refine_diff_density_min         -2.217
_refine_diff_density_rms         0.203
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         9659
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0328
_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 
 [0.00000+1.00000exp(2.25(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.1000*P+(0.0135P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                8076
_reflns_number_total             9659
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049212dsi20040617_104231.cif
_cod_data_source_block           amg1129s
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
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_cod_database_code               4311918