Diiodotetrakis[tris(dimethylamino)phosphine oxide-<i>O</i>]bismuth(III) Pentaiodide, [BiI~2~{OP(NMe~2~)~3~}~4~][I~5~]
Louis J. Farrugia; Nicholas C. Norman; Nigel L. Pickett; Acta Crystallographica Section C 54 (1998) 476–479; doi:10.1107/S0108270197015485

data_2007146
_publ_section_title
;
 Diiodotetrakis[tris(dimethylamino)phosphine
 oxide-<i>O</i>]bismuth(III) Pentaiodide,
 [BiI~2~{OP(NMe~2~)~3~}~4~][I~5~]
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              476
_journal_page_last               479
_journal_paper_doi               10.1107/S0108270197015485
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '[BiI2 (C6 H18 N3 OP)4][I5]'
_chemical_formula_moiety         'C24 H72 Bi I2 N12 O4 P4,I5'
_chemical_formula_sum            'C24 H72 Bi I7 N12 O4 P4'
_chemical_formula_weight         1814.1
_chemical_name_systematic
;
bis(iodo)tetrakis{tris(dimethylamido)phosphineoxide}bismuth(III) pentaiodide
;
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.775(6)
_cell_length_b                   13.775(6)
_cell_length_c                   30.533(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      15.1
_cell_measurement_theta_min      8.2
_cell_volume                     5794(4)
_computing_cell_refinement       'CAD4 Express'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1992)'
_computing_data_reduction        'XCAD-4 (Harms & Wocadlo, 1996)'
_computing_molecular_graphics
;
ORTEP3 for Windows (Farrugia, 1997),
CAMERON (Watkin et al., 1993)
;
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al, 1996)'
_diffrn_ambient_temperature      291(2)
_diffrn_measurement_device       'Enraf 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  0.034
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2751
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.92
_exptl_absorpt_correction_T_max  0.304
_exptl_absorpt_correction_T_min  0.109
_exptl_absorpt_correction_type   psi_scans
_exptl_absorpt_process_details
;
[local program based on the method of North, Phillips & Mathews (1968)]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.08
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             3384
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.78
_refine_diff_density_min         -1.10_(1.08\%A_from_Bi1)
_refine_ls_abs_structure_details 'Flack (1983) parameter = -0.029(11)'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.001
_refine_ls_goodness_of_fit_obs   1.081
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_restrained_S_obs      1.081
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_obs          .0305
_refine_ls_shift/esd_max         -0.005
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0374P)^2^ ] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0765
_refine_ls_wR_factor_obs         .0659
_reflns_number_observed          950
_reflns_number_total             1422
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bm1163.cif
_cod_data_source_block           bibl
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0374P)^2^ ] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0374P)^2^ ]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5793(3)
_cod_database_code               2007146