Different Ways To Distort a Tetracapped Tetrahedron on Route to Forming an E4M4 Cubane: The Case of [E4(Pd(PPh2Me)2)4][Ph2EX2]2 (E = Sb, X = Cl; E = Bi, X = Br)
Joseph L. Stark; Brian Harms; Ilse Guzman-Jimenez; Kenton H. Whitmire; Régis Gautier; Jean-François Halet; Jean-Yves Saillard; Journal of the American Chemical Society 121 (1999) 4409–4418; doi:10.1021/ja982902u

data_4116379
_publ_contact_author
; 
Dr. Kenton. H. Whitmire
Chemistry Department MS 60
Rice University
6100 Main Street
Houston TX 77005-1892
U.S.A.
;
_publ_contact_author_email       whitmir@rice.edu
_publ_contact_author_fax         (1)-713-737-5652
_publ_contact_author_phone       (1)-713-737-5650
_publ_section_title
;
 Different Ways To Distort a Tetracapped Tetrahedron on Route to Forming
 an E4M4 Cubane: The Case of [E4(Pd(PPh2Me)2)4][Ph2EX2]2 (E = Sb, X = Cl;
 E = Bi, X = Br)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4409
_journal_page_last               4418
_journal_paper_doi               10.1021/ja982902u
_journal_volume                  121
_journal_year                    1999
_chemical_formula_moiety
;
[Bi4(Pd((C6H5)2PCH3)2)4][(C6H5)2BiBr2]2
;
_chemical_formula_sum            'C128 H124 Bi6 Br4 P8 Pd4'
_chemical_formula_weight         3909.15
_chemical_name_systematic
; 
 [( 3-(Bis(diphenylmethylphosphine)palldium)-tetrabismuth][Dibromo-
 diphenyl bismuth]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                84.75(3)
_cell_angle_beta                 77.78(3)
_cell_angle_gamma                85.59(3)
_cell_formula_units_Z            2
_cell_length_a                   14.395(3)
_cell_length_b                   14.974(3)
_cell_length_c                   32.363(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      7.32
_cell_measurement_theta_min      3.67
_cell_volume                     6777(3)
_computing_cell_refinement       'TEXSAN 5.0'
_computing_data_collection       'TEXSAN 5.0'
_computing_data_reduction        'TEXSAN 5.0'
_computing_molecular_graphics    SHELXTL-PLUS
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measurement_device       'Rigaku AFC5-S'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_sigmaI/netI    0.1167
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            19468
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.593
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.7528
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_description       cube
_exptl_crystal_F_000             3668
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         2.080
_refine_diff_density_min         -1.583
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.039
_refine_ls_goodness_of_fit_obs   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1284
_refine_ls_number_reflns         18463
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.053
_refine_ls_restrained_S_obs      1.114
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_obs          0.0550
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0641P)^2^+67.8493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1658
_refine_ls_wR_factor_obs         0.1358
_reflns_number_observed          11442
_reflns_number_total             18468
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja982902u_1.cif
_cod_data_source_block           bi4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0641P)^2^+67.8493P] 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^)+( 0.0641P)^2^+67.8493P]
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        6777.3(24)
_cod_database_code               4116379