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_4116380
_publ_contact_author
; 
Dr. Kenton. H. Whitmire
Chemistry Department MS 60
Rice University
6100 Main Street
Houston TX 77005-1892
U.S.A.
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_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_structural
; 
[Sb4(Pd((C6H5)2PCH3)2)4][(C6H5)2SbCl2]2
;
_chemical_formula_sum            'C130 H128 Cl4 O0.5 P8 Pd4 Sb6'
_chemical_formula_weight         3243.98
_chemical_name_systematic
; 
 [tetrakis[u3-(bis(diphenylmethylphposphine)palladium)] tetraantimony]
 bis[diphenyldidichloroantimony]
;
_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                85.08(3)
_cell_angle_beta                 77.96(3)
_cell_angle_gamma                85.23(3)
_cell_formula_units_Z            2
_cell_length_a                   14.176(3)
_cell_length_b                   14.770(3)
_cell_length_c                   32.465(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      5.75
_cell_measurement_theta_min      3.40
_cell_volume                     6609(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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            18094
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.959
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.6280
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       block
_exptl_crystal_F_000             3180
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.494
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.108
_refine_ls_goodness_of_fit_obs   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1291
_refine_ls_number_reflns         17244
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.153
_refine_ls_restrained_S_obs      1.137
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_obs          0.0386
_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^)+( 0.0569P)^2^+32.5742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1334
_refine_ls_wR_factor_obs         0.1206
_reflns_number_observed          14690
_reflns_number_total             17260
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja982902u_2.cif
_cod_data_source_block           sb4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0569P)^2^+32.5742P] 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^)+( 0.0569P)^2^+32.5742P]
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        6608.6(23)
_cod_original_formula_sum        'C130 H128 Cl4 O0.50 P8 Pd4 Sb6'
_cod_database_code               4116380