Regioselective versus complete chalcogen transfer reactions of the bis(bidentate) phosphine cis,trans,cis-1,2,3,4-tetrakis(diphenylphosphino)cyclobutane: full characterization of new, hemilabile ligands and their complexes with palladium(II) and platinum(II)
Thomas Stampfl; Rene Gutmann; Georg Czermak; Christoph Langes; Alexander Dumfort; Holger Kopacka; Karl-Hans Ongania; Peter Brüggeller; Dalton Trans.  (2003) 3425–3435; doi:10.1039/b305775e

data_7013229
_publ_section_title
;
 Regioselective versus complete chalcogen transfer reactions of the
 bis(bidentate) phosphine
 cis,trans,cis-1,2,3,4-tetrakis(diphenylphosphino)cyclobutane: full
 characterization of new, hemilabile ligands and their complexes with
 palladium(II) and platinum(II)
;
_journal_issue                   17
_journal_name_full               'Dalton Trans.'
_journal_page_first              3425
_journal_page_last               3435
_journal_paper_doi               10.1039/b305775e
_journal_year                    2003
_chemical_formula_moiety         'C52 H44 P4 Se4 x 0.5 C7 H8'
_chemical_formula_sum            'C55.5 H48 P4 Se4'
_chemical_formula_weight         1154.71
_chemical_name_systematic        dppcbSe4
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   38.730(3)
_cell_length_b                   38.730(3)
_cell_length_c                   13.281(2)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     19922(4)
_computing_cell_refinement       'Software of the Siemens P4'
_computing_data_collection       'Siemens P4'
_computing_data_reduction        'Software of the Siemens P4'
_computing_molecular_graphics    'SHELXTL PLUS'
_computing_publication_material  'SHELXTL PLUS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device_type  'Siemens P4'
_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  0.031
_diffrn_reflns_av_sigmaI/netI    0.2358
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            10844
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.109
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.779
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular solid'
_exptl_crystal_F_000             9232
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         6281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0848
_reflns_number_gt                2168
_reflns_number_total             6281
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            b305775e.txt
_cod_data_source_block           IV
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'Psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        19921(4)
_cod_original_sg_symbol_H-M      I4(1)/a
_cod_database_code               7013229
_diffrn_measured_fraction        0.990