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_7013231
_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 Cl4 P4 Pt2 Se2 x 0.5 C52 H44 Cl4 P4 Pt2 x 5.5 C3 H7 N O'
_chemical_formula_sum            'C94.5 H104.5 Cl6 N5.5 O5.5 P6 Pt3 Se2'
_chemical_formula_weight         2547.12
_chemical_name_systematic        '[Pt2Cl4(2,3-trans-dppcbSe2-P,P',Se,Se')]'
_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-97
_cell_angle_alpha                68.799(2)
_cell_angle_beta                 80.929(2)
_cell_angle_gamma                87.253(2)
_cell_formula_units_Z            2
_cell_length_a                   14.9398(5)
_cell_length_b                   18.8634(6)
_cell_length_c                   19.2668(6)
_cell_measurement_reflns_used    117578
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      21.491
_cell_measurement_theta_min      0.998
_cell_volume                     4998.6(3)
_computing_cell_refinement       'Denzo and Scalepack'
_computing_data_collection       'Kappa CCD'
_computing_data_reduction        'Denzo and Scalepack'
_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      223(2)
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       'phi- and 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  0.025
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20732
_diffrn_reflns_theta_full        21.54
_diffrn_reflns_theta_max         21.54
_diffrn_reflns_theta_min         0.998
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.215
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   Sortav
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.690
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1145
_refine_ls_number_reflns         10537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+22.3382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                7403
_reflns_number_total             10537
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            b305775e.txt
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7013231
_diffrn_measured_fraction        0.990