Stereospecific Diphosphination of Activated Acetylenes: A General Route to Backbone-Functionalized, Chelating 1,2-Diphosphinoethenes
Dodds, Deborah L.; Haddow, Mairi F.; Orpen, A. Guy; Pringle, Paul G.; Woodward, Gary; Organometallics 25 (2006) 5937–; doi:10.1021/om060716o

data_4074509
_publ_section_title
;
 Stereospecific Diphosphination of Activated Acetylenes:&#x00A0; A General
 Route to Backbone-Functionalized, Chelating 1,2-Diphosphinoethenes
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5937
_journal_paper_doi               10.1021/om060716o
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C30 H50 Cl2 O4 P2 Pt, C H Cl3'
_chemical_formula_sum            'C31 H51 Cl5 O4 P2 Pt'
_chemical_formula_weight         922.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 94.133(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2422(10)
_cell_length_b                   19.2312(19)
_cell_length_c                   14.6945(11)
_cell_measurement_reflns_used    16143
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.453
_cell_measurement_theta_min      2.262
_cell_volume                     3732.4(5)
_computing_cell_refinement       'Bruker SMART V5.625 (Bruker, 2001)'
_computing_data_collection       'Bruker SMART V5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT V6.02 (Bruker, 1999)'
_computing_molecular_graphics    'Bruker SHELXTL V6.14 (Bruker AXS, 2003)'
_computing_publication_material  'Bruker SHELXTL V6.14 (Bruker AXS, 2003)'
_computing_structure_refinement  'SHELXL V6.12 (Bruker 2001)'
_computing_structure_solution    'SHELXS V6.12 (Bruker 2001)'
_diffrn_ambient_temperature      446(2)
_diffrn_detector_area_resol_mean 8.5
_diffrn_measured_fraction_theta_full 0.727
_diffrn_measured_fraction_theta_max 0.727
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0560
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24867
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.236
_exptl_absorpt_correction_T_max  0.650000
_exptl_absorpt_correction_T_min  0.331872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.167
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         6245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0165P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0678
_reflns_number_gt                4672
_reflns_number_total             6245
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060716osi20060807_013747.cif
_cod_data_source_block           8b_robinsonsad
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4074509