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_4074512
_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         'C26 H34 Cl2 O4 P2 Pd, C H Cl3'
_chemical_formula_sum            'C27 H35 Cl5 O4 P2 Pd'
_chemical_formula_weight         769.14
_chemical_name_systematic
; 
 ? 
;
_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                90.783(9)
_cell_angle_beta                 104.471(8)
_cell_angle_gamma                109.036(9)
_cell_formula_units_Z            2
_cell_length_a                   8.844(3)
_cell_length_b                   11.587(5)
_cell_length_c                   17.470(7)
_cell_measurement_reflns_used    9148
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.541
_cell_measurement_theta_min      2.416
_cell_volume                     1629.8(11)
_computing_cell_refinement       'Bruker SMART V5.054 (Bruker, 1998)'
_computing_data_collection       'Bruker SMART V5.054 (Bruker, 1998)'
_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      173(2)
_diffrn_detector_area_resol_mean 8.2
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17320
_diffrn_reflns_theta_full        27.69
_diffrn_reflns_theta_max         27.69
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_T_max  0.800000
_exptl_absorpt_correction_T_min  0.681716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.1'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.147
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         7465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0442P)^2^+0.8806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                6207
_reflns_number_total             7465
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060716osi20060807_013850.cif
_cod_data_source_block           9c_dld194sad
_cod_database_code               4074512