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_4074508
_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 O4 P2'
_chemical_formula_sum            'C30 H50 O4 P2'
_chemical_formula_weight         536.64
_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                100.44(3)
_cell_angle_beta                 94.37(3)
_cell_angle_gamma                115.06(3)
_cell_formula_units_Z            2
_cell_length_a                   11.359(2)
_cell_length_b                   11.784(2)
_cell_length_c                   12.843(3)
_cell_measurement_reflns_used    5651
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.482
_cell_measurement_theta_min      2.364
_cell_volume                     1508.7(7)
_computing_cell_refinement       'Bruker SMART V5.628 (Bruker, 2005)'
_computing_data_collection       'Bruker SMART V5.628 (Bruker, 2005)'
_computing_data_reduction        'Bruker SAINT V6.41 (Bruker, 2002)'
_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      100(2)
_diffrn_detector_area_resol_mean 8.5
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17343
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.176
_exptl_absorpt_correction_T_max  0.980000
_exptl_absorpt_correction_T_min  0.924230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Bruker AXS, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         6908
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0447P)^2^+0.7627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1023
_reflns_number_gt                6076
_reflns_number_total             6908
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060716osi20060807_013727.cif
_cod_data_source_block           3b_dld267sad
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4074508