Diphosphination of Electron Poor Alkenes
Hajdók, Imre; Lissner, Falk; Nieger, Martin; Strobel, Sabine; Gudat, Dietrich; Organometallics 28 (2009) 1644–; doi:10.1021/om801179k

data_4068960
_publ_section_title
;
 Diphosphination of Electron Poor Alkenes
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1644
_journal_paper_doi               10.1021/om801179k
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C39.4 H43 Cl4.8 N3 O2 P2 Pd'
_chemical_formula_weight         927.00
_chemical_name_common            'C38 H43 Cl2 N3 O2 P2 Pd, 1.4 CH2Cl2'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 124.4580(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.8659(7)
_cell_length_b                   15.3565(4)
_cell_length_c                   20.4915(4)
_cell_measurement_reflns_used    204283
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      1.02
_cell_volume                     8268.1(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.1237
_diffrn_reflns_av_sigmaI/netI    0.0593
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            78598
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         3.60
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  0.9278
_exptl_absorpt_correction_T_min  0.7815
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'HABITUS, W. Herrendorf, Univ. Giessen, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3784
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.846
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.00004(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         10258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0281P)^2^+52.3894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                8329
_reflns_number_total             10258
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801179k_si_001.cif
_cod_data_source_block           c:\crystal\x-red\ihnov07
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4068960