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

data_4068962
_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_moiety         'C34 H44 Cl2 N2 O4 P2 Pd, 1.5(C3 H7 N O)'
_chemical_formula_sum            'C38.5 H54.5 Cl2 N3.5 O5.5 P2 Pd'
_chemical_formula_weight         893.60
_chemical_name_systematic
; 
 [Dimethyl 2-(1,3-dineopentyl-1,2-dihydro-benzo[c][1,3,2]diazaphosphol-2-yl)-
 3-(diphenylphosphino)succinate dichloro palladium(II)
;
_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                 94.36(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.899(2)
_cell_length_b                   14.033(1)
_cell_length_c                   25.170(2)
_cell_measurement_reflns_used    157
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     8417.0(11)
_computing_cell_refinement       'DIRAX (Duisenberg, 1992)'
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction        'EVALCCD (Duisenberg et al, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 1 deg.'
_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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            54901
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.7485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             3712
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.410
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         7421
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0702
_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^)+(0.0000P)^2^+350.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1699
_refine_ls_wR_factor_ref         0.1706
_reflns_number_gt                7156
_reflns_number_total             7421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801179k_si_003.cif
_cod_data_source_block           dg030_hy_compound_11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C38.50 H54.50 Cl2 N3.50 O5.50 P2 Pd'
_cod_database_code               4068962