Palladium Complexes Bearing Novel Strongly Bent Trans-Spanning Diphosphine Ligands: Synthesis, Characterization, and Catalytic Activity
Olga Grossman; Clarit Azerraf; Dmitri Gelman; Organometallics 25 (2006) 375–381; doi:10.1021/om050906j

data_4063286
_publ_section_title
;
 Palladium Complexes Bearing Novel Strongly Bent Trans-Spanning
 Diphosphine Ligands: Synthesis, Characterization, and Catalytic
 Activity
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              375
_journal_page_last               381
_journal_paper_doi               10.1021/om050906j
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C32 H40 Cl4 P2 Pd2, 3(C H Cl3)'
_chemical_formula_sum            'C35 H43 Cl13 P2 Pd2'
_chemical_formula_weight         1199.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 106.9380(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3648(9)
_cell_length_b                   22.1329(12)
_cell_length_c                   14.2719(8)
_cell_measurement_reflns_used    6734
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.92
_cell_measurement_theta_min      2.30
_cell_volume                     4642.9(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0549
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            52101
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    1.618
_exptl_absorpt_correction_T_max  0.8814
_exptl_absorpt_correction_T_min  0.6339
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'Face-Indexed Absorption Correction, Bruker-XPREP'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.111
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         10150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                7668
_reflns_number_total             10150
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4063286