Reversible Ligand Pairing and Sorting Processes Leading to Heteroligated Palladium(II) Complexes with Hemilabile Ligands
Ulmann, Pirmin A.; Mirkin, Chad A.; DiPasquale, Antonio G.; Liable-Sands, Louise M.; Rheingold, Arnold L.; Organometallics 28 (2009) 1068–; doi:10.1021/om801060m

data_4068735
_publ_section_title
;
 Reversible Ligand Pairing and Sorting Processes Leading to Heteroligated
 Palladium(II) Complexes with Hemilabile Ligands
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1068
_journal_paper_doi               10.1021/om801060m
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C36 H38 B2 Cl2 F8 P2 Pd S2'
_chemical_formula_weight         947.64
_chemical_name_systematic
; 

 [k2-(Ph2PCH2CH2SMe)-k2-(Ph2PCH2CH2SPh)Pd](BF4)2 

;
_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                 115.2870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   37.697(4)
_cell_length_b                   13.4866(12)
_cell_length_c                   17.6277(17)
_cell_measurement_reflns_used    9202
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      20.84
_cell_measurement_theta_min      2.31
_cell_volume                     8103.3(14)
_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      208(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16887
_diffrn_reflns_theta_full        20.84
_diffrn_reflns_theta_max         20.84
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_T_max  0.9362
_exptl_absorpt_correction_T_min  0.8375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             3824
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_platon_squeeze_details
; 

 SQUEEZE (PLATON, A.Spek) was used to treat diffuse solvent 

 contributions.  Total electron count found = 632/unit cell.  Calculated 

 for 8 BF4- (one of two counterions) and 8 CH2Cl2 (the re'xtal solvent) 

 = 656/unit cell.  The intensive properties (density, F(000), etc.) 

 reflect these contributions.

;
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         4239
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                3662
_reflns_number_total             4239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801060m_si_002.cif
_cod_data_source_block           complex12
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        8103.3(13)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4068735