Ligand-Dependent Selective Formation of Unique Silylpalladium Complexes by the Reaction of 1-(Dimethylsilyl)-2-silylbenzene and [{1,2-C6H4(SiMe2)(SiH2)}Pd(R2PCH2CH2PR2)]
Li, Yong-Hua; Shimada, Shigeru; Organometallics 29 (2010) 4406–; doi:10.1021/om100626k

data_4066784
_publ_section_title
;
 Ligand-Dependent Selective Formation of Unique Silylpalladium Complexes
 by the Reaction of 1-(Dimethylsilyl)-2-silylbenzene and
 [{1,2-C6H4(SiMe2)(SiH2)}Pd(R2PCH2CH2PR2)]
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4406
_journal_paper_doi               10.1021/om100626k
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C26 H46 P2 Pd Si4 '
_chemical_formula_sum            'C26 H46 P2 Pd Si4'
_chemical_formula_weight         639.34
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-05-16
_audit_creation_method           'by CrystalStructure 3.8'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.7495(9)
_cell_length_b                   18.0326(10)
_cell_length_c                   11.3822(7)
_cell_measurement_reflns_used    85480
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      2.5
_cell_volume                     3232.6(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean '8.366 [pixels/mm]'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18806
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.27
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  0.8575
_exptl_absorpt_correction_T_min  0.8442
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS; Sheldrick 1996
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1336.00
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.86
_refine_diff_density_min         -0.45
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2676 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.003(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     307
_refine_ls_number_reflns         6527
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.0020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0120P)^2^+3.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0589
_reflns_number_gt                6308
_reflns_number_total             6527
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om100626k_si_001.cif
_cod_data_source_block           complex-7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom & difmap' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_formula_sum        'C26 H46 P2 Pd Si4 '
_cod_database_code               4066784