Chiral Palladium(II)−Bis(trichlorosilyl) Complexes. Synthesis, Structure, and Combined QM/MM Computational Studies
Woo, Tom K.; Pioda, Giorgio; Rothlisberger, Ursula; Togni, Antonio; Organometallics 19 (2000) 2144–; doi:10.1021/om000130g

data_4077495
_publ_section_title
;
 Chiral Palladium(II)&#x2212;Bis(trichlorosilyl) Complexes. Synthesis,
 Structure, and Combined QM/MM Computational Studies
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2144
_journal_paper_doi               10.1021/om000130g
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C35 H33 Cl8 Fe N2 P Pd Si2'
_chemical_formula_weight         1014.63
_chemical_name_systematic
;
Bis(trichlorosilyl)-{1-{(R)-1-[(S)-2-(diphenylphosphino-kP)ferrocenyl]ethyl}-
3-phenyl-5-methyl-1H-pyrazole-kN}palladium (5)
;
_space_group_IT_number           145
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_atom_sites_solution_hydrogens   'ref U'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   17.966(12)
_cell_length_b                   17.966(12)
_cell_length_c                   10.785(7)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      1.31
_cell_volume                     3015(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Siemens SMART Platform (CCD detector)'
_diffrn_measurement_method       w-scan
_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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22036
_diffrn_reflns_theta_full        29.94
_diffrn_reflns_theta_max         29.94
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    1.469
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_meas      '? '
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1524
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.029(19)
_refine_ls_extinction_coef       0.0024(3)
_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   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         10037
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.608
_refine_ls_shift/su_mean         0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+2.8890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                9051
_reflns_number_total             10037
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000130g.cif
_cod_data_source_block           '[PPFPy(Me,Ph)Pd(SiCl3)2]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
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_sg_symbol_H-M      P32
_cod_database_code               4077495