7-Azaindol-1-yl(organo)silanes and Their PdCl2Complexes: Pd-Capped Tetrahedral Silicon Coordination Spheres and Paddlewheels with a Pd–Si Axis
Wahlicht, Sven; Brendler, Erica; Heine, Thomas; Zhechkov, Lyuben; Wagler, Jörg; Organometallics 33 (2014) 2479–; doi:10.1021/om401220m

data_4083213
_publ_section_title
;
 7-Azaindol-1-yl(organo)silanes and Their PdCl2Complexes: Pd-Capped
 Tetrahedral Silicon Coordination Spheres and Paddlewheels with a Pd--Si
 Axis
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2479
_journal_paper_doi               10.1021/om401220m
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         '2(C28 H20 Cl2 N8 Pd Si), 3(C H Cl3)'
_chemical_formula_sum            'C59 H43 Cl13 N16 Pd2 Si2'
_chemical_formula_weight         1705.92
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.086(5)
_cell_angle_beta                 79.007(5)
_cell_angle_gamma                63.664(4)
_cell_formula_units_Z            1
_cell_length_a                   9.0791(6)
_cell_length_b                   10.3656(6)
_cell_length_c                   19.8345(13)
_cell_measurement_reflns_used    15630
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.43
_cell_measurement_theta_min      2.38
_cell_volume                     1639.20(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS-2T'
_diffrn_measurement_method       '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  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18337
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    1.170
_exptl_absorpt_correction_T_max  0.9643
_exptl_absorpt_correction_T_min  0.8365
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XShape
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             850
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.664
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.268
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         7150
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.256
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0744
_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^)+(0.0000P)^2^+12.5365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1579
_reflns_number_gt                6119
_reflns_number_total             7150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401220m_si_002.cif
_cod_data_source_block           (paddlewheel)2(CHCl3)3
_cod_depositor_comments
'Adding full bibliography for 4083204--4083216.cif.'
_cod_original_cell_volume        1639.20(18)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4083213