<i>trans</i>-Dichlorobis(10-dodecyl-9-phospha-10-silatriptycene-κ<i>P</i>)palladium(II)
Hayato Tsuji; Tomoyuki Inoue; Shohei Sase; Kohei Tamao; Acta Crystallographica Section E 62 (2006) m535–m537; doi:10.1107/S1600536806004958

data_2208390
_publ_section_title
<i>trans</i>-Dichlorobis(10-dodecyl-9-phospha-10-silatriptycene-\k<i>P</i>)palladium(II)
_journal_coeditor_code           NG2002
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m535
_journal_page_last               m537
_journal_paper_doi               10.1107/S1600536806004958
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Pd Cl2 (C30 H37 P Si)2]'
_chemical_formula_moiety         'C60 H74 Cl2 P2 Pd Si2'
_chemical_formula_sum            'C60 H74 Cl2 P2 Pd Si2'
_chemical_formula_weight         1090.61
_chemical_melting_point          .505E-305
_chemical_name_systematic
;
trans-Dichlorobis(10-dodecyl-9-phospha-10-silatriptycene-\kP)palladium(II)
;
_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
_cell_angle_alpha                106.403(10)
_cell_angle_beta                 92.296(10)
_cell_angle_gamma                102.087(9)
_cell_formula_units_Z            1
_cell_length_a                   9.253(6)
_cell_length_b                   10.897(7)
_cell_length_c                   14.311(9)
_cell_measurement_reflns_used    3738
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      3.06
_cell_volume                     1346.0(15)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2004)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL97 and Yadokari-XG (Wakita, 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Saturn70 CCD (4 \\times 4 bin mode)'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14206
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_T_max  0.9713
_exptl_absorpt_correction_T_min  0.8917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.280
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+0.108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0797
_reflns_number_gt                4405
_reflns_number_total             4993
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng2002.cif
_cod_data_source_block           I
_cod_database_code               2208390
_cod_database_fobs_code          2208390