[2,2'-Bis(diphenylphosphanyl)-1,1'-binaphthyl-κ^2^<i>P</i>,<i>P</i>']chlorido(4-methylphenylsulfonyl-κ<i>S</i>)palladium(II) dichloromethane trisolvate monohydrate
Shrestha, Ruja; Brennessel, William W.; Weix, Daniel J.; Acta Crystallographica Section E 67 (2011) m1830–; doi:10.1107/S1600536811049889

data_2232572
_publ_section_title
;
 [2,2'-Bis(diphenylphosphanyl)-1,1'-binaphthyl-\k^2^<i>P</i>,<i>P</i>']chlorido(4-methylphenylsulfonyl-\k<i>S</i>)palladium(II)
 dichloromethane trisolvate monohydrate
;
_journal_coeditor_code           BR2184
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1830
_journal_paper_doi               10.1107/S1600536811049889
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Pd (C7 H7 O2 S) Cl (C44 H32 P2)], 3C H2 Cl2, H2 O'
_chemical_formula_moiety         'C51 H39 Cl O2 P2 Pd S, 3(C H2 Cl2), H2 O'
_chemical_formula_sum            'C54 H47 Cl7 O3 P2 Pd S'
_chemical_formula_weight         1192.47
_chemical_name_common            weixrs01
_chemical_name_systematic
;
[2,2'-Bis(diphenylphosphanyl)-1,1'-binaphthyl-\k^2^<i>P</i>,<i>P</i>']
chlorido(4-methylphenylsulfonyl-\k<i>S</i>)palladium(II) dichloromethane
trisolvate monohydrate
;
_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                101.808(2)
_cell_angle_beta                 101.339(2)
_cell_angle_gamma                109.743(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7273(12)
_cell_length_b                   13.7474(13)
_cell_length_c                   16.533(3)
_cell_measurement_reflns_used    9765
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      37.97
_cell_measurement_theta_min      2.32
_cell_volume                     2551.8(6)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       'area detector, \w scans at different \f'
_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  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0705
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55527
_diffrn_reflns_theta_full        34.97
_diffrn_reflns_theta_max         34.97
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  0.9492
_exptl_absorpt_correction_T_min  0.7544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.124
_refine_diff_density_min         -1.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         22145
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0590P)^2^+0.5385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1277
_reflns_number_gt                15533
_reflns_number_total             22145
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br2184.cif
_cod_data_source_block           I
_cod_original_cell_volume        2551.8(5)
_cod_database_code               2232572
_cod_database_fobs_code          2232572