[1,2-Bis(diphenylphosphanyl)ethane-κ^2^<i>P</i>,<i>P</i>']{2-[(4-nitrobenzoylmethyl)diphenylphosphanyl]phenyl-κ^2^<i>C</i>,<i>C</i>'}palladium(II) trifluoromethanesulfonate‒dichloromethane‒<i>n</i>-hexane (1/1/0.5)
Rizzoli, Corrado; Karami, Kazem; Borzooie, Farzaneh; Acta Crystallographica Section E 67 (2011) m416–m417; doi:10.1107/S1600536811008075

data_2229887
_publ_section_title
;
 [1,2-Bis(diphenylphosphanyl)ethane-\k^2^<i>P</i>,<i>P</i>']{2-[(4-nitrobenzoylmethyl)diphenylphosphanyl]phenyl-\k^2^<i>C</i>,<i>C</i>'}palladium(II)
 trifluoromethanesulfonate--dichloromethane--<i>n</i>-hexane (1/1/0.5)
;
_journal_coeditor_code           ZJ2004
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m416
_journal_page_last               m417
_journal_paper_doi               10.1107/S1600536811008075
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Pd (C26 H19 N O3 P) (C26 H24 P2)] C F3 O3 S, C H2 Cl2, 0.5C6 H14'
_chemical_formula_moiety
'C52 H43 N O3 P3 Pd +, C F3 O3 S -, C H2 Cl2, 0.5(C6 H14)'
_chemical_formula_sum            'C57 H52 Cl2 F3 N O6 P3 Pd S'
_chemical_formula_weight         1206.27
_chemical_name_systematic
;
[1,2-Bis(diphenylphosphanyl)ethane-\k^2^<i>P</i>,<i>P</i>']{2-[(4-
nitrobenzoylmethyl)diphenylphosphanyl]phenyl-
\k^2^<i>C</i>,<i>C</i>'}palladium(II)
trifluoromethanesulfonate--dichloromethane--<i>n</i>-hexane (1/1/0.5)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 91.6675(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4063(7)
_cell_length_b                   14.2445(8)
_cell_length_c                   31.3633(17)
_cell_measurement_reflns_used    1226
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      23.40
_cell_measurement_theta_min      6.25
_cell_volume                     5540.2(5)
_computing_cell_refinement       '<i>APEX2</i> (Bruker, 2008)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2008)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2008)'
_computing_molecular_graphics
;
<i>ORTEP-3 for Windows</i> (Farrugia, 1997) and
<i>SCHAKAL97</i> (Keller, 1997)
;
_computing_publication_material
;
<i>SHELXL97</i> (Sheldrick, 2008) and <i>PARST95</i> (Nardelli,
1995)
;
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SIR97</i> (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker APEXII CCD'
_diffrn_measurement_method       \w
_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  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            62924
_diffrn_reflns_theta_full        25.71
_diffrn_reflns_theta_max         25.71
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2468
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.382
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         10529
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0291
_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^)+(0.0380P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0761
_reflns_number_gt                8106
_reflns_number_total             10529
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zj2004.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2229887
_cod_database_fobs_code          2229887