<i>trans</i>-(6-Amino-2-pyridinio)iodobis(triphenylphosphine)palladium(II) iodide ethyl acetate solvate
Clegg, William; Horsburgh, Lynne; Acta Crystallographica Section E 59 (2003) m700–m702; doi:10.1107/S1600536803017252

data_2202352
_publ_section_title
;
 <i>trans</i>-(6-Amino-2-pyridinio)iodobis(triphenylphosphine)palladium(II)
 iodide ethyl acetate solvate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m700
_journal_page_last               m702
_journal_paper_doi               10.1107/S1600536803017252
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Pd (C5 H6 N2) (C18 H15 P}2] I, C4 H8 O2'
_chemical_formula_moiety         'C41 H36 I N2 P2 Pd 1+, I 1-, C4 H8 O2'
_chemical_formula_sum            'C45 H44 I2 N2 O2 P2 Pd'
_chemical_formula_weight         1066.96
_chemical_name_systematic
;
trans-(6-amino-2-pyridinio)iodobis(triphenylphosphine)palladium(II) iodide
ethyl acetate solvate
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0297(9)
_cell_length_b                   16.9603(10)
_cell_length_c                   17.2897(11)
_cell_measurement_reflns_used    13025
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.8
_cell_measurement_theta_min      2.2
_cell_volume                     4407.3(5)
_computing_cell_refinement       'local programs'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker SMART 1K CCD'
_diffrn_measurement_method       'narrow-frame \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14181
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.80
_diffrn_reflns_theta_min         1.81
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.932
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.280
_refine_diff_density_min         -0.705
_refine_ls_abs_structure_details 'Flack (1983); 2220 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.005(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         5016
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0393P)^2^+0.905P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                4828
_reflns_number_total             5016
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6322.cif
_cod_data_source_block           I
_cod_database_code               2202352
_cod_database_fobs_code          2202352