Dichlorido(4,7-diaza-1-azoniacyclononane-κ^2^<i>N</i>^4^,<i>N</i>^7^)palladium(II) <i>p</i>-toluenesulfonate
Anthony, Timothy A.; Arman, Hadi D.; Walmsley, Judith A.; Acta Crystallographica Section E 66 (2010) m638–m639; doi:10.1107/S1600536810016533

data_2226305
_publ_section_title
;
 Dichlorido(4,7-diaza-1-azoniacyclononane-\k^2^<i>N</i>^4^,<i>N</i>^7^)palladium(II)
 <i>p</i>-toluenesulfonate
;
_journal_coeditor_code           TK2666
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m638
_journal_page_last               m639
_journal_paper_doi               10.1107/S1600536810016533
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Pd Cl2 (C6 H16 N3)] (C7 H7 O3 S)'
_chemical_formula_moiety         'C6 H16 Cl2 N3 Pd +, C7 H7 O3 S -'
_chemical_formula_sum            'C13 H23 Cl2 N3 O3 Pd S'
_chemical_formula_weight         478.70
_chemical_name_systematic
;
Dichlorido(4,7-diaza-1-azoniacyclononane-
\k^2^<i>N</i>^4^,<i>N</i>^7^)palladium(II)
<i>p</i>-toluenesulfonate
;
_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                92.149(3)
_cell_angle_beta                 92.301(3)
_cell_angle_gamma                103.084(4)
_cell_formula_units_Z            2
_cell_length_a                   6.6663(11)
_cell_length_b                   7.0023(11)
_cell_length_c                   19.646(3)
_cell_measurement_reflns_used    4441
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      40.2243
_cell_measurement_theta_min      2.9900
_cell_volume                     891.5(2)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2005)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  '<i>publCIF</i> (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      98(2)
_diffrn_detector_area_resol_mean 14.286
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Rigaku AFC12 Kappa goniometer'
_diffrn_measurement_method       \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  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6224
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.99
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.473
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.977
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0070P)^2^+4.1000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0665
_reflns_number_gt                3941
_reflns_number_total             3998
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            tk2666.cif
_cod_data_source_block           I
_cod_database_code               2226305
_cod_database_fobs_code          2226305