<i>cyclo</i>-Tetrakis(μ~2~-<small>D</small>-penicillaminato-κ^4^<i>N</i>,<i>S</i>:<i>O</i>,<i>S</i>)tetrapalladium(II) 9.75-hydrate
Yokoi, Anzu; Yoshinari, Nobuto; Konno, Takumi; Acta Crystallographica Section E 69 (2013) m288–m289; doi:10.1107/S160053681301088X

data_2237906
_publ_section_title
;
 <i>cyclo</i>-Tetrakis(\m~2~-<small>D</small>-penicillaminato-\k^4^<i>N</i>,<i>S</i>:<i>O</i>,<i>S</i>)tetrapalladium(II)
 9.75-hydrate
;
_journal_coeditor_code           IS5266
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m288
_journal_page_last               m289
_journal_paper_doi               10.1107/S160053681301088X
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Pd4 (C5 H9 N O2 S)4], 9.75H2 O'
_chemical_formula_moiety         'C20 H36 N4 O8 Pd4 S4, 9.75(H2 O)'
_chemical_formula_sum            'C20 H55.5 N4 O17.75 Pd4 S4'
_chemical_formula_weight         1190.025
_chemical_name_systematic
'<i>cyclo</i>-Tetrakis(\m~2~-<i>D</i>-penicillaminato-\k^4^<i>N</i>,<i>S</i>:<i>O</i>,<i>S</i>)tetrapalladium(II) 9.75-hydrate'
_space_group_IT_number           1
_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                113.527(8)
_cell_angle_beta                 98.425(7)
_cell_angle_gamma                108.557(8)
_cell_formula_units_Z            2
_cell_length_a                   12.4517(3)
_cell_length_b                   13.2680(4)
_cell_length_c                   15.1666(11)
_cell_measurement_reflns_used    20017
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.05
_cell_volume                     2067.3(3)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 2000)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 2000)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 2000)'
_computing_molecular_graphics
'<i>Yadokari-XG 2009</i> (Kabuto <i>et al.</i>, 2009)'
_computing_publication_material
'<i>Yadokari-XG 2009</i> (Kabuto <i>et al.</i>, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20447
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    1.982
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1187
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.519
_refine_diff_density_min         -0.682
_refine_ls_abs_structure_details 'Flack (1983), 6026 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.024(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1052
_refine_ls_number_reflns         15410
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0317P)^2^+0.9989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0621
_reflns_number_gt                15064
_reflns_number_total             15410
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            is5266.cif
_cod_data_source_block           I
_cod_database_code               2237906
_cod_database_fobs_code          2237906