<i>trans</i>-Bis(3,5-diaza-1-azonia-7-phosphaadamantane-κ<i>P</i>)bis(thiocyanato-κ<i>S</i>)palladium(II) bis(thiocyanate)
Meij, Anna M. M.; Otto, Stefanus; Roodt, Andreas; Acta Crystallographica Section C 59 (2003) m352–m354; doi:10.1107/S010827010301521X

data_2013422
_publ_section_title
;<i>trans</i>-Bis(3,5-diaza-1-azonia-7-phosphaadamantane-\k<i>P</i>)bis(thiocyanato-\k<i>S</i>)palladium(II)
 bis(thiocyanate)
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m352
_journal_page_last               m354
_journal_paper_doi               10.1107/S010827010301521X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Pd (N C S)2 (C6 H13 N3 P)2] (N C S)2'
_chemical_formula_moiety         'C14 H26 N8 P2 Pd S2 2+, 2C N S 1-'
_chemical_formula_sum            'C16 H26 N10 P2 Pd S4'
_chemical_formula_weight         655.05
_chemical_name_systematic
;
trans-bis(3,5-diaza-1-azonia-7-phosphaadamantane-
\kP)bis(thiocyanato-\kS)palladium(II) bis(thiocyanate)
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.96(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.5170(15)
_cell_length_b                   12.733(3)
_cell_length_c                   12.956(3)
_cell_measurement_reflns_used    2294
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.25
_cell_volume                     1235.4(5)
_computing_cell_refinement       Collect
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction        Collect
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       '\w and \f scans'
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6468
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_T_max  0.8254
_exptl_absorpt_correction_T_min  0.7060
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_meas      1.746
_exptl_crystal_density_method    'flotation in CH~2~I~2~/C~6~H~6~'
_exptl_crystal_description       rectangles
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.414
_refine_ls_extinction_coef       0.0021(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.000
_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^+0.7680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0569
_reflns_number_gt                2179
_reflns_number_total             2766
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa1019.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1235.4(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2013422
_cod_database_fobs_code          2013422