<i>cis</i>-[1,4-Bis(diphenylphosphino)butane](μ-tetrathiotungstato)palladium(II) <i>N</i>,<i>N</i>'-dimethylformamide hemisolvate hemihydrate
Liang, Kai; Li, Yi-Zhi; Zheng, He-Gen; Xin, Xin-Quan; Acta Crystallographica Section C 59 (2003) m310–m312; doi:10.1107/S0108270103013507

data_2013443
_publ_section_title
;<i>cis</i>-[1,4-Bis(diphenylphosphino)butane](\m-tetrathiotungstato)palladium(II)
 <i>N</i>,<i>N</i>'-dimethylformamide hemisolvate hemihydrate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m310
_journal_page_last               m312
_journal_paper_doi               10.1107/S0108270103013507
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac
'[Pd W S4 (C28 H28 P2)], 0.5C3 H7 N1 O1, 0.5H2 O'
_chemical_formula_moiety         'C28 H28 P2 Pd S4 W, 0.5C3 H7 N1 O1, 0.5H2 O'
_chemical_formula_sum            'C29.5 H32.5 N0.5 O P2 Pd S4 W'
_chemical_formula_weight         890.49
_chemical_name_systematic
;
Cis-{[1,4-(diphenylphosphine-P,P')butane]
[\m-(tetrathiotungstate-S,S')]}Pd(II)0.5N,N'-dimethylformamide 0.5hydrate
;
_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                 98.440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1780(10)
_cell_length_b                   19.566(2)
_cell_length_c                   19.705(2)
_cell_measurement_reflns_used    878
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.50
_cell_measurement_theta_min      2.33
_cell_volume                     3500.2(6)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17162
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.149
_exptl_absorpt_correction_T_max  0.436
_exptl_absorpt_correction_T_min  0.385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.683
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0377
_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^)+(0.06P)^2^+1.99P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                4371
_reflns_number_total             6153
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ga1018.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C29.50 H32.50 N0.50 O P2 Pd S4 W'
_cod_database_code               2013443
_cod_database_fobs_code          2013443