(4-<i>tert</i>-Butyl-2-methylthiosemicarbazido)(<i>O</i>-methyldithiophosphato)palladium(II)
Janča, Michal; Taraba, Jan; Příhoda, Jiří; Acta Crystallographica Section E 58 (2002) m245–m247; doi:10.1107/S1600536802007237

data_2201114
_publ_section_title
(4-<i>tert</i>-Butyl-2-methylthiosemicarbazido)(<i>O</i>-methyldithiophosphato)palladium(II)
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m245
_journal_page_last               m247
_journal_paper_doi               10.1107/S1600536802007237
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Pd (C6 H14 N3 O1 S2) (C1 H3 O1 P1 S1)]'
_chemical_formula_moiety         'C7 H17 N3 O2 P S3 Pd'
_chemical_formula_sum            'C7 H17 N3 O2 P Pd S3'
_chemical_formula_weight         408.79
_chemical_name_systematic
(4-tert-butyl-2-methylthiosemicarbazido)(O-methyldithiophosphato)palladium(II)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 105.23(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.889(3)
_cell_length_b                   10.854(2)
_cell_length_c                   11.120(2)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.84
_cell_measurement_theta_min      11.01
_cell_volume                     1501.0(6)
_computing_cell_refinement       'KM-4 Software'
_computing_data_collection       'KM-4 Software (Kuma, 1997)'
_computing_data_reduction        'KM-4 Software'
_computing_molecular_graphics    'XP in SHELXTL'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type
;
Kuma KM-4 CCD diffractometer with a CCD camera and an Oxford Cryosystems
low-temperature device
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_sigmaI/netI    0.0738
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9041
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.38
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.754
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.184
_refine_diff_density_min         -1.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2636
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0398P)^2^+3.35P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1104
_reflns_number_gt                2249
_reflns_number_total             2636
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv6108.cif
_cod_data_source_block           2
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0398P)^2^+3.35P] where P = (Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0398P)^2^+3.35P] where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1501.0(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2201114
_cod_database_fobs_code          2201114