#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:16:52 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179835 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/31/7013183.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7013183
loop_
_publ_author_name
'Kim, Yong-Joo'
'Han, Jin-Taek'
'Kang, Seok'
'Han, Won Seok'
'Lee, Soon W.'
_publ_section_title
;
 Reactivity of di(azido)bis(phosphine) complexes of Ni(ii), Pd(ii) and
 Pt(ii) toward organic isothiocyanates: synthesis, structures, and
 properties of bis(tetrazole-thiolato) and bis(isothiocyanato)
 complexes
;
_journal_issue                   17
_journal_name_full               'Dalton Transactions'
_journal_page_first              3357
_journal_paper_doi               10.1039/b305341p
_journal_year                    2003
_chemical_formula_sum            'C20 H28 N8 P2 Pd S2'
_chemical_formula_weight         612.96
_chemical_name_systematic
;
?
;
_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                 100.531(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.1906(14)
_cell_length_b                   17.205(3)
_cell_length_c                   12.664(2)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.55
_cell_measurement_theta_min      7.30
_cell_volume                     1326.1(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω 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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2545
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.02
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  0.4770
_exptl_absorpt_correction_T_min  0.4630
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0264
_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/[σ²(Fo²)+(0.0222P)²+0.9816P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0675
_reflns_number_gt                2032
_reflns_number_total             2320
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305341p.txt
_cod_data_source_block           abspd
_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 
;
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               7013183
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.0000 0.0000 0.5000 0.03171(10) Uani 1 2 d S . .
S1 S 0.15170(14) -0.01511(4) 0.68077(6) 0.04803(19) Uani 1 1 d . . .
P1 P 0.16872(12) -0.11118(4) 0.44738(6) 0.03988(17) Uani 1 1 d . . .
N1 N -0.1214(4) -0.14169(15) 0.6675(2) 0.0531(6) Uani 1 1 d . . .
N2 N -0.1359(5) -0.20618(17) 0.7282(3) 0.0651(8) Uani 1 1 d . . .
N3 N 0.0180(5) -0.20772(15) 0.8117(2) 0.0605(7) Uani 1 1 d . . .
N4 N 0.1410(4) -0.14264(13) 0.80702(19) 0.0443(6) Uani 1 1 d . . .
C1 C 0.3206(6) -0.1770(2) 0.5450(3) 0.0745(11) Uani 1 1 d . . .
H1A H 0.2267 -0.1954 0.5922 0.089 Uiso 1 1 calc R . .
H1B H 0.4441 -0.1503 0.5861 0.089 Uiso 1 1 calc R . .
H1C H 0.3715 -0.2204 0.5086 0.089 Uiso 1 1 calc R . .
C2 C -0.0178(6) -0.17569(18) 0.3642(3) 0.0696(10) Uani 1 1 d . . .
H2A H -0.1314 -0.1915 0.4020 0.083 Uiso 1 1 calc R . .
H2B H 0.0608 -0.2206 0.3468 0.083 Uiso 1 1 calc R . .
H2C H -0.0824 -0.1494 0.2992 0.083 Uiso 1 1 calc R . .
C3 C 0.3739(8) -0.0850(2) 0.3699(4) 0.0941(15) Uani 1 1 d . . .
H3A H 0.4784 -0.0504 0.4110 0.113 Uiso 1 1 calc R . .
H3B H 0.3049 -0.0597 0.3049 0.113 Uiso 1 1 calc R . .
H3C H 0.4479 -0.1310 0.3526 0.113 Uiso 1 1 calc R . .
C4 C 0.0524(5) -0.10245(16) 0.7173(2) 0.0409(6) Uani 1 1 d . . .
C5 C 0.3277(5) -0.12621(16) 0.8897(2) 0.0468(7) Uani 1 1 d . . .
C6 C 0.3129(7) -0.1415(2) 0.9960(3) 0.0679(10) Uani 1 1 d . . .
H10 H 0.1852 -0.1617 1.0140 0.081 Uiso 1 1 calc R . .
C7 C 0.4962(9) -0.1253(3) 1.0745(3) 0.0851(14) Uani 1 1 d . . .
H9 H 0.4912 -0.1357 1.1461 0.102 Uiso 1 1 calc R . .
C8 C 0.6850(8) -0.0941(3) 1.0484(3) 0.0831(13) Uani 1 1 d . . .
H8 H 0.8047 -0.0829 1.1021 0.100 Uiso 1 1 calc R . .
C9 C 0.6953(6) -0.0799(2) 0.9444(3) 0.0679(10) Uani 1 1 d . . .
H7 H 0.8224 -0.0586 0.9270 0.082 Uiso 1 1 calc R . .
C10 C 0.5184(6) -0.09670(19) 0.8636(3) 0.0560(8) Uani 1 1 d . . .
H6 H 0.5282 -0.0881 0.7921 0.067 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Pd1 S1 180.0 3_556 . ?
S1 Pd1 P1 86.09(3) 3_556 . ?
S1 Pd1 P1 93.91(3) . . ?
S1 Pd1 P1 93.91(3) 3_556 3_556 ?
S1 Pd1 P1 86.09(3) . 3_556 ?
P1 Pd1 P1 180.00(3) . 3_556 ?
C4 S1 Pd1 105.25(10) . . ?
C2 P1 C3 106.1(2) . . ?
C2 P1 C1 102.23(18) . . ?
C3 P1 C1 101.5(2) . . ?
C2 P1 Pd1 113.61(12) . . ?
C3 P1 Pd1 110.38(14) . . ?
C1 P1 Pd1 121.47(12) . . ?
C4 N1 N2 106.1(3) . . ?
N3 N2 N1 111.4(3) . . ?
N2 N3 N4 106.4(2) . . ?
C4 N4 N3 108.2(2) . . ?
C4 N4 C5 131.1(2) . . ?
N3 N4 C5 120.7(2) . . ?
N1 C4 N4 107.9(2) . . ?
N1 C4 S1 128.0(2) . . ?
N4 C4 S1 124.1(2) . . ?
C10 C5 C6 120.8(3) . . ?
C10 C5 N4 120.4(3) . . ?
C6 C5 N4 118.7(3) . . ?
C5 C6 C7 117.7(4) . . ?
C8 C7 C6 121.4(4) . . ?
C9 C8 C7 119.8(4) . . ?
C8 C9 C10 120.7(4) . . ?
C5 C10 C9 119.6(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 S1 2.3248(8) 3_556 ?
Pd1 S1 2.3248(8) . ?
Pd1 P1 2.3341(8) . ?
Pd1 P1 2.3341(8) 3_556 ?
S1 C4 1.719(3) . ?
P1 C2 1.797(3) . ?
P1 C3 1.798(4) . ?
P1 C1 1.809(3) . ?
N1 C4 1.328(4) . ?
N1 N2 1.362(4) . ?
N2 N3 1.288(4) . ?
N3 N4 1.361(3) . ?
N4 C4 1.357(4) . ?
N4 C5 1.439(4) . ?
C5 C10 1.379(5) . ?
C5 C6 1.390(4) . ?
C6 C7 1.394(6) . ?
C7 C8 1.380(6) . ?
C8 C9 1.352(5) . ?
C9 C10 1.387(5) . ?
