#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:28:31 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180507 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/76/7217683.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_7217683
loop_
_publ_author_name
'Gupta, Ajit N.'
'Kumar, Vinod'
'Singh, Vikram'
'Manar, Krishna K.'
'Drew, Michael G. B.'
'Singh, Nanhai'
_publ_section_title
;
 Intermolecular anagostic interactions in group 10 metal dithiocarbamates
;
_journal_issue                   39
_journal_name_full               CrystEngComm
_journal_page_first              9299
_journal_paper_doi               10.1039/C4CE01263A
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C28 H26 N4 Pd S4'
_chemical_formula_weight         653.17
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_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                75.41(8)
_cell_angle_beta                 80.37(8)
_cell_angle_gamma                72.19(8)
_cell_formula_units_Z            1
_cell_length_a                   6.503(6)
_cell_length_b                   10.171(9)
_cell_length_c                   11.709(10)
_cell_measurement_reflns_used    5245
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.09
_cell_volume                     710.1(12)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_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  0.1473
_diffrn_reflns_av_sigmaI/netI    0.1823
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5245
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.924
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.266
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0775
_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/[σ²(Fo²)+(0.0686P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.2144
_reflns_number_gt                1479
_reflns_number_total             3100
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce01263a2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7217680--7217684.cif.'
_cod_original_cell_volume        710.2(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7217683
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
S11 S -0.1576(3) 0.0289(2) -0.17339(18) 0.0561(6) Uani 1 1 d . . .
S13 S -0.1844(3) -0.1735(2) 0.04480(17) 0.0553(6) Uani 1 1 d . . .
Pd1 Pd 0.0000 0.0000 0.0000 0.0510(3) Uani 1 2 d S . .
C12 C -0.2685(11) -0.1054(8) -0.0978(6) 0.0463(17) Uani 1 1 d . . .
N14 N -0.3997(10) -0.1533(7) -0.1401(5) 0.0508(15) Uani 1 1 d . . .
C21 C -0.4881(13) -0.0753(9) -0.2567(7) 0.059(2) Uani 1 1 d . . .
H21A H -0.4674 0.0186 -0.2762 0.071 Uiso 1 1 calc R . .
H21B H -0.6429 -0.0648 -0.2485 0.071 Uiso 1 1 calc R . .
C22 C -0.3799(12) -0.1503(9) -0.3590(6) 0.0533(19) Uani 1 1 d . B .
C23 C -0.5033(15) -0.1752(11) -0.4305(7) 0.074(3) Uani 1 1 d . . .
H23 H -0.6533 -0.1490 -0.4132 0.088 Uiso 1 1 calc R A 1
C24 C -0.4206(18) -0.2362(12) -0.5258(8) 0.099(4) Uani 0.28(7) 1 d P B 1
H24 H -0.5112 -0.2544 -0.5699 0.119 Uiso 0.28(7) 1 calc PR B 1
N24 N -0.4206(18) -0.2362(12) -0.5258(8) 0.099(4) Uani 0.72(7) 1 d P B 2
C25 C -0.206(2) -0.2689(16) -0.5539(10) 0.120(5) Uani 1 1 d . . .
H25 H -0.1463 -0.3106 -0.6185 0.145 Uiso 1 1 calc R B 1
C26 C -0.0715(18) -0.2412(16) -0.4871(10) 0.115(5) Uani 1 1 d . B .
H26 H 0.0777 -0.2635 -0.5078 0.138 Uiso 1 1 calc R . .
C27 C -0.1581(16) -0.1817(13) -0.3921(8) 0.089(3) Uani 1 1 d . . .
H27 H -0.0680 -0.1618 -0.3488 0.107 Uiso 1 1 calc R B .
C31 C -0.4947(13) -0.2670(9) -0.0683(7) 0.058(2) Uani 1 1 d . . .
H31B H -0.6439 -0.2254 -0.0403 0.069 Uiso 1 1 calc R . .
H31A H -0.4150 -0.3141 0.0006 0.069 Uiso 1 1 calc R . .
C32 C -0.4889(12) -0.3739(8) -0.1371(6) 0.0490(18) Uani 1 1 d . B .
C37 C -0.2946(14) -0.4746(9) -0.1637(8) 0.070(2) Uani 1 1 d . . .
H37 H -0.1670 -0.4755 -0.1372 0.084 Uiso 1 1 calc R . .
C36 C -0.2898(18) -0.5696(11) -0.2268(9) 0.086(3) Uani 1 1 d . B .
H36 H -0.1576 -0.6328 -0.2444 0.103 Uiso 1 1 calc R . .
C35 C -0.471(2) -0.5766(12) -0.2655(9) 0.093(3) Uani 1 1 d . . .
H35 H -0.4636 -0.6419 -0.3102 0.112 Uiso 1 1 calc R B 1
C34 C -0.6688(16) -0.4826(11) -0.2362(8) 0.083(3) Uani 0.72(7) 1 d P B 1
H34 H -0.7962 -0.4851 -0.2607 0.100 Uiso 0.72(7) 1 calc PR B 1
N34 N -0.6688(16) -0.4826(11) -0.2362(8) 0.083(3) Uani 0.28(7) 1 d P B 2
C33 C -0.6743(13) -0.3863(9) -0.1707(7) 0.064(2) Uani 1 1 d . . .
H33 H -0.8078 -0.3275 -0.1483 0.076 Uiso 1 1 calc R B 1
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'
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
C12 S11 Pd1 86.6(2) . .
C12 S13 Pd1 86.1(3) . .
S13 Pd1 S13 180 . 2
S13 Pd1 S11 75.69(10) . .
S13 Pd1 S11 104.31(10) 2 .
S13 Pd1 S11 104.31(10) . 2
S13 Pd1 S11 75.69(10) 2 2
S11 Pd1 S11 180 . 2
N14 C12 S11 125.3(6) . .
N14 C12 S13 123.2(6) . .
S11 C12 S13 111.6(4) . .
C12 N14 C31 122.3(6) . .
C12 N14 C21 119.4(7) . .
C31 N14 C21 117.5(6) . .
N14 C21 C22 113.1(6) . .
C23 C22 C27 116.4(8) . .
C23 C22 C21 120.4(7) . .
C27 C22 C21 122.8(7) . .
C24 C23 C22 124.2(9) . .
C25 C24 C23 118.2(9) . .
C24 C25 C26 120.5(11) . .
C27 C26 C25 120.0(10) . .
C26 C27 C22 120.6(9) . .
N14 C31 C32 112.3(6) . .
C33 C32 C37 116.1(8) . .
C33 C32 C31 122.3(8) . .
C37 C32 C31 121.5(7) . .
C36 C37 C32 121.3(8) . .
C37 C36 C35 122.4(10) . .
C36 C35 C34 118.0(10) . .
C33 C34 C35 119.7(8) . .
C34 C33 C32 122.3(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S11 C12 1.717(8) .
S11 Pd1 2.339(3) .
S13 C12 1.749(7) .
S13 Pd1 2.333(3) .
Pd1 S13 2.333(3) 2
Pd1 S11 2.339(3) 2
C12 N14 1.315(8) .
N14 C31 1.483(9) .
N14 C21 1.504(9) .
C21 C22 1.537(11) .
C22 C23 1.367(10) .
C22 C27 1.388(11) .
C23 C24 1.364(12) .
C24 C25 1.334(14) .
C25 C26 1.398(14) .
C26 C27 1.357(13) .
C31 C32 1.496(10) .
C32 C33 1.379(9) .
C32 C37 1.407(11) .
C37 C36 1.347(12) .
C36 C35 1.358(13) .
C35 C34 1.397(14) .
C34 C33 1.377(11) .
