#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:50:11 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180098 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/44/7054420.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_7054420
loop_
_publ_author_name
'Ehsan, Muhammad Ali'
'Ming, Huang Nay'
'McKee, Vickie'
'Peiris, Thalge Anton Nirmal'
'Wijayantha-Kahagala-Gamage, Upul'
'Arifin, Zainudin'
'Mazhar, Muhammad'
_publ_section_title
;
 Vysotskite structured photoactive palladium sulphide thin films from
 dithiocarbamate derivatives
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4083
_journal_paper_doi               10.1039/C4NJ00564C
_journal_volume                  38
_journal_year                    2014
_chemical_formula_sum            'C31 H49 N3 Pd S4'
_chemical_formula_weight         698.37
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 104.023(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9610(13)
_cell_length_b                   14.0277(19)
_cell_length_c                   12.1552(16)
_cell_measurement_reflns_used    3121
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.77
_cell_measurement_theta_min      2.26
_cell_volume                     1647.8(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16333
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.347
_diffrn_reflns_theta_min         2.256
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2009/1, Sheldrick, G.M., (2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         4109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[σ²(Fo²)+(0.0438P)²] 
 where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3135
_reflns_number_total             4109
_reflns_threshold_expression     'I > 2σ(I)'
_cod_duplicate_entry             7054230
_cod_data_source_file            c4nj00564c2.cif
_cod_data_source_block           Complex_2(p1)
_cod_database_code               7054420
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.824
_shelx_estimated_absorpt_t_max   0.877
_shelxl_version_number           2012-9
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.5000 0.5000 0.5000 0.02289(8) Uani 1 2 d S . P . .
S1 S 0.29497(6) 0.43575(5) 0.39469(5) 0.02969(15) Uani 1 1 d . . . . .
S2 S 0.56729(6) 0.37897(4) 0.39431(5) 0.02556(14) Uani 1 1 d . . . . .
C1 C 0.3927(2) 0.35557(16) 0.33886(19) 0.0227(5) Uani 1 1 d . . . . .
N1 N 0.34478(19) 0.28685(14) 0.26479(16) 0.0233(4) Uani 1 1 d . . . . .
C2 C 0.1947(2) 0.26188(18) 0.2254(2) 0.0273(5) Uani 1 1 d . . . . .
H2 H 0.1908 0.2050 0.1752 0.033 Uiso 1 1 calc R U . . .
C3 C 0.1345(3) 0.22920(19) 0.3227(2) 0.0330(6) Uani 1 1 d . . . . .
H3A H 0.1436 0.2809 0.3795 0.040 Uiso 1 1 calc R U . . .
H3B H 0.1867 0.1732 0.3602 0.040 Uiso 1 1 calc R U . . .
C4 C -0.0193(3) 0.2026(2) 0.2784(3) 0.0407(7) Uani 1 1 d . . . . .
H4A H -0.0273 0.1457 0.2291 0.049 Uiso 1 1 calc R U . . .
H4B H -0.0592 0.1866 0.3432 0.049 Uiso 1 1 calc R U . . .
C5 C -0.1000(3) 0.2844(2) 0.2119(3) 0.0427(7) Uani 1 1 d . . . . .
H5A H -0.1983 0.2657 0.1843 0.051 Uiso 1 1 calc R U . . .
H5B H -0.0958 0.3404 0.2622 0.051 Uiso 1 1 calc R U . . .
C6 C -0.0415(3) 0.3108(2) 0.1120(2) 0.0397(7) Uani 1 1 d . . . . .
H6A H -0.0952 0.3645 0.0703 0.048 Uiso 1 1 calc R U . . .
H6B H -0.0508 0.2558 0.0596 0.048 Uiso 1 1 calc R U . . .
C7 C 0.1119(2) 0.33939(19) 0.1507(2) 0.0321(6) Uani 1 1 d . . . . .
H7A H 0.1498 0.3496 0.0835 0.038 Uiso 1 1 calc R U . . .
H7B H 0.1202 0.4000 0.1936 0.038 Uiso 1 1 calc R U . . .
C8 C 0.4459(2) 0.22556(16) 0.22565(19) 0.0228(5) Uani 1 1 d . . . . .
H8 H 0.5354 0.2613 0.2422 0.027 Uiso 1 1 calc R U . . .
C9 C 0.4070(3) 0.20643(18) 0.0979(2) 0.0302(6) Uani 1 1 d . . . . .
H9A H 0.3209 0.1682 0.0775 0.036 Uiso 1 1 calc R U . . .
H9B H 0.3904 0.2675 0.0560 0.036 Uiso 1 1 calc R U . . .
C10 C 0.5247(3) 0.15243(19) 0.0655(2) 0.0334(6) Uani 1 1 d . . . . .
H10A H 0.4975 0.1369 -0.0164 0.040 Uiso 1 1 calc R U . . .
H10B H 0.6075 0.1939 0.0787 0.040 Uiso 1 1 calc R U . . .
C11 C 0.5613(3) 0.06065(19) 0.1330(2) 0.0378(6) Uani 1 1 d . . . . .
H11A H 0.6434 0.0314 0.1143 0.045 Uiso 1 1 calc R U . . .
H11B H 0.4834 0.0152 0.1110 0.045 Uiso 1 1 calc R U . . .
C12 C 0.5917(3) 0.0784(2) 0.2605(2) 0.0363(6) Uani 1 1 d . . . . .
H12A H 0.6783 0.1156 0.2846 0.044 Uiso 1 1 calc R U . . .
H12B H 0.6055 0.0166 0.3010 0.044 Uiso 1 1 calc R U . . .
C13 C 0.4729(3) 0.13291(18) 0.2929(2) 0.0300(5) Uani 1 1 d . . . . .
H13A H 0.3882 0.0932 0.2762 0.036 Uiso 1 1 calc R U . . .
H13B H 0.4979 0.1471 0.3751 0.036 Uiso 1 1 calc R U . . .
N20 N 0.3590(3) 0.5171(2) -0.0063(3) 0.0484(7) Uani 0.5 1 d . . P A 1
C20 C 0.3590(3) 0.5171(2) -0.0063(3) 0.0484(7) Uani 0.5 1 d . . P A 2
H20 H 0.2639 0.5286 -0.0104 0.058 Uiso 0.5 1 calc R U P A 2
C21 C 0.4461(4) 0.4815(2) 0.0886(3) 0.0480(8) Uani 1 1 d . . . . .
H21 H 0.4105 0.4678 0.1526 0.058 Uiso 1 1 calc R U . A 1
C22 C 0.5836(3) 0.4647(2) 0.0955(3) 0.0481(8) Uani 1 1 d . . . . .
H22 H 0.6402 0.4398 0.1638 0.058 Uiso 1 1 calc R U . . .
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
S1 Pd1 S1 180.0 3_666 .
S1 Pd1 S2 104.85(2) 3_666 .
S1 Pd1 S2 75.15(2) . .
S1 Pd1 S2 75.15(2) 3_666 3_666
S1 Pd1 S2 104.85(2) . 3_666
S2 Pd1 S2 180.0 . 3_666
C1 S1 Pd1 88.01(8) . .
C1 S2 Pd1 87.52(8) . .
N1 C1 S1 126.50(17) . .
N1 C1 S2 124.21(17) . .
S1 C1 S2 109.29(13) . .
C1 N1 C8 118.51(18) . .
C1 N1 C2 123.67(19) . .
C8 N1 C2 117.61(18) . .
N1 C2 C3 111.92(19) . .
N1 C2 C7 112.22(19) . .
C3 C2 C7 114.8(2) . .
C2 C3 C4 110.3(2) . .
C5 C4 C3 110.9(2) . .
C6 C5 C4 110.8(2) . .
C5 C6 C7 111.4(2) . .
C2 C7 C6 110.5(2) . .
N1 C8 C13 111.54(19) . .
N1 C8 C9 113.67(19) . .
C13 C8 C9 111.28(19) . .
C10 C9 C8 109.1(2) . .
C11 C10 C9 112.2(2) . .
C10 C11 C12 111.9(2) . .
C11 C12 C13 111.4(2) . .
C8 C13 C12 109.5(2) . .
C21 N20 C22 115.9(3) . 3_665
N20 C21 C22 122.6(3) . .
C20 C22 C21 121.5(3) 3_665 .
N20 C22 C21 121.5(3) 3_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 S1 2.3140(6) 3_666
Pd1 S1 2.3141(6) .
Pd1 S2 2.3237(6) .
Pd1 S2 2.3237(6) 3_666
S1 C1 1.730(2) .
S2 C1 1.738(2) .
C1 N1 1.326(3) .
N1 C8 1.487(3) .
N1 C2 1.496(3) .
C2 C3 1.521(3) .
C2 C7 1.525(3) .
C3 C4 1.542(3) .
C4 C5 1.517(4) .
C5 C6 1.515(4) .
C6 C7 1.538(3) .
C8 C13 1.524(3) .
C8 C9 1.530(3) .
C9 C10 1.526(3) .
C10 C11 1.523(4) .
C11 C12 1.525(4) .
C12 C13 1.538(3) .
N20 C21 1.359(4) .
N20 C22 1.367(4) 3_665
C21 C22 1.372(4) .
C22 C20 1.367(4) 3_665
C22 N20 1.367(4) 3_665
