#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:47:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180096 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/42/7054232.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_7054232
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            'C16 H28 N2 Pd S4'
_chemical_formula_weight         483.04
_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                 114.6960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9199(7)
_cell_length_b                   11.0292(7)
_cell_length_c                   10.1444(7)
_cell_measurement_reflns_used    3958
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.51
_cell_measurement_theta_min      2.88
_cell_volume                     1008.37(12)
_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 0.937
_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  0.0298
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11825
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.804
_diffrn_reflns_theta_min         2.412
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.335
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6719
_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    1.591
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         3217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0262
_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/[σ²(Fo²)+(0.0335P)²+0.0751P] 
 where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2767
_reflns_number_total             3217
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4nj00564c2.cif
_cod_data_source_block           complex_4(p3r)
_cod_depositor_comments
'Adding full bibliography for 7054229--7054232.cif.'
_cod_database_code               7054232
#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   0.706
_shelx_estimated_absorpt_t_max   0.776
_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
Pd1 Pd 1.0000 0.0000 1.0000 0.01690(6) Uani 1 2 d S . P
S1 S 0.87449(4) 0.06787(4) 0.76174(5) 0.02241(10) Uani 1 1 d . . .
S2 S 0.75458(5) 0.02191(4) 0.96658(5) 0.02183(9) Uani 1 1 d . . .
C1 C 0.71887(17) 0.07598(14) 0.79591(17) 0.0175(3) Uani 1 1 d . . .
N1 N 0.58869(14) 0.11999(13) 0.70459(14) 0.0184(3) Uani 1 1 d . . .
C2 C 0.57087(19) 0.17457(17) 0.56660(18) 0.0250(4) Uani 1 1 d . . .
H2A H 0.5154 0.1190 0.4869 0.038 Uiso 1 1 calc R U .
H2B H 0.6688 0.1900 0.5681 0.038 Uiso 1 1 calc R U .
H2C H 0.5166 0.2512 0.5525 0.038 Uiso 1 1 calc R U .
C3 C 0.46457(16) 0.13096(14) 0.74922(17) 0.0175(3) Uani 1 1 d . . .
H3 H 0.4815 0.0699 0.8274 0.021 Uiso 1 1 calc R U .
C5 C 0.34195(18) 0.26488(17) 0.86660(19) 0.0240(3) Uani 1 1 d . . .
H5A H 0.3402 0.3478 0.9031 0.029 Uiso 1 1 calc R U .
H5B H 0.3632 0.2076 0.9480 0.029 Uiso 1 1 calc R U .
C4 C 0.46427(17) 0.25616(15) 0.81312(18) 0.0205(3) Uani 1 1 d . . .
H4A H 0.5617 0.2713 0.8949 0.025 Uiso 1 1 calc R U .
H4B H 0.4485 0.3189 0.7383 0.025 Uiso 1 1 calc R U .
C6 C 0.19049(19) 0.23553(16) 0.7451(2) 0.0247(4) Uani 1 1 d . . .
H6A H 0.1639 0.2984 0.6687 0.030 Uiso 1 1 calc R U .
H6B H 0.1143 0.2362 0.7842 0.030 Uiso 1 1 calc R U .
C7 C 0.19253(17) 0.11114(16) 0.67910(18) 0.0227(3) Uani 1 1 d . . .
H7A H 0.2085 0.0476 0.7531 0.027 Uiso 1 1 calc R U .
H7B H 0.0951 0.0961 0.5973 0.027 Uiso 1 1 calc R U .
C8 C 0.31471(17) 0.10276(16) 0.62472(17) 0.0211(3) Uani 1 1 d . . .
H8A H 0.3164 0.0202 0.5871 0.025 Uiso 1 1 calc R U .
H8B H 0.2946 0.1612 0.5447 0.025 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
S2 Pd1 S2 180.0 . 3_757
S2 Pd1 S1 75.080(14) . .
S2 Pd1 S1 104.919(14) 3_757 .
S2 Pd1 S1 104.919(14) . 3_757
S2 Pd1 S1 75.081(14) 3_757 3_757
S1 Pd1 S1 180.00(2) . 3_757
S2 Pd1 H2C 84.3 . 4_666
S2 Pd1 H2C 95.7 3_757 4_666
S1 Pd1 H2C 81.1 . 4_666
S1 Pd1 H2C 98.9 3_757 4_666
C1 S1 Pd1 86.75(5) . .
C1 S2 Pd1 86.88(5) . .
N1 C1 S1 124.87(12) . .
N1 C1 S2 124.04(12) . .
S1 C1 S2 111.08(9) . .
C1 N1 C2 120.73(13) . .
C1 N1 C3 120.42(13) . .
C2 N1 C3 118.28(12) . .
N1 C3 C4 110.65(13) . .
N1 C3 C8 112.10(13) . .
C4 C3 C8 111.20(13) . .
C4 C5 C6 111.10(14) . .
C5 C4 C3 110.57(13) . .
C5 C6 C7 110.77(14) . .
C8 C7 C6 111.66(14) . .
C3 C8 C7 109.48(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 S2 2.3261(5) .
Pd1 S2 2.3261(5) 3_757
Pd1 S1 2.3319(4) .
Pd1 S1 2.3319(4) 3_757
Pd1 H2C 2.7872 4_666
S1 C1 1.7201(16) .
S2 C1 1.7223(16) .
C1 N1 1.3273(19) .
N1 C2 1.465(2) .
N1 C3 1.4837(19) .
C3 C4 1.526(2) .
C3 C8 1.527(2) .
C5 C4 1.525(2) .
C5 C6 1.528(2) .
C6 C7 1.530(2) .
C7 C8 1.530(2) .
