#------------------------------------------------------------------------------
#$Date: 2021-12-14 12:44:23 +0200 (Tue, 14 Dec 2021) $
#$Revision: 271414 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/57/1565761.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_1565761
loop_
_publ_author_name
'Mlowe, Sixberth'
'Shombe, Ginena B.'
'Akerman, Matthew P.'
'Mubofu, Egid B.'
'O'Brien, Paul'
'Mashazi, Philani'
'Nyokong, Tebello'
'Revaprasadu, Neerish'
_publ_section_title
;
 Morphological influence of deposition routes on lead sulfide thin films
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119116
_journal_paper_doi               10.1016/j.ica.2019.119116
_journal_volume                  498
_journal_year                    2019
_chemical_formula_moiety         'C12 H20 N2 Pb S4'
_chemical_formula_sum            'C12 H20 N2 Pb S4'
_chemical_formula_weight         527.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P -2ac -2n'
_space_group_name_H-M_alt        'P n 21 a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.086(3)
_cell_length_b                   22.565(4)
_cell_length_c                   4.4482(7)
_cell_measurement_reflns_used    3573
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      1.8
_cell_volume                     1614.6(5)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2012)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2012)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      102(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Incoatec microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            12885
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.240
_diffrn_reflns_theta_min         1.805
_exptl_absorpt_coefficient_mu    10.955
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADAB, Bruker, 2014'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.171
_exptl_crystal_description       needle
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.400
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.048(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3822
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0202
_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)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0420
_refine_ls_wR_factor_ref         0.0427
_reflns_Friedel_coverage         0.953
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                3573
_reflns_number_total             3822
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2019-498-119116.cif
_cod_data_source_block           1
_cod_original_cell_volume        1614.6(4)
_cod_database_code               1565761
_shelx_shelxl_version_number     2014/7
_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   0.058
_shelx_estimated_absorpt_t_max   0.353
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, y, -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
Pb1 Pb 0.36562(2) 0.72116(3) 0.51677(3) 0.01309(6) Uani 1 1 d . . . . .
S3 S 0.49611(7) 0.71443(6) 0.1280(3) 0.0113(3) Uani 1 1 d . . . . .
S2 S 0.23470(7) 0.72924(6) 0.1323(3) 0.0117(3) Uani 1 1 d . . . . .
S4 S 0.39129(8) 0.60793(6) 0.2234(3) 0.0176(3) Uani 1 1 d . . . . .
S1 S 0.34007(8) 0.83522(6) 0.2361(4) 0.0173(3) Uani 1 1 d . . . . .
C12 C 0.5230(3) 0.5447(2) -0.1520(13) 0.0149(11) Uani 1 1 d . . . . .
H12A H 0.5111 0.5422 -0.3700 0.018 Uiso 1 1 calc R U . . .
H12B H 0.4742 0.5291 -0.0421 0.018 Uiso 1 1 calc R U . . .
N1 N 0.1955(3) 0.83705(19) -0.0619(10) 0.0121(9) Uani 1 1 d . . . . .
C6 C 0.1196(3) 0.8115(3) -0.1920(15) 0.0128(13) Uani 1 1 d . . . . .
H6A H 0.1129 0.7701 -0.1220 0.015 Uiso 1 1 calc R U . . .
H6B H 0.1241 0.8111 -0.4139 0.015 Uiso 1 1 calc R U . . .
N2 N 0.5366(3) 0.60699(18) -0.0681(10) 0.0125(9) Uani 1 1 d . . . . .
C7 C 0.4800(3) 0.6387(2) 0.0808(12) 0.0110(10) Uani 1 1 d . . . . .
C2 C 0.2097(3) 0.8993(2) -0.1455(14) 0.0156(12) Uani 1 1 d . . . . .
H2A H 0.2180 0.9023 -0.3655 0.019 Uiso 1 1 calc R U . . .
H2B H 0.2606 0.9140 -0.0453 0.019 Uiso 1 1 calc R U . . .
C5 C 0.0435(3) 0.8483(2) -0.0975(12) 0.0125(11) Uani 1 1 d . . . . .
H5A H -0.0066 0.8326 -0.1997 0.015 Uiso 1 1 calc R U . . .
H5B H 0.0350 0.8442 0.1220 0.015 Uiso 1 1 calc R U . . .
C3 C 0.1358(3) 0.9375(3) -0.0529(14) 0.0166(13) Uani 1 1 d . . . . .
H3A H 0.1441 0.9783 -0.1285 0.020 Uiso 1 1 calc R U . . .
H3B H 0.1329 0.9393 0.1692 0.020 Uiso 1 1 calc R U . . .
C4 C 0.0538(3) 0.9132(2) -0.1752(13) 0.0160(12) Uani 1 1 d . . . . .
H4A H 0.0070 0.9361 -0.0892 0.019 Uiso 1 1 calc R U . . .
H4B H 0.0525 0.9181 -0.3963 0.019 Uiso 1 1 calc R U . . .
C1 C 0.2516(3) 0.8044(2) 0.0882(11) 0.0103(10) Uani 1 1 d . . . . .
C11 C 0.5994(4) 0.5069(2) -0.0782(13) 0.0183(12) Uani 1 1 d . . . . .
H11A H 0.6060 0.5045 0.1428 0.022 Uiso 1 1 calc R U . . .
H11B H 0.5908 0.4662 -0.1552 0.022 Uiso 1 1 calc R U . . .
C10 C 0.6783(3) 0.5324(2) -0.2151(14) 0.0168(12) Uani 1 1 d . . . . .
H10A H 0.6756 0.5292 -0.4369 0.020 Uiso 1 1 calc R U . . .
H10B H 0.7270 0.5094 -0.1449 0.020 Uiso 1 1 calc R U . . .
C9 C 0.6884(3) 0.5971(2) -0.1254(12) 0.0156(11) Uani 1 1 d . . . . .
H9A H 0.6986 0.5996 0.0938 0.019 Uiso 1 1 calc R U . . .
H9B H 0.7373 0.6140 -0.2298 0.019 Uiso 1 1 calc R U . . .
C8 C 0.6122(3) 0.6332(3) -0.2035(14) 0.0113(12) Uani 1 1 d . . . . .
H8A H 0.6194 0.6742 -0.1291 0.014 Uiso 1 1 calc R U . . .
H8B H 0.6058 0.6348 -0.4247 0.014 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'
Pb Pb -3.3944 10.1111 '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 Pb1 S3 101.61(4) . .
S2 Pb1 S1 63.79(4) . .
S3 Pb1 S1 83.40(4) . .
S2 Pb1 S4 83.47(4) . .
S3 Pb1 S4 63.59(4) . .
S1 Pb1 S4 127.65(4) . .
C7 S3 Pb1 90.96(18) . .
C1 S2 Pb1 90.85(17) . .
C7 S4 Pb1 85.85(18) . .
C1 S1 Pb1 85.58(17) . .
N2 C12 C11 111.0(4) . .
N2 C12 H12A 109.4 . .
C11 C12 H12A 109.4 . .
N2 C12 H12B 109.4 . .
C11 C12 H12B 109.4 . .
H12A C12 H12B 108.0 . .
C1 N1 C6 122.7(4) . .
C1 N1 C2 123.0(4) . .
C6 N1 C2 113.8(4) . .
N1 C6 C5 110.1(5) . .
N1 C6 H6A 109.6 . .
C5 C6 H6A 109.6 . .
N1 C6 H6B 109.6 . .
C5 C6 H6B 109.6 . .
H6A C6 H6B 108.2 . .
C7 N2 C12 122.5(4) . .
C7 N2 C8 123.2(4) . .
C12 N2 C8 113.6(4) . .
N2 C7 S4 122.4(4) . .
N2 C7 S3 119.0(4) . .
S4 C7 S3 118.6(3) . .
N1 C2 C3 110.5(4) . .
N1 C2 H2A 109.5 . .
C3 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
C3 C2 H2B 109.5 . .
H2A C2 H2B 108.1 . .
C4 C5 C6 111.8(5) . .
C4 C5 H5A 109.2 . .
C6 C5 H5A 109.2 . .
C4 C5 H5B 109.2 . .
C6 C5 H5B 109.2 . .
H5A C5 H5B 107.9 . .
C2 C3 C4 111.9(5) . .
C2 C3 H3A 109.2 . .
C4 C3 H3A 109.2 . .
C2 C3 H3B 109.2 . .
C4 C3 H3B 109.2 . .
H3A C3 H3B 107.9 . .
C5 C4 C3 111.1(4) . .
C5 C4 H4A 109.4 . .
C3 C4 H4A 109.4 . .
C5 C4 H4B 109.4 . .
C3 C4 H4B 109.4 . .
H4A C4 H4B 108.0 . .
N1 C1 S1 121.8(4) . .
N1 C1 S2 119.2(4) . .
S1 C1 S2 119.0(3) . .
C10 C11 C12 111.9(4) . .
C10 C11 H11A 109.2 . .
C12 C11 H11A 109.2 . .
C10 C11 H11B 109.2 . .
C12 C11 H11B 109.2 . .
H11A C11 H11B 107.9 . .
C11 C10 C9 110.3(4) . .
C11 C10 H10A 109.6 . .
C9 C10 H10A 109.6 . .
C11 C10 H10B 109.6 . .
C9 C10 H10B 109.6 . .
H10A C10 H10B 108.1 . .
C8 C9 C10 111.7(4) . .
C8 C9 H9A 109.3 . .
C10 C9 H9A 109.3 . .
C8 C9 H9B 109.3 . .
C10 C9 H9B 109.3 . .
H9A C9 H9B 107.9 . .
N2 C8 C9 110.9(5) . .
N2 C8 H8A 109.5 . .
C9 C8 H8A 109.5 . .
N2 C8 H8B 109.5 . .
C9 C8 H8B 109.5 . .
H8A C8 H8B 108.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 S2 2.7192(13) .
Pb1 S3 2.7237(12) .
Pb1 S1 2.8899(16) .
Pb1 S4 2.8984(16) .
S3 C7 1.740(5) .
S2 C1 1.730(5) .
S4 C7 1.710(5) .
S1 C1 1.714(5) .
C12 N2 1.471(6) .
C12 C11 1.532(7) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
N1 C1 1.343(6) .
N1 C6 1.469(6) .
N1 C2 1.471(6) .
C6 C5 1.537(7) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
N2 C7 1.335(6) .
N2 C8 1.480(6) .
C2 C3 1.525(7) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C5 C4 1.515(6) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C3 C4 1.528(7) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C11 C10 1.520(8) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C10 C9 1.524(7) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C9 C8 1.511(7) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C1 N1 C6 C5 130.1(5) . . . .
C2 N1 C6 C5 -57.5(6) . . . .
C11 C12 N2 C7 -134.0(5) . . . .
C11 C12 N2 C8 54.8(6) . . . .
C12 N2 C7 S4 7.2(7) . . . .
C8 N2 C7 S4 177.6(4) . . . .
C12 N2 C7 S3 -171.9(4) . . . .
C8 N2 C7 S3 -1.6(7) . . . .
Pb1 S4 C7 N2 171.3(4) . . . .
Pb1 S4 C7 S3 -9.6(3) . . . .
Pb1 S3 C7 N2 -170.7(4) . . . .
Pb1 S3 C7 S4 10.2(3) . . . .
C1 N1 C2 C3 -130.3(5) . . . .
C6 N1 C2 C3 57.4(6) . . . .
N1 C6 C5 C4 54.3(6) . . . .
N1 C2 C3 C4 -53.4(6) . . . .
C6 C5 C4 C3 -52.2(6) . . . .
C2 C3 C4 C5 51.9(7) . . . .
C6 N1 C1 S1 179.6(4) . . . .
C2 N1 C1 S1 8.0(7) . . . .
C6 N1 C1 S2 0.0(7) . . . .
C2 N1 C1 S2 -171.6(4) . . . .
Pb1 S1 C1 N1 172.0(4) . . . .
Pb1 S1 C1 S2 -8.3(3) . . . .
Pb1 S2 C1 N1 -171.5(4) . . . .
Pb1 S2 C1 S1 8.8(3) . . . .
N2 C12 C11 C10 -53.3(6) . . . .
C12 C11 C10 C9 53.2(6) . . . .
C11 C10 C9 C8 -54.3(6) . . . .
C7 N2 C8 C9 132.9(5) . . . .
C12 N2 C8 C9 -56.0(6) . . . .
C10 C9 C8 N2 55.1(6) . . . .
