Morphological influence of deposition routes on lead sulfide thin films
Mlowe, Sixberth; Shombe, Ginena B.; Akerman, Matthew P.; Mubofu, Egid B.; O'Brien, Paul; Mashazi, Philani; Nyokong, Tebello; Revaprasadu, Neerish; Inorganica Chimica Acta 498 (2019) 119116–; doi:10.1016/j.ica.2019.119116

data_1565761
_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       '\w and \f-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/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_estimated_absorpt_t_min   0.058
_shelx_estimated_absorpt_t_max   0.353