Synthesis of (Bi1−xSbx)2S3 solid solutions via thermal decomposition of bismuth and antimony piperidinedithiocarbamates
Kun, Walter N.; McNaughter, Paul D.; Nyamen, Linda D.; Spencer, Ben F.; O'Brien, Paul; Ndifon, Peter T.; Revaprasadu, Neerish; RSC Advances 9 (2019) 15836–; doi:10.1039/C9RA01127G

data_7232806
_publ_section_title
;
 Synthesis of (Bi1&#x2212;xSbx)2S3 solid solutions via thermal
 decomposition of bismuth and antimony piperidinedithiocarbamates
;
_journal_issue                   28
_journal_name_full               'RSC Advances'
_journal_page_first              15836
_journal_paper_doi               10.1039/C9RA01127G
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C18 H30 N3 S6 Sb'
_chemical_formula_sum            'C18 H30 N3 S6 Sb'
_chemical_formula_weight         602.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-01-09 deposited with the CCDC.    2019-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.4771(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6331(3)
_cell_length_b                   11.84939(19)
_cell_length_c                   12.12535(19)
_cell_measurement_reflns_used    12093
_cell_measurement_temperature    150
_cell_measurement_theta_max      68.1830
_cell_measurement_theta_min      2.5900
_cell_volume                     2416.54(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -79.00 -53.00   1.00    1.00    --    5.00 -73.00 -75.00   26
  2  \w      6.00  31.00   1.00    1.00    --    5.00  73.00  53.00   25
  3  \w    -30.00  -5.00   1.00    1.00    --  -45.10  73.00  53.00   25
  4  \w    -95.00 -70.00   1.00    1.00    --  -45.10 -73.00 -75.00   25
  5  \w   -106.00 -81.00   1.00    1.00    -- -107.20  73.00  53.00   25
  6  \w   -157.00-132.00   1.00    1.00    -- -107.20 -73.00 -75.00   25
  7  \w   -123.00  -8.00   1.00    1.00    --  -45.10 -43.00 -37.16  115
  8  \w   -134.00 -16.00   1.00    1.00    --  -45.10 -57.00-120.00  118
  9  \w   -139.00 -18.00   1.00    1.00    -- -107.20  57.00  60.00  121
 10  \w   -139.00 -19.00   1.00    1.00    -- -107.20  57.00-150.00  120
 11  \w   -177.00-151.00   1.00    1.00    -- -107.20 -57.00 -60.00   26
 12  \w   -124.00 -99.00   1.00    1.00    -- -107.20 -57.00 -60.00   25
 13  \w   -197.00 -19.00   1.00    1.00    -- -107.20   0.00-180.00  178
 14  \w   -140.00-115.00   1.00    1.00    -- -107.20  38.00  30.00   25
 15  \w   -145.00-120.00   1.00    1.00    -- -107.20  38.00  60.00   25
 16  \w   -100.00 -57.00   1.00    1.00    -- -107.20  38.00  60.00   43
 17  \w    -47.00 -22.00   1.00    1.00    -- -107.20  38.00  60.00   25
 18  \w   -122.00 -96.00   1.00    1.00    -- -107.20  76.00 -30.00   26
 19  \w    -76.00 -51.00   1.00    1.00    -- -107.20  76.00 -30.00   25
 20  \w    -74.00 -49.00   1.00    1.00    -- -107.20  57.00 150.00   25
 21  \w    -74.00 -49.00   1.00    1.00    -- -107.20  57.00   0.00   25
 22  \w   -150.00-103.00   1.00    1.00    -- -107.20 -57.00 -30.00   47
 23  \w   -129.00-103.00   1.00    1.00    -- -107.20 -57.00   0.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0409370000
_diffrn_orient_matrix_UB_12      -0.1044876000
_diffrn_orient_matrix_UB_13      -0.0320090000
_diffrn_orient_matrix_UB_21      -0.0446957000
_diffrn_orient_matrix_UB_22      0.0194372000
_diffrn_orient_matrix_UB_23      -0.1288266000
_diffrn_orient_matrix_UB_31      0.0686909000
_diffrn_orient_matrix_UB_32      0.0748307000
_diffrn_orient_matrix_UB_33      -0.0113550000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16485
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.245
_diffrn_reflns_theta_min         2.627
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.983
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform and methanol'
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.00034(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0172
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+1.2335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0422
_refine_ls_wR_factor_ref         0.0426
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4281
_reflns_number_total             4406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra01127g2.cif
_cod_data_source_block           s4967r
_cod_database_code               7232806
_publcif_datablock.id            {780335c4-71b8-497e-9067-2b6c6a08093c}
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.454
_shelx_estimated_absorpt_t_min   0.235
_reflns_odcompleteness_completeness 99.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00C(H00A,H00B), C00F(H00C,H00D), C00G(H00E,H00F), C00H(H00G,H00H), C00I(H00I,
 H00J), C00J(H00K,H00L), C00K(H00M,H00N), C00L(H00O,H00P), C00M(H00Q,H00R),
 C00N(H00S,H00T), C00O(H00U,H00V), C00P(H00W,H00X), C00Q(H00Y,H), C00R(H00Z,HA),
  C00S(H00,HB)
;
_shelx_res_checksum              10307
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.319
_oxdiff_exptl_absorpt_empirical_full_min 0.791
_publcif_funding_html
;
;