Structural Investigations of α-MnS Nanocrystals and Thin Films Synthesized from Manganese(II) Xanthates by Hot Injection, Solvent-Less Thermolysis, and Doctor Blade Routes.
Alanazi, Abdulaziz M.; McNaughter, Paul D.; Alam, Firoz; Vitorica-Yrezabal, Inigo J; Whitehead, George F. S.; Tuna, Floriana; O'Brien, Paul; Collison, David; Lewis, David J.; ACS omega 6 (2021) 27716–27725; doi:10.1021/acsomega.1c02907

data_4519117
_publ_section_title
;
 Structural Investigations of \a-MnS Nanocrystals and Thin Films
 Synthesized from Manganese(II) Xanthates by Hot Injection, Solvent-Less
 Thermolysis, and Doctor Blade Routes.
;
_journal_issue                   42
_journal_name_full               'ACS omega'
_journal_page_first              27716
_journal_page_last               27725
_journal_paper_doi               10.1021/acsomega.1c02907
_journal_volume                  6
_journal_year                    2021
_chemical_formula_moiety         'C18 H38 Mn N2 O2 S4'
_chemical_formula_sum            'C18 H38 Mn N2 O2 S4'
_chemical_formula_weight         497.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                70.704(4)
_cell_angle_beta                 78.932(4)
_cell_angle_gamma                72.591(4)
_cell_formula_units_Z            2
_cell_length_a                   7.5898(4)
_cell_length_b                   11.8599(5)
_cell_length_c                   16.0804(7)
_cell_measurement_reflns_used    6405
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      71.7360
_cell_measurement_theta_min      5.6890
_cell_volume                     1296.59(11)
_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_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.977
_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   -130.00 -35.00   1.00    1.00    --  -45.10 -34.00  26.92   95
  2  \w    -90.00 -15.00   1.00    1.00    --  -45.10 -38.00 -90.00   75
  3  \w      8.00  43.00   1.00    1.00    --  -45.10  57.00 -90.00   35
  4  \w    -76.00  28.00   1.00    1.00    --  -45.10  57.00-180.00  104
  5  \w    -67.00  -9.00   1.00    1.00    --  -45.10  57.00 -90.00   58
  6  \w   -127.00 -93.00   1.00    1.00    --  -45.10 -38.00 -90.00   34
  7  \w   -121.00 -93.00   1.00    2.00    -- -107.20  76.00-150.00   28
  8  \w   -114.00 -88.00   1.00    2.00    -- -107.20  76.00  30.00   26
  9  \w   -146.00 -64.00   1.00    2.00    -- -107.20  76.00 -90.00   82
 10  \w   -144.00-117.00   1.00    2.00    -- -107.20  76.00  30.00   27
 11  \w   -136.00 -25.00   1.00    2.00    -- -107.20  57.00-150.00  111
 12  \w    -81.00 -19.00   1.00    2.00    -- -107.20  76.00  30.00   62
 13  \w   -196.00 -19.00   1.00    2.00    -- -107.20  19.00  60.00  177
 14  \w   -139.00-107.00   1.00    2.00    -- -107.20  76.00 -60.00   32
 15  \w   -118.00 -61.00   1.00    2.00    -- -107.20  76.00-180.00   57
 16  \w   -144.00 -38.00   1.00    2.00    -- -107.20  76.00   0.00  106
 17  \w   -135.00 -72.00   1.00    2.00    -- -107.20  57.00 150.00   63
 18  \w    -69.00 -42.00   1.00    2.00    -- -107.20  76.00 -60.00   27
 19  \w    -46.00 -18.00   1.00    2.00    -- -107.20  76.00-150.00   28
 20  \w    -60.00 -35.00   1.00    2.00    -- -107.20  76.00 -90.00   25
 21  \w   -192.00-123.00   1.00    2.00    -- -107.20 -19.00 -30.00   69
 22  \w   -119.00 -56.00   1.00    2.00    -- -107.20 -19.00 -30.00   63
 23  \w   -135.00 -21.00   1.00    2.00    -- -107.20  76.00  90.00  114
 24  \w   -108.00 -83.00   1.00    2.00    -- -107.20  38.00  60.00   25
 25  \w    -64.00 -39.00   1.00    2.00    -- -107.20  38.00  60.00   25
 26  \w    -59.00 -33.00   1.00    2.00    -- -107.20  57.00-120.00   26
 27  \w   -143.00-103.00   1.00    2.00    -- -107.20  76.00 -30.00   40
 28  \w   -197.00-152.00   1.00    2.00    -- -107.20  19.00  90.00   45
 29  \w   -104.00 -77.00   1.00    2.00    -- -107.20 -38.00 120.00   27
;
_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      -0.0621352000
_diffrn_orient_matrix_UB_12      0.1217782000
_diffrn_orient_matrix_UB_13      0.0250000000
_diffrn_orient_matrix_UB_21      0.0991236000
_diffrn_orient_matrix_UB_22      0.0639977000
_diffrn_orient_matrix_UB_23      -0.0881734000
_diffrn_orient_matrix_UB_31      -0.1790323000
_diffrn_orient_matrix_UB_32      0.0364370000
_diffrn_orient_matrix_UB_33      -0.0448910000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14258
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.063
_diffrn_reflns_theta_min         2.927
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.262
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74276
_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    1.275
_exptl_crystal_description       plate
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.013
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4999
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0413P)^2^+0.2668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4661
_reflns_number_total             4999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c02907_si_005.cif
_cod_data_source_block           s4952r
_cod_original_cell_volume        1296.60(11)
_cod_database_code               4519117
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.327
_reflns_odcompleteness_completeness 98.80
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B), C6(H6A,H6B), C7(H7A,H7B), C5(H5A,H5B), C8(H8A,
 H8B), C16(H16A,H16B), C15(H15A,H15B), C14(H14A,H14B), C17(H17A,H17B)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C25(H25A,H25B,
 H25C), C9(H9A,H9B,H9C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              25669
_shelx_hkl_checksum              64972
_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 1.361
_oxdiff_exptl_absorpt_empirical_full_min 0.762