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_4519115
_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         'C16 H34 Mn N2 O2 S4'
_chemical_formula_sum            'C16 H34 Mn N2 O2 S4'
_chemical_formula_weight         469.63
_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'
_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                90
_cell_angle_beta                 102.885(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5433(3)
_cell_length_b                   21.2751(5)
_cell_length_c                   9.3308(2)
_cell_measurement_reflns_used    3959
_cell_measurement_temperature    150
_cell_measurement_theta_max      71.7270
_cell_measurement_theta_min      3.6440
_cell_volume                     2427.32(10)
_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 0.998
_diffrn_measured_fraction_theta_max 0.986
_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    101.00 126.00   1.00    1.00    --   37.00  60.00-150.00   25
  2  \w    -51.00 119.00   1.00    1.00    --   37.00  57.00 150.00  170
  3  \w    -51.00   6.00   1.00    1.00    --   37.00  57.00 -30.00   57
  4  \w     18.00  44.00   1.00    1.00    --   37.00  60.00 -90.00   26
  5  \w     63.00  88.00   1.00    1.00    --   37.00  60.00-150.00   25
  6  \w    -51.00  -9.00   1.00    1.00    --   37.00  60.00-150.00   42
  7  \w     10.00 124.00   1.00    1.00    --   37.00  57.00 -30.00  114
  8  \w     81.00 109.00   1.00    1.00    --  108.90  60.00-120.00   28
  9  \w     71.00 197.00   1.00    1.00    --  108.90  60.00-180.00  126
 10  \w    111.00 198.00   1.00    1.00    --  108.90  46.00-180.00   87
 11  \w     20.00  55.00   1.00    1.00    --  108.90  60.00-180.00   35
 12  \w    158.00 195.00   1.00    1.00    --  108.90  60.00-150.00   37
 13  \w    104.00 195.00   1.00    1.00    --  108.90  11.00-150.00   91
 14  \w     22.00  68.00   1.00    1.00    --  108.90  46.00-180.00   46
 15  \w     21.00 198.00   1.00    1.00    --  108.90  23.00  30.00  177
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1234034000
_diffrn_orient_matrix_UB_12      0.0092244000
_diffrn_orient_matrix_UB_13      0.0631644000
_diffrn_orient_matrix_UB_21      0.0201157000
_diffrn_orient_matrix_UB_22      -0.0699729000
_diffrn_orient_matrix_UB_23      -0.0274014000
_diffrn_orient_matrix_UB_31      0.0159668000
_diffrn_orient_matrix_UB_32      0.0162065000
_diffrn_orient_matrix_UB_33      -0.1546838000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11697
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.093
_diffrn_reflns_theta_min         3.615
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.728
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35308
_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    1.285
_exptl_crystal_description       plate
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4724
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+0.4599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3860
_reflns_number_total             4724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c02907_si_004.cif
_cod_data_source_block           s4950l
_cod_database_code               4519115
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.366
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
C17 \\sim C17A \\sim C18A \\sim C18: within 2A with sigma of 0.002 and sigma
for terminal atoms of 0.004
3. Others
 Sof(C17)=Sof(H17D)=Sof(H17E)=Sof(C18)=Sof(H18D)=Sof(H18E)=Sof(C16)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C15A)=Sof(H15D)=
 Sof(H15E)=Sof(H15F)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=1-FVAR(1)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C20A)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=Sof(C19A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C0AA)=Sof(H16A)=
 Sof(H16B)=Sof(H16C)=Sof(C17A)=Sof(H1AA)=Sof(H1AB)=Sof(C18A)=Sof(H0AA)=
 Sof(H0AB)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C8(H8A,H8B), C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C9(H9A,H9B),
 C17A(H1AA,H1AB), C18A(H0AA,H0AB), C17(H17D,H17E), C18(H18D,H18E)
4.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C5(H5A,H5B,H5C), C20A(H17A,H17B,
 H17C), C19A(H18A,H18B,H18C), C0AA(H16A,H16B,H16C), C16(H16D,H16E,H16F),
 C19(H19A,H19B,H19C), C15A(H15D,H15E,H15F), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              61936
_shelx_hkl_checksum              66290
_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 2.080
_oxdiff_exptl_absorpt_empirical_full_min 0.609