Synthesis of nanostructured powders and thin films of iron sulfide from molecular precursors
Almanqur, Laila; Vitorica-yrezabal, Inigo; Whitehead, George; Lewis, David J.; O'Brien, Paul; RSC Advances 8 (2018) 29096–; doi:10.1039/C8RA04917C

data_7231384
_publ_section_title
;
 Synthesis of nanostructured powders and thin films of iron sulfide from
 molecular precursors
;
_journal_issue                   51
_journal_name_full               'RSC Advances'
_journal_page_first              29096
_journal_paper_doi               10.1039/C8RA04917C
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C12 H21 Fe O3 S6'
_chemical_formula_sum            'C12 H21 Fe O3 S6'
_chemical_formula_weight         461.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-06-04 deposited with the CCDC.
2018-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.469(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8787(2)
_cell_length_b                   9.6899(2)
_cell_length_c                   21.8298(5)
_cell_measurement_reflns_used    18787
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.1540
_cell_measurement_theta_min      2.2920
_cell_volume                     2047.90(8)
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.892
_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      1.00  33.00   1.00    1.00    --    5.00  49.00  -5.00   32
  2  \w    -71.00 -34.00   1.00    1.00    --   -7.70 -49.00-152.00   37
  3  \w     37.00  63.00   1.00    1.00    --    5.00  57.00 -90.00   26
  4  \w      0.00  44.00   1.00    1.00    --    5.00 -76.00 -60.00   44
  5  \w     27.00  53.00   1.00    1.00    --    5.00  57.00  60.00   26
  6  \w    -80.00 -18.00   1.00    1.00    --    5.00 -76.00 -60.00   62
  7  \w    -97.00  33.00   1.00    1.00    --   -7.70 -76.00 -30.00  130
  8  \w    -36.00  82.00   1.00    1.00    --   -7.70  57.00  60.00  118
  9  \w    -40.00  81.00   1.00    1.00    --   -7.70  38.00-180.00  121
;
_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      -0.0536281000
_diffrn_orient_matrix_UB_12      0.0083852000
_diffrn_orient_matrix_UB_13      0.0170071000
_diffrn_orient_matrix_UB_21      -0.0435305000
_diffrn_orient_matrix_UB_22      -0.0431532000
_diffrn_orient_matrix_UB_23      -0.0216971000
_diffrn_orient_matrix_UB_31      0.0243875000
_diffrn_orient_matrix_UB_32      -0.0585400000
_diffrn_orient_matrix_UB_33      0.0184147000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            36718
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.994
_diffrn_reflns_theta_min         2.130
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.354
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75947
_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 dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       plate
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         5332
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0231
_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^)+(0.0220P)^2^+0.8728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0517
_refine_ls_wR_factor_ref         0.0537
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4708
_reflns_number_total             5332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra04917c2.cif
_cod_data_source_block           s5053r
_cod_database_code               7231384
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         FeS6O3C10H10
_shelx_estimated_absorpt_t_max   0.773
_shelx_estimated_absorpt_t_min   0.614
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C19(H19), C5(H5), C12(H12)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C6(H6A,H6B,
 H6C), C8(H8A,H8B,H8C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              75435
_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 1.425
_oxdiff_exptl_absorpt_empirical_full_min 0.632