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_7231383
_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 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             2017-10-20
_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                 102.292(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9928(3)
_cell_length_b                   15.6007(3)
_cell_length_c                   9.13185(19)
_cell_measurement_reflns_used    15438
_cell_measurement_temperature    150.00(2)
_cell_measurement_theta_max      26.3970
_cell_measurement_theta_min      2.6160
_cell_volume                     1947.76(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      150.00(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -34.00  18.00   1.00    1.00    --    5.00  76.00-180.00   52
  2  \w    -72.00 -41.00   1.00    1.00    --    5.00 -57.00 120.00   31
  3  \w    -93.00  26.00   1.00    1.00    --   -7.80 -57.00-150.00  119
  4  \w     44.00  82.00   1.00    1.00    --   -7.80  76.00  60.00   38
  5  \w    -43.00  42.00   1.00    1.00    --   -7.80  76.00  60.00   85
  6  \w    -76.00  27.00   1.00    1.00    --   -7.80 -38.00  30.00  103
  7  \w    -97.00 -21.00   1.00    1.00    --   -7.80 -57.00  30.00   76
;
_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      -0.0409509000
_diffrn_orient_matrix_UB_12      0.0265100000
_diffrn_orient_matrix_UB_13      0.0016991000
_diffrn_orient_matrix_UB_21      -0.0314789000
_diffrn_orient_matrix_UB_22      -0.0358605000
_diffrn_orient_matrix_UB_23      -0.0178405000
_diffrn_orient_matrix_UB_31      0.0049770000
_diffrn_orient_matrix_UB_32      -0.0088445000
_diffrn_orient_matrix_UB_33      0.0774322000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            27884
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         1.981
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.423
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74712
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       block
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.522
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0177
_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^)+(0.0207P)^2^+0.7954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0439
_refine_ls_wR_factor_ref         0.0446
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3726
_reflns_number_total             3978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra04917c2.cif
_cod_data_source_block           s4988r
_cod_database_code               7231383
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Fe S2 C6 H6 O'
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C10(H10A,H10B), C7(H7A,H7B), C11(H11A,H11B), C6(H6A,
 H6B)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              29070
_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 1.378
_oxdiff_exptl_absorpt_empirical_full_min 0.679