Facile hydrogen atom abstraction and sulfide formation in a methyl-thiolate capped iron-sulfur-carbonyl cluster.
Shupp, J. Patrick; Rose, Michael J.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 23–26; doi:10.1039/c9dt04098f

data_7703087
_publ_section_title
;
 Facile hydrogen atom abstraction and sulfide formation in a
 methyl-thiolate capped iron-sulfur-carbonyl cluster.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              23
_journal_page_last               26
_journal_paper_doi               10.1039/c9dt04098f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C12 H7 Fe3 O9 S, C28 H40 K O10'
_chemical_formula_sum            'C40 H47 Fe3 K O19 S'
_chemical_formula_weight         1070.48
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-25 deposited with the CCDC.	2019-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                63.000(3)
_cell_angle_beta                 70.310(2)
_cell_angle_gamma                87.375(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6950(3)
_cell_length_b                   15.2437(4)
_cell_length_c                   15.3863(4)
_cell_measurement_reflns_used    19490
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4680
_cell_measurement_theta_min      1.8080
_cell_volume                     2282.27(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_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   -110.00  24.00   0.50   45.00    --  -20.00 -60.00 120.00  268
  2  \w    -50.00  70.00   0.50   45.00    --  -20.00  60.00 240.00  240
  3  \w    -85.00   5.00   0.50   45.00    --  -20.00 -60.00   0.00  180
  4  \w    -50.00  70.00   0.50   45.00    --  -20.00  60.00   0.00  240
  5  \w   -110.00  70.00   0.50   45.00    --  -20.00   0.00 120.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0331438000
_diffrn_orient_matrix_UB_12      -0.0252974000
_diffrn_orient_matrix_UB_13      0.0333630000
_diffrn_orient_matrix_UB_21      0.0556042000
_diffrn_orient_matrix_UB_22      0.0189276000
_diffrn_orient_matrix_UB_23      -0.0435465000
_diffrn_orient_matrix_UB_31      0.0052875000
_diffrn_orient_matrix_UB_32      0.0421204000
_diffrn_orient_matrix_UB_33      0.0073478000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32217
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.589
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.153
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       needle
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         10390
_refine_ls_number_restraints     384
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0409P)^2^+1.1262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9130
_reflns_number_total             10390
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04098f2.cif
_cod_data_source_block           kfe3sipr
_cod_original_cell_volume        2282.27(12)
_cod_database_code               7703087
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C48H32O10SKFe3
_reflns_odcompleteness_completeness 99.26
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C010(H010)
3.b Secondary CH2 refined with riding coordinates:
 C00U(H00A,H00B), C00V(H00C,H00D), C013(H01A,H01B), C014(H01C,H01D), C015(H01E,
 H01F), C016(H01G,H01H), C019(H01I,H01J), C01B(H01K,H01L), C01F(H01O,H01P),
 C01I(H01Q,H01R), C01L(H01T,H01U), C01M(H01V,H01W), C01O(H01Y,HB), C01R(H01,HE),
  C01S(H0AA,HF)
3.c Aromatic/amide H refined with riding coordinates:
 C00R(H00R), C00S(H00S), C00Y(H00Y), C00Z(H00Z), C018(H018), C01J(H01S),
 C01N(H01X), C01P(H01Z)
3.d Idealised Me refined as rotating group:
 C01K(H1AA,H,HA), C01Q(H2AA,HC,HD)
;
_shelx_res_checksum              59831
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.701
_oxdiff_exptl_absorpt_empirical_full_min 0.586