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_7703088
_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         'C14 Fe5 O14 S2, 2(C28 H40 K O10), C4 H10 O'
_chemical_formula_sum            'C74 H90 Fe5 K2 O35 S2'
_chemical_formula_weight         1961.02
_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             2019-11-21
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2019-11-25 deposited with the CCDC.	2019-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                80.089(3)
_cell_angle_beta                 83.912(4)
_cell_angle_gamma                72.768(4)
_cell_formula_units_Z            2
_cell_length_a                   11.7472(7)
_cell_length_b                   15.4129(6)
_cell_length_c                   25.0874(8)
_cell_measurement_reflns_used    14145
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      25.3170
_cell_measurement_theta_min      1.7960
_cell_volume                     4266.3(3)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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   0.00  268
  2  \w   -110.00  24.00   0.50   45.00    --  -20.00 -60.00 120.00  268
  3  \w    -81.00  22.00   0.50   45.00    --  -20.00 -60.00 240.00  206
  4  \w    -81.00  70.00   0.50   45.00    --  -20.00   0.00   0.00  302
  5  \w   -110.00  70.00   0.50   45.00    --  -20.00   0.00 240.00  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      0.0594392000
_diffrn_orient_matrix_UB_12      -0.0008584000
_diffrn_orient_matrix_UB_13      -0.0092326000
_diffrn_orient_matrix_UB_21      0.0027950000
_diffrn_orient_matrix_UB_22      -0.0352656000
_diffrn_orient_matrix_UB_23      -0.0153597000
_diffrn_orient_matrix_UB_31      -0.0216070000
_diffrn_orient_matrix_UB_32      0.0336172000
_diffrn_orient_matrix_UB_33      -0.0224988000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49043
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.726
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55388
_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            brown
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       plate
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.786
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1065
_refine_ls_number_reflns         15547
_refine_ls_number_restraints     708
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1202
_refine_ls_R_factor_gt           0.0820
_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^)+(0.1168P)^2^+16.0252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2029
_refine_ls_wR_factor_ref         0.2281
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10721
_reflns_number_total             15547
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04098f2.cif
_cod_data_source_block           K2Fe5S2
_cod_database_code               7703088
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C74H88K2O35S2Fe5
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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 Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C01B(H01B,H01C), C01C(H01D,H01E), C01D(H01F,H01G), C01G(H01I,
 H01J), C01I(H01K,H01L), C01K(H01N,H01O), C01L(H01P,H01Q), C01M(H01R,H01S),
 C01N(H01T,H01U), C01Q(H01W,H01X), C01V(H1,H), C01W(H2,HA), C01X(H3,HB), C2(H2A,
 H2B), C021(H02A,H02B), C02C(H02C,H02D), C02D(H02E,H02F), C02E(H02G,H02H),
 C02F(H02I,H02J), C02H(H02K,H02L), C02M(H02M,H02N), C02N(H02O,H02P), C02Q(H02Q,
 H02R), C02S(H02S,H02T), C02U(H02U,H02V), C02V(H02W,H02X), C02Z(H4,HC), C028(H5,
 HD), C029(H6,HE), C030(H03A,H03B), C036(H03C,H03D), C035(H03H,H03I), C039(H03J,
 H03K)
3.b Aromatic/amide H refined with riding coordinates:
 C01A(H01A), C01E(H01H), C01J(H01M), C01P(H01V), C01R(H01Y), C01S(H01Z),
 C01U(H01), C019(H019), C02W(H02Y), C02X(H02Z), C02Y(H02), C031(H031),
 C033(H033), C034(H034), C037(H037), C038(H038)
3.c Idealised Me refined as rotating group:
 C02T(H7,HF,HG), C03A(H03E,H03F,H03G)
;
_shelx_res_checksum              86712
_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 1.845
_oxdiff_exptl_absorpt_empirical_full_min 0.663