Transfer of hydrosulfide from thiols to iron(ii): a convenient synthetic route to nonheme diiron(ii)-hydrosulfide complexes.
Pal, Nabhendu; Majumdar, Amit; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5903–5908; doi:10.1039/c8dt04092c

data_7048480
_publ_section_title
;
 Transfer of hydrosulfide from thiols to iron(ii): a convenient synthetic
 route to nonheme diiron(ii)-hydrosulfide complexes.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5903
_journal_page_last               5908
_journal_paper_doi               10.1039/c8dt04092c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C49 H66 Fe2 N12 O4 S, 3(B F4)'
_chemical_formula_sum            'C49 H66 B3 F12 Fe2 N12 O4 S'
_chemical_formula_weight         1291.32
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-03 deposited with the CCDC.
2019-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                67.164(9)
_cell_angle_beta                 72.810(9)
_cell_angle_gamma                76.576(9)
_cell_formula_units_Z            2
_cell_length_a                   13.584(4)
_cell_length_b                   14.829(4)
_cell_length_c                   19.058(5)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.66
_cell_measurement_theta_min      2.37
_cell_volume                     3349.8(16)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2016)'
_computing_data_collection       'APEX2 v2017.3-0 (Bruker-Axs,2016)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2016)'
_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    'ShelXD (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker D8VENTURE with PHOTON II Detector'
_diffrn_measurement_method       'phi, omega and kappa scan'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_unetI/netI     0.0971
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32546
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.837
_diffrn_reflns_theta_min         2.340
_diffrn_source_type              Micro-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1397 before and 0.0991 after correction.
The Ratio of minimum to maximum transmission is 0.7915.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1334
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.379
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         12753
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.0913
_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^)+(0.1476P)^2^+5.9357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2535
_refine_ls_wR_factor_ref         0.2793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8935
_reflns_number_total             12753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04092c2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7048480--7048483.cif.'
_cod_original_cell_volume        3349.9(17)
_cod_database_code               7048480
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.880
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All S(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 S1-H1
 1.2 with sigma of 0.02
 C27B-C29B
 2.4 with sigma of 0.02
 C26-C29B
 2.5 with sigma of 0.02
 C30-C25 = C26-C25 = C27A-C26 = C27B-C26 = C28A-C27A = C28B-C27B = C29A-C28A =
 C29B-C28B = C30-C29A = C30-C29B
 1.366 with sigma of 0.02
 C25-C27B
 2.359 with sigma of 0.02
 C27A-C25
 2.359 with sigma of 0.02
 C30-C29A = C29A-C28A
 1.36 with sigma of 0.02
 C29A-C27A
 2.39 with sigma of 0.02
 C29B-C27B
 2.39 with sigma of 0.02
 C29A-C28A
 1.35 with sigma of 0.02
 C29B-C26
 2.82 with sigma of 0.02
 C26-C29A
 2.82 with sigma of 0.02
 C28A-C27A
 1.38 with sigma of 0.02
 C30-C27A
 2.74 with sigma of 0.02
 C30-C27B
 2.74 with sigma of 0.02
 F10A-B3A \\sim F10B-B3B \\sim F11B-B3B \\sim F11A-B3A \\sim F12A-B3A \\sim
F12B-B3B \\sim F9B-B3B ~
 F9A-B3A
 with sigma of 0.02
 F5-B2 \\sim F6A-B2 \\sim F6B-B2 \\sim F7B-B2 \\sim F7A-B2 \\sim F8A-B2 \\sim
F8B-B2
 with sigma of 0.02
 F1-B1 \\sim F2-B1 \\sim F4B-B1 \\sim F4A-B1 \\sim F3B-B1 \\sim F3A-B1
 with sigma of 0.02
 C21A-C21 \\sim C21B-C21
 with sigma of 0.02
 N12A-C46 \\sim N12B-C46
 with sigma of 0.02
 N12A-C48A \\sim N12B-C48B \\sim N12B-C47B \\sim N12A-C47A
 with sigma of 0.02
 C30-C25 \\sim C30-C29B \\sim C29B-C28B \\sim C28B-C27B \\sim C27B-C26 \\sim
C30-C29A \\sim C29A-C28A
 \\sim C28A-C27A \\sim C27A-C26 \\sim C26-C25
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F4A) = Uanis(F4B)
Uanis(F3A) = Uanis(F3B)
Uanis(F5) = Uanis(F6B) = Uanis(F6A) = Uanis(F7B) = Uanis(F7A) = Uanis(F8B) =
Uanis(F8A)
Uanis(C21) = Uanis(C21A) = Uanis(C21B)
Uanis(C47B) = Uanis(C47A) = Uanis(C48A) = Uanis(C48B)
Uanis(N12B) = Uanis(N12A)
Uanis(C46) = Uanis(N12B) = Uanis(N12A) = Uanis(C48A) = Uanis(C48B) =
Uanis(C47B) = Uanis(C47A)
Uanis(C31) = Uanis(C32A) = Uanis(C32B)
Uanis(B3B) = Uanis(B3A)
Uanis(F12B) = Uanis(F12A) = Uanis(F11B) = Uanis(F11A) = Uanis(F9B) = Uanis(F9A)
= Uanis(F10B) = Uanis(F10A)
Uanis(B2) = Uanis(B3B) = Uanis(B3A)
Uanis(C10) = Uanis(C25) = Uanis(N7) = Uanis(C30) = Uanis(C29A) = Uanis(C29B) =
Uanis(C28B) = Uanis(C28A) = Uanis(C27B) = Uanis(C27A) = Uanis(C26)
Uanis(O1) = Uanis(O2)
Uanis(N7) = Uanis(N8)
Uanis(C9) = Uanis(C10)
Uanis(C24) = Uanis(N7)
4. Others
 Sof(N12B)=Sof(H21C)=Sof(H21D)=Sof(C21B)=Sof(H21H)=Sof(H21I)=Sof(H21J)=
 Sof(H26A)=Sof(C27B)=Sof(H27B)=Sof(C28B)=Sof(H28B)=Sof(C29B)=Sof(H29B)=
 Sof(H31C)=Sof(H31D)=Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(H46A)=
 Sof(C47B)=Sof(H47D)=Sof(H47E)=Sof(H47F)=Sof(C48B)=Sof(H48D)=Sof(H48E)=
 Sof(H48F)=Sof(F3B)=Sof(F4B)=Sof(F6B)=Sof(F7B)=Sof(F8B)=Sof(F9B)=Sof(F10B)=
 Sof(F11B)=Sof(F12B)=Sof(B3B)=1-FVAR(1)
 Sof(N12A)=Sof(H21A)=Sof(H21B)=Sof(C21A)=Sof(H21E)=Sof(H21F)=Sof(H21G)=
 Sof(H26)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(H31A)=
 Sof(H31B)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(H46)=Sof(C47A)=Sof(H47A)=
 Sof(H47B)=Sof(H47C)=Sof(C48A)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(F3A)=Sof(F4A)=
 Sof(F6A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=Sof(B3A)=
 FVAR(1)
5.a Rotating group:
 O2(H2A,H2B)
5.b Ternary CH refined with riding coordinates:
 C1(H1A)
5.c Secondary CH2 refined with riding coordinates:
 C2(H2C,H2D), C3(H3A,H3B), C11(H11A,H11B), C13(H13A,H13B), C21(H21A,H21B),
 C21(H21C,H21D), C22(H22A,H22B), C23(H23A,H23B), C31(H31A,H31B), C31(H31C,H31D),
  C33(H33A,H33B), C41(H41A,H41B)
5.d Me refined with riding coordinates:
 C47A(H47A,H47B,H47C), C47B(H47D,H47E,H47F), C48A(H48A,H48B,H48C), C48B(H48D,
 H48E,H48F)
5.e Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C16(H16), C17(H17), C18(H18), C19(H19),
 C26(H26), C26(H26A), C27A(H27A), C28A(H28A), C29A(H29A), C27B(H27B),
 C28B(H28B), C29B(H29B), C36(H36), C37(H37), C38(H38), C39(H39), C43(H43),
 C46(H46), C46(H46A)
5.f Tetrahedral OH refined with riding coordinates:
 S1(H1)
5.g Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C21A(H21E,H21F,H21G), C21B(H21H,H21I,H21J), C32A(H32A,
 H32B,H32C), C32B(H32D,H32E,H32F), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C)
;
_shelx_res_checksum              87153
_shelx_fab_checksum              80308
_olex2_submission_special_instructions 'No special instructions were received'