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_7048483
_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         'C46 H59 Fe2 N11 O3 S, 2(B F4)'
_chemical_formula_sum            'C46 H59 B2 F8 Fe2 N11 O3 S'
_chemical_formula_weight         1131.42
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-04 deposited with the CCDC.
2019-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.816(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9837(16)
_cell_length_b                   22.878(3)
_cell_length_c                   16.0002(16)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.15
_cell_measurement_theta_min      2.26
_cell_volume                     5071.2(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.1543
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            129203
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.746
_diffrn_reflns_theta_min         2.196
_diffrn_source_type              Micro-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1258 before and 0.0963 after correction.
The Ratio of minimum to maximum transmission is 0.8803.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.732
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.613
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         9652
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.623
_refine_ls_R_factor_all          0.2097
_refine_ls_R_factor_gt           0.1418
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4088
_refine_ls_wR_factor_ref         0.4539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5473
_reflns_number_total             9652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04092c2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7048480--7048483.cif.'
_cod_database_code               7048483
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.862
_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
 C45B-C44B
 2.41 with sigma of 0.02
 C2A-C1 \\sim C2B-C1 \\sim C23A-C1 \\sim C23B-C1
 with sigma of 0.02
 N6-C23A \\sim N6-C23B \\sim N1-C2A \\sim N1-C2B
 with sigma of 0.02
 N6-C23A \\sim N6-C23B \\sim N1-C2A \\sim N1-C2B \\sim N1-C13B \\sim N1-C13A
\\sim N6-C24B \\sim N6-C24A
 with sigma of 0.02
 C35-C34A \\sim C35-C34B
 with sigma of 0.02
 N6-C34B \\sim N6-C34A
 with sigma of 0.02
 C22B-C21B \\sim C22A-C21A
 with sigma of 0.02
 C25-C24A \\sim C25-C24B
 with sigma of 0.02
 C14A-C13A \\sim C14B-C13B
 with sigma of 0.02
 N4-C14A \\sim N4-C14B \\sim N5A-C14A \\sim N5B-C14B
 with sigma of 0.02
 N4-C15 \\sim N5A-C20 \\sim N5B-C20
 with sigma of 0.02
 C43A-C42 \\sim C43B-C42
 with sigma of 0.02
 N11-C45B \\sim N11-C45A \\sim N11-C44A \\sim N11-C44B
 with sigma of 0.02
 F4A-B1 \\sim F4B-B1 \\sim F3A-B1 \\sim F3B-B1 \\sim F2A-B1 \\sim F2B-B1
 with sigma of 0.02
 F5B-B2 \\sim F5A-B2 \\sim F7B-B2 \\sim F7A-B2 \\sim F8-B2 \\sim F6A-B2 \\sim
F6B-B2
 with sigma of 0.02
 N4-C14A \\sim N5A-C14A \\sim N5B-C14B \\sim N4-C14B
 with sigma of 0.02
 N5A-C20 \\sim N5B-C20 \\sim N4-C15
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C23A) = Uanis(C23B) = Uanis(C2A) = Uanis(C2B) = Uanis(C13A) = Uanis(C13B)
= Uanis(C14A) = Uanis(C14B) = Uanis(C24B) = Uanis(C24A)
Uanis(C34A) = Uanis(C34B)
Uanis(C22A) = Uanis(C22B) = Uanis(C21B) = Uanis(C21A)
Uanis(N4) = Uanis(N5A) = Uanis(N5B) = Uanis(C21A) = Uanis(C21B) = Uanis(C22A) =
Uanis(C22B)
Uanis(C14A) = Uanis(C14B) = Uanis(C15) = Uanis(C20) = Uanis(C19) = Uanis(C18) =
Uanis(C17) = Uanis(C16)
Uanis(C45B) = Uanis(C45A) = Uanis(C44B) = Uanis(C44A) = Uanis(N11) = Uanis(C46)
= Uanis(O3)
Uanis(C42) = Uanis(C43B) = Uanis(C43A)
Uanis(F6A) = Uanis(F6B) = Uanis(F7B) = Uanis(F7A) = Uanis(F5B) = Uanis(F5A) =
Uanis(F8)
Uanis(F3B) = Uanis(F3A) = Uanis(F1) = Uanis(F2A) = Uanis(F2B) = Uanis(F4A) =
Uanis(F4B)
Uanis(B2) = Uanis(B1)
4. Others
 Sof(N5B)=Sof(H1B)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C13B)=Sof(H13C)=Sof(H13D)=
 Sof(C14B)=Sof(C21B)=Sof(H21C)=Sof(H21D)=Sof(C22B)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=Sof(C23B)=Sof(H23C)=Sof(H23D)=Sof(C24B)=Sof(H24C)=Sof(H24D)=
 Sof(C34B)=Sof(H34C)=Sof(H34D)=Sof(H42C)=Sof(H42D)=Sof(C43B)=Sof(H43D)=
 Sof(H43E)=Sof(H43F)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(F7B)=
 Sof(C44B)=Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C45B)=Sof(H45D)=Sof(H45E)=
 Sof(H45F)=1-FVAR(1)
 Sof(N5A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C13A)=Sof(H13A)=Sof(H13B)=
 Sof(C14A)=Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(C22A)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(C24A)=Sof(H24A)=Sof(H24B)=
 Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H42A)=Sof(H42B)=Sof(C43A)=Sof(H43A)=
 Sof(H43B)=Sof(H43C)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(F7A)=
 Sof(C44A)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C45A)=Sof(H45A)=Sof(H45B)=
 Sof(H45C)=FVAR(1)
5.a Rotating group:
 O2(H2A,H2B)
5.b Ternary CH refined with riding coordinates:
 C1(H1A), C1(H1B)
5.c Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C2B(H2BA,H2BB), C3(H3A,H3B), C11(H11A,H11B), C13A(H13A,H13B),
 C13B(H13C,H13D), C21A(H21A,H21B), C21B(H21C,H21D), C23A(H23A,H23B), C23B(H23C,
 H23D), C24A(H24A,H24B), C24B(H24C,H24D), C32(H32A,H32B), C34A(H34A,H34B),
 C34B(H34C,H34D), C42(H42A,H42B), C42(H42C,H42D)
5.d Me refined with riding coordinates:
 C22A(H22A,H22B,H22C), C22B(H22D,H22E,H22F), C43A(H43A,H43B,H43C), C43B(H43D,
 H43E,H43F), C44A(H44A,H44B,H44C), C44B(H44D,H44E,H44F)
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),
 C27(H27), C28(H28), C29(H29), C30(H30), C37(H37), C38(H38), C39(H39), C40(H40),
  C46(H46)
5.f Tetrahedral OH refined with riding coordinates:
 S1(H1)
5.g Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C33(H33A,H33B,H33C), C45A(H45A,H45B,H45C), C45B(H45D,
 H45E,H45F)
;
_shelx_res_checksum              76203
_olex2_submission_special_instructions 'No special instructions were received'