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_7048482
_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 H64 Fe2 N12 O3 S, 2(B F4), 2(C3 H7 N O)'
_chemical_formula_sum            'C55 H78 B2 F8 Fe2 N14 O5 S'
_chemical_formula_weight         1332.69
_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                102.922(5)
_cell_angle_beta                 96.739(5)
_cell_angle_gamma                98.616(6)
_cell_formula_units_Z            2
_cell_length_a                   12.226(2)
_cell_length_b                   15.384(3)
_cell_length_c                   18.398(3)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.51
_cell_measurement_theta_min      2.33
_cell_volume                     3293.6(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 0.980
_diffrn_measured_fraction_theta_max 0.971
_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  0.0653
_diffrn_reflns_av_unetI/netI     0.0866
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.971
_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       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26542
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.619
_diffrn_reflns_theta_min         2.300
_diffrn_source_type              Micro-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1305 before and 0.0859 after correction.
The Ratio of minimum to maximum transmission is 0.6169.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         12066
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1296
_refine_ls_R_factor_gt           0.0918
_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^)+(0.0520P)^2^+20.1470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2053
_refine_ls_wR_factor_ref         0.2338
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8328
_reflns_number_total             12066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04092c2.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 7048480--7048483.cif.'
_cod_original_cell_volume        3293.5(10)
_cod_database_code               7048482
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.889
_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. Restrained distances
 S1-H1
 1.2 with sigma of 0.02
 N12-C48B \\sim N12-C48A \\sim N12-C49A \\sim N12-C49B
 with sigma of 0.02
 F4B-B1 \\sim F4A-B1
 with sigma of 0.02
 F5-B2 \\sim F7B-B2 \\sim F7A-B2 \\sim F6A-B2 \\sim F6B-B2 \\sim F8A-B2 \\sim
F8B-B2
 with sigma of 0.02
 C2A-C1 \\sim C23A-C1 \\sim C2B-C1 \\sim C23B-C1
 with sigma of 0.02
 N6-C23A \\sim N6-C23B \\sim N1-C2B \\sim N1-C2A
 with sigma of 0.02
 N6-C24A \\sim N6-C24B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C47) = Uanis(C48A) = Uanis(C48B) = Uanis(C49A) = Uanis(C49B)
Uanis(F5) = Uanis(F7B) = Uanis(F7A) = Uanis(F6A) = Uanis(F6B) = Uanis(F8B) =
Uanis(F8A)
Uanis(F1) = Uanis(F4A) = Uanis(F4B)
Uanis(C23A) = Uanis(C2A) = Uanis(C2B) = Uanis(C23B) = Uanis(C24A) = Uanis(C24B)
Uanis(N7) = Uanis(N8)
4. Others
 Sof(H1B)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C23B)=Sof(H23C)=Sof(H23D)=Sof(C24B)=
 Sof(H24C)=Sof(H24D)=Sof(C48B)=Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(C49B)=
 Sof(H49D)=Sof(H49E)=Sof(H49F)=Sof(F4B)=Sof(F6B)=Sof(F7B)=Sof(F8B)=1-FVAR(1)
 Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(C24A)=
 Sof(H24A)=Sof(H24B)=Sof(C48A)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C49A)=
 Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(F4A)=Sof(F6A)=Sof(F7A)=Sof(F8A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1A), C1(H1B)
5.b Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C2B(H2BA,H2BB), C3(H3A,H3B), C11(H11A,H11B), C13(H13A,H13B),
 C21(H21A,H21B), C23A(H23A,H23B), C23B(H23C,H23D), C24A(H24A,H24B), C24B(H24C,
 H24D), C32(H32A,H32B), C34(H34A,H34B), C42(H42A,H42B)
5.c 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),
  C44(H44), C47(H47), C50(H50), C53(H53)
5.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C33(H33A,H33B,H33C), C43(H43A,H43B,
 H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C48A(H48A,H48B,H48C),
 C48B(H48D,H48E,H48F), C49A(H49A,H49B,H49C), C49B(H49D,H49E,H49F), C51(H51A,
 H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C)
;
_shelx_res_checksum              19376
_shelx_fab_checksum              4670
_olex2_submission_special_instructions 'No special instructions were received'