Controlling the Reactivity of Bifunctional Ligands: Carboxylate-Bridged Nonheme Diiron(II) Complexes Bearing Free Thiol Groups.
Pal, Nabhendu; Majumdar, Amit; Inorganic chemistry 55 (2016) 3181–3191; doi:10.1021/acs.inorgchem.6b00316

data_4347539
_publ_section_title
;
 Controlling the Reactivity of Bifunctional Ligands: Carboxylate-Bridged
 Nonheme Diiron(II) Complexes Bearing Free Thiol Groups.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3181
_journal_page_last               3191
_journal_paper_doi               10.1021/acs.inorgchem.6b00316
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C46 H54 Fe2 N10 O3 S, 2(B F4)'
_chemical_formula_sum            'C46 H54 B2 F8 Fe2 N10 O3 S'
_chemical_formula_weight         1112.37
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-09-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.023(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9029(14)
_cell_length_b                   22.561(2)
_cell_length_c                   15.7300(16)
_cell_measurement_reflns_used    8202
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.37
_cell_measurement_theta_min      2.25
_cell_volume                     4906.7(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.7-1 (Bruker-Axs,2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            62736
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.872
_diffrn_reflns_theta_min         1.584
_diffrn_source_type              'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1140 before and 0.0558 after correction.
The Ratio of minimum to maximum transmission is 0.9094.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.480
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         9451
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0745
_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^)+(0.0738P)^2^+20.0112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1811
_refine_ls_wR_factor_ref         0.2007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6638
_reflns_number_total             9451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00316_si_002.cif
_cod_data_source_block           3Mercapto
_cod_original_cell_volume        4906.7(9)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4347539
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.847
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3A-C11A \\sim N3B-C11B
 with sigma of 0.02
 N10A-C42A \\sim N10B-C42B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2B) = Uanis(C3B) = Uanis(C3A) = Uanis(C2A)
Uanis(C4A) = Uanis(C4B) = Uanis(N3A) = Uanis(N3B) = Uanis(C11A) = Uanis(C11B) =
Uanis(C12A) = Uanis(C12B)
Uanis(C25) = Uanis(C24B) = Uanis(C24A)
Uanis(C35A) = Uanis(C35B)
Uanis(N9) = Uanis(N10B) = Uanis(N10A)
Uanis(C43B) = Uanis(C42B)
Uanis(C21) = Uanis(C22) = Uanis(C43A) = Uanis(C42A)
Uanis(C23A) = Uanis(C23B)
Uanis(C14) = Uanis(C13B) = Uanis(C13A)
Uanis(C33A) = Uanis(C33B)
Uanis(C32) = Uanis(C33B) = Uanis(C33A)
Uanis(C45B) = Uanis(C45A) = Uanis(C46B) = Uanis(C46A)
Uanis(F2) = Uanis(F3A) = Uanis(F3B)
Uanis(F5) = Uanis(F6B) = Uanis(F6A)
Uanis(F8A) = Uanis(F8B)
4. Others
 Sof(H1B)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=1-FVAR(1)
 Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=FVAR(1)
 Sof(C4B)=Sof(C11B)=Sof(H11C)=Sof(H11D)=Sof(C12B)=Sof(H12D)=Sof(H12E)=
 Sof(H12F)=Sof(C13B)=Sof(H13C)=Sof(H13D)=Sof(N3B)=1-FVAR(2)
 Sof(C4A)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C12A)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(N3A)=FVAR(2)
 Sof(C23B)=Sof(H23C)=Sof(H23D)=Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(H32C)=
 Sof(H32D)=Sof(C33B)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C34B)=Sof(H34C)=
 Sof(H34D)=Sof(C35B)=Sof(C42B)=Sof(H42C)=Sof(H42D)=Sof(C43B)=Sof(H43D)=
 Sof(H43E)=Sof(H43F)=Sof(N10B)=1-FVAR(3)
 Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H32A)=
 Sof(H32B)=Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34A)=Sof(H34A)=
 Sof(H34B)=Sof(C35A)=Sof(C42A)=Sof(H42A)=Sof(H42B)=Sof(C43A)=Sof(H43A)=
 Sof(H43B)=Sof(H43C)=Sof(N10A)=FVAR(3)
 Sof(C45B)=Sof(H45C)=Sof(H45D)=Sof(C46B)=Sof(H46C)=Sof(H46D)=Sof(H1BB)=1-FVAR(4)
 Sof(C45A)=Sof(H45A)=Sof(H45B)=Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(H1AA)=FVAR(4)
 Sof(F6B)=Sof(F8B)=Sof(F3B)=1-FVAR(5)
 Sof(F6A)=Sof(F8A)=Sof(F3A)=FVAR(5)
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), C3A(H3AA,H3AB), C3B(H3BA,H3BB), C11A(H11A,
 H11B), C11B(H11C,H11D), C13A(H13A,H13B), C13B(H13C,H13D), C21(H21A,H21B),
 C23A(H23A,H23B), C23B(H23C,H23D), C24A(H24A,H24B), C24B(H24C,H24D), C32(H32A,
 H32B), C32(H32C,H32D), C34A(H34A,H34B), C34B(H34C,H34D), C42A(H42A,H42B),
 C42B(H42C,H42D), C45A(H45A,H45B), C45B(H45C,H45D), C46A(H46A,H46B), C46B(H46C,
 H46D)
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)
5.d Tetrahedral OH refined with riding coordinates:
 S1(H1AA), S1(H1BB)
5.e Idealised Me refined as rotating group:
 C12A(H12A,H12B,H12C), C12B(H12D,H12E,H12F), C22(H22A,H22B,H22C), C33A(H33A,
 H33B,H33C), C33B(H33D,H33E,H33F), C43A(H43A,H43B,H43C), C43B(H43D,H43E,H43F)
;
_shelx_res_checksum              46569
_shelx_hkl_checksum              21631
_olex2_submission_special_instructions 'No special instructions were received'