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_4347534
_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         'C44 H52 Fe2 N10 O S, C3 H7 N O, 2(B F4)'
_chemical_formula_sum            'C47 H59 B2 F8 Fe2 N11 O2 S'
_chemical_formula_weight         1127.43
_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                 98.310(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.083(3)
_cell_length_b                   23.097(5)
_cell_length_c                   16.129(3)
_cell_measurement_reflns_used    4157
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.26
_cell_measurement_theta_min      2.18
_cell_volume                     5191.3(18)
_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 0.995
_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  0.0837
_diffrn_reflns_av_unetI/netI     0.1023
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19521
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.804
_diffrn_reflns_theta_min         1.551
_diffrn_source_type              'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1134 before and 0.0616 after correction.
The Ratio of minimum to maximum transmission is 0.7347.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.019
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         9949
_refine_ls_number_restraints     177
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.1979
_refine_ls_R_factor_gt           0.1121
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3192
_refine_ls_wR_factor_ref         0.3790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4673
_reflns_number_total             9949
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00316_si_002.cif
_cod_data_source_block           SMe
_cod_original_cell_volume        5191.1(18)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4347534
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.888
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C5A-C10A \\sim C9A-C10A \\sim C9A-C8A \\sim C8A-C7A \\sim C7A-C6A \\sim C6A-C5A
 with sigma of 0.02
 C6B-C5B \\sim C7B-C6B \\sim C8B-C7B \\sim C9B-C8B \\sim C9B-C10B \\sim C5B-C10B
 with sigma of 0.02
 Fe1-N2B \\sim Fe1-N2A
 with sigma of 0.02
 C4B-C3B \\sim C4B-N2B \\sim C4B-N3B
 with sigma of 0.02
 C4A-C3B \\sim C4A-N2B \\sim C4A-N3B
 with sigma of 0.02
 C3B-N2B \\sim N2B-N3B \\sim C3B-N3B
 with sigma of 0.02
 C12B-C12A \\sim C11A-C11B
 with sigma of 0.02
 N1A-C3A \\sim N1B-C3B
 with sigma of 0.02
 N1A-C13A \\sim N1B-C13B
 with sigma of 0.02
 C4B-C3B \\sim C4A-C3A
 with sigma of 0.02
 N2B-C5B \\sim N2A-C5A \\sim N3B-C10B \\sim N3A-C10A
 with sigma of 0.02
 N3B-C11B \\sim N3A-C11A
 with sigma of 0.02
 C12B-C11B \\sim C12A-C11A
 with sigma of 0.02
 N10A-C42A \\sim N10B-C42B
 with sigma of 0.02
 C43A-C42A \\sim C43B-C42B
 with sigma of 0.02
 Fe2-N9B \\sim Fe2-N9A
 with sigma of 0.02
 N6B-C34B \\sim N6B-C23B \\sim N6A-C34A \\sim N6A-C24
 with sigma of 0.02
 C35A-C34A \\sim C35B-C34B
 with sigma of 0.02
 N10A-C35A \\sim N10B-C35B \\sim N9A-C35A \\sim N9B-C35B
 with sigma of 0.02
 N9A-C36A \\sim N9B-C36B \\sim N10B-C41B \\sim N10A-C41A
 with sigma of 0.02
 C41B-C40B \\sim C40B-C39B \\sim C39B-C38B \\sim C38B-C37B \\sim C37B-C36B
\\sim C41B-C36B
 with sigma of 0.02
 C41A-C40A \\sim C40A-C39A \\sim C39A-C38A \\sim C38A-C37A \\sim C37A-C36A
\\sim C41A-C36A
 with sigma of 0.02
 F3A-B1A \\sim F3B-B1B \\sim F1A-B1A \\sim F1B-B1B \\sim F4A-B1A \\sim F4B-B1B
\\sim F2A-B1A \\sim F2B-B1B
 with sigma of 0.02
 F7B-B2 \\sim F7A-B2 \\sim F5B-B2 \\sim F6A-B2 \\sim F6B-B2 \\sim F5A-B2 \\sim
F8A-B2 \\sim F8B-B2
 with sigma of 0.02
 O1-C1A \\sim O1-C1B
 with sigma of 0.02
 N5-C21A \\sim N5-C21B
 with sigma of 0.02
 C22B-C21B \\sim C22A-C21A
 with sigma of 0.02
 N11-C46 \\sim N11-C45A \\sim N11-C45B
 with sigma of 0.02
3. Restrained planarity
 C36B, C37B, C38B, C39B, C41B, C40B
 with sigma of 0.1
 C36A, C41A, C40A, C39A, C38A, C37A
 with sigma of 0.1
 C9B, C10B, C5B, C6B, C7B, C8B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C23A) = Uanis(C23B)
Uanis(C2A) = Uanis(C2B) = Uanis(C3A) = Uanis(C3B)
Uanis(C10A) = Uanis(C5A) = Uanis(C6A) = Uanis(C6B) = Uanis(C5B) = Uanis(C7A) =
Uanis(C7B) = Uanis(C8A) = Uanis(C8B) = Uanis(C9B) = Uanis(C9A) = Uanis(C10B)
Uanis(N2B) = Uanis(N2A) = Uanis(N3B) = Uanis(N3A) = Uanis(N1B) = Uanis(N1A) =
Uanis(C4A) = Uanis(C4B) = Uanis(C12B) = Uanis(C12A) = Uanis(C11B) = Uanis(C11A)
Uanis(C13A) = Uanis(C13B)
Uanis(C14) = Uanis(C13B) = Uanis(C13A)
Uanis(C21A) = Uanis(C21B) = Uanis(C22A) = Uanis(C22B)
Uanis(N5) = Uanis(C21A) = Uanis(C21B) = Uanis(C22A) = Uanis(C22B)
Uanis(C18) = Uanis(C17) = Uanis(C19)
Uanis(S1A) = Uanis(S1B)
Uanis(C44A) = Uanis(C44B)
Uanis(C34A) = Uanis(C34B)
Uanis(C35A) = Uanis(C35B)
Uanis(C43A) = Uanis(C43B) = Uanis(C42A) = Uanis(C42B)
Uanis(N6A) = Uanis(N6B) = Uanis(N9A) = Uanis(N9B) = Uanis(N10A) = Uanis(N10B)
Uanis(C39A) = Uanis(C39B) = Uanis(C38A) = Uanis(C38B) = Uanis(C37A) =
Uanis(C37B) = Uanis(C36A) = Uanis(C36B) = Uanis(C41A) = Uanis(C41B) =
Uanis(C40A) = Uanis(C40B)
Uanis(B1A) = Uanis(B1B)
Uanis(F2A) = Uanis(F2B) = Uanis(F3A) = Uanis(F3B) = Uanis(F4A) = Uanis(F4B) =
Uanis(F1A) = Uanis(F1B)
Uanis(F6B) = Uanis(F6A)
Uanis(F7A) = Uanis(F7B) = Uanis(F5A) = Uanis(F5B) = Uanis(F8A) = Uanis(F8B) =
Uanis(F6B) = Uanis(F6A)
Uanis(C33A) = Uanis(C33B)
Uanis(C1A) = Uanis(C1B)
Uanis(C46) = Uanis(C45A) = Uanis(C45B)
5. Others
 Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=
 Sof(C4B)=Sof(C5B)=Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8B)=
 Sof(C9B)=Sof(H9B)=Sof(C10B)=Sof(C11B)=Sof(H11C)=Sof(H11D)=Sof(C12B)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=Sof(C13B)=Sof(H13C)=Sof(H13D)=Sof(C21B)=Sof(H21C)=
 Sof(H21D)=Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C23B)=Sof(H23C)=
 Sof(H23D)=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(C36B)=
 Sof(C37B)=Sof(H37B)=Sof(C38B)=Sof(H38B)=Sof(C39B)=Sof(H39B)=Sof(C40B)=
 Sof(H40B)=Sof(C41B)=Sof(C42B)=Sof(H42C)=Sof(H42D)=Sof(C43B)=Sof(H43D)=
 Sof(H43E)=Sof(H43F)=Sof(N1B)=Sof(N2B)=Sof(N3B)=Sof(N6B)=Sof(N9B)=Sof(N10B)=
 Sof(C45B)=Sof(H45D)=Sof(H45E)=Sof(H45F)=1-FVAR(1)
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=
 Sof(C4A)=Sof(C5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=
 Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C12A)=Sof(H12A)=
 Sof(H12B)=Sof(H12C)=Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(C21A)=Sof(H21A)=
 Sof(H21B)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23A)=Sof(H23A)=
 Sof(H23B)=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(C36A)=
 Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(H39A)=Sof(C40A)=
 Sof(H40A)=Sof(C41A)=Sof(C42A)=Sof(H42A)=Sof(H42B)=Sof(C43A)=Sof(H43A)=
 Sof(H43B)=Sof(H43C)=Sof(N1A)=Sof(N2A)=Sof(N3A)=Sof(N6A)=Sof(N9A)=Sof(N10A)=
 Sof(C45A)=Sof(H45A)=Sof(H45B)=Sof(H45C)=FVAR(1)
 Sof(C44B)=Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(S1B)=1-FVAR(2)
 Sof(C44A)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(S1A)=FVAR(2)
 Sof(B1B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(F7B)=
 Sof(F8B)=1-FVAR(3)
 Sof(B1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(F7A)=
 Sof(F8A)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C1A(H1A), C1B(H1B)
6.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), C21A(H21A,H21B),
 C21B(H21C,H21D), C23A(H23A,H23B), C23B(H23C,H23D), C24(H24A,H24B), C24(H24C,
 H24D), C32(H32A,H32B), C32(H32C,H32D), C34A(H34A,H34B), C34B(H34C,H34D),
 C42A(H42A,H42B), C42B(H42C,H42D)
6.c Aromatic/amide H refined with riding coordinates:
 C6A(H6A), C6B(H6B), C7A(H7A), C7B(H7B), C8A(H8A), C8B(H8B), C9A(H9A),
 C9B(H9B), C16(H16), C17(H17), C18(H18), C19(H19), C27(H27), C28(H28), C29(H29),
  C30(H30), C37A(H37A), C37B(H37B), C38A(H38A), C38B(H38B), C39A(H39A),
 C39B(H39B), C40A(H40A), C40B(H40B), C47(H47)
6.d Idealised Me refined as rotating group:
 C12A(H12A,H12B,H12C), C12B(H12D,H12E,H12F), C22A(H22A,H22B,H22C), C22B(H22D,
 H22E,H22F), C33A(H33A,H33B,H33C), C33B(H33D,H33E,H33F), C43A(H43A,H43B,H43C),
 C43B(H43D,H43E,H43F), C44A(H44A,H44B,H44C), C44B(H44D,H44E,H44F), C45A(H45A,
 H45B,H45C), C45B(H45D,H45E,H45F), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              85003
_shelx_hkl_checksum              5743
_olex2_submission_special_instructions 'No special instructions were received'