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_4347540
_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         'C51 H64 Fe2 N10 O3 S, 2(B F4)'
_chemical_formula_sum            'C51 H64 B2 F8 Fe2 N10 O3 S'
_chemical_formula_weight         1182.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                104.020(5)
_cell_angle_beta                 93.043(4)
_cell_angle_gamma                106.951(4)
_cell_formula_units_Z            2
_cell_length_a                   13.068(2)
_cell_length_b                   13.342(2)
_cell_length_c                   17.830(3)
_cell_measurement_reflns_used    1884
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.76
_cell_measurement_theta_min      2.28
_cell_volume                     2859.3(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 0.992
_diffrn_measured_fraction_theta_max 0.984
_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  0.0962
_diffrn_reflns_av_unetI/netI     0.1324
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29469
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.740
_diffrn_reflns_theta_min         1.644
_diffrn_source_type              'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1002 before and 0.0565 after correction.
The Ratio of minimum to maximum transmission is 0.8524.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         10753
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1637
_refine_ls_R_factor_gt           0.0792
_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^)+(0.1075P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1898
_refine_ls_wR_factor_ref         0.2272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5184
_reflns_number_total             10753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00316_si_002.cif
_cod_data_source_block           Mercaptooctanoic
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4347540
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.941
_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
 C48A-C47 \\sim C49A-C48A \\sim C50A-C49A \\sim C51A-C50A \\sim C47-C48B \\sim
C48B-C49B \\sim C49B-
 C50B \\sim C50B-C51B \\sim C51A-C50A
 with sigma of 0.02
 F8A-B2 \\sim F8B-B2 \\sim F5A-B2 \\sim F5B-B2 \\sim F7B-B2 \\sim F7A-B2 \\sim
F6B-B2 \\sim F6A-B2
 with sigma of 0.02
 C37-C36 \\sim C38B-C37 \\sim C38A-C37 \\sim C39B-C38B \\sim C39A-C38A \\sim
C40B-C39B \\sim C40A-C39A
 \\sim C41B-C40B \\sim C41A-C40A \\sim C41B-C36 \\sim C41A-C36
 with sigma of 0.02
 S1-C51B \\sim S1-C51A
 with sigma of 0.02
 C46-C45 \\sim C47-C46 \\sim C48A-C47 \\sim C48B-C47 \\sim C49B-C48B \\sim
C49A-C48A \\sim C50A-C49A ~
 C50B-C49B \\sim C51B-C50B \\sim C51A-C50A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C50B) = Uanis(C50A) = Uanis(C51B) = Uanis(C51A)
Uanis(C44) = Uanis(C45) = Uanis(C46) = Uanis(C47) = Uanis(C48B) = Uanis(C48A) =
Uanis(C49A) = Uanis(C49B)
Uanis(C20) = Uanis(C19) = Uanis(C18) = Uanis(C17) = Uanis(C16) = Uanis(C15)
Uanis(F6A) = Uanis(F6B) = Uanis(F7A) = Uanis(F7B)
Uanis(F5A) = Uanis(F5B) = Uanis(F8B) = Uanis(F8A)
Uanis(F2) = Uanis(F4A) = Uanis(F4B) = Uanis(F1A) = Uanis(F1B) = Uanis(F3A) =
Uanis(F3B)
Uanis(N9) = Uanis(N10B) = Uanis(N10A) = Uanis(C43B) = Uanis(C43A) = Uanis(C42B)
= Uanis(C42A)
Uanis(C36) = Uanis(C38A) = Uanis(C38B) = Uanis(C39A) = Uanis(C39B) =
Uanis(C40A) = Uanis(C41A) = Uanis(C41B) = Uanis(C40B)
Uanis(C3) = Uanis(C24)
4. Others
 Sof(H37A)=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(H47C)=Sof(H47D)=Sof(C48B)=Sof(H48C)=Sof(H48D)=Sof(C49B)=
 Sof(H49C)=Sof(H49D)=Sof(N10B)=1-FVAR(1)
 Sof(H37)=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(H47A)=Sof(H47B)=Sof(C48A)=Sof(H48A)=Sof(H48B)=Sof(C49A)=
 Sof(H49A)=Sof(H49B)=Sof(N10A)=FVAR(1)
 Sof(C50B)=Sof(H50C)=Sof(H50D)=Sof(C51B)=Sof(H51C)=Sof(H51D)=Sof(H1B)=1-FVAR(2)
 Sof(C50A)=Sof(H50A)=Sof(H50B)=Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(H1A)=FVAR(2)
 Sof(F5B)=Sof(F6B)=Sof(F7B)=Sof(F8B)=Sof(F1B)=Sof(F3B)=Sof(F4B)=1-FVAR(3)
 Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(F8A)=Sof(F1A)=Sof(F3A)=Sof(F4A)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C11(H11A,H11B), C13(H13A,H13B), C21(H21A,H21B),
 C23(H23A,H23B), C24(H24A,H24B), C32(H32A,H32B), C34(H34A,H34B), C42A(H42A,
 H42B), C42B(H42C,H42D), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
 C47(H47C,H47D), C48A(H48A,H48B), C48B(H48C,H48D), C49A(H49A,H49B), C49B(H49C,
 H49D), C50A(H50A,H50B), C50B(H50C,H50D), C51A(H51A,H51B), C51B(H51C,H51D)
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), C37(H37A), C38A(H38A),
 C38B(H38B), C39A(H39A), C39B(H39B), C40A(H40A), C40B(H40B)
5.d Tetrahedral OH refined with riding coordinates:
 S1(H1A), S1(H1B)
5.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C33(H33A,H33B,H33C), C43A(H43A,H43B,
 H43C), C43B(H43D,H43E,H43F)
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_shelx_res_checksum              21414
_shelx_hkl_checksum              80932
_olex2_submission_special_instructions 'No special instructions were received'