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_4347536
_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         'C47 H58 Fe2 N10 O S, C3 H7 N O, 2(B F4)'
_chemical_formula_sum            'C50 H65 B2 F8 Fe2 N11 O2 S'
_chemical_formula_weight         1169.51
_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             2015-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                112.044(13)
_cell_angle_beta                 92.360(13)
_cell_angle_gamma                99.652(13)
_cell_formula_units_Z            2
_cell_length_a                   13.243(7)
_cell_length_b                   15.246(9)
_cell_length_c                   16.716(9)
_cell_measurement_reflns_used    6338
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.46
_cell_measurement_theta_min      2.17
_cell_volume                     3064(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.985
_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  0.0469
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30838
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.651
_diffrn_reflns_theta_min         1.323
_diffrn_source_type              'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1138 before and 0.0493 after correction.
The Ratio of minimum to maximum transmission is 0.9070.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.170
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         11450
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0796
_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^)+(0.1083P)^2^+5.1409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2080
_refine_ls_wR_factor_ref         0.2223
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8082
_reflns_number_total             11450
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00316_si_002.cif
_cod_data_source_block           StBu
_cod_database_code               4347536
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.837
_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
 F5-B2 \\sim F7A-B2 \\sim F7A-B2 \\sim F8A-B2 \\sim F8A-B2 \\sim F6A-B2 \\sim
F6A-B2
 with sigma of 0.02
 F1B-B1B \\sim F2B-B1B \\sim F3B-B1B \\sim F3A-B1A \\sim F1A-B1A \\sim F2A-B1A
\\sim F4B-B1B \\sim F4A-B1A
 with sigma of 0.02
 C23B-C1B \\sim C2B-C1B \\sim C2A-C1A \\sim C23A-C1A
 with sigma of 0.02
 N1-C2A \\sim N1-C2B \\sim N6-C23A \\sim N6-C23B
 with sigma of 0.02
 C43-C42 \\sim C33B-C32B \\sim C33A-C32A
 with sigma of 0.02
 N6-C23B \\sim N6-C23A
 with sigma of 0.02
 C46A-C44 \\sim C46A-C44 \\sim C45A-C44 \\sim C45A-C44 \\sim C47A-C44
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C11B) = Uanis(C11A)
Uanis(C4) = Uanis(C11A) = Uanis(C11B) = Uanis(C12B) = Uanis(C12A)
Uanis(F5) = Uanis(F6B) = Uanis(F6A) = Uanis(F7B) = Uanis(F7A) = Uanis(F8A) =
Uanis(F8B)
Uanis(B1B) = Uanis(B1A)
Uanis(F1B) = Uanis(F1A) = Uanis(F2B) = Uanis(F2A) = Uanis(F3B) = Uanis(F3A) =
Uanis(F4B) = Uanis(F4A)
Uanis(O1B) = Uanis(O1A)
Uanis(C23B) = Uanis(C23A) = Uanis(C1B) = Uanis(C1A) = Uanis(C2B) = Uanis(C2A)
Uanis(C32A) = Uanis(C33A) = Uanis(C32B) = Uanis(C33B)
Uanis(C26) = Uanis(C31) = Uanis(C32A) = Uanis(C32B) = Uanis(C33B) = Uanis(C33A)
Uanis(C15) = Uanis(C13)
Uanis(N7) = Uanis(C26) = Uanis(C25) = Uanis(N8) = Uanis(C31)
Uanis(C25) = Uanis(C24) = Uanis(C34) = Uanis(C35)
Uanis(C45A) = Uanis(C45A) = Uanis(C47A) = Uanis(C46A) = Uanis(C46A) =
Uanis(C47A)
Uanis(C44) = Uanis(C45B) = Uanis(C45A) = Uanis(C47A) = Uanis(C47B) =
Uanis(C46A) = Uanis(C46B)
4. Others
 Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C11B)=Sof(H11D)=Sof(H11E)=
 Sof(C12B)=Sof(H12C)=Sof(H12D)=Sof(H12E)=Sof(C23B)=Sof(H23C)=Sof(H23D)=
 Sof(C32B)=Sof(H32C)=Sof(H32D)=Sof(C33B)=Sof(H33D)=Sof(H33E)=Sof(H33F)=
 Sof(C45B)=Sof(H45D)=Sof(H45E)=Sof(H45F)=Sof(C46B)=Sof(H46D)=Sof(H46E)=
 Sof(H46F)=Sof(C47B)=Sof(H47D)=Sof(H47E)=Sof(H47F)=Sof(O1B)=1-FVAR(1)
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C11A)=Sof(H11A)=Sof(H11B)=
 Sof(H11C)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(C23A)=Sof(H23A)=Sof(H23B)=
 Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 Sof(C45A)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C46A)=Sof(H46A)=Sof(H46B)=
 Sof(H46C)=Sof(C47A)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(O1A)=FVAR(1)
 Sof(F6B)=Sof(F7B)=Sof(F8B)=Sof(B1B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=1-
 FVAR(2)
 Sof(F6A)=Sof(F7A)=Sof(F8A)=Sof(B1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C1A(H1A), C1B(H1B)
5.b Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C2B(H2BA,H2BB), C3(H3A,H3B), C11B(H11D,H11E), C12A(H12A,H12B),
  C13(H13A,H13B), C21(H21A,H21B), C23A(H23A,H23B), C23B(H23C,H23D), C24(H24A,
 H24B), C32A(H32A,H32B), C32B(H32C,H32D), 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),
  C50(H50)
5.d Idealised Me refined as rotating group:
 C11A(H11A,H11B,H11C), C12B(H12C,H12D,H12E), C22(H22A,H22B,H22C), C33A(H33A,
 H33B,H33C), C33B(H33D,H33E,H33F), C43(H43A,H43B,H43C), C45A(H45A,H45B,H45C),
 C45B(H45D,H45E,H45F), C46A(H46A,H46B,H46C), C46B(H46D,H46E,H46F), C47A(H47A,
 H47B,H47C), C47B(H47D,H47E,H47F), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              77068
_shelx_hkl_checksum              58085
_olex2_submission_special_instructions 'No special instructions were received'