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_4347541
_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 H56 Fe2 N10 O4, 2(B F4)'
_chemical_formula_sum            'C47 H56 B2 F8 Fe2 N10 O4'
_chemical_formula_weight         1110.33
_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                 97.040(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7884(10)
_cell_length_b                   22.7777(17)
_cell_length_c                   15.8097(12)
_cell_measurement_reflns_used    2123
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.61
_cell_measurement_theta_min      2.27
_cell_volume                     4927.9(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.992
_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  0.1608
_diffrn_reflns_av_unetI/netI     0.1230
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            50198
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.788
_diffrn_reflns_theta_min         1.576
_diffrn_source_type              'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1098 before and 0.0689 after correction.
The Ratio of minimum to maximum transmission is 0.8670.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         9379
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1704
_refine_ls_R_factor_gt           0.0832
_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^)+(0.0736P)^2^+17.1750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1762
_refine_ls_wR_factor_ref         0.2172
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4891
_reflns_number_total             9379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00316_si_002.cif
_cod_data_source_block           GHB
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4347541
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.866
_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, All O(H) groups
2. Restrained distances
 N3B-C11B \\sim N3A-C11A
 with sigma of 0.02
 C12B-C11B \\sim C12A-C11A
 with sigma of 0.02
 N3B-C11B \\sim N3A-C11A
 with sigma of 0.02
 N1-C13B \\sim N1-C13A \\sim N1-C3B \\sim N1-C3A \\sim N1-C2B \\sim N1-C2A
 with sigma of 0.02
 N6-C23B \\sim N6-C23A \\sim N6-C34B \\sim N6-C34A \\sim N6-C24A \\sim N6-C24B
 with sigma of 0.02
 N10A-C35A \\sim N10B-C35B \\sim N9-C35A \\sim N9-C35B
 with sigma of 0.02
 N10B-C42B \\sim N10A-C43A
 with sigma of 0.02
 C43A-C42A \\sim C43B-C42B
 with sigma of 0.02
 C14-C13B \\sim C14-C13A
 with sigma of 0.02
 C4B-C3B \\sim C4A-C3A
 with sigma of 0.02
 C35B-C34B \\sim C35A-C34A
 with sigma of 0.02
 F4-B1 \\sim F3B-B1 \\sim F3A-B1 \\sim F1A-B1 \\sim F2A-B1 \\sim F2B-B1 \\sim
F1B-B1
 with sigma of 0.02
 F8-B2 \\sim F5B-B2 \\sim F5A-B2 \\sim F6-B2 \\sim F7-B2
 with sigma of 0.02
 O4A-C47 \\sim O4B-C47
 with sigma of 0.02
 C22A-C21 \\sim C22B-C21
 with sigma of 0.02
 C33A-C32 \\sim C33B-C32
 with sigma of 0.02
 C12A-C11A \\sim C12B-C11B
 with sigma of 0.02
 N3B-C11B \\sim N3A-C11A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C23B) = Uanis(C23A)
Uanis(C2B) = Uanis(C2A)
Uanis(C3B) = Uanis(C3A)
Uanis(N2) = Uanis(C4B) = Uanis(C4A) = Uanis(N3B) = Uanis(N3A)
Uanis(C14) = Uanis(C13B) = Uanis(C13A)
Uanis(C21) = Uanis(C22B) = Uanis(C22A)
Uanis(C32) = Uanis(C33A) = Uanis(C33B)
Uanis(C25) = Uanis(C24B) = Uanis(C24A)
Uanis(C34B) = Uanis(C34A)
Uanis(N9) = Uanis(N10B) = Uanis(N10A) = Uanis(C42B) = Uanis(C43A) = Uanis(C42A)
= Uanis(C43B) = Uanis(C35A) = Uanis(C35B)
Uanis(C41) = Uanis(C36) = Uanis(C37) = Uanis(C38) = Uanis(C39) = Uanis(C40)
Uanis(F4) = Uanis(F2A) = Uanis(F2B) = Uanis(F3A) = Uanis(F3B) = Uanis(F1A) =
Uanis(F1B)
Uanis(F5A) = Uanis(F5B)
Uanis(F8) = Uanis(F5A) = Uanis(F5B)
Uanis(O4A) = Uanis(O4B)
Uanis(C12B) = Uanis(C12A) = Uanis(C11B) = Uanis(C11A)
4. Others
 Sof(H1B)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(C4B)=
 Sof(C11B)=Sof(H11C)=Sof(H11D)=Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=
 Sof(C13B)=Sof(H13C)=Sof(H13D)=Sof(H21C)=Sof(H21D)=Sof(C22B)=Sof(H22D)=
 Sof(H22E)=Sof(H22F)=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(H42D)=Sof(H42E)=
 Sof(C43B)=Sof(H43C)=Sof(H43D)=Sof(H43E)=Sof(N3B)=Sof(N10B)=1-FVAR(1)
 Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=
 Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=
 Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(H21A)=Sof(H21B)=Sof(C22A)=Sof(H22A)=
 Sof(H22B)=Sof(H22C)=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(H42C)=Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(N3A)=Sof(N10A)=FVAR(1)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F5B)=1-FVAR(2)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F5A)=FVAR(2)
 Sof(H47C)=Sof(H47D)=Sof(O4B)=Sof(H4B)=1-FVAR(3)
 Sof(H47A)=Sof(H47B)=Sof(O4A)=Sof(H4A)=FVAR(3)
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),
 C21(H21C,H21D), C23A(H23A,H23B), C23B(H23C,H23D), C24A(H24A,H24B), C24B(H24C,
 H24D), C32(H32A,H32B), C32(H32C,H32D), C34A(H34A,H34B), C34B(H34C,H34D),
 C42B(H42D,H42E), C43A(H43A,H43B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,
 H47B), C47(H47C,H47D)
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 Idealised Me refined with riding coordinates:
 C12A(H12A,H12B,H12C), C12B(H12D,H12E,H12F)
5.e Idealised Me refined as rotating group:
 C22A(H22A,H22B,H22C), C22B(H22D,H22E,H22F), C33A(H33A,H33B,H33C), C33B(H33D,
 H33E,H33F), C42A(H42A,H42B,H42C), C43B(H43C,H43D,H43E)
5.f Idealised tetrahedral OH refined as rotating group:
 O4A(H4A), O4B(H4B)
;
_shelx_res_checksum              95862
_shelx_hkl_checksum              70558
_olex2_submission_special_instructions 'No special instructions were received'