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_4347537
_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         'C52 H61 Fe2 N11 O2 S, 2(B F4)'
_chemical_formula_sum            'C52 H61 B2 F8 Fe2 N11 O2 S'
_chemical_formula_weight         1189.49
_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                 97.948(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0909(11)
_cell_length_b                   22.8058(18)
_cell_length_c                   18.7389(14)
_cell_measurement_reflns_used    3099
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      15.63
_cell_measurement_theta_min      2.19
_cell_volume                     6387.2(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 0.992
_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  0.1382
_diffrn_reflns_av_unetI/netI     0.1161
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            67157
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.029
_diffrn_reflns_theta_min         1.415
_diffrn_source_type              'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1016 before and 0.0690 after correction.
The Ratio of minimum to maximum transmission is 0.8551.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.042
_refine_diff_density_min         -0.948
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         12499
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1695
_refine_ls_R_factor_gt           0.0924
_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^)+(0.1567P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2503
_refine_ls_wR_factor_ref         0.2896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5768
_reflns_number_total             12499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00316_si_002.cif
_cod_data_source_block           SPh
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4347537
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.897
_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
 N11-C52A \\sim N11-C52B \\sim N11-C51B \\sim N11-C51A
 with sigma of 0.02
 F4A-B1A \\sim F4B-B1B \\sim F2B-B1B \\sim F2A-B1A \\sim F1B-B1B \\sim F1A-B1A
\\sim F3B-B1B \\sim F3A-B1A
 with sigma of 0.02
 F8B-B2B \\sim F8A-B2A
 with sigma of 0.02
 F7B-B2B \\sim F7A-B2A
 with sigma of 0.02
 F6B-B2B \\sim F6A-B2A
 with sigma of 0.02
 F5B-B2B \\sim F5A-B2A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(B2B) = Uanis(B2A)
Uanis(F5B) = Uanis(F5A)
Uanis(F8B) = Uanis(F8A) = Uanis(F6A) = Uanis(F6B)
Uanis(F1A) = Uanis(F1B) = Uanis(F4B) = Uanis(F4A) = Uanis(F3B) = Uanis(F2B) =
Uanis(F2A) = Uanis(F3A) = Uanis(B1A) = Uanis(B1B)
Uanis(F7A) = Uanis(F7B)
Uanis(C52A) = Uanis(C52B) = Uanis(C51A) = Uanis(C51B)
Uanis(C29) = Uanis(C30)
4. Others
 Sof(C51B)=Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(C52B)=Sof(H52D)=Sof(H52E)=
 Sof(H52F)=1-FVAR(1)
 Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C52A)=Sof(H52A)=Sof(H52B)=
 Sof(H52C)=FVAR(1)
 Sof(B1B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=1-FVAR(2)
 Sof(B1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=FVAR(2)
 Sof(B2B)=Sof(F5B)=Sof(F6B)=Sof(F7B)=Sof(F8B)=1-FVAR(3)
 Sof(B2A)=Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(F8A)=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), 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),
  C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50)
5.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C33(H33A,H33B,H33C), C43(H43A,H43B,
 H43C), C51A(H51A,H51B,H51C), C51B(H51D,H51E,H51F), C52A(H52A,H52B,H52C),
 C52B(H52D,H52E,H52F)
;
_shelx_res_checksum              10822
_shelx_hkl_checksum              95855
_olex2_submission_special_instructions 'No special instructions were received'