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_4347543
_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 H70 Fe2 N13 O4, 3(B F4), C3 H7 N O'
_chemical_formula_sum            'C55 H77 B3 F12 Fe2 N14 O5'
_chemical_formula_weight         1386.43
_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             2015-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4975)
;
_cell_angle_alpha                78.693(6)
_cell_angle_beta                 86.825(5)
_cell_angle_gamma                68.870(5)
_cell_formula_units_Z            2
_cell_length_a                   12.779(5)
_cell_length_b                   15.586(7)
_cell_length_c                   17.908(8)
_cell_measurement_reflns_used    4211
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.22
_cell_measurement_theta_min      2.26
_cell_volume                     3262(2)
_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 0.990
_diffrn_measured_fraction_theta_max 0.950
_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  0.1346
_diffrn_reflns_av_unetI/netI     0.1522
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43475
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.796
_diffrn_reflns_theta_min         1.160
_diffrn_source_type              'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1773 before and 0.0648 after correction.
The Ratio of minimum to maximum transmission is 0.6484.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       0.0168(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         13251
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1922
_refine_ls_R_factor_gt           0.0919
_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^)+(0.1421P)^2^+2.0996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2275
_refine_ls_wR_factor_ref         0.2901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6333
_reflns_number_total             13251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00316_si_002.cif
_cod_data_source_block           3DMF
_cod_database_code               4347543
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.873
_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
 O2-C44 \\sim O3B-C47B \\sim O3A-C47A
 with sigma of 0.02
 N11-C44 \\sim N12B-C47B \\sim N12A-C47A
 with sigma of 0.02
 N11-C45 \\sim N12A-C48A \\sim N12A-C49A \\sim N12B-C48B \\sim N12B-C49B
 with sigma of 0.02
 C33B-C32 \\sim C33A-C32
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3A) = Uanis(O3B)
Uanis(C47B) = Uanis(C47A)
Uanis(C49B) = Uanis(C48B)
Uanis(C48A) = Uanis(C49A)
Uanis(N11) = Uanis(N12B) = Uanis(N12A)
Uanis(C47B) = Uanis(C49B) = Uanis(C48B)
Uanis(C47A) = Uanis(C49A) = Uanis(C48A)
Uanis(O2) = Uanis(O3A) = Uanis(O3B)
Uanis(C45) = Uanis(C46) = Uanis(C47B) = Uanis(C47A) = Uanis(C49A) = Uanis(C49B)
= Uanis(C48B) = Uanis(C48A)
Uanis(F3) = Uanis(F4A) = Uanis(F4B)
Uanis(F11A) = Uanis(F11B)
Uanis(F12A) = Uanis(F12B)
Uanis(F10A) = Uanis(F10B)
Uanis(C32) = Uanis(C33B) = Uanis(C33A)
4. Others
 Sof(C47B)=Sof(H47B)=Sof(C48B)=Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(C49B)=
 Sof(H49D)=Sof(H49E)=Sof(H49F)=Sof(N12B)=Sof(O3B)=1-FVAR(1)
 Sof(C47A)=Sof(H47A)=Sof(C48A)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C49A)=
 Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(N12A)=Sof(O3A)=FVAR(1)
 Sof(F10B)=Sof(F11B)=Sof(F12B)=Sof(F4B)=1-FVAR(2)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=Sof(F4A)=FVAR(2)
 Sof(H32C)=Sof(H32D)=Sof(C33B)=Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(3)
 Sof(H32A)=Sof(H32B)=Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(H33C)=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), C32(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),
  C44(H44), C47A(H47A), C47B(H47B), C50(H50), C53(H53)
5.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C33A(H33A,H33B,H33C), C33B(H33D,
 H33E,H33F), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C),
 C48A(H48A,H48B,H48C), C48B(H48D,H48E,H48F), C49A(H49A,H49B,H49C), C49B(H49D,
 H49E,H49F), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C),
 C55(H55A,H55B,H55C)
;
_shelx_res_checksum              53808
_shelx_hkl_checksum              61092
_olex2_submission_special_instructions 'No special instructions were received'