Regioselectivity in ligand substitution reactions on diiron complexes governed by nucleophilic and electrophilic ligand properties.
Bethel, Ryan D.; Crouthers, Danielle J.; Hsieh, Chung-Hung; Denny, Jason A.; Hall, Michael B.; Darensbourg, Marcetta Y.; Inorganic chemistry 54 (2015) 3523–3535; doi:10.1021/acs.inorgchem.5b00072

data_4346024
_publ_section_title
;
 Regioselectivity in ligand substitution reactions on diiron complexes
 governed by nucleophilic and electrophilic ligand properties.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3523
_journal_page_last               3535
_journal_paper_doi               10.1021/acs.inorgchem.5b00072
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C28 H30 Fe2 N3 O5 S2, B F4'
_chemical_formula_sum            'C28 H30 B F4 Fe2 N3 O5 S2'
_chemical_formula_weight         751.18
_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
_cell_angle_alpha                90
_cell_angle_beta                 92.210(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0777(17)
_cell_length_b                   26.614(5)
_cell_length_c                   13.759(3)
_cell_measurement_reflns_used    9689
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      23.15
_cell_measurement_theta_min      2.64
_cell_volume                     3321.6(11)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            62106
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.255
_diffrn_reflns_theta_min         1.667
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1122 before and 0.0760 after correction.
The Ratio of minimum to maximum transmission is 0.6890.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.127
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         5960
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0695P)^2^+10.7648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4608
_reflns_number_total             5960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00072_si_002.cif
_cod_data_source_block           2-IMes
_cod_original_cell_volume        3321.5(11)
_cod_database_code               4346024
_shelx_estimated_absorpt_t_max   0.901
_shelx_estimated_absorpt_t_min   0.701
_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
 F2A-B4A \\sim F1-B4 \\sim F1A-B4A \\sim F4A-B4A \\sim F3A-B4A \\sim F4-B4
\\sim F3-B4 \\sim F2-B4
 with sigma of 0.02
 F1-F2 \\sim F2-F3 \\sim F3-F4 \\sim F1A-F2A \\sim F2A-F3A \\sim F3A-F4A \\sim
F4A-F1A \\sim F4-F1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(B4) = Uanis(F1) = Uanis(F2) = Uanis(F3) = Uanis(F4) = Uanis(B4A) =
Uanis(F1A) = Uanis(F2A) = Uanis(F3A) = Uanis(F4A)
4. Others
 Sof(B4A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=1-FVAR(1)
 Sof(B4)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C5(H5A,H5B), C6(H6A,H6B)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C18(H18), C19(H19), C22(H22), C25(H25)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C24(H24A,H24B,H24C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              9619
_shelx_hkl_checksum              27811