Electron Hopping through Double-Exchange Coupling in a Mixed-Valence Diiminobenzoquinone-Bridged Fe2 Complex.
Gaudette, Alexandra I.; Jeon, Ie-Rang; Anderson, John S.; Grandjean, Fernande; Long, Gary J.; Harris, T. David; Journal of the American Chemical Society 137 (2015) 12617–12626; doi:10.1021/jacs.5b07251

data_4124748
_publ_section_title
;
 Electron Hopping through Double-Exchange Coupling in a Mixed-Valence
 Diiminobenzoquinone-Bridged Fe2 Complex.
;
_journal_issue                   39
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12617
_journal_page_last               12626
_journal_paper_doi               10.1021/jacs.5b07251
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         '2(C32 H33 Br Fe N5 O), 2(C32 H12 B F24)'
_chemical_formula_sum            'C128.07 H90.04 B2 Br2 F48 Fe2 N10 O2'
_chemical_formula_weight         3006.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-06-15 # Formatted by publCIF

;
_cell_angle_alpha                88.986(2)
_cell_angle_beta                 88.420(2)
_cell_angle_gamma                78.267(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2741(5)
_cell_length_b                   20.2397(8)
_cell_length_c                   26.2330(10)
_cell_measurement_temperature    100
_cell_volume                     6377.8(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.656
_diffrn_measured_fraction_theta_max 0.972
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_laue_measured_fraction_full 0.656
_diffrn_reflns_laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26420
_diffrn_reflns_point_group_measured_fraction_full 0.656
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         54.300
_diffrn_reflns_theta_min         1.685
_exptl_absorpt_coefficient_mu    3.685
_exptl_absorpt_correction_T_max  0.7507
_exptl_absorpt_correction_T_min  0.6861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0486 before and 0.0417 after correction.
The Ratio of minimum to maximum transmission is 0.9139.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       plate
_exptl_crystal_F_000             3017
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.250
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1895
_refine_ls_number_reflns         15160
_refine_ls_number_restraints     2172
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0901
_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^)+(0.1475P)^2^+23.0356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2418
_refine_ls_wR_factor_ref         0.2594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12000
_reflns_number_total             15160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b07251_si_002.cif
_cod_data_source_block           aig79
_cod_database_code               4124748
_publcif_datablock.id            {7eab92cb-37f4-4dbf-b07a-30b348fcafd6}
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.837
_shelx_estimated_absorpt_t_min   0.615
_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
 F11-C96 \\sim F12-C96 \\sim F10-C96
 with sigma of 0.02
 F12-C96 \\sim F11-C96 \\sim F10-C96
 with sigma of 0.02
 F12-C96 \\sim F11-C96 \\sim F10-C96 \\sim F9-C95 \\sim F8-C95 \\sim F7-C95
 with sigma of 0.02
 N2-C20 \\sim C21-C22 \\sim C23-C24
 with sigma of 0.02
 F9-C95 \\sim F8-C95 \\sim F7-C95 \\sim F6-C79 \\sim F4-C79 \\sim F5-C79
 with sigma of 0.02
 F11-C96 \\sim F10-C96 \\sim F12-C96 \\sim F17-C87 \\sim F16-C87 \\sim F18-C87
 with sigma of 0.02
 F8-C95 \\sim F7-C95 \\sim F9-C95
 with sigma of 0.02
 N2-C20 \\sim C21-C22 \\sim C23-C24
 with sigma of 0.02
 C20-C21 \\sim C22-C23 \\sim C24-N2 \\sim C27-C28 \\sim C29-C30 \\sim C31-N3
 with sigma of 0.02
 C23-C24 \\sim C23-C22 \\sim C22-C21 \\sim C21-C20 \\sim N2-C20 \\sim N2-C24
\\sim N9-C45 \\sim C46-C45 ~
 C46-C47 \\sim C48-C47 \\sim C48-C49 \\sim N9-C49
 with sigma of 0.02
 C37-C38 \\sim C38-C39 \\sim C40-C41 \\sim C40-C39 \\sim C41-C36 \\sim C37-C36
 with sigma of 0.02
 C48-C49 \\sim C48-C47 \\sim C46-C47 \\sim C46-C45 \\sim N9-C45 \\sim N9-C49
 with sigma of 0.02
 C131-C121 \\sim C130-C131 \\sim C130-C129 \\sim C129-C123
 with sigma of 0.02
 C130-C132 \\sim F52-C132 \\sim F54-C132 \\sim F53-C132
 with sigma of 0.02
 C69-F29 \\sim C69-F30 \\sim C69-F28 \\sim F29-F30 \\sim F29-F28 \\sim F30-F28
 with sigma of 0.04
 C71-C69 \\sim C71-F29 \\sim C71-F30 \\sim C71-F28
 with sigma of 0.02
 F27-F25 \\sim F27-F26 \\sim F25-F26
 with sigma of 0.04
 C3A-C69 \\sim C3A-F27 \\sim C3A-F25 \\sim C3A-F26
 with sigma of 0.02
 C67-F22 \\sim F22-F24 \\sim F22-F23 \\sim F24-F23
 with sigma of 0.04
 C72-C67 \\sim C72-F22 \\sim C72-F24 \\sim C72-F23
 with sigma of 0.02
3. Restrained planarity
 C49, C47, C48, C46, C45, N9
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C48) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(C50) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(C132) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C50) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C47)
\\sim Ueq, Uanis(C46) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(C63) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C60)
\\sim Ueq, Uanis(C59) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(C104) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C3A)=Sof(F27)=Sof(F25)=Sof(F26)=1-FVAR(1)
 Sof(C71)=Sof(F29)=Sof(F30)=Sof(F28)=FVAR(1)
 Sof(C1AB)=Sof(F20)=Sof(F21)=Sof(F19)=1-FVAR(2)
 Sof(F22)=Sof(F24)=Sof(F23)=Sof(C72)=FVAR(2)
 Sof(F55)=Sof(F56)=Sof(F57)=Sof(C127)=Sof(C126)=Sof(H126)=Sof(C125)=Sof(C124)=
 Sof(H124)=1-FVAR(3)
 Sof(C129)=Sof(H129)=Sof(C130)=Sof(C131)=Sof(H131)=Sof(C132)=Sof(F52)=Sof(F53)=
 Sof(F54)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C19(H19a,H19b), C26(H26a,H26b), C44(H44a,H44b), C58(H58a,H58b), C51(H51a,
 H51b), C12(H12a,H12b)
7.b Aromatic/amide H refined with riding coordinates:
 C114(H114), C98(H98), C94(H94), C90(H90), C118(H118), C122(H122), C92(H92),
 C106(H106), C6(H6), C8(H8), C102(H102), C110(H110), C7(H7), C39(H39), C28(H28),
  C21(H21), C38(H38), C78(H78), C100(H100), C74(H74), C116(H116), C40(H40),
 C108(H108), C86(H86), C70(H70), C22(H22), C23(H23), C47(H47), C76(H76),
 C30(H30), C55(H55), C29(H29), C16(H16), C53(H53), C66(H66), C15(H15), C84(H84),
  C14(H14), C60(H60), C46(H46), C54(H54), C62(H62), C48(H48), C61(H61),
 C68(H68), C82(H82), C126(H126), C124(H124), C129(H129), C131(H131)
7.c Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C25(H25a,H25b,H25c), C10(H10a,H10b,H10c), C32(H32a,H32b,
 H32c), C42(H42a,H42b,H42c), C43(H43a,H43b,H43c), C57(H57a,H57b,H57c), C18(H18a,
 H18b,H18c), C64(H64a,H64b,H64c), C50(H50a,H50b,H50c)
;
_shelx_res_checksum              60468
_shelx_hkl_checksum              63623
_olex2_submission_special_instructions 'No special instructions were received'