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_4124749
_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
'C64 H66 Br2 Fe2 N10 O2, 3(C32 H12 B F24), C H2 Cl2'
_chemical_formula_sum            'C161 H104 B3 Br2 Cl2 F72 Fe2 N10 O2'
_chemical_formula_weight         3953.39
_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             2015-07-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                74.978(12)
_cell_angle_beta                 89.070(15)
_cell_angle_gamma                71.113(9)
_cell_formula_units_Z            4
_cell_length_a                   16.461(6)
_cell_length_b                   23.978(9)
_cell_length_c                   46.22(2)
_cell_measurement_reflns_used    6428
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      50.51
_cell_measurement_theta_min      20.42
_cell_volume                     16625(11)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_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_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.718
_diffrn_measured_fraction_theta_max 0.718
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0986
_diffrn_reflns_av_unetI/netI     0.1929
_diffrn_reflns_laue_measured_fraction_full 0.718
_diffrn_reflns_laue_measured_fraction_max 0.718
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            40251
_diffrn_reflns_point_group_measured_fraction_full 0.718
_diffrn_reflns_point_group_measured_fraction_max 0.718
_diffrn_reflns_theta_full        51.094
_diffrn_reflns_theta_max         51.094
_diffrn_reflns_theta_min         20.415
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    3.487
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.4122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1336 before and 0.0758 after correction.
The Ratio of minimum to maximum transmission is 0.5496.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear bluish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       plate
_exptl_crystal_F_000             7900
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4651
_refine_ls_number_reflns         25727
_refine_ls_number_restraints     4536
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.2146
_refine_ls_R_factor_gt           0.1286
_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^)+(0.1056P)^2^+159.1499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2952
_refine_ls_wR_factor_ref         0.3524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13872
_reflns_number_total             25727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b07251_si_003.cif
_cod_data_source_block           aig84redo
_cod_database_code               4124749
_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
 C0CL-C0BA
 1.5 with sigma of 0.02
 Cl4-C27 = C27-Cl8
 1.47 with sigma of 0.02
 C27-Cl4 = C27-Cl8
 1.77 with sigma of 0.02
 C6AA-F070
 1.33 with sigma of 0.02
 F08R-C6AA = F0BJ-C6AA
 1.33 with sigma of 0.02
 F0BI-C6AA
 1.33 with sigma of 0.02
3. 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
4. Others
 Sof(F0BJ)=1-FVAR(1)
 Sof(F0BI)=FVAR(1)
 Sof(F0)=1-FVAR(2)
 Sof(F0D6)=FVAR(2)
 Sof(F1)=1-FVAR(3)
 Sof(F069)=FVAR(3)
 Sof(F2)=1-FVAR(4)
 Sof(F08P)=FVAR(4)
 Fixed Sof: F0BL(0.5) F40(0.5) F4(0.5) F9(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C034(H03a,H03b), C037(H03c,H03d), C043(H04a,H04b), C05R(H05d,H05f), C06H(H06e,
 H06g), C06W(H06n,H06o), C071(H07a,H07b), C079(H07j,H07k), C09A(H09a,H09b),
 C0AY(H0Ad,H0Ae), C0BQ(H0Bf,H0Bg), C0CF(H0Ch,H0Ci), C3ba(H3ba,H3bb), C27(H27a,
 H27b)
5.b Aromatic/amide H refined with riding coordinates:
 C029(H029), C02M(H02M), C035(H035), C03E(H03E), C03K(H03K), C03M(H03M),
 C03R(H03R), C041(H041), C042(H042), C047(H047), C04A(H04g), C04B(H04d),
 C04C(H04C), C04D(H04e), C04F(H04F), C04H(H04H), C04K(H04K), C04L(H04L),
 C04M(H04M), C04R(H04R), C04T(H04T), C04U(H04U), C053(H053), C05E(H05E),
 C05G(H05j), C05H(H05k), C05L(H05L), C05M(H05M), C05O(H05O), C05Q(H05Q),
 C05V(H05V), C05W(H05W), C05Z(H05Z), C060(H060), C064(H064), C066(H066),
 C067(H067), C06C(H06d), C06D(H06s), C06F(H06F), C06G(H06u), C06I(H06v),
 C06L(H06t), C06X(H06X), C075(H075), C07A(H07l), C07F(H07F), C07G(H07m),
 C07K(H07n), C07O(H07O), C07P(H07P), C07Q(H07Q), C080(H080), C081(H081),
 C083(H083), C087(H087), C089(H089), C08D(H08t), C08E(H08j), C08I(H08q),
 C08K(H08s), C08L(H08v), C08N(H08r), C08U(H08U), C08W(H08W), C091(H091),
 C092(H092), C093(H093), C095(H095), C09B(H09c), C09G(H09G), C09H(H09H),
 C09I(H09I), C09O(H09O), C09Q(H09Q), C0A0(H0A0), C0A1(H0A1), C0A5(H0A5),
 C0A8(H0A8), C0AF(H0AF), C0AO(H0AO), C0AP(H0AP), C0AS(H0AS), C0AT(H0AT),
 C0AU(H0AU), C0AW(H0AW), C0AZ(H0AZ), C0B4(H0B4), C0B8(H0B8), C0BC(H0Bd),
 C0BD(H0Bm), C0BE(H0BE), C0BJ(H0BJ), C0BK(H0BK), C0BN(H0BN), C0BS(H0BS),
 C0BU(H0BU), C0BY(H0BY), C0BZ(H0BZ), C0C1(H0C1), C0C5(H0C5), C0C6(H0C6),
 C0CB(H0CB), C0CQ(H0CQ), C0CU(H0CU), C0CW(H0CW), C0CZ(H0CZ), C0D0(H0D0),
 C24(H24), C2AA(H2AA), C3AA(H3AA), C19(H19), C31(H31), C1AA(H1AA), C29(H29),
 C33(H33), C40(H40), C25(H25), C37(H37), C2ba(H2ba)
5.c Idealised Me refined as rotating group:
 C05A(H05g,H05h,H05i), C05C(H05a,H05b,H05c), C061(H06a,H06b,H06c), C063(H06p,
 H06q,H06r), C06N(H06h,H06i,H06j), C06V(H06k,H06l,H06m), C074(H07g,H07h,H07i),
 C076(H07c,H07d,H07e), C085(H08a,H08b,H08c), C08A(H08d,H08e,H08f), C08B(H08g,
 H08h,H08i), C08G(H08n,H08o,H08p), C08X(H08k,H08l,H08m), C0AG(H0Aa,H0Ab,H0Ac),
 C0BO(H0Ba,H0Bb,H0Bc), C0BX(H0Bh,H0Bi,H0Bl), C0C4(H0Ca,H0Cc,H0Cd), C0CC(H0Ce,
 H0Cf,H0Cg), C0CJ(H0Cj,H0Ck,H0Cl), C7AA(H7Aa,H7Ab,H7Ac)
;
_shelx_res_checksum              3814
_shelx_hkl_checksum              51437
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'