Mono- and Dinuclear Neutral and Cationic Iron(II) Compounds Supported by an Amidinato-diolefin Ligand: Characterization and Catalytic Application
Lichtenberg, Crispin; Adelhardt, Mario; Wörle, Michael; Büttner, Torsten; Meyer, Karsten; Grützmacher, Hansjörg; Organometallics 34 (2015) 3079–; doi:10.1021/acs.organomet.5b00395

data_4085922
_publ_section_title
;
 Mono- and Dinuclear Neutral and Cationic Iron(II) Compounds Supported by
 an Amidinato-diolefin Ligand: Characterization and Catalytic Application
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3079
_journal_paper_doi               10.1021/acs.organomet.5b00395
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C37 H28 Br2 Fe1 N2'
_chemical_formula_sum            'C37 H28 Br2 Fe N2'
_chemical_formula_weight         716.28
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-12-18
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.0230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.2501(2)
_cell_length_b                   15.8949(2)
_cell_length_c                   22.6296(3)
_cell_measurement_temperature    100.0
_cell_volume                     6090.30(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            85600
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.903
_diffrn_reflns_theta_min         1.366
_exptl_absorpt_coefficient_mu    3.149
_exptl_absorpt_correction_T_max  0.8622
_exptl_absorpt_correction_T_min  0.6740
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for
absorption correction.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.819
_refine_diff_density_min         -1.343
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     783
_refine_ls_number_reflns         17561
_refine_ls_number_restraints     1152
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.0720
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0766P)^2^+35.5125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.2010
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10985
_reflns_number_total             17561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00395_si_003.cif
_cod_data_source_block           Compound_7
_cod_depositor_comments
'Adding full bibliography for 4085916--4085926.cif.'
_cod_database_code               4085922
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.834
_shelx_estimated_absorpt_t_min   0.495
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C62) = Uanis(C65)
Uanis(C7A) = Uanis(C17)
Uanis(C8A) = Uanis(C30)
Uanis(C9A) = Uanis(C29)
Uanis(C10A) = Uanis(C28)
Uanis(C11A) = Uanis(C27)
Uanis(C6A) = Uanis(C18)
Uanis(C16) = Uanis(C1A)
Uanis(N1A) = Uanis(N2)
Uanis(C5A) = Uanis(C19)
Uanis(C4A) = Uanis(C20)
Uanis(C21) = Uanis(C3A)
Uanis(C12A) = Uanis(C26)
Uanis(C13A) = Uanis(C25)
Uanis(C14A) = Uanis(C24)
Uanis(C2A) = Uanis(C22)
Uanis(C32A) = Uanis(C32)
Uanis(C33A) = Uanis(C37)
Uanis(C34A) = Uanis(C36)
Uanis(C35) = Uanis(C35A)
Uanis(C37A) = Uanis(C33)
Uanis(C34) = Uanis(C36A)
Uanis(C31) = Uanis(C31A)
Uanis(N2A) = Uanis(N1)
Uanis(C2) = Uanis(C22A)
Uanis(C3) = Uanis(C21A)
Uanis(C12) = Uanis(C26A)
Uanis(C25A) = Uanis(C14)
Uanis(C14) = Uanis(C24A)
Uanis(C15) = Uanis(C23A)
Uanis(C3) = Uanis(C20A)
Uanis(C4) = Uanis(C20A)
Uanis(C5) = Uanis(C19A)
Uanis(C18A) = Uanis(C6)
Uanis(C7) = Uanis(C17A)
Uanis(C30A) = Uanis(C8)
Uanis(C29A) = Uanis(C9)
Uanis(C28A) = Uanis(C10)
Uanis(C11) = Uanis(C27A)
Uanis(Br1) = Uanis(Br2A)
Uanis(C23) = Uanis(C15A)
Uanis(C24) = Uanis(C14A)
Uanis(Fe1) = Uanis(Fe1A)
Uanis(C40A) = Uanis(C55)
Uanis(C54) = Uanis(C39A)
Uanis(C52A) = Uanis(C67)
Uanis(C66) = Uanis(C51A)
Uanis(C50A) = Uanis(C65)
Uanis(C49A) = Uanis(C64)
Uanis(C44A) = Uanis(C59)
Uanis(C45A) = Uanis(C60)
Uanis(C62) = Uanis(C47A)
Uanis(C58) = Uanis(C43A)
Uanis(C48A) = Uanis(C63)
Uanis(C47A) = Uanis(C62)
Uanis(C46A) = Uanis(C61)
Uanis(C68) = Uanis(C68A)
Uanis(N4A) = Uanis(N3)
Uanis(N4) = Uanis(N3A)
Uanis(C70A) = Uanis(C74)
Uanis(C73) = Uanis(C71A)
Uanis(C72) = Uanis(C72A)
Uanis(C71) = Uanis(C73A)
Uanis(C69) = Uanis(C69A)
Uanis(C70) = Uanis(C74A)
Uanis(C57) = Uanis(C42A)
Uanis(C53) = Uanis(C38A)
Uanis(C41) = Uanis(C56A)
Uanis(C42) = Uanis(C57A)
Uanis(C55A) = Uanis(C40)
Uanis(C54A) = Uanis(C39)
Uanis(C38) = Uanis(C53A)
Uanis(C55A) = Uanis(C40)
Uanis(C54A) = Uanis(C39)
Uanis(C64A) = Uanis(C49)
Uanis(C65A) = Uanis(C50)
Uanis(C66A) = Uanis(C51)
Uanis(C67A) = Uanis(C52)
Uanis(C53A) = Uanis(C38)
Uanis(C44) = Uanis(C59A)
Uanis(C45) = Uanis(C60A)
Uanis(C43) = Uanis(C58A)
Uanis(C63A) = Uanis(C48)
Uanis(C46) = Uanis(C61A)
Uanis(C63A) = Uanis(C48)
Uanis(C62A) = Uanis(C47)
Uanis(C56) = Uanis(C41A)
Uanis(Br4A) = Uanis(Br3)
Uanis(Br4A) = Uanis(Br3)
Uanis(Br4A) = Uanis(Br3)
Uanis(Fe2) = Uanis(Fe2A)
4. Rigid body (RIGU) restrains
 C16A, C22A, C21A, C17A, C18A, C27A, C20A, C28A, C19A, C30A, C23A, C24A, C26A,
 C25A, C29A, N2A, C31A, C1A, C7A, C2A, C8A, C15A, C9A, C13A, C14A, C32A, C33A,
 C34A, C35A, C37A, C36A, N1A, C4A, C6A, C3A, C5A, C11A, C12A, C10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C44A, C43A, C42A, C48A, C46A, C45A, C47A, C50A, C39A, C52A, C49A, C51A, C38A,
 C41A, C40A, C68A, C69A, C70A, C72A, C71A, C74A, C73A, N3A, N4A, C53A, C59A,
 C54A, C58A, C62A, C57A, C55A, C60A, C56A, C61A, C63A, C64A, C67A, C66A, C65A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C31A)=Sof(Fe1A)=Sof(Br1A)=Sof(Br2A)=Sof(C16A)=Sof(H16A)=Sof(C22A)=
 Sof(C21A)=Sof(C17A)=Sof(C18A)=Sof(C27A)=Sof(H27A)=Sof(C20A)=Sof(H20A)=
 Sof(C28A)=Sof(H28A)=Sof(C19A)=Sof(H19A)=Sof(C30A)=Sof(H30A)=Sof(C23A)=
 Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C26A)=Sof(H26A)=Sof(C25A)=Sof(H25A)=Sof(C1A)=
 Sof(H1A)=Sof(C7A)=Sof(C4A)=Sof(H4A)=Sof(C6A)=Sof(C2A)=Sof(C3A)=Sof(C5A)=
 Sof(H5A)=Sof(C8A)=Sof(H8A)=Sof(C15A)=Sof(H15A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=
 Sof(H12A)=Sof(C9A)=Sof(H9A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=Sof(C10A)=
 Sof(H10A)=Sof(C32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=Sof(C35A)=
 Sof(H35A)=Sof(C37A)=Sof(H37A)=Sof(C36A)=Sof(H36A)=Sof(C29A)=Sof(H29A)=Sof(N2A)=
 Sof(H2A)=Sof(N1A)=1-FVAR(1)
 Sof(Fe1)=Sof(Br1)=Sof(Br2)=Sof(C16)=Sof(H16)=Sof(C22)=Sof(C21)=Sof(C17)=
 Sof(C18)=Sof(C27)=Sof(H27)=Sof(C20)=Sof(H20)=Sof(C28)=Sof(H28)=Sof(C19)=
 Sof(H19)=Sof(C30)=Sof(H30)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C26)=
 Sof(H26)=Sof(C25)=Sof(H25)=Sof(C1)=Sof(H1)=Sof(C7)=Sof(C4)=Sof(H4)=Sof(C6)=
 Sof(C2)=Sof(C3)=Sof(C5)=Sof(H5)=Sof(C8)=Sof(H8)=Sof(C15)=Sof(H15)=Sof(C11)=
 Sof(H11)=Sof(C12)=Sof(H12)=Sof(C9)=Sof(H9)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=
 Sof(C10)=Sof(H10)=Sof(C32)=Sof(C33)=Sof(H33)=Sof(C31)=Sof(C34)=Sof(H34)=
 Sof(C35)=Sof(H35)=Sof(C37)=Sof(H37)=Sof(C36)=Sof(H36)=Sof(C29)=Sof(H29)=
 Sof(N2)=Sof(H2)=Sof(N1)=FVAR(1)
 Sof(C44A)=Sof(C43A)=Sof(C68A)=Sof(C69A)=Sof(C70A)=Sof(H70A)=Sof(C72A)=
 Sof(H72A)=Sof(C42A)=Sof(H42A)=Sof(C48A)=Sof(H48A)=Sof(C53A)=Sof(H53A)=
 Sof(C59A)=Sof(C46A)=Sof(H46A)=Sof(C45A)=Sof(H45A)=Sof(C71A)=Sof(H71A)=
 Sof(C74A)=Sof(H74A)=Sof(C54A)=Sof(C47A)=Sof(H47A)=Sof(C58A)=Sof(C62A)=
 Sof(H62A)=Sof(C57A)=Sof(H57A)=Sof(C73A)=Sof(H73A)=Sof(C55A)=Sof(C60A)=
 Sof(H60A)=Sof(C56A)=Sof(H56A)=Sof(C61A)=Sof(H61A)=Sof(C63A)=Sof(H63A)=
 Sof(C64A)=Sof(H64A)=Sof(C67A)=Sof(H67A)=Sof(C66A)=Sof(H66A)=Sof(C50A)=
 Sof(H50A)=Sof(C39A)=Sof(C52A)=Sof(H52A)=Sof(C49A)=Sof(H49A)=Sof(C51A)=
 Sof(H51A)=Sof(C38A)=Sof(H38A)=Sof(C41A)=Sof(H41A)=Sof(C40A)=Sof(C65A)=
 Sof(H65A)=Sof(Fe2A)=Sof(Br3A)=Sof(Br4A)=Sof(N3A)=Sof(N4A)=Sof(H4AA)=1-FVAR(2)
 Sof(C44)=Sof(C43)=Sof(C68)=Sof(C69)=Sof(C70)=Sof(H70)=Sof(C72)=Sof(H72)=
 Sof(C42)=Sof(H42)=Sof(C48)=Sof(H48)=Sof(C53)=Sof(H53)=Sof(C59)=Sof(C46)=
 Sof(H46)=Sof(C45)=Sof(H45)=Sof(C71)=Sof(H71)=Sof(C74)=Sof(H74)=Sof(C54)=
 Sof(C47)=Sof(H47)=Sof(C58)=Sof(C62)=Sof(H62)=Sof(C57)=Sof(H57)=Sof(C73)=
 Sof(H73)=Sof(C55)=Sof(C60)=Sof(H60)=Sof(C56)=Sof(H56)=Sof(C61)=Sof(H61)=
 Sof(C63)=Sof(H63)=Sof(C64)=Sof(H64)=Sof(C67)=Sof(H67)=Sof(C66)=Sof(H66)=
 Sof(C50)=Sof(H50)=Sof(C39)=Sof(C52)=Sof(H52)=Sof(C49)=Sof(H49)=Sof(C51)=
 Sof(H51)=Sof(C38)=Sof(H38)=Sof(C41)=Sof(H41)=Sof(C40)=Sof(C65)=Sof(H65)=
 Sof(Fe2)=Sof(Br3)=Sof(Br4)=Sof(N3)=Sof(N4)=Sof(H4B)=FVAR(2)
6.a Free rotating group:
 C31A(Fe1A,Br1A,Br2A,C16A,C22A,C21A,C17A,C18A,C27A,C20A,C28A,C19A,C30A,C23A,
 C24A,C26A,C25A,C1A,C7A,C4A,C6A,C2A,C3A,C5A,C8A,C15A,C11A,C12A,C9A,C13A,C14A,
 C10A,C32A,C33A,C34A,C35A,C37A,C36A,C29A,N2A,N1A), C44A(C43A,C68A,C69A,C70A,
 C72A,C42A,C48A,C53A,C59A,C46A,C45A,C71A,C74A,C54A,C47A,C58A,C62A,C57A,C73A,
 C55A,C60A,C56A,C61A,C63A,C64A,C67A,C66A,C50A,C39A,C52A,C49A,C51A,C38A,C41A,
 C40A,C65A,Fe2A,Br3A,Br4A,N3A,N4A)
6.b Ternary CH refined with riding coordinates:
 C16(H16), C1(H1), C4(H4), C5(H5), C16A(H16A), C1A(H1A), C4A(H4A), C5A(H5A),
 C42(H42), C53(H53), C38(H38), C41(H41), C42A(H42A), C53A(H53A), C38A(H38A),
 C41A(H41A)
6.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C20(H20), C28(H28), C19(H19), C30(H30), C23(H23), C24(H24),
 C26(H26), C25(H25), C8(H8), C15(H15), C11(H11), C12(H12), C9(H9), C13(H13),
 C14(H14), C10(H10), C33(H33), C27A(H27A), C20A(H20A), C28A(H28A), C19A(H19A),
 C30A(H30A), C23A(H23A), C24A(H24A), C26A(H26A), C25A(H25A), C8A(H8A),
 C15A(H15A), C11A(H11A), C12A(H12A), C9A(H9A), C13A(H13A), C14A(H14A),
 C10A(H10A), C33A(H33A), C34A(H34A), C35A(H35A), C37A(H37A), C36A(H36A),
 C29A(H29A), N2A(H2A), C34(H34), C35(H35), C37(H37), C36(H36), C70(H70),
 C72(H72), C48(H48), C46(H46), C45(H45), C71(H71), C74(H74), C47(H47), C62(H62),
  C57(H57), C73(H73), C60(H60), C56(H56), C61(H61), C63(H63), C64(H64),
 C67(H67), C66(H66), C50(H50), C52(H52), C49(H49), C51(H51), C65(H65), C29(H29),
  N2(H2), N4(H4B), C70A(H70A), C72A(H72A), C48A(H48A), C46A(H46A), C45A(H45A),
 C71A(H71A), C74A(H74A), C47A(H47A), C62A(H62A), C57A(H57A), C73A(H73A),
 C60A(H60A), C56A(H56A), C61A(H61A), C63A(H63A), C64A(H64A), C67A(H67A),
 C66A(H66A), C50A(H50A), C52A(H52A), C49A(H49A), C51A(H51A), C65A(H65A),
 N4A(H4AA)
;
_shelx_res_checksum              83595
_shelx_hkl_checksum              11193
_olex2_submission_special_instructions 'No special instructions were received'