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_4085924
_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
'4(C37 H27 Br2 Fe N2), 4(C16 H36 N), 6(C4 H8 O)'
_chemical_formula_sum            'C236 H300 Br8 Fe4 N12 O6'
_chemical_formula_weight         4263.54
_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             2014-10-20
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                61.992(3)
_cell_angle_beta                 71.252(3)
_cell_angle_gamma                83.089(3)
_cell_formula_units_Z            1
_cell_length_a                   15.5268(5)
_cell_length_b                   20.3772(7)
_cell_length_c                   21.4660(6)
_cell_measurement_reflns_used    9647
_cell_measurement_temperature    105.5(3)
_cell_measurement_theta_max      28.6150
_cell_measurement_theta_min      3.0730
_cell_volume                     5674.3(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      105.5(3)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -23.00   48.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9467   77.0000   30.0000 71

  2 omega  -50.00   30.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9467   77.0000  -90.0000 80

  3 omega  -36.00   48.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9467   77.0000  -30.0000 84

  4 omega   -8.00   36.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154   77.0000   30.0000 44

  5 omega   -7.00   89.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154   77.0000  120.0000 96

  6 omega    3.00   68.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154   77.0000 -150.0000 65

  7 omega  -47.00  -20.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9467   38.0000 -180.0000 27
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0230293000
_diffrn_orient_matrix_UB_12      0.0117104000
_diffrn_orient_matrix_UB_13      -0.0381068000
_diffrn_orient_matrix_UB_21      0.0333714000
_diffrn_orient_matrix_UB_22      -0.0267889000
_diffrn_orient_matrix_UB_23      0.0094481000
_diffrn_orient_matrix_UB_31      -0.0261999000
_diffrn_orient_matrix_UB_32      -0.0264900000
_diffrn_orient_matrix_UB_33      0.0004047000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0750
_diffrn_reflns_Laue_measured_fraction_full 0.929
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45957
_diffrn_reflns_point_group_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.350
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.901
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.715
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       plate
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.559
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1171
_refine_ls_number_reflns         20740
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1065P)^2^+8.8822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1832
_refine_ls_wR_factor_ref         0.2056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14031
_reflns_number_total             20740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00395_si_003.cif
_cod_data_source_block           Compound_8_1.5THF
_cod_depositor_comments
'Adding full bibliography for 4085916--4085926.cif.'
_cod_database_code               4085924
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         FeBr2N3C40H40
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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
 C112-C113
 1.5 with sigma of 0.02
 C112-C111
 1.5 with sigma of 0.02
 C114-C113
 1.5 with sigma of 0.02
 C111-O2
 1.42 with sigma of 0.02
 O2-C114
 1.42 with sigma of 0.02
 C93-C92
 1.52 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C85, C86
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(H92C)=Sof(H92D)=Sof(C93)=Sof(H93C)=Sof(H93D)=Sof(C94)=Sof(H94A)=Sof(H94B)=
 Sof(H94C)=1-FVAR(1)
 Sof(H92A)=Sof(H92B)=Sof(C93A)=Sof(H93A)=Sof(H93B)=Sof(C94A)=Sof(H94D)=
 Sof(H94E)=Sof(H94F)=FVAR(1)
 Fixed Sof: O2(0.5) C111(0.5) H11C(0.5) H11D(0.5) C114(0.5) H11E(0.5)
 H11F(0.5) C112(0.5) H11G(0.5) H11H(0.5) C113(0.5) H11I(0.5) H11J(0.5) O4(0.5)
 C121(0.5) H12A(0.5) H12B(0.5) C122(0.5) H12C(0.5) H12D(0.5) C120(0.5)
 H12E(0.5) H12F(0.5) C119(0.5) H11S(0.5) H11T(0.5)
5.a Ternary CH refined with riding coordinates:
 C16(H16), C53(H53), C38(H38), C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C103(H10A,H10B), C99(H99A,H99B), C91(H91A,H91B), C95(H95A,H95B), C96(H96A,
 H96B), C104(H10C,H10D), C105(H10E,H10F), C92(H92A,H92B), C92(H92C,H92D),
 C97(H97A,H97B), C101(H10J,H10K), C100(H10L,H10M), C80(H80A,H80B), C88(H88A,
 H88B), C87(H87A,H87B), C75(H75A,H75B), C89(H89A,H89B), C81(H81A,H81B),
 C79(H79A,H79B), C83(H83A,H83B), C77(H77A,H77B), C76(H76A,H76B), C85(H85A,H85B),
  C84(H84A,H84B), C107(H10Q,H10R), C108(H10S,H10T), C109(H10U,H10V), C110(H11A,
 H11B), C111(H11C,H11D), C114(H11E,H11F), C112(H11G,H11H), C113(H11I,H11J),
 C115(H11K,H11L), C118(H11M,H11N), C116(H11O,H11P), C117(H11Q,H11R), C121(H12A,
 H12B), C122(H12C,H12D), C120(H12E,H12F), C119(H11S,H11T), C93A(H93A,H93B),
 C93(H93C,H93D)
5.c Aromatic/amide H refined with riding coordinates:
 C30(H30), C45(H45), C67(H67), C15(H15), C23(H23), C27(H27), C46(H46),
 C19(H19), C29(H29), C66(H66), C61(H61), C20(H20), C52(H52), C33(H33), C8(H8),
 C60(H60), C41(H41), C14(H14), C24(H24), C48(H48), C74(H74), C63(H63), C4(H4),
 C25(H25), C11(H11), C28(H28), C57(H57), C26(H26), C65(H65), C64(H64), C62(H62),
  C34(H34), C13(H13), C36(H36), C42(H42), C47(H47), C37(H37), C56(H56), C9(H9),
 C35(H35), C12(H12), C70(H70), C5(H5), C10(H10), C71(H71), C73(H73), C51(H51),
 C49(H49), C72(H72), C50(H50)
5.d Idealised Me refined as rotating group:
 C98(H98A,H98B,H98C), C106(H10G,H10H,H10I), C102(H10N,H10O,H10P), C90(H90A,
 H90B,H90C), C82(H82A,H82B,H82C), C86(H86A,H86B,H86C), C78(H78A,H78B,H78C),
 C94(H94A,H94B,H94C), C94A(H94D,H94E,H94F)
;
_shelx_res_checksum              69755
_shelx_hkl_checksum              23265
_olex2_submission_special_instructions 'No special instructions were received'