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_4085921
_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         '2(C32 H12 B F24), C24 H48 Fe O6, 3(C4 H8 O)'
_chemical_formula_sum            'C100 H96 B2 F48 Fe O9'
_chemical_formula_weight         2431.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4975)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.256(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.7267(17)
_cell_length_b                   17.4831(8)
_cell_length_c                   24.6865(16)
_cell_measurement_temperature    104(4)
_cell_volume                     10482.4(12)
_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      104(4)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  Xcalibur
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0816
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            29247
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.683
_diffrn_reflns_theta_min         2.854
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91148
_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            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_description       plate
_exptl_crystal_F_000             4944
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.070
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         14202
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1436
_refine_ls_R_factor_gt           0.0995
_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^)+(0.1261P)^2^+30.8045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2428
_refine_ls_wR_factor_ref         0.2770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9238
_reflns_number_total             14202
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00395_si_003.cif
_cod_data_source_block           Compound_6
_cod_depositor_comments
'Adding full bibliography for 4085916--4085926.cif.'
_cod_original_cell_volume        10482.4(11)
_cod_database_code               4085921
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.840(2) 0.160(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
3. Restrained distances
 F2-F3 \\sim F2-F1 \\sim F3-F1
 with sigma of 0.02
 C19B-F2B \\sim C19B-F1B \\sim C19B-F3B
 with sigma of 0.02
 C35B-F13B \\sim C35B-F15B \\sim C35B-F14B
 with sigma of 0.02
 F13B-F15B \\sim F13B-F14B \\sim F15B-F14B
 with sigma of 0.02
 C35-F14 \\sim C35-F15 \\sim C35-F13
 with sigma of 0.02
 F14-F15 \\sim F14-F13 \\sim F15-F13
 with sigma of 0.02
 C19-F3 \\sim C19-F1 \\sim C19-F2
 with sigma of 0.02
4. Rigid bond restraints
 C35, F14, F15, F13, F15B, F13B, F14B, C35B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F15B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F14B) \\sim Ueq, Uanis(F13B) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(F13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F13) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F14) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C19) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C6) = Uanis(C7B) = Uanis(C7) = Uanis(C6B)
Uanis(F20B) = Uanis(F21B) = Uanis(F19B) = Uanis(F20) = Uanis(F21) = Uanis(F19)
Uanis(F1) = Uanis(F2) = Uanis(F3)
Uanis(F3B) = Uanis(F2B) = Uanis(F1B)
Uiso(C51) = Uiso(C50) = Uiso(C52) = Uiso(O6) = Uiso(C49)
6. Rigid body (RIGU) restrains
 C28, F10, F11, F12, F11B, F12B, F10B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C44, F24, F22, F23, F23B, F22B, F24B, F19C, F21C, F20C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35, F14, F15, F13, F15B, F13B, F14B, C35B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(H5BC)=Sof(H5BD)=Sof(H8BC)=Sof(H8BD)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(C6B)=
 Sof(H6BA)=Sof(H6BB)=1-FVAR(1)
 Sof(H5AA)=Sof(H5AB)=Sof(H8AA)=Sof(H8AB)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=
 Sof(H7A)=Sof(H7B)=FVAR(1)
 Sof(F2B)=Sof(F1B)=Sof(F3B)=1-FVAR(2)
 Sof(F3)=Sof(F1)=Sof(F2)=FVAR(2)
 Sof(F11B)=Sof(F12B)=Sof(F10B)=1-FVAR(3)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(3)
 Sof(F20B)=Sof(F21B)=Sof(F19B)=1-FVAR(4)
 Sof(F21)=Sof(F19)=Sof(F20)=FVAR(4)
 Sof(C46)=Sof(H46C)=Sof(H46D)=Sof(O5B)=Sof(C47)=Sof(H47C)=Sof(H47D)=Sof(C45)=
 Sof(H45C)=Sof(H45D)=Sof(C48)=Sof(H48C)=Sof(H48D)=1-FVAR(5)
 Sof(O5)=Sof(C47B)=Sof(H47A)=Sof(H47B)=Sof(C46B)=Sof(H46A)=Sof(H46B)=Sof(C48B)=
 Sof(H48A)=Sof(H48B)=Sof(C45B)=Sof(H45A)=Sof(H45B)=FVAR(5)
 Sof(F15B)=Sof(F13B)=Sof(F14B)=Sof(C35B)=1-FVAR(6)
 Sof(C35)=Sof(F14)=Sof(F15)=Sof(F13)=FVAR(6)
 Sof(C19B)=1-FVAR(7)
 Sof(C19)=FVAR(7)
 Fixed Sof: F24(0.4723) F22(0.4723) F23(0.4723) F23B(0.2946) F22B(0.2946)
 F24B(0.2946) F19C(0.2331) F21C(0.2331) F20C(0.2331) O6(0.5) C52(0.5) H52A(0.5)
 H52B(0.5) C51(0.5) H51A(0.5) H51B(0.5) C50(0.5) H50A(0.5) H50B(0.5) C49(0.5)
 H49A(0.5) H49B(0.5)
8.a Free rotating group:
 O6(C52,C51,C50,C49,C1,O1,C2)
8.b Secondary CH2 refined with riding coordinates:
 C5(H5AA,H5AB), C5(H5BC,H5BD), C8(H8AA,H8AB), C8(H8BC,H8BD), C3(H3A,H3B),
 C12(H12A,H12B), C11(H11A,H11B), C10(H10A,H10B), C9(H9A,H9B), C47B(H47A,H47B),
 C46B(H46A,H46B), C48B(H48A,H48B), C45B(H45A,H45B), C6(H6A,H6B), C7(H7A,H7B),
 C7B(H7BA,H7BB), C6B(H6BA,H6BB), C4(H4A,H4B), C46(H46C,H46D), C47(H47C,H47D),
 C45(H45C,H45D), C48(H48C,H48D), C52(H52A,H52B), C51(H51A,H51B), C50(H50A,H50B),
  C49(H49A,H49B), C1(H1A,H1B), C2(H2A,H2B)
8.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C40(H40), C38(H38), C22(H22), C26(H26), C24(H24), C14(H14),
 C16(H16), C34(H34), C30(H30), C32(H32), C18(H18)
;
_shelx_res_checksum              84738
_shelx_hkl_checksum              34473
_olex2_submission_special_instructions 'No special instructions were received'