Low-valent iron: an Fe(I) ate compound as a building block for a linear trinuclear Fe cluster
C. Lichtenberg; L. Viciu; M. Vogt; R. E. Rodriguez-Lugo; M. Adelhardt; J. Sutter; M. M. Khusniyarov; K. Meyer; B. de Bruin; E. Billd; H. Grutzmacher; Chem.Commun. 51 (2015) 13890–; doi:10.1039/C5cc04908C

data_7117708
_publ_section_title
;
 Low-valent iron: an Fe(I) ate compound as a building block for a linear
 trinuclear Fe cluster
;
_journal_name_full               Chem.Commun.
_journal_page_first              13890
_journal_paper_doi               10.1039/C5cc04908C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety
'C64 H48 Fe3 N4, 0.186(C6 H14), 0.628(C4 H8 O)'
_chemical_formula_sum            'C67.63 H55.63 Fe3 N4 O0.63'
_chemical_formula_weight         1101.91
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-01-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_audit_update_record
;
2015-06-01 deposited with the CCDC.
2015-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.8932(4)
_cell_length_b                   14.78371(18)
_cell_length_c                   13.25563(18)
_cell_measurement_reflns_used    13522
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.1810
_cell_measurement_theta_min      3.1340
_cell_volume                     5074.22(12)
_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)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_details
;
  1 omega  -24.00    7.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000   60.0000 31

  2 omega   41.00   72.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592  179.0000  -60.0000 31

  3 omega  -12.00   58.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592  -99.0000 -180.0000 70

  4 omega  -46.00   66.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592  -19.0000 -120.0000 112

  5 omega    1.00   26.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   57.0000    0.0000 25

  6 omega   -3.00   95.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   38.0000  -90.0000 98
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0273858000
_diffrn_orient_matrix_UB_12      0.0002628000
_diffrn_orient_matrix_UB_13      0.0024538000
_diffrn_orient_matrix_UB_21      -0.0009337000
_diffrn_orient_matrix_UB_22      0.0366497000
_diffrn_orient_matrix_UB_23      0.0344731000
_diffrn_orient_matrix_UB_31      -0.0008551000
_diffrn_orient_matrix_UB_32      -0.0309324000
_diffrn_orient_matrix_UB_33      0.0408253000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42724
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.792
_diffrn_reflns_theta_min         2.866
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94519
_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_density_diffrn    1.442
_exptl_crystal_description       plate
_exptl_crystal_F_000             2289.7
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 4461 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.007(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         13684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0554P)^2^+1.9521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1168
_reflns_Friedel_coverage         0.714
_reflns_friedel_fraction_full    0.943
_reflns_friedel_fraction_max     0.791
_reflns_number_gt                12054
_reflns_number_total             13684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc04908c2.cif
_cod_data_source_block           compound3
_cod_database_code               7117708
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         C40H40N2Fe
_reflns_odcompleteness_completeness 99.78
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(C68)=Sof(H68A)=
 Sof(H68B)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(O1)=1-FVAR(1)
 Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C71)=Sof(H71A)=
 Sof(H71B)=Sof(H71C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C4(H4), C1(H1), C5(H5), C52(H52), C48(H48), C51(H51), C37(H37), C33(H33),
 C36(H36), C20(H20), C19(H19), C16(H16)
3.b Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B), C70(H70A,H70B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,
 H68B), C65(H65A,H65B)
3.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C28(H28), C29(H29), C30(H30), C8(H8), C9(H9), C27(H27), C10(H10),
 C31(H31), C15(H15), C32(H32), C14(H14), C13(H13), C23(H23), C24(H24), C26(H26),
  C12(H12), C25(H25), C61(H61), C62(H62), C59(H59), C60(H60), C55(H55),
 C56(H56), C58(H58), C57(H57), C47(H47), C44(H44), C46(H46), C45(H45), C40(H40),
  C43(H43), C42(H42), C41(H41), C64(H64), C63(H63)
3.d Idealised Me refined as rotating group:
 C71(H71A,H71B,H71C)
;
_shelx_res_checksum              18594
_olex2_submission_special_instructions 'No special instructions were received'