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_7117709
_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         '4(C64 H48 Fe N4), 3(C4 H8 O), C6 H14'
_chemical_formula_sum            'C274 H230 Fe4 N16 O3'
_chemical_formula_weight         4018.13
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            2
_cell_length_a                   26.9704(3)
_cell_length_b                   17.93806(19)
_cell_length_c                   21.5915(2)
_cell_measurement_reflns_used    34188
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      30.1060
_cell_measurement_theta_min      3.1480
_cell_volume                     10445.90(19)
_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      100.0(2)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_details
;
  1 omega  -95.00  -59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9467  179.0000   90.0000 36

  2 omega   -6.00   20.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9467  -99.0000   60.0000 26

  3 omega  -13.00   95.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154    0.0000  -90.0000 108

  4 omega  -21.00   41.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154  -77.0000   60.0000 62

  5 omega  -47.00   50.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9467   38.0000  -60.0000 97

  6 omega  -25.00   20.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9467  -99.0000 -150.0000 45

  7 omega  -76.00  -51.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9467  120.0000  111.0000 25

  8 omega  -94.00    4.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9467  -38.0000  -60.0000 98
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0123854000
_diffrn_orient_matrix_UB_12      -0.0321962000
_diffrn_orient_matrix_UB_13      0.0111648000
_diffrn_orient_matrix_UB_21      -0.0073293000
_diffrn_orient_matrix_UB_22      0.0090058000
_diffrn_orient_matrix_UB_23      0.0306549000
_diffrn_orient_matrix_UB_31      -0.0220088000
_diffrn_orient_matrix_UB_32      -0.0211032000
_diffrn_orient_matrix_UB_33      -0.0039202000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            114073
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.719
_diffrn_reflns_theta_min         2.886
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95822
_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    1.277
_exptl_crystal_description       block
_exptl_crystal_F_000             4228
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 10777 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.002(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1389
_refine_ls_number_reflns         29546
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+3.9371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1259
_reflns_Friedel_coverage         0.885
_reflns_friedel_fraction_full    0.994
_reflns_friedel_fraction_max     0.875
_reflns_number_gt                25925
_reflns_number_total             29546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc04908c2.cif
_cod_data_source_block           Compound4
_cod_original_cell_volume        10445.89(19)
_cod_database_code               7117709
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         C40H40N2FeO
_reflns_odcompleteness_completeness 99.81
_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. Rigid bond restraints
 C65, N5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C131) \\sim Ueq, Uanis(C141) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
4. Others
 Fixed Sof: C129(0.5) H12A(0.5) H12B(0.5) C130(0.5) H13P(0.5) H13Q(0.5)
 C131(0.5) H13R(0.5) H13S(0.5) C132(0.5) H13T(0.5) H13U(0.5) O1(0.5) C139(0.5)
 H13A(0.5) H13B(0.5) C140(0.5) H14A(0.5) H14B(0.5) C141(0.5) H14C(0.5)
 H14D(0.5) C142(0.5) H14E(0.5) H14F(0.5) H14G(0.5) C137(0.5) H13C(0.5)
 H13D(0.5) H13E(0.5) C138(0.5) H13F(0.5) H13G(0.5)
5.a Ternary CH refined with riding coordinates:
 C97(H97), C65(H65), C112(H112), C80(H80), C48(H48), C33(H33), C16(H16), C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C134(H13H,H13I), C135(H13J,H13K), C136(H13L,H13M), C133(H13N,H13O), C129(H12A,
 H12B), C130(H13P,H13Q), C131(H13R,H13S), C132(H13T,H13U), C139(H13A,H13B),
 C140(H14A,H14B), C141(H14C,H14D), C138(H13F,H13G)
5.c Aromatic/amide H refined with riding coordinates:
 C104(H104), C105(H105), C107(H107), C111(H111), C110(H110), C106(H106),
 C73(H73), C101(H101), C74(H74), C100(H100), C108(H108), C109(H109), C75(H75),
 C123(H123), C124(H124), C126(H126), C125(H125), C116(H116), C76(H76),
 C115(H115), C77(H77), C79(H79), C69(H69), C78(H78), C68(H68), C41(H41),
 C55(H55), C40(H40), C58(H58), C72(H72), C43(H43), C42(H42), C57(H57), C56(H56),
  C122(H122), C119(H119), C121(H121), C120(H120), C87(H87), C88(H88), C90(H90),
 C89(H89), C127(H127), C128(H128), C96(H96), C95(H95), C83(H83), C91(H91),
 C92(H92), C84(H84), C94(H94), C93(H93), C62(H62), C28(H28), C60(H60), C59(H59),
  C29(H29), C30(H30), C27(H27), C31(H31), C32(H32), C64(H64), C63(H63),
 C20(H20), C23(H23), C26(H26), C19(H19), C8(H8), C9(H9), C11(H11), C15(H15),
 C5(H5), C4(H4), C13(H13), C12(H12), C14(H14), C10(H10), C47(H47), C46(H46),
 C44(H44), C45(H45), C36(H36), C37(H37), C24(H24), C25(H25), C61(H61), C51(H51),
  C52(H52)
5.d Idealised Me refined as rotating group:
 C142(H14E,H14F,H14G), C137(H13C,H13D,H13E)
;
_shelx_res_checksum              71853
_olex2_submission_special_instructions 'No special instructions were received'