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_7117710
_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         'C38 H30, C6 H14'
_chemical_formula_sum            'C44 H44'
_chemical_formula_weight         572.79
_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
_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                71.996(4)
_cell_angle_beta                 79.884(3)
_cell_angle_gamma                82.754(4)
_cell_formula_units_Z            2
_cell_length_a                   10.4488(4)
_cell_length_b                   12.4887(6)
_cell_length_c                   13.5525(6)
_cell_measurement_reflns_used    4367
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.2060
_cell_measurement_theta_min      3.1820
_cell_volume                     1650.87(13)
_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 0.999
_diffrn_measurement_details
;
  1 omega  -15.00   20.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000   30.0000 35

  2 omega  -12.00   14.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000 -150.0000 26

  3 omega  -25.00   12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000 -180.0000 37

  4 omega  -47.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592  -57.0000  -90.0000 91

  5 omega    2.00   88.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   38.0000 -180.0000 86

  6 omega   13.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   57.0000   30.0000 78

  7 omega   36.00   68.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592  179.0000  -60.0000 32

  8 omega   63.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   57.0000   60.0000 28

  9 omega   32.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592 -179.0000  150.0000 57
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0055957000
_diffrn_orient_matrix_UB_12      0.0164989000
_diffrn_orient_matrix_UB_13      -0.0541561000
_diffrn_orient_matrix_UB_21      -0.0258747000
_diffrn_orient_matrix_UB_22      -0.0520541000
_diffrn_orient_matrix_UB_23      0.0067171000
_diffrn_orient_matrix_UB_31      -0.0638921000
_diffrn_orient_matrix_UB_32      0.0246104000
_diffrn_orient_matrix_UB_33      0.0107431000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16692
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.275
_diffrn_reflns_theta_min         3.047
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98498
_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    1.152
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         8179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0391P)^2^+0.3192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1356
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5709
_reflns_number_total             8179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc04908c2.cif
_cod_data_source_block           Compound5
_cod_database_code               7117710
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         C40H40N2Fe1LiCl
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C20(H20)
2.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C42(H42A,H42B), C41(H41A,H41B), C40(H40A,H40B)
2.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C24(H24), C25(H25), C34(H34), C9(H9), C32(H32), C6(H6),
 C5(H5), C7(H7), C28(H28), C15(H15), C38(H38), C4(H4), C30(H30), C13(H13),
 C3(H3), C29(H29), C31(H31), C35(H35), C19(H19), C18(H18), C16(H16), C11(H11),
 C37(H37), C10(H10), C12(H12), C17(H17), C36(H36)
2.d Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              42986
_olex2_submission_special_instructions 'No special instructions were received'