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_7117707
_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         'C44 H48 Fe N2 Na O3, 0.5(C6 H14)'
_chemical_formula_sum            'C47 H55 Fe N2 Na O3'
_chemical_formula_weight         774.76
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_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                 99.180(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.2714(4)
_cell_length_b                   16.1257(3)
_cell_length_c                   24.0679(4)
_cell_measurement_temperature    103(4)
_cell_volume                     8149.9(3)
_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      103(4)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       '\w and \p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.876
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            70645
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.641
_diffrn_reflns_theta_min         2.865
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.424
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87790
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       needle
_exptl_crystal_F_000             3296
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1037
_refine_ls_number_reflns         22055
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0562P)^2^+10.0211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1478
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                16337
_reflns_number_total             22055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc04908c2.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
;

2023-11-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C94 H110 Fe2 N4 Na2 O6'
_cod_original_formula_weight         1549.53
_cod_original_formula_moiety         '2(C44 H48 Fe N2 Na O3), C6 H14'
_cod_original_formula_units_Z            4
_cod_database_code               7117707
_shelxl_version_number           2013-4
_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. Restrained distances
 C83A-C82A
 1.5 with sigma of 0.02
 C83A-C84A
 1.5 with sigma of 0.02
 C82A-C81A
 1.5 with sigma of 0.02
 C38A-C39A
 1.5 with sigma of 0.02
 C37A-C38A
 1.5 with sigma of 0.02
 C40A-C39A
 1.5 with sigma of 0.02
 C37A-O2A
 1.4 with sigma of 0.02
 O2A-C40A
 1.4 with sigma of 0.02
 C91-C92
 1.54 with sigma of 0.02
 C92-C93
 1.54 with sigma of 0.02
 C93-C94
 1.54 with sigma of 0.02
 C90-C91
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C83) \\sim Ueq, Uanis(C86) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C84A) = Uanis(C83A) = Uanis(C82A) = Uanis(C81A)
Uanis(C40A) = Uanis(C39A) = Uanis(C38A) = Uanis(C37A)
4. Others
 Sof(O5A)=Sof(C84A)=Sof(H84C)=Sof(H84D)=Sof(C83A)=Sof(H83C)=Sof(H83D)=
 Sof(C82A)=Sof(H82C)=Sof(H82D)=Sof(C81A)=Sof(H81C)=Sof(H81D)=1-FVAR(1)
 Sof(O5)=Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(C82)=
 Sof(H82A)=Sof(H82B)=Sof(C83)=Sof(H83A)=Sof(H83B)=FVAR(1)
 Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C39A)=
 Sof(H39C)=Sof(H39D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=Sof(O2A)=1-FVAR(2)
 Sof(O2)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C40)=
 Sof(H40A)=Sof(H40B)=Sof(C39)=Sof(H39A)=Sof(H39B)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C4(H4), C5(H5), C20(H20), C19(H19), C16(H16), C1(H1), C63(H63), C60(H60),
 C64(H64), C45(H45), C49(H49), C48(H48)
5.b Secondary CH2 refined with riding coordinates:
 C79(H79A,H79B), C80(H80A,H80B), C78(H78A,H78B), C77(H77A,H77B), C44(H44A,
 H44B), C33(H33A,H33B), C41(H41A,H41B), C42(H42A,H42B), C37(H37A,H37B),
 C38(H38A,H38B), C40(H40A,H40B), C39(H39A,H39B), C43(H43A,H43B), C34(H34A,H34B),
  C36(H36A,H36B), C87(H87A,H87B), C84(H84A,H84B), C86(H86A,H86B), C88(H88A,
 H88B), C85(H85A,H85B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B),
 C93(H93A,H93B), C92(H92A,H92B), C91(H91A,H91B), C90(H90A,H90B), C84A(H84C,
 H84D), C83A(H83C,H83D), C82A(H82C,H82D), C81A(H81C,H81D), C37A(H37C,H37D),
 C38A(H38C,H38D), C39A(H39C,H39D), C40A(H40C,H40D)
5.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C9(H9), C10(H10), C8(H8), C12(H12), C15(H15), C13(H13), C14(H14),
 C27(H27), C30(H30), C28(H28), C29(H29), C32(H32), C23(H23), C31(H31), C26(H26),
  C25(H25), C24(H24), C70(H70), C67(H67), C68(H68), C75(H75), C76(H76),
 C73(H73), C69(H69), C71(H71), C72(H72), C74(H74), C55(H55), C54(H54), C52(H52),
  C59(H59), C53(H53), C57(H57), C58(H58), C56(H56)
5.d Idealised Me refined as rotating group:
 C94(H94A,H94B,H94C), C89(H89A,H89B,H89C)
;
_shelx_res_checksum              1338
_olex2_submission_special_instructions 'No special instructions were received'