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_7117706
_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         'C32 H24 Br2 Fe N2, C7 H8'
_chemical_formula_sum            'C39 H32 Br2 Fe N2'
_chemical_formula_weight         744.33
_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   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                 107.5140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1652(10)
_cell_length_b                   12.2178(9)
_cell_length_c                   20.8109(16)
_cell_measurement_temperature    100(2)
_cell_volume                     3192.3(4)
_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(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            35088
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.473
_diffrn_reflns_theta_min         1.957
_exptl_absorpt_coefficient_mu    3.007
_exptl_absorpt_correction_T_max  0.5708
_exptl_absorpt_correction_T_min  0.4759
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS - Bruker area detector scaling and absorption correction - V2.10'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       needle
_exptl_crystal_F_000             1504
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.047
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         9251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+1.1754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0901
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                7298
_reflns_number_total             9251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc04908c2.cif
_cod_data_source_block           Compound1
_cod_database_code               7117706
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.571
_shelx_estimated_absorpt_t_min   0.476
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C16(H16)
2.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C24(H24), C7S(H7S), C23(H23), C4S(H4S), C3S(H3S), C30(H30), C5(H5),
 C12(H12), C6S(H6S), C20(H20), C4(H4), C25(H25), C5S(H5S), C19(H19), C15(H15),
 C8(H8), C29(H29), C28(H28), C11(H11), C27(H27), C14(H14), C13(H13), C9(H9),
 C10(H10), C31(H31), C32(H32)
2.c Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC)
;
_shelx_res_checksum              10396
_olex2_submission_special_instructions 'No special instructions were received'