Synthesis and Elaboration of the Dinuclear Iron-Imide Cluster Core [Fe2(μ-NR)2]2+
Jeremiah S. Duncan; Michael J. Zdilla; Sonny C. Lee; Inorganic Chemistry 46 (2007) 1071–1080; doi:10.1021/ic061133+

data_4327208
_publ_contact_author_address
;                                                                               
 Department of Chemistry
 University of Waterloo
 200 University Avenue West
 Waterloo, Ontario  N2L 3G1
 CANADA  
;
_publ_contact_author_email       sclee@uwaterloo.ca
_publ_contact_author_fax         519-746-0435
_publ_contact_author_name        'Sonny C. Lee'
_publ_contact_author_phone       '519-885-1211 x7501'
_publ_section_title
;
 Synthesis and Elaboration of the Dinuclear Iron-Imide Cluster Core
 [Fe2(\m-NR)2]2+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1071
_journal_page_last               1080
_journal_paper_doi               10.1021/ic061133+
_journal_volume                  46
_journal_year                    2007
_chemical_compound_source        'Chemical synthesis, S.C. Lee lab'
_chemical_formula_moiety
'(Fe 2+)4 (Fe 3+)3 (C4H9N 2-)4 (Cl -)8 (C4H10O2)6'
_chemical_formula_structural     (Fe3Cl4(O2C4H10)5)(Fe4(NC4H9)4Cl4)2(C4H10O2)
_chemical_formula_sum            'C56 H132 Cl12 Fe11 N8 O12'
_chemical_formula_weight         2149.45
_chemical_name_common            '[Fe3Cl4(DME)5][Fe4(mu3-NtBu)4Cl4]2.DME'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 119.177(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.2691(10)
_cell_length_b                   27.751(2)
_cell_length_c                   19.3230(12)
_cell_measurement_reflns_used    15241
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21.50
_cell_measurement_theta_min      1.32
_cell_volume                     9958.1(11)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'CIFTAB, Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15241
_diffrn_reflns_theta_max         21.50
_diffrn_reflns_theta_min         1.32
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.920
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       needles
_exptl_crystal_F_000             4440
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.755
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1005
_refine_ls_number_reflns         7734
_refine_ls_number_restraints     511
_refine_ls_restrained_S_all      1.018
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_obs          0.0658
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+107.6406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1566
_refine_ls_wR_factor_obs         0.1444
_reflns_number_observed          6079
_reflns_number_total             7734
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic0611332Bsi20060622_121538_06.cif
_cod_data_source_block           '[Fe3Cl4(DME)5][Fe4(mu3-NtBu)4Cl4]2.DME'
_cod_original_cell_volume        9958.0(11)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4327208