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_4327207
_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
'(C16H36N 1+)2 (Fe 3+)2 (C9H11N 2-)2 (Cl 1-)4 (C2H3N)4'
_chemical_formula_structural     (C16H36N)2(Fe2(NC9H11)2(Cl)4(C2H3N)4
_chemical_formula_sum            'C58 H106 Cl4 Fe2 N8'
_chemical_formula_weight         1169.01
_chemical_name_common            (NBu4)2[Fe2(mu-NMes)2Cl4].4MeCN
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 122.2710(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.3740(9)
_cell_length_b                   21.0290(9)
_cell_length_c                   16.3194(6)
_cell_measurement_reflns_used    17225
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.49
_cell_measurement_theta_min      1.41
_cell_volume                     6782.4(5)
_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  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_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  0.0690
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17225
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.41
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.66205
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       parallelopippeds
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.031
_refine_ls_goodness_of_fit_obs   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         4412
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.035
_refine_ls_restrained_S_obs      1.093
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_obs          0.0489
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1426
_refine_ls_wR_factor_obs         0.1225
_reflns_number_observed          3011
_reflns_number_total             4413
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic0611332Bsi20060622_121538_05.cif
_cod_data_source_block           (NBu4)2[Fe2(mu-NMes)2Cl4].4MeCN
_cod_database_code               4327207