Iron-Arylimide Clusters [Fem(NAr)nCl4]2- (m,n= 2, 2; 3, 4; 4, 4) from a Ferric Amide Precursor: Synthesis, Characterization, and Comparison to Fe-S Chemistry
Jeremiah S. Duncan; Tamim M. Nazif; Atul K. Verma; Sonny C. Lee; Inorganic Chemistry 42 (2003) 1211–1224; doi:10.1021/ic025825j

data_4313144
_publ_section_title
;
 Iron-Arylimide Clusters [Fem(NAr)nCl4]2- (m,n= 2, 2; 3, 4; 4, 4) from a
 Ferric Amide Precursor: Synthesis, Characterization, and Comparison to
 Fe-S Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1211
_journal_page_last               1224
_journal_paper_doi               10.1021/ic025825j
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        'Chemical synthesis, S.C. Lee lab'
_chemical_formula_moiety
'(Li 1+) (C12H32LiN4)2 (Fe 3+) (Cl1-)2 (C6H18NSi2 1-)2'
_chemical_formula_structural     (Li(C6H16N2)2)FeCl2(N(SiC3H9)2)2
_chemical_formula_sum            'C24 H68 Cl2 Fe Li N6 Si4'
_chemical_formula_weight         686.89
_chemical_name_common            '[Li(TMEDA)2]{FeCl2[N(TMS)2]2}'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.7900(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.2815(4)
_cell_length_b                   22.4243(4)
_cell_length_c                   19.525
_cell_measurement_reflns_used    32350
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      1.06
_cell_volume                     8382.9(2)
_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  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14647
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         1.06
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.7490
_exptl_absorpt_correction_T_min  0.7093
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            redish-orange
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.030
_refine_ls_goodness_of_fit_obs   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         14647
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_restrained_S_obs      1.121
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_obs          0.0505
_refine_ls_shift/esd_max         0.008
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1433
_refine_ls_wR_factor_obs         0.1225
_reflns_number_observed          9263
_reflns_number_total             14647
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic025825j-2_s1_3.cif
_cod_data_source_block           '[Li(TMEDA)2]{FeCl2[N(TMS)2]2}'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        8383.1(2)
_cod_database_code               4313144