A Cheap Metal for a "Noble" Task: Preparative and Mechanistic Aspects of Cycloisomerization and Cycloaddition Reactions Catalyzed by Low-Valent Iron Complexes
Alois Fürstner; Keisuke Majima; Rubén Martín; Helga Krause; Egmont Kattnig; Richard Goddard; Christian W. Lehmann; Journal of the American Chemical Society 130 (2008) 1992–2004; doi:10.1021/ja0777180

data_4107423
_publ_section_title
;
 A Cheap Metal for a "Noble" Task: Preparative and Mechanistic Aspects of
 Cycloisomerization and Cycloaddition Reactions Catalyzed by Low-Valent
 Iron Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1992
_journal_page_last               2004
_journal_paper_doi               10.1021/ja0777180
_journal_volume                  130
_journal_year                    2008
_chemical_compound_source        tetrahydrofuran
_chemical_formula_moiety         'C9 H13 Fe 1-, Li 1+, C6 H16 N2'
_chemical_formula_sum            'C15 H29 Fe Li N2'
_chemical_formula_weight         300.19
_chemical_name_systematic
; 
 tetramethyl-ethylenediamine-lithium-bis-ethylene-cyclopentadienyl-iron
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                MJM-MC-193-01
_audit_creation_date             2007-09-05
_cell_angle_alpha                94.945(1)
_cell_angle_beta                 98.755(1)
_cell_angle_gamma                107.135(1)
_cell_formula_units_Z            2
_cell_length_a                   8.1030(2)
_cell_length_b                   9.4613(2)
_cell_length_c                   11.1671(2)
_cell_measurement_reflns_used    37181
_cell_measurement_temperature    100
_cell_measurement_theta_max      40.25
_cell_measurement_theta_min      2.91
_cell_volume                     800.77(3)
_computing_cell_refinement       'Denzo / Scalepack (Otwinowski 1997)'
_computing_data_collection       'Collect software (Nonius, 1998)'
_computing_data_reduction        'Denzo / Scalepack (Otwinowski 1997)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 18.18
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD \w-scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.3 mm focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29174
_diffrn_reflns_theta_full        37.47
_diffrn_reflns_theta_max         37.47
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_T_max  0.93035
_exptl_absorpt_correction_T_min  0.86537
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'XPREP, Siemens (1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         8064
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+0.3209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0927
_reflns_number_gt                7358
_reflns_number_total             8064
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0777180-file002.cif
_cod_data_source_block           5952
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               4107423