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_4107422
_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        toluene
_chemical_formula_moiety         'C38 H35 Fe'
_chemical_formula_sum            'C38 H35 Fe'
_chemical_formula_weight         547.51
_chemical_name_systematic
; 
 tetraphenyl-cyclobutadiene-pentamethyl-cyclopentadienyl-iron
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                KHS-HD-010-01
_audit_creation_date             2007-09-06
_cell_angle_alpha                90.0
_cell_angle_beta                 113.860(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   13.7287(5)
_cell_length_b                   14.0318(6)
_cell_length_c                   15.9173(5)
_cell_measurement_reflns_used    52183
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      2.91
_cell_volume                     2804.23(19)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1072
_diffrn_reflns_av_sigmaI/netI    0.0856
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            51290
_diffrn_reflns_theta_full        33.19
_diffrn_reflns_theta_max         33.19
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_T_max  0.97921
_exptl_absorpt_correction_T_min  0.93442
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'XPREP, Siemens (1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         10702
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0338P)^2^+2.1497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                6640
_reflns_number_total             10702
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0777180-file001.cif
_cod_data_source_block           5955
_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_cell_volume        2804.23(18)
_cod_original_sg_symbol_Hall     '-p 2yn'
_cod_database_code               4107422