Synthesis and Reactivity of Sterically Encumbered Diazaferrocenes
Kreye, Markus; Baabe, Dirk; Schweyen, Peter; Freytag, Matthias; Daniliuc, Constantin G.; Jones, Peter G.; Walter, Marc D.; Organometallics 32 (2013) 5887–; doi:10.1021/om400474e

data_4081533
_publ_section_title
;
 Synthesis and Reactivity of Sterically Encumbered Diazaferrocenes
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5887
_journal_paper_doi               10.1021/om400474e
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C34 H58 F6 Fe Sb'
_chemical_formula_weight         758.40
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.070(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.6586(10)
_cell_length_b                   14.7578(8)
_cell_length_c                   12.1964(8)
_cell_measurement_reflns_used    8859
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.7540
_cell_measurement_theta_min      3.7540
_cell_volume                     3432.2(4)
_computing_cell_refinement
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_collection
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_reduction
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31772
_diffrn_reflns_theta_full        75.00
_diffrn_reflns_theta_max         76.00
_diffrn_reflns_theta_min         3.79
_exptl_absorpt_coefficient_mu    10.091
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+3.4723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0753
_reflns_number_gt                3259
_reflns_number_total             3584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400474e_si_004.cif
_cod_data_source_block           mk82
_cod_original_cell_volume        3432.2(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4081533