Low-Valent Pentafulvene Titanium Dinitrogen Complex as a Precursor for Cationic Titanium Complexes
Scherer, Axel; Haase, Detlev; Saak, Wolfgang; Beckhaus, Rüdiger; Meetsma, Auke; Bouwkamp, Marco W.; Organometallics 28 (2009) 6969–; doi:10.1021/om900875e

data_4070501
_publ_section_title
;
 Low-Valent Pentafulvene Titanium Dinitrogen Complex as a Precursor for
 Cationic Titanium Complexes
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6969
_journal_paper_doi               10.1021/om900875e
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C51 H49 B F15 O2 Ti'
_chemical_formula_weight         1037.61
_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                 115.070(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.0821(17)
_cell_length_b                   13.4214(4)
_cell_length_c                   25.5905(14)
_cell_measurement_temperature    153(2)
_cell_volume                     9358.6(9)
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_collection       'IPDS (Stoe, 1999)'
_computing_data_reduction        'XRED (Stoe, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Stoe IPDS'
_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  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40486
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_T_max  0.9171
_exptl_absorpt_correction_T_min  0.8481
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4264
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         8835
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1115P)^2^+8.0056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1760
_reflns_number_gt                6493
_reflns_number_total             8835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900875e_si_001.cif
_cod_data_source_block           ADABET2
_cod_original_cell_volume        9358.6(8)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4070501