Tetrabenzo[a,c,g,i]fluorenyllithium and η5-Tetrabenzo[a,c,g,i]fluorenyltitanium Complexes
Schröder, Kai; Haase, Detlev; Saak, Wolfgang; Lützen, Arne; Beckhaus, Rüdiger; Wichmann, Silke; Schellenberg, Jürgen; Organometallics 25 (2006) 3824–; doi:10.1021/om0602613

data_4075379
_publ_section_title
;
 Tetrabenzo[a,c,g,i]fluorenyllithium and
 \h5-Tetrabenzo[a,c,g,i]fluorenyltitanium Complexes
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3824
_journal_paper_doi               10.1021/om0602613
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C59 H36 Cl2'
_chemical_formula_weight         815.78
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.980(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8807(8)
_cell_length_b                   20.0576(8)
_cell_length_c                   14.8992(10)
_cell_measurement_temperature    153(2)
_cell_volume                     3873.1(4)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31892
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  0.9628
_exptl_absorpt_correction_T_min  0.9390
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRED (Stoe, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         7507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0448P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                4918
_reflns_number_total             7507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0602613si20060323_092143.cif
_cod_data_source_block           TITBF
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4075379