Tetrabenzo[a,c,g,i]fluorenyltitanium(III) and -(IV) Complexes: Syntheses, Reactions, and Catalytic Application
Schröder, Kai; Haase, Detlev; Saak, Wolfgang; Beckhaus, Ruediger; Kretschmer, Winfried P.; Lützen, Arne; Organometallics 27 (2008) 1859–; doi:10.1021/om7012293

data_4071058
_publ_section_title
;
 Tetrabenzo[a,c,g,i]fluorenyltitanium(III) and -(IV) Complexes: Syntheses,
 Reactions, and Catalytic Application
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1859
_journal_paper_doi               10.1021/om7012293
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C50.5 H34 Cl2 O Ti'
_chemical_formula_weight         775.58
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                92.982(10)
_cell_angle_beta                 95.251(10)
_cell_angle_gamma                109.988(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5715(8)
_cell_length_b                   12.8182(10)
_cell_length_c                   16.3538(14)
_cell_measurement_temperature    153(2)
_cell_volume                     1870.2(3)
_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 0.940
_diffrn_measured_fraction_theta_max 0.927
_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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17200
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.412
_exptl_absorpt_correction_T_max  0.9296
_exptl_absorpt_correction_T_min  0.8364
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRED (Stoe, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             802
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.397
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         6865
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0801P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                5378
_reflns_number_total             6865
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7012293-file007.cif
_cod_data_source_block           DCP252
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C50.50 H34 Cl2 O Ti'
_cod_database_code               4071058