[6,6'-Bis(1,1-dimethylethyl)-4,4'-dimethyl-2,2'-methylenediphenolato-κ^2^<i>O</i>,<i>O</i>']dichlorido(9<i>H</i>-fluoren-9-ol-κ<i>O</i>)titanium(IV)–fluorene–diethyl ether (1/0.5/1)
Nielson, Alastair J.; Shen, Chaohong; Waters, Joyce M.; Acta Crystallographica Section E 69 (2013) m673–m674; doi:10.1107/S1600536813030249

data_2238842
_publ_section_title
;
 [6,6'-Bis(1,1-dimethylethyl)-4,4'-dimethyl-2,2'-methylenediphenolato-\k^2^<i>O</i>,<i>O</i>']dichlorido(9<i>H</i>-fluoren-9-ol-\k<i>O</i>)titanium(IV)--fluorene--diethyl
 ether (1/0.5/1)
;
_journal_coeditor_code           BV2226
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m673
_journal_page_last               m674
_journal_paper_doi               10.1107/S1600536813030249
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac
'[Ti Cl2 (C23 H30 O2) (C13 H10 O1)], C4 H10 O, 0.5C13 H10'
_chemical_formula_moiety
'[Ti Cl2 (C23 H30 O2) (C13 H10 O1)], C4 H10 O, 0.5(C13 H10)'
_chemical_formula_sum            'C46.5 H55 Cl2 O4 Ti'
_chemical_formula_weight         796.71
_chemical_name_systematic
'[6,6'-Bis(1,1-dimethylethyl)-4,4'-dimethyl-2,2'-methylenediphenolato-\k^2^<i>O</i>,<i>O</i>']dichlorido(9<i>H</i>-fluoren-9-ol-\k<i>O</i>)titanium(IV)--fluorene--diethyl ether (1/0.5/1)'
_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                110.28(3)
_cell_angle_beta                 109.22(3)
_cell_angle_gamma                91.72(3)
_cell_formula_units_Z            2
_cell_length_a                   12.710(3)
_cell_length_b                   13.227(3)
_cell_length_c                   14.431(3)
_cell_measurement_reflns_used    5551
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     2120.2(11)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS90 (Sheldrick, 2008)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Siemens SMART'
_diffrn_measurement_method       'Area detector \w scans'
_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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18146
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.369
_exptl_absorpt_correction_T_max  0.9711
_exptl_absorpt_correction_T_min  0.9037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Irregular fragment'
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.367
_refine_ls_extinction_coef       0.0008(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     531
_refine_ls_number_reflns         7432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0268P)^2^+1.2664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                6033
_reflns_number_total             7432
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            bv2226.cif
_cod_data_source_block           I
_cod_original_cell_volume        2120.2(7)
_cod_original_formula_sum        'C46.50 H55 Cl2 O4 Ti'
_cod_database_code               2238842