Synthesis and Structural Characterization of Lithium and Titanium Complexes Bearing a Bulky Aryloxide Ligand Based on a Rigid Fused-Ring s-Hydrindacene Skeleton.
Kanazawa, Shoya; Ohira, Taishi; Goda, Shun; Hayakawa, Naoki; Tanikawa, Tomoharu; Hashizume, Daisuke; Ishida, Yutaka; Kawaguchi, Hiroyuki; Matsuo, Tsukasa; Inorganic chemistry 55 (2016) 6643–6652; doi:10.1021/acs.inorgchem.6b00762

data_4344902
_publ_section_title
;
 Synthesis and Structural Characterization of Lithium and Titanium
 Complexes Bearing a Bulky Aryloxide Ligand Based on a Rigid Fused-Ring
 s-Hydrindacene Skeleton.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6643
_journal_page_last               6652
_journal_paper_doi               10.1021/acs.inorgchem.6b00762
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C32 H53 Cl2 O3 Ti'
_chemical_formula_sum            'C32 H53 Cl2 O3 Ti'
_chemical_formula_weight         604.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.037(17)
_cell_length_b                   12.339(9)
_cell_length_c                   23.767(18)
_cell_measurement_reflns_used    13962
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      31.5738
_cell_measurement_theta_min      1.6323
_cell_volume                     6463(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    SHELXLE
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku AFC-10 with Saturn70'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32040
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         3.014
_diffrn_source                   'Fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.1233
_exptl_crystal_colour            'Pale Green'
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       Block
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.30(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         11304
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0778
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0969P)^2^+5.7260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1865
_refine_ls_wR_factor_ref         0.2134
_reflns_Friedel_coverage         0.954
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                8109
_reflns_number_total             11304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00762_si_008.cif
_cod_data_source_block           shelxl
_cod_database_code               4344902
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.922
_shelx_estimated_absorpt_t_max   0.938
_shelx_res_checksum              98445
_shelx_hkl_checksum              21586