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_4344907
_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         'C84 H135 Li3 O3'
_chemical_formula_sum            'C84 H135 Li3 O3'
_chemical_formula_weight         1213.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 108.362(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.929(10)
_cell_length_b                   12.248(3)
_cell_length_c                   33.721(8)
_cell_measurement_reflns_used    12278
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.08
_cell_measurement_theta_min      1.10
_cell_volume                     15260(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    SHELXLE
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1439
_diffrn_reflns_av_unetI/netI     0.1038
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            119190
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         3.055
_diffrn_source                   'Fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.986
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   NUMABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.057
_exptl_crystal_description       Block
_exptl_crystal_F_000             5376
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.147
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.388
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         17499
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.388
_refine_ls_R_factor_all          0.1895
_refine_ls_R_factor_gt           0.1643
_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^)+(0.0785P)^2^+55.6862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3058
_refine_ls_wR_factor_ref         0.3236
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14629
_reflns_number_total             17499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00762_si_004.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_cell_volume        15259(6)
_cod_database_code               4344907
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.987
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              13354
_shelx_hkl_checksum              41395