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_4344903
_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         'C28 H46 O'
_chemical_formula_sum            'C28 H46 O'
_chemical_formula_weight         398.65
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.287(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.295(2)
_cell_length_b                   7.9904(10)
_cell_length_c                   31.829(4)
_cell_measurement_reflns_used    6325
_cell_measurement_temperature    90
_cell_measurement_theta_max      32.5008
_cell_measurement_theta_min      1.2805
_cell_volume                     4903.3(10)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    SHELXLE
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku AFC-8 with Saturn70'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12145
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.9954
_exptl_absorpt_correction_T_min  0.9808
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         5588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0591P)^2^+3.0462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1495
_reflns_number_gt                3955
_reflns_number_total             5588
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00762_si_002.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        4903.2(11)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4344903