Syntheses, Characterizations, and X-ray Structures of Alkali Metal Derivatives of Titanium(IV) Neopentoxides
Timothy J. Boyle; Todd M. Alam; Cory J. Tafoya; Eric R. Mechenbier; Joseph W. Ziller; Inorganic Chemistry 38 (1999) 2422–2428; doi:10.1021/ic981143d

data_4322009
_publ_section_title
;
 Syntheses, Characterizations, and X-ray Structures of Alkali Metal
 Derivatives of Titanium(IV) Neopentoxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2422
_journal_page_last               2428
_journal_paper_doi               10.1021/ic981143d
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C50 H110 Li2 O10 Ti2'
_chemical_formula_weight         981.06
_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           SHELXTL
_cell_angle_alpha                75.39(2)
_cell_angle_beta                 73.31(2)
_cell_angle_gamma                71.65(2)
_cell_formula_units_Z            1
_cell_length_a                   10.656(3)
_cell_length_b                   12.202(5)
_cell_length_c                   13.266(3)
_cell_measurement_reflns_used    31
_cell_measurement_temperature    158
_cell_measurement_theta_max      12.52
_cell_measurement_theta_min      3.25
_cell_volume                     1543.2(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        CARESS
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      158
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
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_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.056
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       Plate
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
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_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_obs          0.0506
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_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+1.7823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1373
_refine_ls_wR_factor_obs         0.1199
_reflns_number_observed          3012
_reflns_number_total             4026
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981143d_1.cif
_cod_data_source_block           snl43
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+1.7823P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+1.7823P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1543.3(8)
_cod_database_code               4322009