X-ray Structure and Raman Spectrum of [Ti4(μ3-O)2(μ2-OiPr)2(OiPr)8(acac)2]: Presence of a Ti4(μ3-O)2(μ2-OiPr)2 Ladder-like Core
Paul D. Moran; Clifton E. F. Rickard; Graham A. Bowmaker; Ralph P. Cooney; John R. Bartlett; James L. Woolfrey; Inorganic Chemistry 37 (1998) 1417–1419; doi:10.1021/ic970942d

data_4322711
_publ_section_title
;
 X-ray Structure and Raman Spectrum of
 [Ti4(\m3-O)2(\m2-OiPr)2(OiPr)8(acac)2]: Presence of a
 Ti4(\m3-O)2(\m2-OiPr)2 Ladder-like Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1417
_journal_page_last               1419
_journal_paper_doi               10.1021/ic970942d
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C20 H42 O8 Ti2'
_chemical_formula_weight         506.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.000(10)
_cell_angle_beta                 105.19(2)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   12.056(4)
_cell_length_b                   15.846(2)
_cell_length_c                   14.758(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      12.0
_cell_measurement_theta_min      8.5
_cell_volume                     2720.9(11)
_computing_cell_refinement       'CAD-4 software'
_computing_data_collection       'CAD-4 software'
_computing_data_reduction        'Local software'
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4962
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        2.5
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.062
_refine_ls_goodness_of_fit_obs   1.067
_refine_ls_hydrogen_treatment    'Riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_restrained_S_obs      1.067
_refine_ls_R_factor_all          0.1248
_refine_ls_R_factor_obs          0.0671
_refine_ls_shift/esd_max         0.184
_refine_ls_shift/esd_mean        0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1567P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2431
_refine_ls_wR_factor_obs         0.1928
_reflns_number_observed          2996
_reflns_number_total             4696
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970942d.cif
_cod_data_source_block           C20H42O8Ti2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1567P)^2^+0.0000P] 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^)+(0.1567P)^2^+0.0000P] 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        2720.9(10)
_cod_database_code               4322711