Crystal structure of μ-oxido-1,1'κ^2^<i>O</i>:<i>O</i>-bis{tetra-μ-oxido-1:2κ^2^<i>O</i>:<i>O</i>;1:3κ^2^<i>O</i>:<i>O</i>;2:3κ^4^<i>O</i>:<i>O</i>-tris[1,2,3(η^5^)-pentamethylcyclopentadienyl]-<i>trianglo</i>-trititanium(IV)}
Pérez-Redondo, Adrián; Martín, Avelino; Acta Crystallographica Section E 71 (2015) m97–; doi:10.1107/S2056989015004041

data_2240520
_publ_section_title
;
 Crystal structure of
 \m-oxido-1,1'\k^2^<i>O</i>:<i>O</i>-bis{tetra-\m-oxido-1:2\k^2^<i>O</i>:<i>O</i>;1:3\k^2^<i>O</i>:<i>O</i>;2:3\k^4^<i>O</i>:<i>O</i>-tris[1,2,3(\h^5^)-pentamethylcyclopentadienyl]-<i>trianglo</i>-trititanium(IV)}
;
_journal_coeditor_code           RZ5150
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m97
_journal_paper_doi               10.1107/S2056989015004041
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Ti6 O9 (C10 H15)6]'
_chemical_formula_moiety         'C60 H90 O9 Ti6'
_chemical_formula_sum            'C60 H90 O9 Ti6'
_chemical_formula_weight         1242.71
_chemical_name_systematic
\m-Oxido-1,1'\k^2^<i>O</i>:<i>O</i>-bis{tetra-\m-oxido-1:2\k^2^<i>O</i>:<i>O</i>;1:3\k^2^<i>O</i>:<i>O</i>;2:3\k^4^<i>O</i>:<i>O</i>-tris-[1,2,3(\h^5^)-pentamethylcyclopentadienyl]-<i>trianglo</i>-trititanium(IV)}
_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     other
_atom_sites_solution_secondary   difmap
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.265(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.086(6)
_cell_length_b                   11.414(4)
_cell_length_c                   17.900(5)
_cell_measurement_reflns_used    169
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     6229(3)
_computing_cell_refinement
;
Dirax/lsq (Duisenberg <i>et al.</i>, 2000)
;
_computing_data_collection
;
COLLECT (Nonius, 1998)
;
_computing_data_reduction
;
EvalCCD (Duisenberg <i>et al.</i>, 2003)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
WinGX (Farrugia, 2012) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL-2014/7 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT-2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1206
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            64311
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.505
_diffrn_reflns_theta_min         3.075
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Blessing, 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.419
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     354
_refine_ls_number_reflns         7159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+19.8847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1329
_reflns_number_gt                5059
_reflns_number_total             7159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rz5150sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2240520
_cod_database_fobs_code          2240520