Organotitanoxanes with Unique Structure among Transition-Element Organometallic Oxide Derivatives
Olga Buitrago; Marta E. G. Mosquera; Gerardo Jiménez; Tomás Cuenca; Inorganic Chemistry 47 (2008) 3940–3942; doi:10.1021/ic8003646

data_4305113
_publ_contact_author
;      Marta E. G. Mosquera
       Departamento de Qu\'imica Inorg\'anica
       Facultad de Farmacia
       Universidad de Alcal\'a
       Campus Universitario
       28871 Alcal\'a de Henares
       Spain
;
_publ_contact_author_email       martaeg.mosquera@uah.es
_publ_contact_author_fax         '0034 91 8854683'
_publ_contact_author_phone       '0034 91 8854779'
_publ_section_title
;
Organotitanoxanes with Unique Structure among Transition-Element
Organometallic Oxide Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3940
_journal_page_last               3942
_journal_paper_doi               10.1021/ic8003646
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C50 H86 Cl2 O7 Si4 Ti4'
_chemical_formula_weight         1174.05
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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           SHELXL-97
_cell_angle_alpha                65.561(7)
_cell_angle_beta                 77.952(15)
_cell_angle_gamma                85.307(10)
_cell_formula_units_Z            2
_cell_length_a                   12.484(2)
_cell_length_b                   15.7680(9)
_cell_length_c                   17.217(4)
_cell_measurement_reflns_used    167
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21.54
_cell_measurement_theta_min      3.846
_cell_volume                     3017.5(9)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0631
_diffrn_reflns_av_sigmaI/netI    0.1098
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            58326
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.448
_exptl_crystal_size_mid          0.292
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         13709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1210
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+0.4689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1617
_reflns_number_gt                8071
_reflns_number_total             13709
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8003646-file003_3.cif
_cod_data_source_block           4.C6H6
_cod_database_code               4305113