Single-Source Materials for Metal-Doped Titanium Oxide: Syntheses, Structures, and Properties of a Series of Heterometallic Transition-Metal Titanium Oxo Cages
Salvador Eslava; Mary McPartlin; Richard I. Thomson; Jeremy M. Rawson; Dominic S. Wright; Inorganic Chemistry 49 (2010) 11532–11540; doi:10.1021/ic101687m

data_4317335
_publ_contact_author_address
;
 University of Cambridge
 Department of Chemistry   
 Lensfield Road
 Cambridge
 CB2 1EW
 England   
;
_publ_contact_author_email       se296@cam.ac.uk
_publ_contact_author_name        'S. Eslava'
_publ_contact_author_phone       00441223763122
_publ_section_title
;
 Single-Source Materials for Metal-Doped Titanium Oxide: Syntheses,
 Structures, and Properties of a Series of Heterometallic Transition-Metal
 Titanium Oxo Cages
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11532
_journal_page_last               11540
_journal_paper_doi               10.1021/ic101687m
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety
'C30 H75 Cl3 Mn2 O16 Ti4,0.5(C4 H8 O), 0.5(C2 H6 O)'
_chemical_formula_sum            'C33 H82 Cl3 Mn2 O17 Ti4'
_chemical_formula_weight         1158.82
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 92.1820(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.72430(10)
_cell_length_b                   20.4895(3)
_cell_length_c                   23.5632(3)
_cell_measurement_reflns_used    141723
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      1.00
_cell_volume                     5656.37(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            56607
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.167
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2420
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         9906
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+14.6481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1818
_refine_ls_wR_factor_ref         0.1923
_reflns_number_gt                7677
_reflns_number_total             9906
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101687m_si_001_7.cif
_cod_data_source_block           6
_cod_database_code               4317335