Extending the Family of Titanium Heterometallic-oxo-alkoxy Cages
Salvador Eslava; Benjamin P. R. Goodwill; Mary McPartlin; Dominic S. Wright; Inorganic Chemistry 50 (2011) 5655–5662; doi:10.1021/ic200350j

data_4325406
_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_section_title
;
 Extending the Family of Titanium Heterometallic-oxo-alkoxy Cages
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5655
_journal_page_last               5662
_journal_paper_doi               10.1021/ic200350j
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C40 H100 Mo4 O36 Ti8'
_chemical_formula_sum            'C40 H100 Mo4 O36 Ti8'
_chemical_formula_weight         1924.16
_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                 112.548(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.2373(5)
_cell_length_b                   16.2385(7)
_cell_length_c                   16.7247(6)
_cell_measurement_reflns_used    51196
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.02
_cell_volume                     3571.1(2)
_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 0.889
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_sigmaI/netI    0.0783
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17138
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         3.53
_exptl_absorpt_coefficient_mu    1.600
_exptl_absorpt_correction_T_max  1.022
_exptl_absorpt_correction_T_min  0.575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.644
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         7670
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0754
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1087P)^2^+13.8488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2085
_refine_ls_wR_factor_ref         0.2218
_reflns_number_gt                5687
_reflns_number_total             7670
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200350j_si_001_5.cif
_cod_data_source_block           5
_cod_database_code               4325406