Polynuclear tantalum oxoalkoxides. Crystal structures of [Ta8O10(OEt)20], [Ta7O9(OPri)17] and [Ta5O7(OBut)11]·C6H5Me
Isaac Abrahams; Donald C. Bradley; Halina Chudzynska; Majid Motevalli; Paul O'Shaughnessy; J. Chem. Soc., Dalton Trans.  (2000) 2685–2691; doi:10.1039/b001797n

data_7009544
_publ_section_title
;
 Polynuclear tantalum oxoalkoxides. Crystal structures of
 [Ta8O10(OEt)20], [Ta7O9(OPri)17] and [Ta5O7(OBut)11]&#x00B7;C6H5Me
;
_journal_issue                   16
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              2685
_journal_page_last               2691
_journal_paper_doi               10.1039/b001797n
_journal_year                    2000
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C44 H99 O18 Ta5 . C7 H8'
_chemical_formula_structural     'C44 H99 O18 TA5 . C7 H8'
_chemical_formula_sum            'C51 H107 O18 Ta5'
_chemical_formula_weight         1913.12
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             2000-02-27T16:38:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                78.78(9)
_cell_angle_beta                 79.79(2)
_cell_angle_gamma                80.63(3)
_cell_formula_units_Z            2
_cell_length_a                   12.421(3)
_cell_length_b                   12.854(2)
_cell_length_c                   22.921(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.42
_cell_measurement_theta_min      11.48
_cell_measurement_wavelength     0.71073
_cell_volume                     3501.4(16)
_computing_cell_refinement       'CAD4/PC (Enraf Nonius, 1992)'
_computing_data_collection       'CAD4/PC (Enraf Nonius, 1992)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_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-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_sigmaI/netI    0.1032
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12901
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.63
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        13
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    7.839
_exptl_absorpt_correction_T_max  0.3086
_exptl_absorpt_correction_T_min  0.085
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1844
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.332
_refine_diff_density_min         -3.108
_refine_diff_density_rms         0.362
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         12284
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1546
_refine_ls_R_factor_gt           0.0876
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1636P)^2^+0.1697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2345
_refine_ls_wR_factor_ref         0.2645
_reflns_number_gt                7245
_reflns_number_total             12284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001797n.txt
_cod_data_source_block           h-tan2j
_cod_original_cell_volume        3501.4(12)
_cod_database_code               7009544
_exptl_absorpt_factor_mur        1.176
_diffrn_standards_decay_corr_max 1.215
_diffrn_standards_decay_corr_min 1