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_7009543
_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         'C51 H119 O26 Ta7'
_chemical_formula_structural     'C51 H119 O26 TA7'
_chemical_formula_sum            'C51 H119 O26 Ta7'
_chemical_formula_weight         2415.11
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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     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             2000-02-29T20:23:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 98.56(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.847(9)
_cell_length_b                   13.626(5)
_cell_length_c                   27.917(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.91
_cell_measurement_theta_min      11.94
_cell_measurement_wavelength     0.71073
_cell_volume                     8218(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.9484E-2
_diffrn_orient_matrix_UB_12      -0.70712E-1
_diffrn_orient_matrix_UB_13      -0.7195E-2
_diffrn_orient_matrix_UB_21      0.9317E-2
_diffrn_orient_matrix_UB_22      -0.15498E-1
_diffrn_orient_matrix_UB_23      0.35374E-1
_diffrn_orient_matrix_UB_31      -0.44339E-1
_diffrn_orient_matrix_UB_32      0.11878E-1
_diffrn_orient_matrix_UB_33      0.00331
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.1062
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            7433
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.48
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        29
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    9.341
_exptl_absorpt_correction_T_max  0.1544
_exptl_absorpt_correction_T_min  0.0479
_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    1.952
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4576
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.875
_refine_diff_density_min         -1.359
_refine_diff_density_rms         0.22
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         7228
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1425
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.056
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0733P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1584
_reflns_number_gt                4128
_reflns_number_total             7228
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001797n.txt
_cod_data_source_block           haltan
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7009543
_exptl_absorpt_factor_mur        1.868
_diffrn_standards_decay_corr_max 1.518
_diffrn_standards_decay_corr_min 1