Synthesis and characterization of tantalum silsesquioxane complexes.
Guillo, Pascal; Fasulo, Meg E.; Lipschutz, Michael I.; Tilley, T. Don; Dalton transactions (Cambridge, England : 2003) 42 (2013) 1991–1995; doi:10.1039/c2dt32601a

data_7020952
_publ_section_title
;
 Synthesis and characterization of tantalum silsesquioxane complexes.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1991
_journal_page_last               1995
_journal_paper_doi               10.1039/c2dt32601a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C66 H84 B F20 N2 O12 Si7 Ta'
_chemical_formula_weight         1865.75
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                102.447(5)
_cell_angle_beta                 90.694(5)
_cell_angle_gamma                94.252(5)
_cell_formula_units_Z            2
_cell_length_a                   14.324(5)
_cell_length_b                   14.832(5)
_cell_length_c                   19.356(5)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.249
_cell_measurement_theta_min      2.501
_cell_volume                     4003(2)
_computing_cell_refinement       'Bruker Apex2 v. 2009.2.1'
_computing_data_collection       'Bruker Apex2 v. 2009.2.1'
_computing_data_reduction        'Bruker Apex2 v. 2009.2.1'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.129
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       '/w and /f scans'
_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  0.0539
_diffrn_reflns_av_sigmaI/netI    0.0791
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26149
_diffrn_reflns_theta_full        25.27
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    1.581
_exptl_absorpt_correction_T_max  0.9253
_exptl_absorpt_correction_T_min  0.9253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1892
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.209
_refine_diff_density_min         -2.517
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1003
_refine_ls_number_reflns         13907
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.0830
_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^)+(0.1276P)^2^+28.8789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2084
_refine_ls_wR_factor_ref         0.2439
_reflns_number_gt                8450
_reflns_number_total             11281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32601a.txt
_cod_data_source_block           5(CH3CN)
_cod_database_code               7020952