Oxygen-Centered Hexatantalum Tetradecaimido Cluster Complexes
Jamin L. Krinsky; Laura L. Anderson; John Arnold; Robert G. Bergman; Inorganic Chemistry 47 (2008) 1053–1066; doi:10.1021/ic701920v

data_4304419
_publ_section_title
;
Oxygen-Centered Hexatantalum Tetradecaimido Cluster Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1053
_journal_page_last               1066
_journal_paper_doi               10.1021/ic701920v
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C90 H75 O5 Si5 Ta, C6 H6'
_chemical_formula_sum            'C96 H81 O5 Si5 Ta'
_chemical_formula_weight         1636.01
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 107.564(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.873(3)
_cell_length_b                   13.937(2)
_cell_length_c                   26.999(4)
_cell_measurement_reflns_used    2046
_cell_measurement_temperature    165(2)
_cell_measurement_theta_max      18.84
_cell_measurement_theta_min      2.53
_cell_volume                     8206(2)
_computing_cell_refinement       'Bruker SAINT v7.07B'
_computing_data_collection       'Bruker SMART v5.631'
_computing_data_reduction        'Bruker SAINT v7.07B'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      165(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_sigmaI/netI    0.1128
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23045
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.58
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.466
_exptl_absorpt_correction_T_max  0.7993
_exptl_absorpt_correction_T_min  0.7387
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.660
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.132(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     965
_refine_ls_number_reflns         11758
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0998
_reflns_number_gt                9832
_reflns_number_total             11758
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701920v-file006.cif
_cod_data_source_block           compound_12
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4304419