Synthesis, Structural and Spectroscopic Characterization, Catalytic Properties, and Thermal Transformations of New Cyclic Di- and Trisiloxanediolato Tantalum Complexes
Kapoor, Ramesh N.; Cervantes-Lee, Francisco; Campana, Charles F.; Haltiwanger, Curtis; Abney, Kent; Pannell, Keith H.; Inorganic Chemistry 45 (2006) 2203–2208; doi:10.1021/ic051274w

data_4331623
_publ_section_title
;
 Synthesis, Structural and Spectroscopic Characterization, Catalytic
 Properties, and Thermal Transformations of New Cyclic Di- and
 Trisiloxanediolato Tantalum Complexes
;
_journal_issue                   5
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2203
_journal_page_last               2208
_journal_paper_doi               10.1021/ic051274w
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C12 H35 O8 Si5 Ta'
_chemical_formula_weight         628.80
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.6917(4)
_cell_length_b                   17.1502(5)
_cell_length_c                   23.9634(7)
_cell_measurement_reflns_used    8470
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.7
_cell_measurement_theta_min      4.7
_cell_volume                     5216.0(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            63757
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    4.474
_exptl_absorpt_correction_T_max  0.5939
_exptl_absorpt_correction_T_min  0.3892
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.705
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         6000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.355
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0845
_reflns_number_gt                4762
_reflns_number_total             6000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051274wsup1.cif
_cod_data_source_block           utep1s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4331623