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_4331625
_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            'C20 H54 O12 Si4 Ta2'
_chemical_formula_weight         960.89
_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                103.649(2)
_cell_angle_beta                 111.626(2)
_cell_angle_gamma                105.234(2)
_cell_formula_units_Z            1
_cell_length_a                   9.2043(8)
_cell_length_b                   10.7671(10)
_cell_length_c                   11.8911(11)
_cell_measurement_temperature    296(2)
_cell_volume                     981.55(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8805
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    5.735
_exptl_absorpt_correction_T_max  0.5227
_exptl_absorpt_correction_T_min  0.3066
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2825
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.840
_refine_ls_shift/su_mean         0.127
_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          0.0933
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                2439
_reflns_number_total             2825
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051274wsup2.cif
_cod_data_source_block           rk858
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_cell_volume        981.55(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4331625