Structural Study of Acidic Metallocavitands and Characterization of their Interactions with Lewis Bases
Christian N. Garon; Serge I. Gorelsky; Olivier Sigouin; Tom K. Woo; Frédéric-Georges Fontaine; Inorganic Chemistry 48 (2009) 1699–1710; doi:10.1021/ic802233e

data_4301516
_publ_contact_author_address
;
      
      D\'epartement de Chimie
      Pavillon Alexandre-Vachon, Local 2257
      Universit\'e Laval
      Qu\'ebec, Canada
      G1K 7P4
;
_publ_contact_author_email       frederic.fontaine@chm.ulaval.ca
_publ_contact_author_fax         418-656-7916
_publ_contact_author_name        'Fr\'ed\'eric-Georges Fontaine'
_publ_contact_author_phone       '418 656-5140'
_publ_section_title
;
Structural Study of Acidic Metallocavitands and Characterization of their
Interactions with Lewis Bases
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1699
_journal_page_last               1710
_journal_paper_doi               10.1021/ic802233e
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C64 H94 B4 O12 Ta2'
_chemical_formula_weight         1460.53
_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                97.783(2)
_cell_angle_beta                 110.332(2)
_cell_angle_gamma                107.834(2)
_cell_formula_units_Z            2
_cell_length_a                   13.6909(19)
_cell_length_b                   16.068(2)
_cell_length_c                   16.587(2)
_cell_measurement_reflns_used    8040
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     3135.3(7)
_computing_cell_refinement       'APEX 2 (Bruker, 2005b)'
_computing_data_collection       'APEX 2 (Bruker, 2005b)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart APEX II CCD'
_diffrn_measurement_method       \w
_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  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33869
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    3.547
_exptl_absorpt_correction_T_max  0.8153
_exptl_absorpt_correction_T_min  0.6182
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'XPREP (Bruker, 2005a)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.696
_refine_diff_density_min         -1.244
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         12272
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0431P)^2^+1.1104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0927
_reflns_number_gt                9055
_reflns_number_total             12272
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802233e_si_002.cif
_cod_data_source_block           cng002
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_original_cell_volume        3135.3(8)
_cod_database_code               4301516