Synthesis of Novel Tantalacalixarene Complexes: First Example of Intramolecular CH Activation of Monodepleted Aromatic Ring
Espinas, Jeff; Pelletier, Jérémie; Jeanneau, Erwan; Darbost, Ulrich; Szeto, Kai C.; Lucas, Christine; Thivolle-Cazat, Jean; Duchamp, Christian; Henriques, Natali; Bouchu, Denis; Basset, Jean-Marie; Chermette, Henry; Bonnamour, Isabelle; Taoufik, Mostafa; Organometallics 30 (2011) 3512–; doi:10.1021/om200140u

data_4064491
_publ_section_title
;
 Synthesis of Novel Tantalacalixarene Complexes: First Example of
 Intramolecular CH Activation of Monodepleted Aromatic Ring
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3512
_journal_paper_doi               10.1021/om200140u
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C66.50 H82.50 O4 Ta1'
_chemical_formula_sum            'C66.5 H82.5 O4 Ta'
_chemical_formula_weight         1126.83
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 105.974(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.653(5)
_cell_length_b                   19.076(5)
_cell_length_c                   21.946(5)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    150
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     5897(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            47482
_diffrn_reflns_theta_full        25.125
_diffrn_reflns_theta_max         27.917
_diffrn_reflns_theta_min         1.439
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.909
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2346
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.82
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1336
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         7700
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001497
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.535 -0.222 -0.516E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0763
_refine_ls_wR_factor_gt          0.0256
_refine_ls_wR_factor_ref         0.0236
_reflns_limit_h_max              18
_reflns_limit_h_min              -19
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                8424
_reflns_number_total             13666
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0289
_oxford_refine_ls_scale          0.23047(12)
_oxford_reflns_number_all        13627
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            om200140u_si_003.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C66.50 H82.50 O4 Ta1'
_cod_database_code               4064491