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_4064490
_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         'C88 H106 Cl4 O6 Ta2'
_chemical_formula_sum            'C88 H106 Cl4 O6 Ta2'
_chemical_formula_weight         1763.51
_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
_cell_angle_alpha                116.445(6)
_cell_angle_beta                 98.994(5)
_cell_angle_gamma                97.308(5)
_cell_formula_units_Z            2
_cell_length_a                   16.3590(10)
_cell_length_b                   17.9810(10)
_cell_length_c                   19.7810(10)
_cell_measurement_reflns_used    10764
_cell_measurement_temperature    150
_cell_measurement_theta_max      62.6212
_cell_measurement_theta_min      4.2331
_cell_volume                     5016.6(6)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_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 0.957
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14984
_diffrn_reflns_theta_full        59.998
_diffrn_reflns_theta_max         62.708
_diffrn_reflns_theta_min         4.237
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.253
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.516
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.70
_refine_diff_density_min         -1.68
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0755
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     982
_refine_ls_number_reflns         13984
_refine_ls_number_restraints     172
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0763
_refine_ls_shift/su_max          0.0042773
_refine_ls_shift/su_mean         0.0005135
_refine_ls_structure_factor_coef Fsqd
_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: 
 0.122E+04 0.187E+04 969. 248. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2087
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.2087
_reflns_limit_h_max              17
_reflns_limit_h_min              -18
_reflns_limit_k_max              18
_reflns_limit_k_min              -20
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                10745
_reflns_number_total             13990
_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   0.0912
_oxford_refine_ls_scale          1.257(8)
_oxford_reflns_number_all        13984
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om200140u_si_002.cif
_cod_data_source_block           1
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4064490