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_4064489
_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_absolute_configuration unk
_chemical_formula_moiety         'C51 H62 O3'
_chemical_formula_sum            'C51 H62 O3'
_chemical_formula_weight         723.01
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 102.71(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.245(2)
_cell_length_b                   22.608(3)
_cell_length_c                   15.123(3)
_cell_measurement_reflns_used    2658
_cell_measurement_temperature    293
_cell_measurement_theta_max      63.9793
_cell_measurement_theta_min      3.9061
_cell_volume                     4417.5(13)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_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      293
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\f & \w scans'
_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  0.057
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6825
_diffrn_reflns_theta_full        58.641
_diffrn_reflns_theta_max         62.384
_diffrn_reflns_theta_min         3.910
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.40
_refine_ls_extinction_coef       18(5)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9765
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         4219
_refine_ls_number_restraints     80
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0807
_refine_ls_shift/su_max          0.0029004
_refine_ls_shift/su_mean         0.0005596
_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: 
 840. 0.131E+04 692. 201. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2046
_refine_ls_wR_factor_gt          0.1643
_refine_ls_wR_factor_ref         0.2046
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              -17
_reflns_number_gt                3111
_reflns_number_total             4222
_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   0.0987
_oxford_refine_ls_scale          1.70(2)
_oxford_reflns_number_all        4219
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om200140u_si_001.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      'C 1 c 1 '
_cod_database_code               4064489