Highly Regioselective Alkyne Cyclotrimerization Catalyzed by Titanium Complexes Supported by Proximally Bridged p-tert-Butylcalix[4]arene Ligands
Oleg V. Ozerov; Folami T. Ladipo; Brian O. Patrick; Journal of the American Chemical Society 121 (1999) 7941–7942; doi:10.1021/ja990740b

data_4116502
_publ_section_title
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 Highly Regioselective Alkyne Cyclotrimerization Catalyzed by Titanium
 Complexes Supported by Proximally Bridged p-tert-Butylcalix[4]arene
 Ligands
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7941
_journal_page_last               7942
_journal_paper_doi               10.1021/ja990740b
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C54 H76 Cl2 O4 Si Ti'
_chemical_formula_weight         936.04
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 124.79(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.750(1)
_cell_length_b                   17.0434(9)
_cell_length_c                   17.1877(9)
_cell_measurement_reflns_used    22618
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.39
_cell_volume                     4991.9(7)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0837
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7735
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.347
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.0008(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.194
_refine_ls_goodness_of_fit_obs   1.258
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4382
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.193
_refine_ls_restrained_S_obs      1.256
_refine_ls_R_factor_all          0.1549
_refine_ls_R_factor_obs          0.1231
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+42.4482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2649
_refine_ls_wR_factor_obs         0.2505
_reflns_number_observed          3542
_reflns_number_total             4382
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja990740b.cif
_cod_data_source_block           k99013
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+42.4482P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+42.4482P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4991.9(4)
_cod_database_code               4116502