Selective synthesis of conformationally restricted mono-cyclopentadienyl titanium(IV) complexes of p-tBu-calix[6]arene
Robert Norman Lamb; Donald C. Craig; Antonella J. Petrella; Colin L. Raston; Nicholas K. Roberts; Chemical communications (Cambridge, England)  (2003) –; doi:10.1039/b301075a

data_7104077
_publ_section_title
;
Selective synthesis of conformationally restricted
mono-cyclopentadienyl titanium(IV) complexes of 
p-tBu-calix[6]arene
;
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/b301075a
_journal_year                    2003
_chemical_formula_moiety         'C71 H83 O6 Ti, C H2 Cl2'
_chemical_formula_sum            'C72 H85 Cl2 O6 Ti'
_chemical_formula_weight         1165.3
_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_type_scat_source
'International Tables for X-ray Crystallography, Vol. IV'
_audit_creation_method           'RAELSPUB and manual entry'
_cell_angle_alpha                81.76(1)
_cell_angle_beta                 69.15(1)
_cell_angle_gamma                89.29(1)
_cell_formula_units_Z            2
_cell_length_a                   13.871(8)
_cell_length_b                   16.411(9)
_cell_length_c                   16.474(9)
_cell_measurement_reflns_used    976
_cell_measurement_temperature    273
_cell_measurement_theta_max      26.04
_cell_measurement_theta_min      2.51
_cell_volume                     3465(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-II, (Johnson, 1976)'
_computing_publication_material  'Local programs'
_computing_structure_refinement  'RAELS, (Rae, 1989)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      273(2)
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            33488
_diffrn_reflns_theta_max         28.36
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.12
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1242.0
_refine_diff_density_max         2.69
_refine_diff_density_min         -0.75
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.04
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     284
_refine_ls_number_reflns         11364
_refine_ls_R_factor_gt           0.116
_refine_ls_shift/su_max          0.016
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(F) + 0.0004F^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.180
_reflns_number_gt                11364
_reflns_number_total             15811
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b301075a.txt
_cod_data_source_block           1
_cod_database_code               7104077