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_7104078
_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         'C76 H88 O6 Ti2,C H2 Cl2'
_chemical_formula_sum            'C77 H90 Cl2 O6 Ti2'
_chemical_formula_weight         1278.3
_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                66.479(4)
_cell_angle_beta                 86.395(5)
_cell_angle_gamma                68.356(5)
_cell_formula_units_Z            2
_cell_length_a                   13.034(1)
_cell_length_b                   16.744(2)
_cell_length_c                   19.276(2)
_cell_measurement_temperature    150
_cell_volume                     3568(2)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_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      150(2)
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method
;
Detector set at 30mm from sample with different 2theta offsets 
1 degree phi exposures for chi=0 degree settings
1 degree omega exposures for chi=90 degree settings
;
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            76059
_diffrn_reflns_theta_max         27.50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.19
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1356.0
_refine_diff_density_max         1.37
_refine_diff_density_min         -1.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.91
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     307
_refine_ls_number_reflns         13583
_refine_ls_R_factor_gt           0.087
_refine_ls_shift/su_max          0.006
_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         0.132
_reflns_number_gt                13583
_reflns_number_total             16318
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b301075a.txt
_cod_data_source_block           2
_cod_database_code               7104078