Titanocene dichloride route to a tetranuclear oxo-bridged monocyclopentadienyl titanium(IV) calix[4]arene complex
Petrella, Antonella J.; Roberts, Nicholas K.; Raston, Colin L.; Thornton-Pett, Mark; Lamb, Robert N.; Chemical Communications (Cambridge, United Kingdom)  (2003) 1238–1239; doi:10.1039/b301313h

data_7113777
_publ_section_title
;
 Titanocene dichloride route to a tetranuclear oxo-bridged
 monocyclopentadienyl titanium(IV) calix[4]arene complex
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   11
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1238
_journal_page_last               1239
_journal_paper_doi               10.1039/b301313h
_journal_year                    2003
_chemical_formula_sum            'C99 H112 O8 Ti4'
_chemical_formula_weight         1621.49
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 122.6460(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   35.1810(4)
_cell_length_b                   13.3310(2)
_cell_length_c                   21.8260(2)
_cell_measurement_temperature    150(2)
_cell_volume                     8619.2(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
;
ORTEP3 for Windows (Farrugia, 1997) 
XSeed (Barbour, 2001)
;
_computing_publication_material  'WC (Thornton-Pett, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0980
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            67155
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.413
_exptl_absorpt_correction_T_max  0.9637
_exptl_absorpt_correction_T_min  0.8076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3432
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0010(2)
_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_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         8460
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+11.1666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1361
_reflns_number_gt                6919
_reflns_number_total             8460
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103665
_cod_data_source_file            b301313h.txt
_cod_data_source_block           compound1
_cod_original_cell_volume        8619.20(18)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7113777