Homo- and Heterometallic Aluminum and Titanium Complexes of Tridentate (OSO) Ligand: Synthesis, Structure, and Catalytic Activity
Janas, Zofia; Jerzykiewicz, Lucjan B.; Sobota, Piotr; Szczegot, Krzysztof; Organometallics 24 (2005) 3987–; doi:10.1021/om050271o

data_4075900
_publ_section_title
;
 Homo- and Heterometallic Aluminum and Titanium Complexes of Tridentate
 (OSO) Ligand:&#x00A0; Synthesis, Structure, and Catalytic Activity
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3987
_journal_paper_doi               10.1021/om050271o
_journal_volume                  24
_journal_year                    2005
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C62 H96 O6 S2 Ti2, C4 H10 O '
_chemical_formula_sum            'C66 H106 O7 S2 Ti2'
_chemical_formula_weight         1171.50
_chemical_name_systematic        ' ?'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                79.10(3)
_cell_angle_beta                 81.80(3)
_cell_angle_gamma                78.79(3)
_cell_formula_units_Z            1
_cell_length_a                   7.011(3)
_cell_length_b                   13.791(6)
_cell_length_c                   17.957(5)
_cell_measurement_reflns_used    6328
_cell_measurement_temperature    100
_cell_measurement_theta_max      26
_cell_measurement_theta_min      3
_cell_volume                     1662.3(11)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2001)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2001)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'SHELXTL-NT (Bruker, 1999)'
_computing_publication_material  'SHELXTL-NT (Bruker, 1999)'
_computing_structure_refinement  'CRYSTALS (Watkin et al., 2003)'
_computing_structure_solution    'SHELXTL-NT (Bruker, 1999)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Kuma KM-4 CCD'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22259
_diffrn_reflns_reduction_process ' ?'
_diffrn_reflns_theta_full        26.79
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.351
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'CrysAlis CCD (Oxford Diffraction, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       ' plate'
_exptl_crystal_F_000             634
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.000186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         4235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.1289
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef F
_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:
 5.67 0.688 5.20 1.46 0.616
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0467
_refine_ls_wR_factor_ref         0.0553
_reflns_number_gt                4235
_reflns_number_total             7739
_reflns_threshold_expression     i>2.00u(i)
_cod_data_source_file            om050271osi20050411_033007.cif
_cod_data_source_block           C66H106O7S2Ti2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_formula_sum        'C66 H106 O7 S2 Ti2 '
_cod_database_code               4075900