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_4075898
_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         'C76 H130 Al2 O14 S2 Ti2 '
_chemical_formula_sum            'C76 H130 Al2 O14 S2 Ti2'
_chemical_formula_weight         1481.76
_chemical_name_systematic        ' ?'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90.30(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.018(3)
_cell_length_b                   21.743(4)
_cell_length_c                   21.141(4)
_cell_measurement_reflns_used    11435
_cell_measurement_temperature    100
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     4145.2(18)
_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
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type
;
Oxford Diffraction KUMA KM4
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Kuma KM4CCD kappa-axis diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28734
_diffrn_reflns_reduction_process ' ?'
_diffrn_reflns_theta_full        21.43
_diffrn_reflns_theta_max         28.57
_diffrn_reflns_theta_min         3.52
_exptl_absorpt_coefficient_mu    0.321
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.280
_refine_diff_density_min         -0.550
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         4655
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1623
_refine_ls_R_factor_gt           0.0737
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 1.93 -1.24 1.24 -0.966E-01 -0.251'

 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:
 1.93 -1.24 1.24 -0.966E-01 -0.251
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0712
_reflns_number_gt                4655
_reflns_number_total             9539
_reflns_threshold_expression     i>2.00u(i)
_cod_data_source_file            om050271osi20050411_033007.cif
_cod_data_source_block           C76H130Al2O14S2Ti2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C76 H130 Al2 O14 S2 Ti2 '
_cod_database_code               4075898