Achiral Tetrahydrosalen Ligands for the Synthesis of C2-Symmetric Titanium Complexes: A Structure and Diastereoselectivity Study
Jaume Balsells; Patrick J. Carroll; Patrick J. Walsh; Inorganic Chemistry 40 (2001) 5568–5574; doi:10.1021/ic010456x

data_4320425
_publ_section_title
;
 Achiral Tetrahydrosalen Ligands for the Synthesis of C2-Symmetric
 Titanium Complexes: A Structure and Diastereoselectivity Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5568
_journal_page_last               5574
_journal_paper_doi               10.1021/ic010456x
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C40 H68 N2 O4 Ti'
_chemical_formula_weight         688.86
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.124(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5777(2)
_cell_length_b                   10.6529(1)
_cell_length_c                   26.2556(2)
_cell_measurement_temperature    293(2)
_cell_volume                     4071.30(7)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            29253
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.249
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.151
_refine_ls_goodness_of_fit_obs   1.172
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_restrained_S_obs      1.172
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_obs          0.0713
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+5.0029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1654
_refine_ls_wR_factor_obs         0.1598
_reflns_number_observed          6487
_reflns_number_total             7170
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010456x_2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+5.0029P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+5.0029P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4320425