Tetranuclear BINOL-Titanium Complex in Selective Direct Aldol Additions
Bernd Schetter; Burkhard Ziemer; Gregor Schnakenburg; Rainer Mahrwald; Journal of Organic Chemistry 73 (2008) 813–819; doi:10.1021/jo7014054

data_4023221
_publ_section_title
;
 Tetranuclear BINOL-Titanium Complex in Selective Direct Aldol Additions
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              813
_journal_page_last               819
_journal_paper_doi               10.1021/jo7014054
_journal_volume                  73
_journal_year                    2008
_chemical_formula_moiety         'C13 H15 Cl O2'
_chemical_formula_sum            'C13 H15 Cl O2'
_chemical_formula_weight         238.70
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 109.81(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.498(3)
_cell_length_b                   8.232(3)
_cell_length_c                   12.746(3)
_cell_measurement_reflns_used    54
_cell_measurement_temperature    180(1)
_cell_measurement_theta_max      16.9.0
_cell_measurement_theta_min      13.1
_cell_volume                     1233.7(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(1)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device       'STOE Stadi4 Diffractometer'
_diffrn_measurement_method
; Scan width (omega) = 2.15 - 2.27, scan ratio 2theta:omega = 0.50
  I(Net) and sigma(I) calculated according to Blessing (1987)
;
_diffrn_radiation_collimation    '0.8 mm'
_diffrn_radiation_detector       'NaI(Tl) Scintillation Counter'
_diffrn_radiation_monochromator  'Planar Graphite'
_diffrn_radiation_polarisn_norm  90
_diffrn_radiation_source         'Sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0117
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2604
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        3.5
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.23
_exptl_absorpt_correction_T_max  0.9210
_exptl_absorpt_correction_T_min  0.8320
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
    Psi Scan Reflections used    Mu * R = 0.05  

    H   K   L   2Theta   Chi   Imin/Imax
   -3  -1   1    11.0   -72.4    0.857
   -3  -3   1    17.9   -77.2    0.842
   -3  -3   2    18.2   -71.5    0.828
    4   4  -1    23.9    77.6    0.861
    5   4   0    26.5    78.6    0.881
   -6  -4   1    28.4   -85.7    0.859
   -7  -4   4    31.1   -76.2    0.868
    6   5   1    33.7    73.3    0.921
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       block
_exptl_crystal_F_000             144
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0010(13)
_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   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+0.7544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1258
_reflns_d_resolution_high        0.811
_reflns_d_resolution_low         11.974
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_observed          1651
_reflns_number_total             2604
_reflns_observed_criterion       I>4sigma(I)
_cod_data_source_file            jo7014054-File005.cif
_cod_data_source_block           d:\roentgen\greg91\greg91
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4023221