Titanium(IV) chloride-mediated carbon-carbon bond-forming reaction between 3,3-dialkylcyclobutanones and aldehydes.
Matsuo, Jun-ichi; Kawano, Mizuki; Okuno, Ryosuke; Ishibashi, Hiroyuki; Organic letters 12 (2010) 3960–3962; doi:10.1021/ol101653b

data_1503180
_publ_section_title
;
 Titanium(IV) chloride-mediated carbon-carbon bond-forming reaction
 between 3,3-dialkylcyclobutanones and aldehydes.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              3960
_journal_page_last               3962
_journal_paper_doi               10.1021/ol101653b
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C20 H35 Cl O2 Si '
_chemical_formula_sum            'C20 H35 Cl O2 Si'
_chemical_formula_weight         371.03
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_cell_angle_alpha                90
_cell_angle_beta                 109.09(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.956(6)
_cell_length_b                   20.04(1)
_cell_length_c                   11.392(7)
_cell_measurement_reflns_used    7026
_cell_measurement_temperature    123.2
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.1
_cell_volume                     2148(2)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    DirectMethod
_diffrn_detector_area_resol_mean 14.46
_diffrn_measured_fraction_theta_full 0.9594
_diffrn_measured_fraction_theta_max 0.9594
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4896
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_exptl_absorpt_coefficient_mu    0.243
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.12
_refine_diff_density_min         -0.32
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2601
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.0019
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00106|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0753
_reflns_number_gt                2601
_reflns_number_total             4772
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol101653b_si_002.cif
_cod_data_source_block           '_matsuo11'
_cod_original_cell_volume        2147(2)
_cod_original_formula_sum        'C20 H35 Cl O2 Si '
_cod_database_code               1503180