Titanium(IV) chloride, zirconium(IV) chloride or boron trichloride and phosphine-promoted Baylis–Hillman reaction of aldehydes with α,β-unsaturated ketone
Shi, Min; Jiang, Jian-Kang; Cui, Shi-Cong; Feng, Yan-Shu; Journal of the Chemical Society, Perkin Transactions 1  (2001) 390–; doi:10.1039/b008105l

data_7213438
_publ_section_title
;
 Titanium(IV) chloride, zirconium(IV) chloride or boron trichloride and
 phosphine-promoted Baylis--Hillman reaction of aldehydes with
 \a,\b-unsaturated ketone
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              390
_journal_paper_doi               10.1039/b008105l
_journal_year                    2001
_chemical_formula_moiety         'C11 H12 Cl N O4 '
_chemical_formula_sum            'C11 H12 Cl N O4'
_chemical_formula_weight         257.67
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.615(1)
_cell_length_b                   14.277(1)
_cell_length_c                   7.838(1)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    297.2
_cell_measurement_theta_max      14.7
_cell_measurement_theta_min      12.7
_cell_volume                     1187.9(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1601
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_standards_decay_%        1.01
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.323
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.15
_refine_diff_density_min         -0.16
_refine_ls_extinction_coef       0.003(5)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     203
_refine_ls_number_reflns         1582
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.0016
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00046|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0515
_reflns_number_gt                1108
_reflns_number_total             1582
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            b008105lsup1.cif
_cod_data_source_block           20000117b
_cod_original_cell_volume        1187.8(3)
_cod_original_sg_symbol_H-M      'P 21 21 21   '
_cod_original_formula_sum        'C11 H12 Cl N O4 '
_cod_database_code               7213438