Recent extensions of the Morita–Baylis–Hillman reaction
Ma, Guang-Ning; Jiang, Jia-Jun; Shi, Min; Wei, Yin; Chemical Communications  (2009) 5496–5514; doi:10.1039/b909405a

data_7111550
_publ_section_title
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 Recent extensions of the Morita--Baylis--Hillman reaction
;
_journal_issue                   37
_journal_name_full               'Chemical Communications'
_journal_page_first              5496
_journal_page_last               5514
_journal_paper_doi               10.1039/b909405a
_journal_year                    2009
_chemical_formula_sum            'C20 H18 Cl N O3 S'
_chemical_formula_weight         387.86
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.925(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.333(5)
_cell_length_b                   8.0254(15)
_cell_length_c                   21.292(4)
_cell_measurement_reflns_used    3007
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      43.085
_cell_measurement_theta_min      5.205
_cell_volume                     3800.7(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1307
_diffrn_reflns_av_sigmaI/netI    0.1162
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19188
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7787
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.475
_exptl_crystal_size_mid          0.366
_exptl_crystal_size_min          0.157
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.096
_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   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         7054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1412
_refine_ls_R_factor_gt           0.1032
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1235P)^2^+10.3257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2926
_refine_ls_wR_factor_ref         0.3099
_reflns_number_gt                4265
_reflns_number_total             7054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b909405asup1.cif
_cod_data_source_block           cd28526
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3800.8(12)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7111550