Phase-transfer catalyzed asymmetric Darzens reaction of cyclic α-chloro ketones
Arai, Shigeru; Shirai, Yoshiki; Shioiri, Takayuki; Ishida, Toshimasa; Chemical Communications  (1999) 49–; doi:10.1039/a808321e

data_7110399
_publ_section_title
;
 Phase-transfer catalyzed asymmetric Darzens reaction of cyclic \a-chloro
 ketones
;
_journal_issue                   1
_journal_name_full               'Chemical Communications'
_journal_page_first              49
_journal_paper_doi               10.1039/a808321e
_journal_year                    1999
_chemical_formula_moiety         'C15 H18 O3 '
_chemical_formula_sum            'C15 H18 O3'
_chemical_formula_weight         246.31
_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'
_audit_creation_date             'Fri Jul 25 12:49:17 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 112.71(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.919(4)
_cell_length_b                   12.587(5)
_cell_length_c                   11.624(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      24.1
_cell_volume                     1338.7(10)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  SHELXL97
_diffrn_ambient_temperature      293.2
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.09322
_diffrn_orient_matrix_UB_12      0.00881
_diffrn_orient_matrix_UB_13      0.01318
_diffrn_orient_matrix_UB_21      -0.05673
_diffrn_orient_matrix_UB_22      -0.00612
_diffrn_orient_matrix_UB_23      -0.09192
_diffrn_orient_matrix_UB_31      -0.00603
_diffrn_orient_matrix_UB_32      -0.07872
_diffrn_orient_matrix_UB_33      0.00862
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.073
_diffrn_reflns_av_sigmaI/netI    0.019
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2441
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         65.25
_diffrn_standards_decay_%        -0.42
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             528.00
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.600
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.27
_refine_diff_density_min         -0.20
_refine_diff_density_rms         0.06
_refine_ls_extinction_coef       0.0046
_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   0.933
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         1878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          -0.0620
_refine_ls_shift/su_mean         0.0150
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2113
_reflns_number_gt                1878
_reflns_number_total             2287
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            808321esup1.cif
_cod_data_source_block           1
_cod_depositor_comments
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The following automatic conversions were performed:
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file
'cod-tools/trunk/perl-scripts/inputs/replacement_tags.lst'.

'_atom_site_calc_flags'
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'cod-tools/trunk/perl-scripts/inputs/replacement_tags.lst'.

'_atom_type_scat_imag'
tag replaced with '_atom_type_scat_dispersion_imag' tag as specified
in the replacement file
'cod-tools/trunk/perl-scripts/inputs/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 3137 2015-03-23 15:08:43Z antanas 
;
_cod_original_cell_volume        1338.8(9)
_cod_original_sg_symbol_H-M      'P 21/a       '
_cod_original_formula_sum        'C15 H18 O3 '
_cod_database_code               7110399