In- or in(I)-employed diastereoselective Reformatsky-type reactions with ketones: 1H NMR investigations on the active species.
Babu, Srinivasarao Arulananda; Yasuda, Makoto; Shibata, Ikuya; Baba, Akio; Organic letters 6 (2004) 4475–4478; doi:10.1021/ol0482846

data_1506965
_publ_section_title
;
 In- or in(I)-employed diastereoselective Reformatsky-type reactions with
 ketones: 1H NMR investigations on the active species.
;
_journal_issue                   24
_journal_name_full               'Organic letters'
_journal_page_first              4475
_journal_page_last               4478
_journal_paper_doi               10.1021/ol0482846
_journal_volume                  6
_journal_year                    2004
_chemical_formula_moiety         'C24 H23 Cl O4 '
_chemical_formula_sum            'C24 H23 Cl O4'
_chemical_formula_weight         410.90
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 90.8136(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4195(3)
_cell_length_b                   21.7175(6)
_cell_length_c                   10.4372(3)
_cell_measurement_reflns_used    22912
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      30.3
_cell_measurement_theta_min      2.2
_cell_volume                     2134.90(11)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 8.00
_diffrn_measured_fraction_theta_full 0.9966
_diffrn_measured_fraction_theta_max 0.9966
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            23431
_diffrn_reflns_theta_full        30.30
_diffrn_reflns_theta_max         30.30
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.650
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.28
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    refall
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_refine_ls_number_reflns         3806
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          3.4183
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1689
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_reflns_threshold_expression     F^2^>2.0\s(F^2^)
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_cod_data_source_block           13a1B
_cod_original_cell_volume        2134.9(1)
_cod_original_formula_sum        'C24 H23 Cl O4 '
_cod_database_code               1506965