α-Ketophosphonates as Ester Surrogates: Isothiourea-Catalyzed Asymmetric Diester and Lactone Synthesis.
Smith, Siobhan R.; Leckie, Stuart M.; Holmes, Reuben; Douglas, James; Fallan, Charlene; Shapland, Peter; Pryde, David; Slawin, Alexandra M. Z.; Smith, Andrew D.; Organic letters 16 (2014) 2506–2509; doi:10.1021/ol500873s

data_1514344
_publ_section_title
;
 \a-Ketophosphonates as Ester Surrogates: Isothiourea-Catalyzed Asymmetric
 Diester and Lactone Synthesis.
;
_journal_issue                   9
_journal_name_full               'Organic letters'
_journal_page_first              2506
_journal_page_last               2509
_journal_paper_doi               10.1021/ol500873s
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C19 H19 Br O4'
_chemical_formula_sum            'C19 H19 Br O4'
_chemical_formula_weight         391.26
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 95.376(14)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   6.050(3)
_cell_length_b                   33.448(15)
_cell_length_c                   8.747(4)
_cell_measurement_reflns_used    4441
_cell_measurement_temperature    93
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.34
_cell_volume                     1762.3(14)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 rc13'
_computing_data_collection
'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 rc13'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
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_diffrn_reflns_av_R_equivalents  0.1258
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_diffrn_reflns_limit_k_min       -40
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_diffrn_reflns_theta_max         25.32
_diffrn_standards_number         0
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_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             800.00
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_exptl_crystal_size_mid          0.030
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_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1524 Friedel Pairs'
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_refine_ls_extinction_method     none
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_refine_ls_shift/su_max          0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1596P)^2^+2.2190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2924
_reflns_number_gt                3341
_reflns_number_total             4687
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol500873s_si_002.cif
_cod_data_source_block           slas7
_cod_depositor_comments          'Adding full bibliography for 1514344.cif.'
_cod_original_cell_volume        1762.3(13)
_cod_database_code               1514344