Chemoselective Intramolecular Carbonyl Ylide Formation through Electronically Differentiated Malonate Diesters.
Nakhla, Mina C.; Lee, Che-Wah; Wood, John L.; Organic letters 17 (2015) 5760–5763; doi:10.1021/acs.orglett.5b02847

data_1555419
_publ_section_title
;
 Chemoselective Intramolecular Carbonyl Ylide Formation through
 Electronically Differentiated Malonate Diesters.
;
_journal_issue                   23
_journal_name_full               'Organic letters'
_journal_page_first              5760
_journal_page_last               5763
_journal_paper_doi               10.1021/acs.orglett.5b02847
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C11 H17 O5'
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_cell_length_c                   16.0124(14)
_cell_measurement_temperature    150(2)
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
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_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_k_min       -14
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_diffrn_reflns_point_group_measured_fraction_full 1.000
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.169
_diffrn_reflns_theta_min         2.162
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       plate
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1458
_refine_ls_R_factor_gt           0.0780
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+1.6909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1823
_refine_ls_wR_factor_ref         0.2192
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1539
_reflns_number_total             2675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5b02847_si_002.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1555419
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.987
_shelx_estimated_absorpt_t_max   0.995
_shelx_res_checksum              68735
_shelx_hkl_checksum              33841