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_1555418
_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            'C17 H16 F6 O9'
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_cell_length_c                   17.3709(12)
_cell_measurement_temperature    150(2)
_cell_volume                     2031.4(2)
_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 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0814
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            133448
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.741
_diffrn_reflns_theta_min         2.346
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.948
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.319
_exptl_crystal_size_min          0.185
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         11591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1225
_refine_ls_R_factor_gt           0.0647
_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^)+(0.0772P)^2^+0.7921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1477
_refine_ls_wR_factor_ref         0.1763
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6965
_reflns_number_total             11591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5b02847_si_003.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1555418
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.949
_shelx_estimated_absorpt_t_max   0.971
_shelx_res_checksum              87079
_shelx_hkl_checksum              26324