The first enantioselective strategy towards speciosins
Peixoto de Abreu Lima, Alejandro; Suescun, Leopoldo; Pandolfi, Enrique; Schapiro, Valeria; New Journal of Chemistry 43 (2019) 3653–; doi:10.1039/C8NJ06158K

data_7058134
_publ_section_title
;
 The first enantioselective strategy towards speciosins
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3653
_journal_paper_doi               10.1039/C8NJ06158K
_journal_volume                  43
_journal_year                    2019
_chemical_absolute_configuration syn
_chemical_formula_sum            'C13 H14 O4'
_chemical_formula_weight         234.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2017-12-26 deposited with the CCDC.
2019-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.100(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9464(3)
_cell_length_b                   6.8743(2)
_cell_length_c                   9.9114(3)
_cell_measurement_reflns_used    105
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      67.7
_cell_measurement_theta_min      26.11
_cell_volume                     609.55(3)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \j scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            22280
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.659
_diffrn_reflns_theta_min         4.461
_diffrn_source                   'Incoatec I\ms Cu microsource'
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker 2013'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       block
_exptl_crystal_F_000             248
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane/dichloromethane'
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.172
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Flack x determined using 770 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.19(14)
_refine_ls_extinction_coef       0.020(3)
_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   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2418
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0451P)^2^+0.1540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                1940
_reflns_number_total             2418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj06158k2.cif
_cod_data_source_block           cu_160711_LS_AP127_L
_cod_depositor_comments          'Adding full bibliography for 7058134.cif.'
_cod_database_code               7058134
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.968
_shelxl_version_number           2014-3
_shelx_res_checksum              74950