Catalytic decarboxylative alkenylation of enolates.
Schröder, Sybrin P; Taylor, Nicholas J.; Jackson, Paula; Franckevičius, Vilius; Organic letters 15 (2013) 3778–3781; doi:10.1021/ol401729m

data_1512212
_publ_section_title
;
 Catalytic decarboxylative alkenylation of enolates.
;
_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3778
_journal_page_last               3781
_journal_paper_doi               10.1021/ol401729m
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C19 H24 O3'
_chemical_formula_sum            'C19 H24 O3'
_chemical_formula_weight         300.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-11-30
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 127.998(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6030(7)
_cell_length_b                   19.3678(5)
_cell_length_c                   7.3303(4)
_cell_measurement_reflns_used    3521
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      27.8099
_cell_measurement_theta_min      2.8019
_cell_volume                     1633.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.9960
_diffrn_measured_fraction_theta_max 0.9960
_diffrn_measurement_details
;
  1 omega  -59.00    0.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.6160  -57.0000  150.0000 59

  2 omega  -83.00   46.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.6160    0.0000 -180.0000 129

  3 omega   59.00   97.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0222 -178.0000    0.0000 38
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0352374000
_diffrn_orient_matrix_UB_12      0.0228412000
_diffrn_orient_matrix_UB_13      0.0948379000
_diffrn_orient_matrix_UB_21      -0.0128751000
_diffrn_orient_matrix_UB_22      0.0270616000
_diffrn_orient_matrix_UB_23      -0.0777518000
_diffrn_orient_matrix_UB_31      -0.0489423000
_diffrn_orient_matrix_UB_32      0.0093040000
_diffrn_orient_matrix_UB_33      -0.0065973000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7641
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         3.00
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.985
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.2456
_exptl_crystal_size_mid          0.1467
_exptl_crystal_size_min          0.0746
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         3889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+0.5677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                3283
_reflns_number_total             3889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol401729m_si_002.cif
_cod_data_source_block           rjkt1214
_cod_original_cell_volume        1633.75(22)
_cod_database_code               1512212
_chemical_oxdiff_formula         'C19 H24 O3'
_chemical_oxdiff_usercomment     'Vil vf450p'
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_olex2_refinement_description
;
;