Reductive Homocondensation of Benzylidene- and Alkylidenepyruvate Esters by a P(NMe2)3-Mediated Tandem Reaction.
Wang, Sunewang Rixin; Radosevich, Alexander T.; Organic letters 15 (2013) 1926–1929; doi:10.1021/ol400576e

data_1511924
_publ_section_title
;
 Reductive Homocondensation of Benzylidene- and Alkylidenepyruvate Esters
 by a P(NMe2)3-Mediated Tandem Reaction.
;
_journal_issue                   8
_journal_name_full               'Organic letters'
_journal_page_first              1926
_journal_page_last               1929
_journal_paper_doi               10.1021/ol400576e
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C28 H32 O5'
_chemical_formula_sum            'C28 H32 O5'
_chemical_formula_weight         448.54
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.506(10)
_cell_angle_beta                 77.945(7)
_cell_angle_gamma                89.988(7)
_cell_formula_units_Z            4
_cell_length_a                   10.046(4)
_cell_length_b                   12.149(5)
_cell_length_c                   22.277(10)
_cell_measurement_reflns_used    5398
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.697
_cell_measurement_theta_min      2.145
_cell_volume                     2593.1(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24116
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.9953
_exptl_absorpt_correction_T_min  0.9854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         12363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1426
_refine_ls_R_factor_gt           0.0712
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1256P)^2^+0.0597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2002
_refine_ls_wR_factor_ref         0.2463
_reflns_number_gt                5885
_reflns_number_total             12363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol400576e_si_003.cif
_cod_data_source_block           rxw5t
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2593(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1511924