Conformations of diester triphenylphosphonium ylides with an ylidic ester or keto and ester ylidic groups
Castañeda, Fernando; Silva, Paul; Bunton, Clifford A.; Garland, María Teresa; Baggio, Ricardo; Acta Crystallographica Section C 67 (2011) o319–o323; doi:10.1107/S0108270111027508

data_2018186
_publ_section_title
;
 Conformations of diester triphenylphosphonium ylides with an ylidic
 ester or keto and ester ylidic groups
;
_journal_coeditor_code           GT3033
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o319
_journal_page_last               o323
_journal_paper_doi               10.1107/S0108270111027508
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C27 H27 O5 P , C2 H4 O2'
_chemical_formula_moiety         'C27 H27 O5 P, C2 H4 O2'
_chemical_formula_sum            'C29 H31 O7 P'
_chemical_formula_weight         522.51
_chemical_name_systematic
;
diethyl 3-oxo-2-(triphenylphosphoranylidene)glutarate acetic acid monosolvate
;
_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           SHELXL97
_cell_angle_alpha                78.191(6)
_cell_angle_beta                 71.505(6)
_cell_angle_gamma                64.285(6)
_cell_formula_units_Z            2
_cell_length_a                   9.957(4)
_cell_length_b                   10.589(4)
_cell_length_c                   14.928(6)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      50.93
_cell_measurement_theta_min      4.83
_cell_volume                     1340.7(9)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  'Bruker SMART? CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.1124
_diffrn_reflns_av_sigmaI/netI    0.1010
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11211
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.356
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         5728
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0898P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1709
_reflns_number_gt                4037
_reflns_number_total             5728
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gt3033.cif
_cod_data_source_block           II
_cod_database_code               2018186