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_2018185
_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'
_chemical_formula_moiety         'C27 H27 O5 P'
_chemical_formula_sum            'C27 H27 O5 P'
_chemical_formula_weight         462.46
_chemical_name_systematic
;
diethyl 3-oxo-2-(triphenylphosphoranylidene)glutarate
;
_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                95.994(2)
_cell_angle_beta                 108.342(2)
_cell_angle_gamma                107.304(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0348(10)
_cell_length_b                   10.3770(11)
_cell_length_c                   13.8951(15)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      50.44
_cell_measurement_theta_min      4.68
_cell_volume                     1152.0(2)
_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 0.991
_diffrn_measured_fraction_theta_max 0.900
_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
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_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9669
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         27.84
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.053
_refine_diff_density_min         -0.358
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_parameters     344
_refine_ls_number_reflns         4935
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0842P)^2^+0.1991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1431
_reflns_number_gt                4077
_reflns_number_total             4935
_reflns_threshold_expression     I>2\s(I)
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_cod_data_source_block           I
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