Differences in the crystal structures of two dialkyl diester triphenylphosphonium ylids
Fernando Castañeda; Carolina Jullian; Clifford A. Bunton; María Teresa Garland; Ricardo Baggio; Acta Crystallographica Section C 63 (2007) o267–o270; doi:10.1107/S0108270107010542

data_2015924
_publ_section_title
;
 Differences in the crystal structures of two dialkyl diester
 triphenylphosphonium ylids
;
_journal_coeditor_code           SQ3064
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o267
_journal_page_last               o270
_journal_paper_doi               10.1107/S0108270107010542
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C23 H21 O4 P'
_chemical_formula_moiety         'C23 H21 O4 P'
_chemical_formula_sum            'C23 H21 O4 P'
_chemical_formula_weight         392.37
_chemical_name_systematic
;
dimethyl 2-(triphenylphosphoranylidene)malonate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.7340(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.1031(8)
_cell_length_b                   14.6961(11)
_cell_length_c                   26.756(2)
_cell_measurement_reflns_used    6277
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.52
_cell_measurement_theta_min      2.28
_cell_volume                     3968.1(5)
_computing_cell_refinement       'SAINT-NT (Bruker, 2001 )'
_computing_data_collection       'SMART-NT (Bruker, 2001)'
_computing_data_reduction        SAINT-NT
_computing_molecular_graphics    'SHELXTL-NT (Bruker, 2001)'
_computing_publication_material  'SHELXTL-NT and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.928
_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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            33032
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.08
_diffrn_reflns_theta_min         1.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         8973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0708P)^2^+0.4925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1451
_reflns_number_gt                6466
_reflns_number_total             8973
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sq3064.cif
_cod_data_source_block           II
_cod_database_code               2015924
_cod_database_fobs_code          2015924