Cyano-stabilized triphenylphosphonium ylids
Fernando Castañeda; Clifford A. Bunton; Ricardo Baggio; María Teresa Garland; Acta Crystallographica Section C 63 (2007) o65–o67; doi:10.1107/S0108270106051201

data_2015766
_publ_section_title
;
 Cyano-stabilized triphenylphosphonium ylids
;
_journal_coeditor_code           SQ3045
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o65
_journal_page_last               o67
_journal_paper_doi               10.1107/S0108270106051201
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C22 H18 N O2 P'
_chemical_formula_moiety         'C22 H18 N O2 P'
_chemical_formula_sum            'C22 H18 N O2 P'
_chemical_formula_weight         359.34
_chemical_name_systematic
;
methyl 2-cyano-2-(trimethylphosphonio)ethenoate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.659(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9601(14)
_cell_length_b                   9.0436(13)
_cell_length_c                   20.708(3)
_cell_measurement_reflns_used    6588
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.24
_cell_volume                     1859.1(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      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\f and \w 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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14118
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.97
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             752
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .24
_exptl_crystal_size_min          .10
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+0.3502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1500
_reflns_number_gt                2645
_reflns_number_total             3659
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sq3045.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               2015766
_cod_database_fobs_code          2015766