Crystal structure of 3-(triphenylphosphoranylidene)-2,5-dihydrofuran-2,5-dione tetrahydrofuran monosolvate
Zagidullin, Almaz; Islamov, Daut; Oshchepkova, Elena; Lonnecke, Peter; Miluykov, Vasili; Acta Crystallographica Section E 74 (2018) 1336–1338; doi:10.1107/S2056989018011775

data_2242619
_publ_section_title
;
 Crystal structure of
 3-(triphenylphosphoranylidene)-2,5-dihydrofuran-2,5-dione tetrahydrofuran
 monosolvate
;
_journal_coeditor_code           RZ5234
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1336
_journal_page_last               1338
_journal_paper_doi               10.1107/S2056989018011775
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C22 H17 O3 P, C4 H8 O'
_chemical_formula_moiety         'C22 H17 O3 P, C4 H8 O'
_chemical_formula_sum            'C26 H25 O4 P'
_chemical_formula_weight         432.43
_chemical_name_systematic
;
3-(Triphenylphosphoranylidene)-2,5-dihydrofuran-2,5-dione
tetrahydrofuran monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.435(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1287(5)
_cell_length_b                   10.5530(4)
_cell_length_c                   17.5838(8)
_cell_measurement_reflns_used    5863
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      32.5463
_cell_measurement_theta_min      3.0269
_cell_volume                     2179.57(16)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Agilent Xcalibur Sapphire3 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30663
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.620
_diffrn_reflns_theta_min         3.033
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.99476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.390
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         7381
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+1.6405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1301
_reflns_number_gt                5123
_reflns_number_total             7381
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rz5234sup1.cif
_cod_data_source_block           I
_cod_database_code               2242619
_cod_database_fobs_code          2242619
_shelx_estimated_absorpt_t_min   0.969
_shelx_estimated_absorpt_t_max   0.992
_shelx_hkl_checksum              91005
_shelx_res_checksum              59651