Tris(4-formylphenyl)phosphane oxide tetrahydrofuran hemisolvate
Kakoullis, Jr, James; Fronczek, Frank R.; Maverick, Andrew W.; Acta Crystallographica Section E 69 (2013) o1362–o1363; doi:10.1107/S1600536813020059

data_2238341
_publ_section_title
;
 Tris(4-formylphenyl)phosphane oxide tetrahydrofuran hemisolvate
;
_journal_coeditor_code           FJ2638
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1362
_journal_page_last               o1363
_journal_paper_doi               10.1107/S1600536813020059
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C21 H15 O4 P, 0.5C4 H8 O'
_chemical_formula_moiety         'C21 H15 O4 P, 0.5(C4 H8 O)'
_chemical_formula_sum            'C23 H19 O4.5 P'
_chemical_formula_weight         398.35
_chemical_name_systematic
;
Tris(4-formylphenyl)phosphane oxide tetrahydrofuran hemisolvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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
_cell_angle_beta                 99.018(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.371(3)
_cell_length_b                   13.474(2)
_cell_length_c                   13.436(2)
_cell_measurement_reflns_used    7492
_cell_measurement_temperature    110.0(5)
_cell_measurement_theta_max      33.7
_cell_measurement_theta_min      2.5
_cell_volume                     3821.1(10)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      110.0(5)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f 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  0.023
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36155
_diffrn_reflns_theta_full        33.7
_diffrn_reflns_theta_max         33.7
_diffrn_reflns_theta_min         3.0
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         7598
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.061
_refine_ls_R_factor_gt           0.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+2.5619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.106
_refine_ls_wR_factor_ref         0.116
_reflns_number_gt                5928
_reflns_number_total             7598
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fj2638.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C23 H19 O4.50 P'
_cod_database_code               2238341
_cod_database_fobs_code          2238341