Preparation of Phosphine Oxides with Anthrylphenyl, Pyrenylphenyl, Anthrylethynyl, and Pyrenylethynyl Groups: Luminescent Properties and Conformational Polymorphs
Konno, Ryunosuke; Fujita, Manami; Maekawa, Rima; Masu, Hyuma; Katagiri, Kosuke; CrystEngComm  (2026) –; doi:10.1039/D5CE00837A

data_7251793
_publ_section_title
;
 Preparation of phosphine oxides with anthrylphenyl, pyrenylphenyl,
 anthrylethynyl, and pyrenylethynyl groups: luminescence properties and
 conformational polymorphs
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2455
_journal_page_last               2467
_journal_paper_doi               10.1039/D5CE00837A
_journal_volume                  28
_journal_year                    2026
_chemical_formula_moiety         'C34 H23 O P'
_chemical_formula_sum            'C34 H23 O P'
_chemical_formula_weight         478.49
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2023-11-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-03-19 deposited with the CCDC.	2026-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.788(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2834(4)
_cell_length_b                   9.4529(2)
_cell_length_c                   14.7171(3)
_cell_measurement_reflns_used    6449
_cell_measurement_temperature    173
_cell_measurement_theta_max      76.5860
_cell_measurement_theta_min      5.1830
_cell_volume                     2369.45(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     31.00  56.00   0.50   27.10    --    0.00  37.00  90.00   50
  2  \w    -10.00  17.00   0.50   27.10    --    0.00  37.00  90.00   54
  3  \w    -26.00  89.00   0.50   27.10    --    0.00  37.00 150.00  230
  4  \w    -68.00   1.00   0.50   27.10    --    0.00 -37.00-180.00  138
  5  \w     84.00 178.00   0.50  108.42    --  101.00  45.00 -90.00  188
  6  \w     75.00 140.00   0.50  108.42    --  101.00  45.00 150.00  130
  7  \w     74.00 166.00   0.50  108.42    --  101.00  77.00 -60.00  184
  8  \w     75.00 190.00   0.50  108.42    --  101.00  45.00-150.00  230
  9  \w     95.00 178.00   0.50  108.42    --  101.00  45.00-120.00  166
 10  \w     82.00 108.00   0.50  108.42    --  101.00  45.00 120.00   52
 11  \w     61.00 126.00   0.50  108.42    --  101.00 -77.00-180.00  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0777497000
_diffrn_orient_matrix_UB_12      0.0439410000
_diffrn_orient_matrix_UB_13      -0.0609754000
_diffrn_orient_matrix_UB_21      -0.0457131000
_diffrn_orient_matrix_UB_22      -0.0928967000
_diffrn_orient_matrix_UB_23      0.0585378000
_diffrn_orient_matrix_UB_31      -0.0067989000
_diffrn_orient_matrix_UB_32      0.1264567000
_diffrn_orient_matrix_UB_33      0.0643434000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13136
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.415
_diffrn_reflns_theta_min         5.194
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.225
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0382
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1352
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4160
_reflns_number_total             4881
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00837a2.cif
_cod_data_source_block           exp_1443
_cod_depositor_comments
'Adding full bibliography for 7251788--7251793.cif.'
_cod_original_cell_volume        2369.48(10)
_cod_database_code               7251793
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C34H23OP
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C5(H5), C12(H12), C14(H14), C15(H15), C21(H21),
 C18(H18), C31(H31), C20(H20), C8(H8), C16(H16), C30(H30), C11(H11), C17(H17),
 C9(H9), C23(H23), C10(H10), C24(H24), C28(H28), C26(H26), C27(H27)
;
_shelx_res_checksum              11011
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.176
_oxdiff_exptl_absorpt_empirical_full_min 0.871