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_7251791
_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         'C30 H19 O P'
_chemical_formula_sum            'C30 H19 O P'
_chemical_formula_weight         426.42
_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             2023-12-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2025-03-19 deposited with the CCDC.	2026-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.7870(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.70743(11)
_cell_length_b                   11.37805(14)
_cell_length_c                   21.6228(3)
_cell_measurement_reflns_used    6335
_cell_measurement_temperature    173
_cell_measurement_theta_max      76.8980
_cell_measurement_theta_min      4.3800
_cell_volume                     2131.33(5)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.966
_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    -21.00   6.00   0.50    0.71    --    0.00  68.00  94.00   54
  2  \w    -88.00 -16.00   0.50    0.71    --    0.00 -57.00-120.00  144
  3  \w    -16.00  88.00   0.50    0.71    --    0.00  57.00 -90.00  208
  4  \w     23.00  48.00   0.50    0.71    --    0.00  68.00  94.00   50
  5  \w     85.00 133.00   0.50    2.84    --  101.00  61.00-150.00   96
  6  \w    139.00 165.00   0.50    2.84    --  101.00  61.00-150.00   52
  7  \w     37.00 113.00   0.50    2.84    --  101.00 -61.00-120.00  152
  8  \w     16.00 127.00   0.50    2.84    --  101.00 -82.00  90.00  222
  9  \w     12.00 128.00   0.50    2.84    --  101.00 -61.00  90.00  232
 10  \w     12.00 166.00   0.50    2.84    --  101.00  15.00  60.00  308
;
_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      -0.0358313000
_diffrn_orient_matrix_UB_12      -0.0916055000
_diffrn_orient_matrix_UB_13      0.0490505000
_diffrn_orient_matrix_UB_21      -0.1112240000
_diffrn_orient_matrix_UB_22      0.0872368000
_diffrn_orient_matrix_UB_23      0.0267758000
_diffrn_orient_matrix_UB_31      -0.1340239000
_diffrn_orient_matrix_UB_32      -0.0481899000
_diffrn_orient_matrix_UB_33      -0.0448072000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11624
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.291
_diffrn_reflns_theta_min         4.110
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.294
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71327
_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    1.329
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+1.0130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1377
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3841
_reflns_number_total             4366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00837a2.cif
_cod_data_source_block           exp_1457
_cod_depositor_comments
'Adding full bibliography for 7251788--7251793.cif.'
_cod_database_code               7251791
_chemical_oxdiff_formula         C30H19OP
_reflns_odcompleteness_completeness 99.93
_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:
 C24(H24), C20(H20), C5(H5), C30(H30), C4(H4), C26(H26), C7(H7), C15(H15),
 C8(H8), C22(H22), C21(H21), C12(H12), C27(H27), C14(H14), C23(H23), C10(H10),
 C11(H11), C28(H28), C29(H29)
;
_shelx_res_checksum              59724
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method loop
_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 1.465
_oxdiff_exptl_absorpt_empirical_full_min 0.702