Preparation, single-crystal structure and room-temperature phosphorescence of a covalent organic polymer containing Te-O-P bonds.
Xue, Miaomiao; Ye, Guigui; Zhang, Lei; Dong, Qiang; Lee, Chun-Sing; Li, Zhen; Zhang, Qichun; Chemical science 16 (2025) 5260–5265; doi:10.1039/d4sc07210c

data_1573936
_publ_section_title
;
 Preparation, single-crystal structure and room-temperature
 phosphorescence of a covalent organic polymer containing Te-O-P bonds.
;
_journal_issue                   12
_journal_name_full               'Chemical science'
_journal_page_first              5260
_journal_page_last               5265
_journal_paper_doi               10.1039/d4sc07210c
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C48 H40 O12 P4 Te2'
_chemical_formula_sum            'C48 H40 O12 P4 Te2'
_chemical_formula_weight         1187.88
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-01-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-04-30 deposited with the CCDC.	2025-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                93.7232(11)
_cell_angle_beta                 99.2727(11)
_cell_angle_gamma                91.1692(13)
_cell_formula_units_Z            2
_cell_length_a                   9.41547(15)
_cell_length_b                   10.53235(17)
_cell_length_c                   23.2502(2)
_cell_measurement_reflns_used    15890
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      67.9990
_cell_measurement_theta_min      3.8490
_cell_volume                     2269.61(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'Image Plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.963
_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    -23.00 131.00   0.50    1.82    --   42.80   3.00 -99.00  308
  2  \w    -19.00   6.00   0.50    1.82    --   42.80  -3.00  84.00   50
  3  \w     94.00 183.00   0.50    7.30    --   94.00   3.00 -99.00  178
  4  \w     36.00  72.00   0.50    7.30    --   94.00   3.00 -99.00   72
  5  \w     17.00  71.00   0.50    1.82    --   42.80  54.00-150.00  108
  6  \w    -45.00   7.00   0.50    1.82    --   42.80 -77.00  90.00  104
  7  \w    -47.00  13.00   0.50    1.82    --   42.80 -54.00 -60.00  120
  8  \w     78.00 104.00   0.50    1.82    --   42.80  54.00-150.00   52
  9  \w     14.00  67.00   0.50    1.82    --   42.80 -82.00  90.00  106
 10  \w     32.00  70.00   0.50    1.82    --   42.80 -82.00  30.00   76
 11  \w     15.00  65.00   0.50    1.82    --   42.80 -65.00  30.00  100
 12  \w    -26.00   1.00   0.50    1.82    --   42.80 -65.00  30.00   54
 13  \w    -47.00  67.00   0.50    1.82    --   42.80 -77.00-180.00  228
 14  \w     -8.00  27.00   0.50    1.82    --   42.80 -77.00 -60.00   70
 15  \w     40.00  70.00   0.50    1.82    --   42.80 -82.00 -90.00   60
 16  \w    -46.00  28.00   0.50    1.82    --   42.80 -82.00 -90.00  148
 17  \w     16.00  85.00   0.50    1.82    --   42.80  43.00   0.00  138
 18  \w     29.00  63.00   0.50    1.82    --   42.80 -82.00-120.00   68
 19  \w      7.00  65.00   0.50    1.82    --   42.80 -82.00   0.00  116
 20  \w     83.00 109.00   0.50    7.30    --   94.00 -82.00 -60.00   52
 21  \w     20.00  55.00   0.50    7.30    --   94.00 -82.00 -60.00   70
 22  \w     27.00  98.00   0.50    7.30    --   94.00 -82.00 -30.00  142
 23  \w      6.00  98.00   0.50    7.30    --   94.00 -82.00   0.00  184
 24  \w      5.00  96.00   0.50    7.30    --   94.00 -82.00-180.00  182
 25  \w      5.00  54.00   0.50    7.30    --   94.00 -42.00  30.00   98
 26  \w     70.00 183.00   0.50    7.30    --   94.00  42.00 -90.00  226
 27  \w     28.00  89.00   0.50    7.30    --   94.00 -82.00-120.00  122
 28  \w     13.00  99.00   0.50    7.30    --   94.00 -82.00  90.00  172
 29  \w      5.00 115.00   0.50    7.30    --   94.00 -82.00 120.00  220
 30  \w     89.00 156.00   0.50    7.30    --   94.00  59.00 -60.00  134
 31  \w     24.00  66.00   0.50    7.30    --   94.00 -82.00 150.00   84
 32  \w     80.00 106.00   0.50    7.30    --   94.00 -82.00 150.00   52
 33  \w      5.00 119.00   0.50    7.30    --   94.00 -42.00-150.00  228
 34  \w    124.00 152.00   0.50    7.30    --   94.00  59.00-180.00   56
 35  \w     84.00 145.00   0.50    7.30    --   94.00  68.00   0.00  122
 36  \w     90.00 116.00   0.50    7.30    --   94.00  59.00-180.00   52
 37  \w     98.00 123.00   0.50    7.30    --   94.00  68.00  60.00   50
 38  \w      6.00 121.00   0.50    7.30    --   94.00 -82.00-150.00  230
 39  \w     92.00 119.00   0.50    7.30    --   94.00 -42.00  30.00   54
 40  \w     53.00  97.00   0.50    7.30    --   94.00 -82.00 -90.00   88
 41  \w     26.00  61.00   0.50    7.30    --   94.00 -82.00  60.00   70
 42  \w     68.00  93.00   0.50    7.30    --   94.00 -82.00  60.00   50
 43  \w      6.00  99.00   0.50    7.30    --   94.00 -82.00  30.00  186
 44  \w     70.00  95.00   0.50    7.30    --   94.00  -3.00  84.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Pro II 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      -0.1540265000
_diffrn_orient_matrix_UB_12      -0.0484576000
_diffrn_orient_matrix_UB_13      0.0028584000
_diffrn_orient_matrix_UB_21      0.0513798000
_diffrn_orient_matrix_UB_22      -0.1379438000
_diffrn_orient_matrix_UB_23      -0.0003960000
_diffrn_orient_matrix_UB_31      0.0338849000
_diffrn_orient_matrix_UB_32      0.0113967000
_diffrn_orient_matrix_UB_33      0.0672366000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24255
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.267
_diffrn_reflns_theta_min         1.930
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.029
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_description       plate
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         8014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0230
_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^)+(0.0190P)^2^+3.6326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7570
_reflns_number_total             8014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07210c2.cif
_cod_data_source_block           CityU_21
_cod_depositor_comments          'Adding full bibliography for 1573936.cif.'
_cod_database_code               1573936
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Te C H O P'
_shelx_estimated_absorpt_t_max   0.197
_shelx_estimated_absorpt_t_min   0.086
_diffrn_oxdiff_digest_frames
;
010381e30f4983c33ba98aa37bedbfb58600026317f
;
_diffrn_oxdiff_digest_hkl
;
01c45e3e438c71c2530478ab3a79dd1e4a91e3
;
_reflns_odcompleteness_completeness 97.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6A), C8(H8), C9(H9), C12(H12A), C17(H17), C18(H18), C19(H19), C20(H20),
 C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48)
2.b Idealised tetrahedral OH refined as rotating group:
 O5(H5), O6(H6), O11(H11), O12(H12)
;
_shelx_res_checksum              89959
_shelx_hkl_checksum              49575
_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 1.381
_oxdiff_exptl_absorpt_empirical_full_min 0.710