A nonconjugated radical polymer with stable red luminescence in the solid state.
Wang, Zhaoyu; Zou, Xinhui; Xie, Yi; Zhang, Haoke; Hu, Lianrui; Chan, Christopher C. S.; Zhang, Ruoyao; Guo, Jing; Kwok, Ryan T. K.; Lam, Jacky W. Y.; Williams, Ian D.; Zeng, Zebing; Wong, Kam Sing; Sherrill, C. David; Ye, Ruquan; Tang, Ben Zhong; Materials horizons 9 (2022) 2564–2571; doi:10.1039/d2mh00808d

data_1567388
_publ_section_title
;
 A nonconjugated radical polymer with stable red luminescence in the solid
 state.
;
_journal_issue                   10
_journal_name_full               'Materials horizons'
_journal_page_first              2564
_journal_page_last               2571
_journal_paper_doi               10.1039/d2mh00808d
_journal_volume                  9
_journal_year                    2022
_chemical_formula_moiety         'C12 H22 N O3'
_chemical_formula_sum            'C12 H22 N O3'
_chemical_formula_weight         228.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-18 deposited with the CCDC.	2022-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.897(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.81660(10)
_cell_length_b                   11.4718(2)
_cell_length_c                   9.5696(2)
_cell_measurement_reflns_used    2336
_cell_measurement_temperature    100.2(8)
_cell_measurement_theta_max      73.2200
_cell_measurement_theta_min      4.7440
_cell_volume                     619.86(2)
_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_environment      N~2~
_diffrn_ambient_temperature      100.2(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_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     24.00 110.00   1.00    3.00    --  106.99 -94.00-180.00   86
  2  \w   -115.00 -25.00   1.00    2.00    --  -40.57 -57.00  60.00   90
  3  \w   -115.00 -90.00   1.00    2.00    --  -40.57-132.00-133.00   25
  4  \w    -64.00  33.00   1.00    2.00    --  -40.57  37.00-150.00   97
  5  \w      1.00  83.00   1.00    2.00    --   40.57 -99.00 -60.00   82
  6  \w     79.00 109.00   1.00    3.00    --  106.99  45.00 150.00   30
  7  \w     49.00 128.00   1.00    3.00    --  106.99 -77.00-120.00   79
  8  \w     40.00 135.00   1.00    3.00    --  106.99 -30.00 -30.00   95
  9  \w    143.00 178.00   1.00    3.00    --  106.99  45.00 150.00   35
 10  \w     30.00 117.00   1.00    3.00    --  106.99 -30.00 150.00   87
 11  \w     78.00 175.00   1.00    3.00    --  106.99  30.00 -30.00   97
 12  \w     42.00 110.00   1.00    3.00    --  106.99 -94.00  60.00   68
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.2466544000
_diffrn_orient_matrix_UB_12      -0.0204755000
_diffrn_orient_matrix_UB_13      -0.1003415000
_diffrn_orient_matrix_UB_21      0.0397321000
_diffrn_orient_matrix_UB_22      -0.1326771000
_diffrn_orient_matrix_UB_23      0.0136331000
_diffrn_orient_matrix_UB_31      -0.1097306000
_diffrn_orient_matrix_UB_32      -0.0018851000
_diffrn_orient_matrix_UB_33      0.1313672000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0099
_diffrn_reflns_av_unetI/netI     0.0105
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3277
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.331
_diffrn_reflns_theta_min         4.760
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91990
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       block
_exptl_crystal_F_000             250
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         1266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0476P)^2^+0.1813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0931
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1210
_reflns_number_total             1266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2mh00808d2.cif
_cod_data_source_block           zwang1cult
_cod_depositor_comments          'Adding full bibliography for 1567388.cif.'
_cod_database_code               1567388
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.884
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: O1(0.5) O2(0.5) H1A(0.5) H1B(0.5) H2(0.5) C3(0.5) H3A(0.5) H3B(0.5)
3.a Ternary CH refined with riding coordinates:
 C2(H2), C4(H4)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              8311
_olex2_date_sample_data_collection 2019-04-30
_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 1.185
_oxdiff_exptl_absorpt_empirical_full_min 0.865