A metal-free 2D layered organic ammonium halide framework realizing full-color persistent room-temperature phosphorescence
Feng, Shangwei; Huang, Qiuqin; Yang, Shuming; Lin, Zhenghuan; Ling, Qidan; Chemical Science  (2021) –; doi:10.1039/D1SC04806F

data_1565074
_publ_section_title
;
 A metal-free 2D layered organic ammonium halide framework realizing
 full-color persistent room-temperature phosphorescence
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC04806F
_journal_year                    2021
_chemical_formula_moiety         '2(Cl), 2(C9 H12 N O2)'
_chemical_formula_sum            'C18 H24 Cl2 N2 O4'
_chemical_formula_weight         403.29
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2b'
_space_group_name_H-M_alt        'P b c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-03-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-30 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.97246(16)
_cell_length_b                   9.0205(2)
_cell_length_c                   36.0997(9)
_cell_measurement_reflns_used    4933
_cell_measurement_temperature    292.9(6)
_cell_measurement_theta_max      72.7540
_cell_measurement_theta_min      3.6110
_cell_volume                     1944.86(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.9(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5148
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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    -65.00  34.00   1.00    7.50    --  -40.45  38.00-120.00   99
  2  \w   -113.00 -12.00   1.00    7.50    --  -40.45 -57.00 -60.00  101
  3  \w    -69.00  33.00   1.00    7.50    --  -40.45  57.00  90.00  102
  4  \w    -92.00  -2.00   1.00    7.50    --  -40.45 125.00 150.00   90
  5  \w     48.00 108.00   1.00   15.00    --  103.24 -94.00  60.00   60
  6  \w     30.00  56.00   1.00   15.00    --  103.24 -30.00-180.00   26
  7  \w     33.00  75.00   1.00   15.00    --  103.24-125.00  30.00   42
  8  \w     38.00  91.00   1.00   15.00    --  103.24 -94.00 150.00   53
  9  \w     39.00 117.00   1.00   15.00    --  103.24-125.00  60.00   78
 10  \w     27.00 135.00   1.00   15.00    --  103.24 -77.00-150.00  108
 11  \w     51.00  81.00   1.00   15.00    --  103.24  15.00 -30.00   30
 12  \w    146.00 171.00   1.00   15.00    --  103.24 125.00-150.00   25
 13  \w     68.00 132.00   1.00   15.00    --  103.24 -30.00-180.00   64
 14  \w     39.00  65.00   1.00   15.00    --  103.24-125.00-120.00   26
 15  \w     95.00 177.00   1.00   15.00    --  103.24  30.00-180.00   82
 16  \w    126.00 152.00   1.00   15.00    --  103.24  15.00 -30.00   26
 17  \w     30.00 126.00   1.00   15.00    --  103.24 -30.00   0.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0715588000
_diffrn_orient_matrix_UB_12      -0.0479649000
_diffrn_orient_matrix_UB_13      0.0391964000
_diffrn_orient_matrix_UB_21      -0.2243933000
_diffrn_orient_matrix_UB_22      -0.0818304000
_diffrn_orient_matrix_UB_23      0.0049521000
_diffrn_orient_matrix_UB_31      0.1052489000
_diffrn_orient_matrix_UB_32      -0.1420283000
_diffrn_orient_matrix_UB_33      -0.0161175000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            11866
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         26.051
_diffrn_reflns_theta_min         2.254
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       needle-like
_exptl_crystal_F_000             848
_refine_diff_density_max         1.353
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Flack x determined using 1531 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.69(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3720
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0884
_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^)+(0.1670P)^2^+2.4771P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2492
_refine_ls_wR_factor_ref         0.2533
_reflns_Friedel_coverage         0.901
_reflns_Friedel_fraction_full    0.949
_reflns_Friedel_fraction_max     0.927
_reflns_number_gt                3476
_reflns_number_total             3720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04806f2.cif
_cod_data_source_block           lqj-20200118-1
_cod_original_cell_volume        1944.86(9)
_cod_database_code               1565074
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C1 H1 O1 N1 Cl1'
_reflns_odcompleteness_completeness 99.90
_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, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C17(H17A,H17B), C19(H19A,H19B), C9(H9A,H9B), C18(H18A,H18B),
 C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C21(H21), C22(H22), C11(H11), C15(H15), C23(H23)
2.c Idealised Me refined as rotating group:
 N20(H20A,H20B,H20C), N2(H2A,H2B,H2C)
;
_shelx_res_checksum              2346
_shelx_hkl_checksum              10548
_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 1.584
_oxdiff_exptl_absorpt_empirical_full_min 0.577