Facile Synthesis of Micro-Scale MOF Host-Guest with Long-Last Phosphorescence and Enhanced Optoelectronic Performance
Yang, Xiao-Gang; Lu, Xiao-Min; Zhai, Zhi-Min; Zhao, Ying; Liu, Xin-Yi; Ma, Lufang; Zang, Shuang-Quan; Chemical Communications  (2019) –; doi:10.1039/C9CC05708K

data_7124043
_publ_section_title
;
 Facile Synthesis of Micro-Scale MOF Host-Guest with Long-Last
 Phosphorescence and Enhanced Optoelectronic Performance
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05708K
_journal_year                    2019
_chemical_formula_moiety         '0.06(C128 H64 O64 Zn16)'
_chemical_formula_sum            'C8 H4 O4 Zn'
_chemical_formula_weight         229.48
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-05 deposited with the CCDC.    2019-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   9.63550(10)
_cell_length_b                   9.63550(10)
_cell_length_c                   32.1835(7)
_cell_measurement_reflns_used    18409
_cell_measurement_temperature    293.37(10)
_cell_measurement_theta_max      28.2010
_cell_measurement_theta_min      4.2170
_cell_volume                     2988.01(8)
_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      air
_diffrn_ambient_temperature      293.37(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -13.25  25.00   0.75    5.00    --  -13.80 -99.00 -30.00   51
  2  \w    -78.00 -30.75   0.75    5.00    --  -13.80 -57.00-180.00   63
  3  \w    -66.00   0.00   0.75    5.00    --  -13.80 122.00  40.21   88
  4  \w     17.00  80.00   0.75    5.00    --   14.82  38.00   0.00   84
  5  \w     -4.00  83.00   0.75    5.00    --   14.82  38.00-150.00  116
  6  \w      3.00  82.50   0.75    5.00    --   14.82  38.00 -60.00  106
  7  \w    -49.00  31.25   0.75    5.00    --   14.82 -57.00-180.00  107
  8  \w     -3.00  83.25   0.75    5.00    --   14.82  38.00 120.00  115
  9  \w     -5.00  63.25   0.75    5.00    --   14.82-116.00  42.00   91
 10  \w    -13.00  58.25   0.75    5.00    --   14.82-106.00 -67.75   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0730369000
_diffrn_orient_matrix_UB_12      -0.0085819000
_diffrn_orient_matrix_UB_13      -0.0010393000
_diffrn_orient_matrix_UB_21      0.0048688000
_diffrn_orient_matrix_UB_22      -0.0119085000
_diffrn_orient_matrix_UB_23      -0.0216993000
_diffrn_orient_matrix_UB_31      0.0078889000
_diffrn_orient_matrix_UB_32      -0.0721285000
_diffrn_orient_matrix_UB_33      0.0037073000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            41879
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.335
_diffrn_reflns_theta_min         3.299
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.258
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31745
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.040
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.631
_refine_diff_density_min         -1.747
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details
;
 Flack x determined using 926 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.464(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         2735
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0644
_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^)+67.7993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1573
_reflns_Friedel_coverage         0.633
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2570
_reflns_number_total             2735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05708k2.cif
_cod_data_source_block           y346
_cod_original_cell_volume        2988.01(9)
_cod_database_code               7124043
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1O1N1Zn1
_shelx_estimated_absorpt_t_max   0.473
_shelx_estimated_absorpt_t_min   0.441
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C8, C10, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C8 \\sim C10 \\sim C16: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C8) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C10(H10), C12(H12), C13(H13), C14(H14)
;
_shelx_res_checksum              280
_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 2.232
_oxdiff_exptl_absorpt_empirical_full_min 0.584