Radical qubits photo-generated in acene-based metal-organic frameworks.
Orihashi, Kana; Yamauchi, Akio; Inoue, Miku; Parmar, Bhavesh; Fujiwara, Saiya; Kimizuka, Nobuo; Asada, Mizue; Nakamura, Toshikazu; Yanai, Nobuhiro; Dalton transactions (Cambridge, England : 2003) 53 (2024) 872–876; doi:10.1039/d3dt03959e

data_7714745
_publ_section_title
;
 Radical qubits photo-generated in acene-based metal-organic frameworks.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              872
_journal_page_last               876
_journal_paper_doi               10.1039/d3dt03959e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C7.625 H4 N0.25 O Zn0.25'
_chemical_formula_sum            'C7.62 H4 N0.25 O Zn0.25'
_chemical_formula_weight         131.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           47
_space_group_name_Hall           '-P 2 2'
_space_group_name_H-M_alt        'P m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-11-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-11-26 deposited with the CCDC.	2023-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.0072(8)
_cell_length_b                   15.9706(8)
_cell_length_c                   18.2207(13)
_cell_measurement_reflns_used    5620
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.9580
_cell_measurement_theta_min      2.4060
_cell_volume                     3203.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.968
_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     30.00  55.00   0.50    0.32    --   43.71-128.00-147.00   50
  2  \w     69.00  95.00   0.50    1.28    --  107.00-136.00 -51.00   52
  3  \w     36.00  91.00   0.50    1.28    --  107.00 -94.00-120.00  110
  4  \w     34.00  92.00   0.50    1.28    --  107.00 -94.00-150.00  116
  5  \w     33.00  92.00   0.50    1.28    --  107.00 -94.00-180.00  118
  6  \w     45.00  70.00   0.50    1.28    --  107.00-128.00-147.00   50
  7  \w    -17.00  19.00   0.50    0.32    --   43.71 -38.00-180.00   72
  8  \w    111.00 136.00   0.50    1.28    --  107.00 128.00 -72.00   50
  9  \w    102.00 127.00   0.50    1.28    --  107.00 136.00  12.00   50
 10  \w    -31.00  20.00   0.50    0.32    --   43.71 -38.00-120.00  102
 11  \w     99.00 125.00   0.50    1.28    --  107.00  30.00-180.00   52
 12  \w     99.00 159.00   0.50    1.28    --  107.00  30.00 -90.00  120
 13  \w    104.00 135.00   0.50    1.28    --  107.00  15.00 -30.00   62
 14  \w    105.00 130.00   0.50    1.28    --  107.00  15.00  60.00   50
 15  \w    -17.00  32.00   0.50    0.32    --  -43.71  38.00-150.00   98
 16  \w    -80.00 -55.00   0.50    0.32    --  -43.71 133.00-165.00   50
 17  \w    -17.00  11.00   0.50    0.32    --  -43.71  38.00 -60.00   56
 18  \w    -88.00 -16.00   0.50    0.32    --  -43.71 128.00 -72.00  144
 19  \w    -72.00 -45.00   0.50    0.32    --  -43.71 136.00  12.00   54
 20  \w   -124.00 -97.00   0.50    1.28    -- -104.00 -15.00-180.00   54
 21  \w   -139.00-113.00   0.50    1.28    -- -104.00-128.00-147.00   52
 22  \w   -138.00 -87.00   0.50    1.28    -- -104.00-136.00 -51.00  102
 23  \w   -122.00 -96.00   0.50    1.28    -- -104.00 -15.00 150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1319311000
_diffrn_orient_matrix_UB_12      0.0026154000
_diffrn_orient_matrix_UB_13      0.0280938000
_diffrn_orient_matrix_UB_21      -0.0469819000
_diffrn_orient_matrix_UB_22      0.0045254000
_diffrn_orient_matrix_UB_23      0.0795602000
_diffrn_orient_matrix_UB_31      0.0014019000
_diffrn_orient_matrix_UB_32      -0.0963107000
_diffrn_orient_matrix_UB_33      0.0046223000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15037
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.456
_diffrn_reflns_theta_min         2.425
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    0.545
_exptl_crystal_description       block
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.086
_refine_diff_density_max         1.984
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3574
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0858
_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^)+(0.1887P)^2^+0.7301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2460
_refine_ls_wR_factor_ref         0.2548
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3103
_reflns_number_total             3574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03959e2.cif
_cod_data_source_block           tcpb-mof_3_auto
_cod_depositor_comments
'Adding full bibliography for 7714745--7714746.cif.'
_cod_database_code               7714745
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.817
_reflns_odcompleteness_completeness 96.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C16-C15 \\sim C15-C10 \\sim C21-C19 \\sim C22-C21
 with sigma of 0.02
 C23-C12 \\sim C23-C19
 with sigma of 0.02
 N15-C16 \\sim N15-C12
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C22, C21, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C16, C15, C10, N15, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C3(0.5) H3(0.5) C1(0.5) H1(0.5) C2(0.5) H2(0.5) C4(0.5) H4(0.5)
 C21(0.25) C9(0.5) H9(0.5) C8(0.5) H8(0.5) C19(0.25) C15(0.25) H15(0.25)
 C10(0.25) H10A(0.25) H10B(0.25) C12(0.125) N15(0.25) C16(0.25) C22(0.25)
6.a Ternary CH refined with riding coordinates:
 C15(H15)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
6.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C3(H3), C1(H1), C2(H2), C4(H4), C9(H9), C8(H8)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              46413
_shelx_hkl_checksum              81541
_shelx_fab_checksum              4549
_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 1.605
_oxdiff_exptl_absorpt_empirical_full_min 0.409