Nonpolar selective emission (NPSE) of carbonyl-bridged rhodols.
Tanioka, Masaru; Mori, Minori; Harada, Mei; Matsuya, Yuji; Kamino, Shinichiro; Chemical communications (Cambridge, England) 60 (2024) 6407–6410; doi:10.1039/d4cc01071j

data_7133102
_publ_section_title
;
 Nonpolar selective emission (NPSE) of carbonyl-bridged rhodols.
;
_journal_issue                   50
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6407
_journal_page_last               6410
_journal_paper_doi               10.1039/d4cc01071j
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C32 H19 N O3'
_chemical_formula_sum            'C32 H19 N O3'
_chemical_formula_weight         465.48
_chemical_name_common            'carbonyl-bridged rhodol'
_chemical_name_systematic        1b
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-06
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2024-02-09 deposited with the CCDC.	2024-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.75825(12)
_cell_length_b                   18.8157(4)
_cell_length_c                   31.7145(6)
_cell_measurement_reflns_used    14013
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      68.1400
_cell_measurement_theta_min      2.7860
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_computing_cell_refinement       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -17.00  31.00   0.50    0.44    --   40.40 -37.00  30.00   96
  2  \w     12.00  60.00   0.50    0.44    --   40.40 -63.00 -30.00   96
  3  \w    -12.00  24.00   0.50    0.44    --   40.40 -12.00 -30.00   72
  4  \w    -21.00   7.00   0.50    0.44    --   40.40 -63.00 -30.00   56
  5  \w     10.00  40.00   0.50    0.44    --   40.40-104.00   0.00   60
  6  \w     11.00  70.00   0.50    0.44    --   40.40-104.00 -30.00  118
  7  \w     28.00  78.00   0.50    0.44    --   40.40-104.00-150.00  100
  8  \w     29.00  57.00   0.50    1.77    --   96.04 -50.00 -60.00   56
  9  \w     35.00  67.00   0.50    1.77    --   96.04 -59.00 -90.00   64
 10  \w     29.00  56.00   0.50    1.77    --   96.04 -50.00 -30.00   54
 11  \w     40.00  75.00   0.50    1.77    --   96.04 -68.00  30.00   70
 12  \w     59.00 105.00   0.50    1.77    --   96.04-117.00  30.00   92
 13  \w     74.00  99.00   0.50    0.44    --   40.40-138.00 120.00   50
 14  \w     45.00  71.00   0.50    0.44    --   40.40-138.00 120.00   52
 15  \w     29.00  55.00   0.50    1.77    --   96.04 -50.00  30.00   52
 16  \w     26.00  52.00   0.50    1.77    --   96.04   0.00  30.00   52
 17  \w     84.00 163.00   0.50    1.77    --   96.04  50.00  60.00  158
 18  \w    137.00 163.00   0.50    1.77    --   96.04  68.00  30.00   52
 19  \w    138.00 163.00   0.50    1.77    --   96.04 117.00  90.00   50
 20  \w     80.00 106.00   0.50    1.77    --   96.04 117.00  90.00   52
 21  \w     72.00  98.00   0.50    1.77    --   96.04  68.00  30.00   52
 22  \w     76.00 164.00   0.50    1.77    --   96.04  68.00  90.00  176
 23  \w     89.00 139.00   0.50    1.77    --   96.04   0.00  30.00  100
 24  \w     74.00 126.00   0.50    1.77    --   96.04  68.00 150.00  104
 25  \w     26.00 100.00   0.50    0.44    --   40.40  50.00  30.00  148
 26  \w     79.00 154.00   0.50    1.77    --   96.04  42.00-150.00  150
 27  \w     29.00  97.00   0.50    0.44    --   40.40  50.00-180.00  136
 28  \w    -11.00  28.00   0.50    0.44    --  -40.71  63.00-180.00   78
 29  \w    -33.00  10.00   0.50    0.44    --   40.40 -12.00 -90.00   86
 30  \w     -7.00  40.00   0.50    0.44    --   40.40 -63.00-150.00   94
 31  \w     29.00 108.00   0.50    1.77    --   96.04-117.00 -30.00  158
 32  \w     -4.00  77.00   0.50    0.44    --   40.40-104.00 120.00  162
 33  \w      2.00  27.00   0.50    0.44    --   40.40 -37.00 150.00   50
 34  \w    -24.00  19.00   0.50    0.44    --   40.40 -37.00  90.00   86
 35  \w    -32.00   8.00   0.50    0.44    --   40.40 -12.00  30.00   80
 36  \w    -60.00 -29.00   0.50    0.44    --  -40.71 -37.00  60.00   62
 37  \w    -24.00  26.00   0.50    0.44    --  -40.71  12.00   0.00  100
 38  \w    -42.00 -17.00   0.50    0.44    --  -40.71  37.00   0.00   50
 39  \w    -57.00 -30.00   0.50    1.77    --  -96.35  50.00-120.00   54
 40  \w    -57.00 -30.00   0.50    1.77    --  -96.35  50.00-150.00   54
 41  \w    -57.00 -30.00   0.50    1.77    --  -96.35  50.00-180.00   54
 42  \w    -69.00 -44.00   0.50    1.77    --  -96.35  59.00 -90.00   50
 43  \w    -83.00 -57.00   0.50    1.77    --  -96.35  77.00-150.00   52
 44  \w    -76.00 -31.00   0.50    1.77    --  -96.35  68.00-120.00   90
 45  \w    -40.00 -15.00   0.50    0.44    --  -40.71  63.00-180.00   50
 46  \w    -23.00  33.00   0.50    0.44    --   40.40 -37.00-150.00  112
 47  \w    -82.00 -28.00   0.50    1.77    --  -96.35  77.00  60.00  108
 48  \w    -68.00 -38.00   0.50    1.77    --  -96.35  59.00 120.00   60
 49  \w   -100.00 -23.00   0.50    1.77    --  -96.35  96.00  90.00  154
 50  \w   -102.00 -49.00   0.50    1.77    --  -96.35  96.00 120.00  106
 51  \w   -110.00 -55.00   0.50    1.77    --  -96.35 117.00 120.00  110
 52  \w   -105.00 -80.00   0.50    0.44    --  -40.71 -37.00  60.00   50
 53  \w   -115.00 -89.00   0.50    1.77    --  -96.35-117.00  60.00   52
 54  \w   -163.00 -91.00   0.50    1.77    --  -96.35 -33.00   0.00  144
 55  \w   -162.00 -80.00   0.50    1.77    --  -96.35 -42.00 -30.00  164
 56  \w   -164.00-100.00   0.50    1.77    --  -96.35 -68.00  90.00  128
 57  \w   -104.00 -26.00   0.50    1.77    --  -96.35  96.00-120.00  156
 58  \w   -104.00 -67.00   0.50    1.77    --  -96.35 117.00-120.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
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'XtaLAB Synergy, Single source at home/near, HyPix3000'
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'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0297173000
_diffrn_orient_matrix_UB_12      -0.0622570000
_diffrn_orient_matrix_UB_13      0.0306887000
_diffrn_orient_matrix_UB_21      -0.0544671000
_diffrn_orient_matrix_UB_22      -0.0528995000
_diffrn_orient_matrix_UB_23      -0.0346204000
_diffrn_orient_matrix_UB_31      0.1885985000
_diffrn_orient_matrix_UB_32      -0.0054907000
_diffrn_orient_matrix_UB_33      -0.0148214000
_diffrn_radiation_monochromator  mirror
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_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            37485
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.443
_diffrn_reflns_theta_min         2.787
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.531
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020)
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            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       plate
_exptl_crystal_F_000             1936
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3/Et2O'
_exptl_crystal_size_max          0.939
_exptl_crystal_size_mid          0.314
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.00031(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0596P)^2^+1.3197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3827
_reflns_number_total             4249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01071j2.cif
_cod_data_source_block           exp_141
_cod_depositor_comments
'Adding full bibliography for 7133100--7133102.cif.'
_cod_original_cell_volume        4629.59(14)
_cod_database_code               7133102
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C9(H9), C4(H4), C2(H2), C29(H29), C10(H10), C32(H32), C30(H30),
 C21(H21), C17(H17), C31(H31), C20(H20), C19(H19), C23(H23), C18(H18), C27(H27),
  C26(H26), C25(H25), C24(H24)
;
_shelx_res_checksum              97535
_shelx_hkl_checksum              15740
_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 1.674
_oxdiff_exptl_absorpt_empirical_full_min 0.736