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_7133100
_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         'C27 H17 N O3'
_chemical_formula_sum            'C27 H17 N O3'
_chemical_formula_weight         403.42
_chemical_name_common            'carbonyl-bridged rhodol'
_chemical_name_systematic        1a
_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             2021-04-26
_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                   7.3843(2)
_cell_length_b                   20.0427(5)
_cell_length_c                   24.5666(6)
_cell_measurement_reflns_used    4641
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      67.6560
_cell_measurement_theta_min      3.6030
_cell_volume                     3635.89(16)
_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 2018/2 (Sheldrick, 2018)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.986
_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  30.00   0.50   40.00    --  -40.71  25.00  30.00  120
  2  \w    -14.00  11.00   0.50   40.00    --  -40.71  43.00 -84.00   50
  3  \w    -56.00 -30.00   0.50  110.00    --  -96.35  50.00  30.00   52
  4  \w    -56.00 -30.00   0.50  110.00    --  -96.35  50.00  60.00   52
  5  \w    -56.00 -31.00   0.50  110.00    --  -96.35  50.00  90.00   50
  6  \w    -57.00 -32.00   0.50  110.00    --  -96.35  50.00 150.00   50
  7  \w    -57.00 -17.00   0.50   40.00    --  -40.71  82.00  52.00   80
  8  \w    -72.00 -47.00   0.50   40.00    --  -40.71 110.00 136.00   50
  9  \w   -100.00 -75.00   0.50  110.00    --  -96.35  82.00  52.00   50
 10  \w    -57.00 -31.00   0.50  110.00    --  -96.35  50.00   0.00   52
 11  \w    -64.00 -24.00   0.50  110.00    --  -96.35  96.00-120.00   80
 12  \w    -69.00 -29.00   0.50  110.00    --  -96.35  59.00-180.00   80
 13  \w   -105.00 -76.00   0.50  110.00    --  -96.35  96.00-120.00   58
 14  \w    -70.00 -30.00   0.50   40.00    --  -40.71 -43.00 123.00   80
 15  \w   -105.00 -80.00   0.50   40.00    --  -40.71 -43.00 123.00   50
 16  \w   -136.00 -86.00   0.50  110.00    --  -96.35-110.00  41.00  100
 17  \w   -160.00 -79.00   0.50  110.00    --  -96.35 -43.00 123.00  162
 18  \w     38.00  63.00   0.50   40.00    --   40.40-110.00  41.00   50
 19  \w     56.00  81.00   0.50   40.00    --   40.40  43.00 -84.00   50
 20  \w    126.00 160.00   0.50  110.00    --   96.04  43.00 -84.00   68
 21  \w     78.00 122.00   0.50  110.00    --   96.04  82.00  52.00   88
 22  \w    107.00 132.00   0.50  110.00    --   96.04 110.00 136.00   50
 23  \w     31.00  56.00   0.50  110.00    --   96.04 -50.00  60.00   50
 24  \w     29.00  54.00   0.50  110.00    --   96.04 -50.00  90.00   50
 25  \w     33.00  59.00   0.50  110.00    --   96.04 -59.00 120.00   52
 26  \w     49.00  76.00   0.50  110.00    --   96.04-110.00  41.00   54
 27  \w     29.00  54.00   0.50  110.00    --   96.04 -50.00 -60.00   50
 28  \w     74.00  99.00   0.50  110.00    --   96.04 -82.00 -68.00   50
 29  \w     62.00  97.00   0.50   40.00    --   40.40-138.00 -30.00   70
 30  \w     25.00  55.00   0.50   40.00    --   40.40-138.00 -30.00   60
 31  \w      5.00  30.00   0.50   40.00    --   40.40 -43.00 123.00   50
 32  \w    -13.00  14.00   0.50   40.00    --   40.40 -25.00  90.00   54
 33  \w     24.00  51.00   0.50   40.00    --   40.40 -82.00 -68.00   54
 34  \w    -27.00  -2.00   0.50   40.00    --   40.40 -12.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0040461000
_diffrn_orient_matrix_UB_12      -0.0665400000
_diffrn_orient_matrix_UB_13      0.0313993000
_diffrn_orient_matrix_UB_21      0.2035461000
_diffrn_orient_matrix_UB_22      0.0096115000
_diffrn_orient_matrix_UB_23      0.0112105000
_diffrn_orient_matrix_UB_31      -0.0453278000
_diffrn_orient_matrix_UB_32      0.0373086000
_diffrn_orient_matrix_UB_33      0.0531084000
_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  0.0370
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12026
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.465
_diffrn_reflns_theta_min         3.598
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.613
_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    1.474
_exptl_crystal_description       plate
_exptl_crystal_F_000             1680
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3/Et2O'
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0839P)^2^+2.3233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1410
_refine_ls_wR_factor_ref         0.1520
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2655
_reflns_number_total             3292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01071j2.cif
_cod_data_source_block           exp_138
_cod_depositor_comments
'Adding full bibliography for 7133100--7133102.cif.'
_cod_database_code               7133100
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00H(H00H), C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L),
 C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R),
 C00T(H00T), C00V(H00V)
2.b Idealised Me refined as rotating group:
 C00U(H00A,H00B,H00C)
;
_shelx_res_checksum              71793
_shelx_hkl_checksum              42304
_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 1.845
_oxdiff_exptl_absorpt_empirical_full_min 0.624