Rh(iii)-catalyzed building up of used heterocyclic cations: facile access to white-light-emitting materials.
Zhang, Jingxian; Sun, Tao; Wang, Kangmin; Hu, Ruike; Zhou, Chunlin; Ge, Haibo; Li, Bijin; Chemical science 15 (2024) 12270–12276; doi:10.1039/d4sc02188f

data_1571808
_publ_section_title
;
 Rh(iii)-catalyzed building up of used heterocyclic cations: facile access
 to white-light-emitting materials.
;
_journal_issue                   31
_journal_name_full               'Chemical science'
_journal_page_first              12270
_journal_page_last               12276
_journal_paper_doi               10.1039/d4sc02188f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         '2(F3 Sb0.5), C39 H26 N O'
_chemical_formula_sum            'C39 H26 F6 N O Sb'
_chemical_formula_weight         760.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-04
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2023-10-03 deposited with the CCDC.	2024-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.9020(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2592(2)
_cell_length_b                   12.03160(10)
_cell_length_c                   18.0659(2)
_cell_measurement_reflns_used    11648
_cell_measurement_temperature    250.01(10)
_cell_measurement_theta_max      70.4060
_cell_measurement_theta_min      2.9750
_cell_volume                     3219.61(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0892
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -20.00  17.00   1.00    1.00    --    0.00  57.00 -90.00   37
  2  \w     27.00  68.00   1.00    1.00    --    0.00  57.00 150.00   41
  3  \w     26.00  60.00   1.00    1.00    --    0.00  57.00 -90.00   34
  4  \w     23.00 102.00   1.00    1.00    --   54.00-125.00  90.00   79
  5  \w     37.00  93.00   1.00    1.00    --   54.00  57.00   0.00   56
  6  \w     66.00 115.00   1.00    1.00    --   54.00  57.00  30.00   49
  7  \w      9.00  71.00   1.00    1.00    --   54.00 -57.00 120.00   62
  8  \w     31.00  80.00   1.00    1.00    --   54.00-125.00 -30.00   49
  9  \w     79.00 130.00   1.00    1.00    --  108.00 -63.00 -30.00   51
 10  \w    100.00 136.00   1.00    1.00    --  108.00  50.00-120.00   36
 11  \w     44.00  73.00   1.00    1.00    --  108.00 -50.00-180.00   29
 12  \w     96.00 122.00   1.00    1.00    --  108.00 -50.00-180.00   26
 13  \w     91.00 177.00   1.00    1.00    --  108.00  38.00  90.00   86
 14  \w     36.00 139.00   1.00    1.00    --  108.00 -25.00 120.00  103
 15  \w     87.00 153.00   1.00    1.00    --  108.00  63.00 -30.00   66
 16  \w     85.00 111.00   1.00    1.00    --  108.00-111.00-150.00   26
 17  \w     42.00  68.00   1.00    1.00    --  108.00-111.00-150.00   26
 18  \w    141.00 173.00   1.00    1.00    --  108.00  63.00  30.00   32
 19  \w     87.00 137.00   1.00    1.00    --  108.00  63.00  30.00   50
 20  \w    117.00 143.00   1.00    1.00    --  108.00 111.00-120.00   26
 21  \w     61.00 137.00   1.00    1.00    --  108.00 -77.00 150.00   76
 22  \w    104.00 158.00   1.00    1.00    --  108.00  50.00   0.00   54
 23  \w    104.00 129.00   1.00    1.00    --  108.00 -63.00 120.00   25
 24  \w     66.00  91.00   1.00    1.00    --  108.00-111.00-120.00   25
 25  \w     70.00 102.00   1.00    1.00    --  108.00-111.00  30.00   32
 26  \w     61.00 129.00   1.00    1.00    --  108.00 -63.00-120.00   68
 27  \w     95.00 126.00   1.00    1.00    --  108.00 -91.00-150.00   31
 28  \w     42.00  67.00   1.00    1.00    --  108.00-111.00 -90.00   25
 29  \w     75.00 100.00   1.00    1.00    --  108.00-111.00 -60.00   25
 30  \w     92.00 118.00   1.00    1.00    --  108.00 -63.00  30.00   26
 31  \w     87.00 112.00   1.00    1.00    --  108.00-111.00  90.00   25
 32  \w     56.00  82.00   1.00    1.00    --  108.00 -50.00-150.00   26
 33  \w    137.00 168.00   1.00    1.00    --  108.00   0.00  30.00   31
 34  \w     71.00  97.00   1.00    1.00    --  108.00   0.00  30.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0896652000
_diffrn_orient_matrix_UB_12      0.0399708000
_diffrn_orient_matrix_UB_13      0.0158197000
_diffrn_orient_matrix_UB_21      0.0453522000
_diffrn_orient_matrix_UB_22      0.1099832000
_diffrn_orient_matrix_UB_23      0.0321956000
_diffrn_orient_matrix_UB_31      -0.0268600000
_diffrn_orient_matrix_UB_32      0.0520144000
_diffrn_orient_matrix_UB_33      -0.0801739000
_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  0.0260
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20747
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.569
_diffrn_reflns_theta_min         2.983
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.391
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.117a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.412
_refine_diff_density_min         -1.744
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.00115(7)
_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   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         6179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0560P)^2^+3.9253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5595
_reflns_number_total             6179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02188f2.cif
_cod_data_source_block           20230703-zjx-61031-250k
_cod_depositor_comments          'Adding full bibliography for 1571808.cif.'
_cod_database_code               1571808
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C39 H26 N O Sb F6'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Sof(F1A)=Sof(F2A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00H(H00H), C00J(H00J), C00M(H00M), C00N(H00N), C00P(H00P),
 C00Q(H00Q), C00R(H00R), C00S(H00S), C00U(H00U), C00V(H00V), C00W(H00W),
 C00X(H00X), C00Z(H00Z), C010(H010), C011(H011), C012(H012), C013(H013),
 C014(H014), C015(H015), C016(H016), C017(H017), C018(H018), C019(H019),
 C01A(H01A), C01B(H01B)
;
_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 1.799
_oxdiff_exptl_absorpt_empirical_full_min 0.765