Synthesis of highly fluorescent helical quinolizinium salts by a Rh-catalyzed cyclotrimerization/C-H activation sequence.
Cadart, Timothée; Feriancová, Lucia; Henke, Petr; Gyepes, Robert; Císařová, Ivana; Kalíková, Květa; Kotora, Martin; Chemical communications (Cambridge, England) 61 (2025) 4662–4665; doi:10.1039/d4cc06512c

data_1573794
_publ_section_title
;
 Synthesis of highly fluorescent helical quinolizinium salts by a
 Rh-catalyzed cyclotrimerization/C-H activation sequence.
;
_journal_issue                   24
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4662
_journal_page_last               4665
_journal_paper_doi               10.1039/d4cc06512c
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C40 H27.98 B Br0.02 N,C40 H27.95 B Br0.05 N'
_chemical_formula_sum            'C80 H55.93 B2 Br0.07 N2 O0'
_chemical_formula_weight         1072.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-07-24 deposited with the CCDC.	2025-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.408(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.5585(7)
_cell_length_b                   9.9428(3)
_cell_length_c                   24.0807(7)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      66.7084
_cell_measurement_theta_min      3.4596
_cell_volume                     6117.6(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTONIII CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios Cu  multilayer optic'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1591
_diffrn_reflns_av_unetI/netI     0.1031
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            65917
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.844
_diffrn_reflns_theta_max         66.844
_diffrn_reflns_theta_min         1.729
_diffrn_source                   'I\mS  micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       bar
_exptl_crystal_F_000             2249
_exptl_crystal_size_max          0.429
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         10814
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0619P)^2^+0.0327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6707
_reflns_number_total             10814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06512c2.cif
_cod_data_source_block           cu_lf38_2a_kotora_sq
_cod_depositor_comments
'Adding full bibliography for 1573791--1573795.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1573794
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.798
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              41134
_shelx_hkl_checksum              92053
_shelx_fab_checksum              25740