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_1573795
_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_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C43 H29 N O2 Pt, 1/3(C5 H12)'
_chemical_formula_sum            'C44.66667 H33 N O2 Pt'
_chemical_formula_weight         810.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                89.964(2)
_cell_angle_beta                 81.068(2)
_cell_angle_gamma                85.594(2)
_cell_formula_units_Z            6
_cell_length_a                   12.7645(6)
_cell_length_b                   18.0822(10)
_cell_length_c                   22.7774(13)
_cell_measurement_reflns_used    9173
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.6863
_cell_measurement_theta_min      2.2594
_cell_volume                     5177.8(5)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTONIII CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_av_unetI/netI     0.0813
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            100825
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.569
_diffrn_reflns_theta_min         1.902
_diffrn_source                   'I\mS  micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.104
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.77
_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            orange
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       needle
_exptl_crystal_F_000             2412
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.013
_refine_diff_density_max         2.363
_refine_diff_density_min         -1.641
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1323
_refine_ls_number_reflns         23812
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+11.6479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16851
_reflns_number_total             23812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06512c2.cif
_cod_data_source_block           mo_lf35_kotora
_cod_depositor_comments
;
Adding full bibliography for 1573791--1573795.cif.

2025-06-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C134 H99 N3 O6 Pt3'
_cod_original_formula_weight         2432.43
_cod_original_formula_moiety         '3(C43 H29 N O2 Pt), C5 H12'
_cod_original_formula_units_Z            2
_cod_database_code               1573795
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.243
_shelx_estimated_absorpt_t_max   0.949
_shelx_res_checksum              82230
_shelx_hkl_checksum              46771