Enantiopure nanohoops through racemic resolution of diketo[n]CPPs by chiral derivatization as precursors to DBP[n]CPPs
Wassy, Daniel; Hermann, Mathias; Wössner, Jan S.; Frédéric, Lucas; Pieters, Grégory; Esser, Birgit; Chemical Science  (2021) –; doi:10.1039/D1SC02718B

data_1563860
_publ_section_title
;
 Enantiopure nanohoops through racemic resolution of diketo[n]CPPs by
 chiral derivatization as precursors to DBP[n]CPPs
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC02718B
_journal_year                    2021
_chemical_formula_moiety         'C30 H20 Br2'
_chemical_formula_sum            'C30 H20 Br2'
_chemical_formula_weight         540.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1ln9j2
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-05-11 deposited with the CCDC.	2021-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.211(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.8475(8)
_cell_length_b                   7.3631(4)
_cell_length_c                   12.8990(8)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.375
_cell_measurement_theta_min      5.200
_cell_volume                     1103.76(12)
_computing_cell_refinement       'SAINT V8.37A'
_computing_data_collection       APEXII
_computing_data_reduction        'SAINT V8.37A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_device_type  'Bruker SMART APEXII QUAZAR'
_diffrn_measurement_method       'Omega and Phi Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19418
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.154
_diffrn_reflns_theta_min         2.137
_diffrn_source                   'INCOATEC Mo  Microsource'
_exptl_absorpt_coefficient_mu    3.689
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.5601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       needle
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.320
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         4425
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.306
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0149P)^2^+1.4104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4010
_reflns_number_total             4425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02718b2.cif
_cod_data_source_block           Esser_MB256_2s1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1563860
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.497
_shelx_estimated_absorpt_t_max   0.809
_shelx_res_checksum              73096
_shelx_hkl_checksum              10337