Modular Synthesis, Host-Guest Complexation and Solvation-Controlled Relaxation of Nanohoops with Donor-Acceptor Structures
Deng, Han; Guo, Zilong; Wang, Yaxin; Li, Ke; Zhou, Qin; Ge, Chang; Xu, Zhanqiang; Sato, Sota; Ma, Xiaonan; Sun, Zhe; Chemical Science  (2022) –; doi:10.1039/D2SC05804A

data_1567963
_publ_section_title
;
 Modular Synthesis, Host-Guest Complexation and Solvation-Controlled
 Relaxation of Nanohoops with Donor-Acceptor Structures
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC05804A
_journal_year                    2022
_chemical_formula_sum            'C154.4 H88.4 Cl1.2 N2'
_chemical_formula_weight         2014.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-03-21 deposited with the CCDC.	2022-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6132(6)
_cell_length_b                   18.7606(12)
_cell_length_c                   32.1149(13)
_cell_measurement_reflns_used    4785
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      51.4110
_cell_measurement_theta_min      2.7330
_cell_volume                     10009.4(8)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_unetI/netI     0.1162
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            25299
_diffrn_reflns_point_group_measured_fraction_full 0.882
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        57.131
_diffrn_reflns_theta_max         57.131
_diffrn_reflns_theta_min         2.752
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.870
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       block
_exptl_crystal_F_000             4197
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 1877 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.09(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1608
_refine_ls_number_reflns         11961
_refine_ls_number_restraints     585
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1498
_refine_ls_R_factor_gt           0.0742
_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^)+(0.1094P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1687
_refine_ls_wR_factor_ref         0.2103
_reflns_Friedel_coverage         0.683
_reflns_Friedel_fraction_full    0.793
_reflns_Friedel_fraction_max     0.793
_reflns_number_gt                6419
_reflns_number_total             11961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05804a2.cif
_cod_data_source_block           049364_DH_3C60_160_a
_cod_original_formula_sum        'C154.40 H88.40 Cl1.20 N2'
_cod_database_code               1567963
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   0.958
_shelx_res_checksum              88726
_shelx_hkl_checksum              78881