Acid/Base-Tunable Unimolecular Chirality Switching of a Pillar[5]azacrown <i>Pseudo</i>[1]Catenane.
Liang, Haozhong; Hua, Bin; Xu, Fan; Gan, Li-She; Shao, Li; Huang, Feihe; Journal of the American Chemical Society 142 (2020) 19772–19778; doi:10.1021/jacs.0c10570

data_4135338
_publ_section_title
;
 Acid/Base-Tunable Unimolecular Chirality Switching of a Pillar[5]azacrown
 <i>Pseudo</i>[1]Catenane.
;
_journal_issue                   46
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19772
_journal_page_last               19778
_journal_paper_doi               10.1021/jacs.0c10570
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'Cl, C51 H60 N3 O12'
_chemical_formula_sum            'C51 H60 Cl N3 O12'
_chemical_formula_weight         942.47
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-05-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.609(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8167(9)
_cell_length_b                   19.4344(18)
_cell_length_c                   20.4342(17)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.32
_cell_volume                     4670.3(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'zju Bruker D8 Venture Ims3.0'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_unetI/netI     0.0777
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40487
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.235
_diffrn_reflns_theta_min         2.261
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1523 before and 0.0800 after correction.
The Ratio of minimum to maximum transmission is 0.6216.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         10318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1106P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1668
_refine_ls_wR_factor_ref         0.1826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7973
_reflns_number_total             10318
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c10570_si_005.cif
_cod_data_source_block           200528_p4s1n3_hcl_0m
_cod_depositor_comments
'Adding full bibliography for 4135334--4135338.cif.'
_cod_database_code               4135338
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.972
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C1(H1A,H1B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B), C25(H25A,H25B),
  C34(H34A,H34B), C43(H43A,H43B)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), C4(H4), C7(H7), C18(H18), C21(H21), C27(H27), C30(H30),
 C36(H36), C39(H39), C46(H46), C49(H49)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C50(H50A,H50B,H50C), C51(H51A,
 H51B,H51C)
;
_shelx_res_checksum              95505
_shelx_hkl_checksum              60143
_olex2_submission_special_instructions 'No special instructions were received'