A Dynamic Tetracationic Macrocycle Exhibiting Photoswitchable Molecular Encapsulation.
Wu, Huang; Chen, Yong; Zhang, Long; Anamimoghadam, Ommid; Shen, Dengke; Liu, Zhichang; Cai, Kang; Pezzato, Cristian; Stern, Charlotte L.; Liu, Yu; Stoddart, J. Fraser; Journal of the American Chemical Society 141 (2019) 1280–1289; doi:10.1021/jacs.8b10526

data_4133511
_publ_section_title
;
 A Dynamic Tetracationic Macrocycle Exhibiting Photoswitchable Molecular
 Encapsulation.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1280
_journal_page_last               1289
_journal_paper_doi               10.1021/jacs.8b10526
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C58 H48 N4, 4(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C62 H54 F24 N6 P4'
_chemical_formula_weight         1462.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.299(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.128(3)
_cell_length_b                   40.070(4)
_cell_length_c                   12.3508(12)
_cell_measurement_reflns_used    8949
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      63.382
_cell_measurement_theta_min      2.788
_cell_volume                     15691(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_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    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      250.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            30284
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        63.889
_diffrn_reflns_theta_max         63.889
_diffrn_reflns_theta_min         1.777
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.740
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.6195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0901 before and 0.0508 after correction. The Ratio of minimum to maximum transmission is 0.8234. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       needle
_exptl_crystal_F_000             5952
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.369
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.644
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     974
_refine_ls_number_reflns         12709
_refine_ls_number_restraints     299
_refine_ls_restrained_S_all      1.690
_refine_ls_R_factor_all          0.1570
_refine_ls_R_factor_gt           0.1348
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4119
_refine_ls_wR_factor_ref         0.4322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8586
_reflns_number_total             12709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10526_si_003.cif
_cod_data_source_block           cx1253b
_cod_database_code               4133511
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.566
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 F7, P2, F8, F9, F10, F11, F12, P4, F17, F18, F19, F20, F21, F22, F15, P3, F14,
  F13, F16, F6, P1, F1, F2, F3, F4, F5, F24, P5, F23, F25, F27, P6, F26, F28
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C49A, C50A, C51A, C46A, C47A, C48A, C49, C50, C51, C46, C47, C48
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Sof(C44A)=Sof(H44A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=Sof(C47A)=Sof(H47A)=
 Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(C50A)=Sof(H50A)=Sof(C51A)=Sof(H51A)=
 Sof(H52A)=1-FVAR(1)
 Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(C47)=Sof(H47)=Sof(C48)=
 Sof(H48)=Sof(C49)=Sof(C50)=Sof(H50)=Sof(C51)=Sof(H51)=Sof(H52)=FVAR(1)
 Fixed Sof: P4(0.5) F17(0.5) F18(0.5) F19(0.5) F20(0.5) F21(0.5) F22(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C31(H31A,H31B), C38(H38A,H38B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24), C25(H25),
  C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34), C36(H36),
 C37(H37), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C44A(H44A),
 C45(H45), C45A(H45A), C47(H47), C47A(H47A), C48(H48), C48A(H48A), C50(H50),
 C50A(H50A), C51(H51), C51A(H51A), C52(H52), C52(H52A), C53(H53), C55(H55),
 C56(H56), C57(H57), C58(H58)
4.c Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              17100
_shelx_hkl_checksum              33596
_shelx_fab_checksum              32028
_olex2_date_sample_data_collection 2018-04-12
_olex2_date_sample_submission    2018-03-29
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id cx1253b
_olex2_submission_special_instructions 'No special instructions were received'