Guest recognition enhanced by lateral interactions
Jiao, Tianyu; Cai, Kang; Liu, Zhichang; Wu, Guangcheng; Shen, Libo; Cheng, Chuyang; Feng, Yuanning; Stern, Charlotte L.; Stoddart, J. Fraser; Li, Hao; Chemical Science  (2019) –; doi:10.1039/C9SC00591A

data_1550924
_publ_section_title
;
 Guest recognition enhanced by lateral interactions
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC00591A
_journal_year                    2019
_chemical_formula_moiety         'C39 H30 N6, 3(C2 F3 O2)'
_chemical_formula_sum            'C45 H30 F9 N6 O6'
_chemical_formula_weight         921.75
_chemical_name_systematic        cage-tfa
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-07-28 deposited with the CCDC.    2019-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.631(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6264(5)
_cell_length_b                   30.4112(12)
_cell_length_c                   14.0126(5)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      63.639
_cell_measurement_theta_min      2.906
_cell_volume                     5707.1(4)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0274
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30865
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        63.815
_diffrn_reflns_theta_max         63.815
_diffrn_reflns_theta_min         2.906
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.6812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0820 before and 0.0450 after correction. The Ratio of minimum to maximum transmission is 0.9054. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.073
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1884
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.099
_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     708
_refine_ls_number_reflns         9551
_refine_ls_number_restraints     379
_refine_ls_restrained_S_all      1.827
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.1063
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3529
_refine_ls_wR_factor_ref         0.3680
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7945
_reflns_number_total             9551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00591a2.cif
_cod_data_source_block           cx1195c
_cod_database_code               1550924
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.835
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F7A-F8A \\sim F8A-F9A \\sim F7A-F9A \\sim F7-F8 \\sim F8-F9 \\sim F7-F9 \\sim
F6-F5 \\sim F6-F4 \\sim F5-F4 ~
 F4A-F5A \\sim F5A-F6A \\sim F4A-F6A
 with sigma of 0.01
 C51A-F4A \\sim C51A-F5A \\sim C51A-F6A \\sim C51-F6 \\sim C51-F5 \\sim C51-F4
 with sigma of 0.01
 C52-C51 \\sim C52A-C51A
 with sigma of 0.01
 F4-C52 \\sim F6-C52 \\sim F5-C52 \\sim F6A-C52A \\sim F4A-C52A \\sim F5A-C52A
\\sim C54-F9 \\sim C54-F8 ~
 C54-F7
 with sigma of 0.01
 O3A-C51A \\sim O4A-C51A \\sim O6-C53 \\sim O5-C53 \\sim O4-C51 \\sim O3-C51
 with sigma of 0.01
 O4A-C52A \\sim O5-C54 \\sim O3A-C52A \\sim O6-C54
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C52A \\sim F4A \\sim F5A \\sim F6A \\sim C51A \\sim O3A \\sim O4A \\sim F6
\\sim F4 \\sim C52 \\sim F5 \\sim C51 \\sim O3 \\sim O4 \\sim F7A \\sim F7
\\sim F9A \\sim F9 \\sim F8A \\sim F8: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. Others
 Sof(F5A)=Sof(F4A)=Sof(C52A)=Sof(F6A)=Sof(C51A)=Sof(O3A)=Sof(O4A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=Sof(O3)=Sof(O4)=Sof(C51)=Sof(C52)=FVAR(1)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(2)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(2)
 Fixed Sof: H13A(0.5) H13B(0.5) H20A(0.5) H20B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C20(H20A,H20B), C33(H33A,H33B), C44(H44A,H44B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C14(H14), C15(H15),
 C18(H18), C19(H19), C22(H22), C23(H23), C28(H28), C29(H29), C31(H31), C32(H32),
  C34(H34), C35(H35), C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43)
;
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.

Total solvent accessible volume / cell = 1871.5 Ang^3^ [32.7%]
Total electron count / cell = 388.9
;
_shelx_res_checksum              67060
_shelx_fab_checksum              80508
_olex2_date_sample_data_collection 2018-03-16
_olex2_date_sample_submission    2018-01-24
_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 cx1195c
_olex2_submission_special_instructions 'No special instructions were received'