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_1550925
_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         'C78 H60 N12, 6(F6 P), 4(C2 H3 N)'
_chemical_formula_sum            'C86 H72 F36 N16 P6'
_chemical_formula_weight         2199.41
_chemical_name_systematic        cage-pf6
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-07-28 deposited with the CCDC.    2019-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                83.509(8)
_cell_angle_beta                 84.344(8)
_cell_angle_gamma                85.297(8)
_cell_formula_units_Z            2
_cell_length_a                   13.9020(14)
_cell_length_b                   19.595(2)
_cell_length_c                   25.262(2)
_cell_measurement_reflns_used    2636
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.576
_cell_measurement_theta_min      3.536
_cell_volume                     6786.7(11)
_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      100.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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_unetI/netI     0.1522
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13490
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        50.834
_diffrn_reflns_theta_max         50.834
_diffrn_reflns_theta_min         1.767
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.525
_exptl_absorpt_correction_T_max  0.749954
_exptl_absorpt_correction_T_min  0.274707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 25968 reflections, Rint = 0.1414
 (6170 with I > 3sig(I), Rint = 0.1202)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_description       needle
_exptl_crystal_F_000             2228
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1302
_refine_ls_number_reflns         13490
_refine_ls_number_restraints     2049
_refine_ls_restrained_S_all      1.899
_refine_ls_R_factor_all          0.2601
_refine_ls_R_factor_gt           0.2253
_refine_ls_shift/su_max          0.002
_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          0.5065
_refine_ls_wR_factor_ref         0.5309
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9336
_reflns_number_total             13490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00591a2.cif
_cod_data_source_block           cx1228_sq
_cod_original_cell_volume        6786.9(12)
_cod_database_code               1550925
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.690(4)
 0.310(4)
2. 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
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(N6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C19(H19A,H19B), C33(H33A,H33B), C44(H44A,H44B), C58(H58A,H58B),
 C69(H69A,H69B)
5.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), C17(H17), C18(H18), C21(H21), C22(H22), C24(H24), C25(H25),
  C28(H28), C29(H29), C31(H31), C32(H32), C34(H34), C35(H35), C37(H37),
 C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C46(H46), C47(H47), C49(H49),
  C50(H50), C53(H53), C54(H54), C56(H56), C57(H57), C59(H59), C60(H60),
 C62(H62), C63(H63), C65(H65), C66(H66), C67(H67), C68(H68), C71(H71), C72(H72),
  C74(H74), C75(H75)
5.c Idealised Me refined as rotating group:
 C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C84(H84A,H84B,H84C), C86(H86A,H86B,
 H86C)
;
_shelx_res_checksum              27229
_shelx_fab_checksum              86649
_platon_squeeze_void_probe_radius 1.20
_olex2_date_sample_data_collection 2018-03-12
_olex2_date_sample_submission    2018-03-05
_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 cx1228
_olex2_submission_special_instructions 'No special instructions were received'