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_1550928
_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
'6(F6 P), C13 H20 O5, 4(C2 H3 N), C78 H60 N12'
_chemical_formula_sum            'C99 H92 F36 N16 O5 P6'
_chemical_formula_weight         2455.70
_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             2019-01-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-09 deposited with the CCDC.    2019-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                72.715(3)
_cell_angle_beta                 85.475(3)
_cell_angle_gamma                81.308(2)
_cell_formula_units_Z            2
_cell_length_a                   13.6331(5)
_cell_length_b                   20.6544(8)
_cell_length_c                   24.9241(10)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.382
_cell_measurement_theta_min      3.234
_cell_volume                     6620.0(5)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2017)'
_computing_data_collection       'APEX2 V2017.3 (Bruker, 2017)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      169.98
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.995
_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  Triumph
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            81234
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.966
_diffrn_reflns_theta_min         3.230
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.060
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0959 before and 0.0618 after correction. The Ratio of minimum to maximum transmission is 0.7248. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       block
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.398
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       0.0047(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.456
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1592
_refine_ls_number_reflns         25036
_refine_ls_number_restraints     1568
_refine_ls_restrained_S_all      1.499
_refine_ls_R_factor_all          0.1782
_refine_ls_R_factor_gt           0.1278
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_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          0.3777
_refine_ls_wR_factor_ref         0.4100
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14205
_reflns_number_total             25036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00591a2.cif
_cod_data_source_block           mjl18182_0m_sq
_cod_database_code               1550928
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.901
_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, All O(H) groups
2. Restrained distances
 O5-C85
 1.4 with sigma of 0.02
 O2-C80
 1.4 with sigma of 0.02
 F11A-F12A \\sim F11A-F10A \\sim F11A-F8A \\sim F11A-F9A \\sim F7A-F12A \\sim
F7A-F10A \\sim F7A-F8A ~
 F7A-F9A \\sim F12A-F10A \\sim F12A-F8A \\sim F10A-F9A \\sim F8A-F9A
 with sigma of 0.02
 P2A-F11A \\sim P2A-F7A \\sim P2A-F12A \\sim P2A-F10A \\sim P2A-F8A \\sim
P2A-F9A
 with sigma of 0.01
 F11-F12 \\sim F11-F10 \\sim F11-F8 \\sim F11-F9 \\sim F7-F12 \\sim F7-F10
\\sim F7-F8 \\sim F7-F9 \\sim F12-
 F10 \\sim F12-F8 \\sim F10-F9 \\sim F8-F9
 with sigma of 0.02
 P2-F11 \\sim P2-F7 \\sim P2-F12 \\sim P2-F10 \\sim P2-F8 \\sim P2-F9
 with sigma of 0.01
3. 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
4. Others
 Sof(P7)=Sof(F37)=Sof(F39)=Sof(F40)=Sof(F38)=Sof(F34A)=Sof(F35A)=1-FVAR(1)
 Sof(F34)=Sof(F35)=Sof(P6)=Sof(F33)=Sof(F31)=Sof(F32)=Sof(F36)=FVAR(1)
 Sof(F11A)=Sof(F7A)=Sof(F12A)=Sof(F10A)=Sof(F8A)=Sof(F9A)=Sof(P2A)=1-FVAR(2)
 Sof(P2)=Sof(F11)=Sof(F7)=Sof(F12)=Sof(F10)=Sof(F8)=Sof(F9)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C85(H85A,H85B), C79(H79A,H79B), C84(H84A,H84B), C81(H81A,H81B), C78(H78A,
 H78B), C82(H82A,H82B), C83(H83A,H83B), C80(H80A,H80B), C4HA(H4HA,H4HB),
 C0IA(H0IA,H0IB), C3JA(H3JA,H3JB), C110(H11A,H11B), C5DA(H5DA,H5DB), C8GA(H8GA,
 H8GB)
5.b Aromatic/amide H refined with riding coordinates:
 C73(H73), C75(H75), C74(H74), C60(H60), C52(H52), C5(H5), C3(H3), C33(H33),
 C62(H62), C39(H39), C10(H10), C14(H14), C61(H61), C51(H51), C35(H35), C17(H17),
  C7(H7), C70(H70), C16(H16), C32(H32), C15(H15), C53(H53), C27(H27), C72(H72),
 C55(H55), C6(H6), C45(H45), C54(H54), C2(H2), C46(H46), C44(H44), C43(H43),
 C63(H63), C49(H49), C36(H36), C9(H9), C24(H24), C69(H69), C66(H66), C65(H65),
 C38(H38), C25(H25), C30(H30), C71(H71), C22(H22), C64(H64), C29(H29), C59(H59),
  C12(H12), C50(H50), C56(H56)
5.c Tetrahedral OH refined with riding coordinates:
 O5(H5A)
5.d Idealised Me refined as rotating group:
 C90(H90A,H90B,H90C), C87(H87A,H87B,H87C), C89(H89A,H89B,H89C), C93(H93A,H93B,
 H93C)
;
_shelx_res_checksum              74810
_shelx_fab_checksum              96295
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'