Post-Synthetic Modification of Nonporous Adaptive Crystals of Pillar[4]arene[1]quinone by Capturing Vaporized Amines.
Li, Errui; Jie, Kecheng; Zhou, Yujuan; Zhao, Run; Huang, Feihe; Journal of the American Chemical Society 140 (2018) 15070–15079; doi:10.1021/jacs.8b10192

data_4133457
_publ_section_title
;
 Post-Synthetic Modification of Nonporous Adaptive Crystals of
 Pillar[4]arene[1]quinone by Capturing Vaporized Amines.
;
_journal_issue                   44
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15070
_journal_page_last               15079
_journal_paper_doi               10.1021/jacs.8b10192
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C61 H82 N2 O10, C5 H13 N'
_chemical_formula_sum            'C66 H95 N3 O10'
_chemical_formula_weight         1090.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                97.3360(10)
_cell_angle_beta                 100.5000(10)
_cell_angle_gamma                113.6740(10)
_cell_formula_units_Z            2
_cell_length_a                   12.4043(3)
_cell_length_b                   12.7618(3)
_cell_length_c                   22.4296(5)
_cell_measurement_reflns_used    9393
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      66.70
_cell_measurement_theta_min      3.97
_cell_volume                     3116.82(13)
_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      173.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            50499
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.709
_diffrn_reflns_theta_max         66.709
_diffrn_reflns_theta_min         3.880
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.3182
_exptl_absorpt_correction_T_min  0.2277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0961 before and 0.0468 after correction.
The Ratio of minimum to maximum transmission is 0.7156.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         10931
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0637
_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^)+(0.0923P)^2^+1.8335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1787
_refine_ls_wR_factor_ref         0.1854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9440
_reflns_number_total             10931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10192_si_006.cif
_cod_data_source_block           171204zd_etp5q_0m
_cod_database_code               4133457
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups,
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C63-C62
 1.5 with sigma of 0.01
 C63-C64
 1.5 with sigma of 0.01
 H3D-H12C
 2.2 with sigma of 0.01
3. Rigid body (RIGU) restrains
 C5, C6, C7, C6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C12A, C12, C13, C13A, C14, C15A, C15, C14A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C62, C63, C64, C65, C66
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H5B)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=
 Sof(H7AC)=1-FVAR(1)
 Sof(H5A)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=
 Sof(H7C)=FVAR(1)
 Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C13A)=Sof(H13A)=
 Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C14A)=Sof(H14D)=Sof(H14E)=
 Sof(H14F)=1-FVAR(2)
 Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13)=Sof(C14)=
 Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(2)
 Sof(H63C)=Sof(H63D)=Sof(H65D)=Sof(H65E)=Sof(H65F)=Sof(H66D)=Sof(H66E)=
 Sof(H66F)=Sof(C64A)=Sof(H64A)=1-FVAR(3)
 Sof(H63A)=Sof(H63B)=Sof(C64)=Sof(H64)=Sof(H65A)=Sof(H65B)=Sof(H65C)=Sof(H66A)=
 Sof(H66B)=Sof(H66C)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C5(H5A), C5(H5B), C13(H13), C64(H64), C13A(H13A), C64A(H64A)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C11(H11A,H11B), C11(H11C,H11D), C12(H12A,H12B),
 C17(H17A,H17B), C20(H20A,H20B), C25(H25A,H25B), C28(H28A,H28B), C31(H31A,H31B),
  C36(H36A,H36B), C39(H39A,H39B), C42(H42A,H42B), C47(H47A,H47B), C50(H50A,
 H50B), C53(H53A,H53B), C58(H58A,H58B), C61(H61A,H61B), C62(H62A,H62B),
 C63(H63C,H63D), C63(H63A,H63B), C12A(H12C,H12D)
5.c Me refined with riding coordinates:
 C65(H65A,H65B,H65C), C65(H65D,H65E,H65F), C66(H66A,H66B,H66C), C66(H66D,H66E,
 H66F)
5.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C22(H22), C27(H27), C33(H33), C38(H38), C44(H44), C49(H49),
 C55(H55), C60(H60)
5.e X=CH2 refined with riding coordinates:
 N3(H3C,H3D)
5.f Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C21(H21A,H21B,H21C), C26(H26A,H26B,H26C), C32(H32A,H32B,H32C), C37(H37A,H37B,
 H37C), C43(H43A,H43B,H43C), C48(H48A,H48B,H48C), C54(H54A,H54B,H54C), C59(H59A,
 H59B,H59C), C6A(H6AA,H6AB,H6AC), C15A(H15D,H15E,H15F), C14A(H14D,H14E,H14F),
 C7A(H7AA,H7AB,H7AC)
;
_shelx_res_checksum              94531
_shelx_hkl_checksum              51561
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'