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_4133455
_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 N'
_chemical_formula_sum            'C66 H82 N3 O10'
_chemical_formula_weight         1077.34
_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             2017-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                97.674(5)
_cell_angle_beta                 99.394(5)
_cell_angle_gamma                113.819(6)
_cell_formula_units_Z            2
_cell_length_a                   12.4803(8)
_cell_length_b                   13.1925(9)
_cell_length_c                   22.0752(12)
_cell_measurement_reflns_used    4050
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      29.3453
_cell_measurement_theta_min      3.1743
_cell_volume                     3199.3(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -74.00   22.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6246  -77.0000   90.0000 96

  2 omega  -38.00   63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6246   77.0000 -150.0000 101

  3 omega  -45.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6246   77.0000  -30.0000 85
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0280352000
_diffrn_orient_matrix_UB_12      -0.0156739000
_diffrn_orient_matrix_UB_13      -0.0326144000
_diffrn_orient_matrix_UB_21      -0.0574762000
_diffrn_orient_matrix_UB_22      -0.0194408000
_diffrn_orient_matrix_UB_23      0.0070540000
_diffrn_orient_matrix_UB_31      0.0022213000
_diffrn_orient_matrix_UB_32      0.0548431000
_diffrn_orient_matrix_UB_33      0.0012878000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20196
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.371
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       block
_exptl_crystal_F_000             1158
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         11621
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1462
_refine_ls_R_factor_gt           0.0907
_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^)+(0.1823P)^2^+0.4120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2591
_refine_ls_wR_factor_ref         0.3215
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6338
_reflns_number_total             11621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10192_si_005.cif
_cod_data_source_block           171110_ler_p5q_c5n
_cod_database_code               4133455
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H O N'
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.964
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 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 = C64-C63 = C65-C64 = C66-C65
 1.53 with sigma of 0.02
 C62-C64
 2.53 with sigma of 0.04
 C63-C65
 2.53 with sigma of 0.04
 C64-C66
 2.53 with sigma of 0.04
 C16-C15 \\sim C17-C16
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C8 \\sim C9 \\sim C10 \\sim C10A \\sim C11A \\sim C11 \\sim C12: within 3.8A
with sigma of 0.01 and sigma for terminal atoms of 0.02
N3 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
C14 \\sim C15 \\sim C16 \\sim C17: within 3.8A with sigma of 0.04 and sigma for
terminal atoms of 0.08
4. Others
 Sof(H9BC)=Sof(H9BD)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C11A)=Sof(H11C)=
 Sof(H11D)=Sof(C10A)=Sof(H10C)=Sof(H10D)=1-FVAR(1)
 Sof(H9AA)=Sof(H9AB)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C10)=Sof(H10A)=
 Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C1(H1A,H1B), C40(H40A,H40B), C47(H47A,H47B), C29(H29A,H29B),
 C18(H18A,H18B), C58(H58A,H58B), C38(H38A,H38B), C60(H60A,H60B), C8(H8A,H8B),
 C36(H36A,H36B), C13(H13A,H13B), C49(H49A,H49B), C14(H14A,H14B), C9(H9AA,H9AB),
 C9(H9BC,H9BD), C27(H27A,H27B), C25(H25A,H25B), C15(H15A,H15B), C10(H10A,H10B),
 C11(H11A,H11B), C16(H16A,H16B), C11A(H11C,H11D), C10A(H10C,H10D)
5.b Aromatic/amide H refined with riding coordinates:
 C53(H53), C45(H45), C42(H42), C34(H34), C31(H31), C20(H20), C23(H23),
 C56(H56), N2(H2), N1(H1)
5.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C39(H39A,H39B,H39C), C59(H59A,H59B,H59C), C50(H50A,H50B,
 H50C), C37(H37A,H37B,H37C), C26(H26A,H26B,H26C), C61(H61A,H61B,H61C), C12(H12A,
 H12B,H12C), C12(H12D,H12E,H12F), C28(H28A,H28B,H28C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              8946
_shelx_hkl_checksum              98150
_olex2_submission_special_instructions 'No special instructions were received'