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_4133458
_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         'C59 H78 N2 O10, O, C4 H11 N'
_chemical_formula_sum            'C63 H89 N3 O11'
_chemical_formula_weight         1064.37
_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
_audit_creation_date             2017-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                96.046(4)
_cell_angle_beta                 101.187(4)
_cell_angle_gamma                114.345(5)
_cell_formula_units_Z            2
_cell_length_a                   12.2429(6)
_cell_length_b                   12.5858(7)
_cell_length_c                   22.1870(9)
_cell_measurement_reflns_used    4744
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      29.3859
_cell_measurement_theta_min      2.9892
_cell_volume                     2989.2(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -74.00   20.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6246  -77.0000  -90.0000 94

  2 omega  -62.00   38.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9371  -38.0000   30.0000 100

  3 omega  -13.00   76.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9371   38.0000 -150.0000 89
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0641382000
_diffrn_orient_matrix_UB_12      0.0328865000
_diffrn_orient_matrix_UB_13      0.0022161000
_diffrn_orient_matrix_UB_21      -0.0112886000
_diffrn_orient_matrix_UB_22      0.0469239000
_diffrn_orient_matrix_UB_23      -0.0102599000
_diffrn_orient_matrix_UB_31      0.0100352000
_diffrn_orient_matrix_UB_32      0.0267360000
_diffrn_orient_matrix_UB_33      0.0316152000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18972
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.995
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92122
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       plate
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.394
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         10886
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.0792
_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^)+(0.1218P)^2^+2.9039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2139
_refine_ls_wR_factor_ref         0.2472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7544
_reflns_number_total             10886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10192_si_003.cif
_cod_data_source_block           170929_ler_p5q_41
_cod_database_code               4133458
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'c h n o p f'
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.963
_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 N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C63-C62 = C62-C61 = C61-C60 = N3-C60
 1.53 with sigma of 0.01
 C63-C61
 2.53 with sigma of 0.02
 C62-C60
 2.53 with sigma of 0.01
 C61-N3
 2.53 with sigma of 0.02
3. Others
 Fixed Sof: O11(0.5) O12(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B), C23(H23A,H23B), C25(H25A,H25B),
  C27(H27A,H27B), C34(H34A,H34B), C36(H36A,H36B), C38(H38A,H38B), C45(H45A,
 H45B), C47(H47A,H47B), C49(H49A,H49B), C56(H56A,H56B), C58(H58A,H58B),
 C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C19(H19), C22(H22), C30(H30), C33(H33), C41(H41), C44(H44),
 C52(H52), C55(H55)
4.c X=CH2 refined with riding coordinates:
 N3(H3A,H3B)
4.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C46(H46A,H46B,H46C), C48(H48A,
 H48B,H48C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C63(H63A,H63B,H63C)
;
_shelx_res_checksum              84139
_shelx_hkl_checksum              28303
_olex2_submission_special_instructions 'No special instructions were received'