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_4133456
_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         'C57 H74 N2 O10, C3 H9 N O0.5'
_chemical_formula_sum            'C60 H83 N3 O10.5'
_chemical_formula_weight         1014.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 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                90
_cell_angle_beta                 94.868(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.251(2)
_cell_length_b                   12.4803(13)
_cell_length_c                   25.254(3)
_cell_measurement_reflns_used    3273
_cell_measurement_temperature    154.7
_cell_measurement_theta_max      29.2711
_cell_measurement_theta_min      2.9345
_cell_volume                     5731.6(11)
_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      154.7
_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  -61.00   34.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7808  -38.0000  -30.0000 95

  2 omega  -15.00   81.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7808   38.0000  150.0000 96
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0019752000
_diffrn_orient_matrix_UB_12      -0.0178212000
_diffrn_orient_matrix_UB_13      -0.0265363000
_diffrn_orient_matrix_UB_21      0.0283358000
_diffrn_orient_matrix_UB_22      0.0377108000
_diffrn_orient_matrix_UB_23      -0.0033461000
_diffrn_orient_matrix_UB_31      0.0267032000
_diffrn_orient_matrix_UB_32      -0.0385829000
_diffrn_orient_matrix_UB_33      0.0089589000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.1129
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22605
_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         2.940
_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  0.81185
_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    1.175
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.061
_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     705
_refine_ls_number_reflns         10434
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.2155
_refine_ls_R_factor_gt           0.1157
_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^)+(0.1113P)^2^+11.8485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2672
_refine_ls_wR_factor_ref         0.3411
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4665
_reflns_number_total             10434
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10192_si_002.cif
_cod_data_source_block           171115_ler_p5q_c3n
_cod_original_cell_volume        5731.5(11)
_cod_original_formula_sum        'C60 H83 N3 O10.50'
_cod_database_code               4133456
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H N O'
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.972
_reflns_odcompleteness_completeness 99.43
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C58A-N3A
 1.53 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N3A \\sim N3 \\sim C58 \\sim C59 \\sim C60: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
N3A \\sim N3 \\sim C58 \\sim C58A \\sim C59A \\sim C59 \\sim C60: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H60D)=Sof(H60E)=Sof(H60F)=Sof(N3A)=Sof(H3AA)=Sof(H11)=Sof(C59A)=Sof(H59C)=
 Sof(H59D)=Sof(C58A)=Sof(H58C)=Sof(H58D)=1-FVAR(1)
 Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(N3)=Sof(H3A)=Sof(H3B)=Sof(C58)=Sof(H58A)=
 Sof(H58B)=Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(1)
 Fixed Sof: O11(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C54(H54A,H54B), C36(H36A,H36B), C47(H47A,H47B), C14(H14A,H14B),
 C25(H25A,H25B), C34(H34A,H34B), C8(H8A,H8B), C43(H43A,H43B), C9(H9A,H9B),
 C56(H56A,H56B), C11(H11A,H11B), C32(H32A,H32B), C21(H21A,H21B), C45(H45A,H45B),
  C12(H12A,H12B), C23(H23A,H23B), C59(H59A,H59B), C58(H58A,H58B), C59A(H59C,
 H59D), C58A(H58C,H58D)
5.b Me refined with riding coordinates:
 C60(H60A,H60B,H60C), C60(H60D,H60E,H60F)
5.c Aromatic/amide H refined with riding coordinates:
 C52(H52), N1(H1), C41(H41), C49(H49), N2(H2), C38(H38), C16(H16), C27(H27),
 C30(H30), C19(H19)
5.d X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N3A(H3AA,H11)
5.e Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C55(H55A,H55B,H55C), C44(H44A,H44B,H44C), C33(H33A,H33B,
 H33C), C46(H46A,H46B,H46C), C10(H10A,H10B,H10C), C35(H35A,H35B,H35C), C13(H13A,
 H13B,H13C), C24(H24A,H24B,H24C), C57(H57A,H57B,H57C)
;
_shelx_res_checksum              20324
_shelx_hkl_checksum              28945
_olex2_submission_special_instructions 'No special instructions were received'