Pillar[5]arene-Based Molecular Recognition Induced Crystal-to-Crystal Transformation and Its Application in Adsorption of Adiponitrile in Water
Shi, Bingbing; Shangguan, Liqing; Wang, Huanhuan; Zhu, Huangtianzhi; Xing, Hao; Liu, Peiren; Liu, Yuezhou; Liu, Jiyong; Huang, Feihe; ACS Materials Letters 1 (2019) 111–; doi:10.1021/acsmaterialslett.9b00163

data_4515190
_publ_section_title
;
 Pillar[5]arene-Based Molecular Recognition Induced Crystal-to-Crystal
 Transformation and Its Application in Adsorption of Adiponitrile in Water
;
_journal_issue                   1
_journal_name_full               'ACS Materials Letters'
_journal_page_first              111
_journal_paper_doi               10.1021/acsmaterialslett.9b00163
_journal_volume                  1
_journal_year                    2019
_chemical_formula_moiety         '2(C75 H82 O14), 5(C2 N)'
_chemical_formula_sum            'C160 H164 N5 O28'
_chemical_formula_weight         2604.95
_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     direct
_audit_creation_date             2018-05-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                83.814(5)
_cell_angle_beta                 74.318(5)
_cell_angle_gamma                87.882(5)
_cell_formula_units_Z            1
_cell_length_a                   11.7229(7)
_cell_length_b                   16.0910(8)
_cell_length_c                   19.5838(11)
_cell_measurement_reflns_used    4647
_cell_measurement_temperature    149.8
_cell_measurement_theta_max      29.3786
_cell_measurement_theta_min      3.3343
_cell_volume                     3535.8(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      149.8
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -88.00   12.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6246  -38.0000  -60.0000 100

  2 omega  -39.00   57.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6246   77.0000   90.0000 96

  3 omega  -18.00   82.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9371   77.0000 -120.0000 100
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0190258000
_diffrn_orient_matrix_UB_12      -0.0420481000
_diffrn_orient_matrix_UB_13      0.0048839000
_diffrn_orient_matrix_UB_21      -0.0357999000
_diffrn_orient_matrix_UB_22      -0.0033892000
_diffrn_orient_matrix_UB_23      0.0357152000
_diffrn_orient_matrix_UB_31      -0.0480219000
_diffrn_orient_matrix_UB_32      -0.0136576000
_diffrn_orient_matrix_UB_33      -0.0114248000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23642
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.341
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90435
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       block
_exptl_crystal_F_000             1383
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         12902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0719
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1066P)^2^+2.0201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1887
_refine_ls_wR_factor_ref         0.2299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7951
_reflns_number_total             12902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tz9b00163_si_002.cif
_cod_data_source_block           180516_sbb_171122_1
_cod_database_code               4515190
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'c h n o'
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.960
_reflns_odcompleteness_completeness 99.54
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C65A)=Sof(H65D)=Sof(H65E)=Sof(H65F)=1-FVAR(1)
 Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=FVAR(1)
 Fixed Sof: C80(0.5) N3(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C1(H1A,H1B), C49(H49A,H49B), C24(H24A,H24B), C26(H26A,H26B),
 C27(H27A,H27B), C25(H25A,H25B), C67(H67A,H67B), C58(H58A,H58B), C9(H9A,H9B),
 C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C38(H38A,H38B), C22(H22A,H22B)
3.b Aromatic/amide H refined with riding coordinates:
 C46(H46), C7(H7), C70(H70), C43(H43), C4(H4), C52(H52), C73(H73), C61(H61),
 C55(H55), C64(H64), C29(H29), C13(H13), C14(H14), C30(H30), C18(H18), C15(H15),
  C34(H34), C19(H19), C20(H20), C35(H35), C31(H31), C36(H36)
3.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C56(H56A,H56B,H56C), C75(H75A,H75B,H75C), C47(H47A,H47B,
 H47C), C74(H74A,H74B,H74C), C66(H66A,H66B,H66C), C57(H57A,H57B,H57C), C23(H23A,
 H23B,H23C), C65(H65A,H65B,H65C), C39(H39A,H39B,H39C), C65A(H65D,H65E,H65F)
;
_shelx_res_checksum              43178
_shelx_hkl_checksum              79668
_olex2_submission_special_instructions 'No special instructions were received'