Linear Positional Isomer Sorting in Nonporous Adaptive Crystals of a Pillar[5]arene.
Jie, Kecheng; Zhou, Yujuan; Li, Errui; Zhao, Run; Liu, Ming; Huang, Feihe; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.7b13156

data_4127185
_publ_section_title
;
 Linear Positional Isomer Sorting in Nonporous Adaptive Crystals of a
 Pillar[5]arene.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b13156
_journal_year                    2018
_chemical_formula_moiety         '4(C55 H70 O10), 4(C5 H10), 2(C0.5 H Cl)'
_chemical_formula_sum            'C241 H322 Cl2 O40'
_chemical_formula_weight         3929.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-29
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.8120(10)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   12.4113(3)
_cell_length_b                   23.1325(5)
_cell_length_c                   22.4665(4)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.74
_cell_measurement_theta_min      3.74
_cell_volume                     6263.7(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      173.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0944
_diffrn_reflns_av_unetI/netI     0.0474
_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       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52648
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.810
_diffrn_reflns_theta_max         66.810
_diffrn_reflns_theta_min         2.784
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.042
_exptl_crystal_F_000             2122
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         11075
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.0764
_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^)+(0.1304P)^2^+3.2920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2172
_refine_ls_wR_factor_ref         0.2538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7050
_reflns_number_total             11075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b13156_si_004.cif
_cod_data_source_block           170417zd_p5_0m
_cod_database_code               4127185
_shelx_shelxl_version_number     2014/7
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl3-Cl1 = Cl1-Cl3A
 2.8 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Cl1, Cl3, Cl3A, C61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=Sof(C56A)=Sof(H56C)=Sof(C57A)=
 Sof(H57A)=Sof(C58A)=Sof(H58A)=Sof(H58B)=Sof(C59A)=Sof(H59D)=Sof(H59E)=
 Sof(H59F)=1-FVAR(1)
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(H58)=Sof(C60)=
 Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=FVAR(1)
 Fixed Sof: Cl1(0.25) Cl3(0.125) Cl3A(0.125) C61(0.25) H61A(0.125) H61B(0.125)
 H61C(0.125) H61D(0.125)
5.a Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B), C9(H9A,H9B), C53(H53A,H53B), C50(H50A,H50B), C20(H20A,H20B),
 C5(H5A,H5B), C12(H12A,H12B), C42(H42A,H42B), C31(H31A,H31B), C23(H23A,H23B),
 C28(H28A,H28B), C34(H34A,H34B), C17(H17A,H17B), C39(H39A,H39B), C45(H45A,H45B),
  C56(H56A,H56B), C58A(H58A,H58B), C61(H61A,H61B), C61(H61C,H61D)
5.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C8(H8), C3(H3), C14(H14), C30(H30), C52(H52), C41(H41), C47(H47),
 C36(H36), C25(H25), C57(H57), C58(H58), C56A(H56C), C57A(H57A)
5.c Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C13(H13A,H13B,H13C), C51(H51A,H51B,H51C), C24(H24A,H24B,
 H24C), C6(H6A,H6B,H6C), C35(H35A,H35B,H35C), C29(H29A,H29B,H29C), C40(H40A,
 H40B,H40C), C46(H46A,H46B,H46C), C18(H18A,H18B,H18C), C60(H60A,H60B,H60C),
 C59(H59A,H59B,H59C), C60A(H60D,H60E,H60F), C59A(H59D,H59E,H59F)
;
_shelx_res_checksum              43359
_shelx_hkl_checksum              54273
_olex2_submission_special_instructions 'No special instructions were received'