Construction of [2]pseudorotaxane and [3]pseudorotaxane based on perbromoethylated pillar[5]arene/pyridinium iodide ion-pair recognition
Shao, Li; Hua, Bin; Liu, Jiyong; Huang, Feihe; Chemical Communications  (2019) –; doi:10.1039/C9CC01984G

data_7123176
_publ_section_title
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 Construction of [2]pseudorotaxane and [3]pseudorotaxane based on
 perbromoethylated pillar[5]arene/pyridinium iodide ion-pair recognition
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC01984G
_journal_year                    2019
_chemical_formula_moiety         'I, C55 H60 Br10 O10, C7 H10 N'
_chemical_formula_sum            'C62 H70 Br10 I N O10'
_chemical_formula_weight         1915.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-01 deposited with the CCDC.    2019-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.527(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9329(4)
_cell_length_b                   25.2167(8)
_cell_length_c                   21.2593(7)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.20
_cell_measurement_theta_min      2.26
_cell_volume                     6888.3(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      170.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1333
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            137005
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.399
_diffrn_reflns_theta_min         2.263
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.320
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1129 before and 0.0637 after correction.
The Ratio of minimum to maximum transmission is 0.6886.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_description       block
_exptl_crystal_F_000             3728
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.029
_refine_diff_density_min         -1.217
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         14115
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1641
_refine_ls_R_factor_gt           0.0892
_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^)+(0.0892P)^2^+60.1102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2083
_refine_ls_wR_factor_ref         0.2511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7639
_reflns_number_total             14115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01984g2.cif
_cod_data_source_block           181023_sl_2_0m
_cod_database_code               7123176
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.518
_shelx_estimated_absorpt_t_min   0.237
_olex2_refinement_description
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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. Uiso/Uaniso restraints and constraints
C43 \\sim C44A \\sim C44: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
3. Others
 Sof(H43C)=Sof(H43D)=Sof(Br8A)=Sof(C44A)=Sof(H44C)=Sof(H44D)=1-FVAR(1)
 Sof(Br8)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=FVAR(1)
 Sof(H22C)=Sof(H22D)=Sof(Br4A)=1-FVAR(2)
 Sof(Br4)=Sof(H22A)=Sof(H22B)=FVAR(2)
 Sof(H33C)=Sof(H33D)=Sof(Br6A)=1-FVAR(3)
 Sof(Br6)=Sof(H33A)=Sof(H33B)=FVAR(3)
 Sof(H31C)=Sof(H31D)=Sof(Br5A)=1-FVAR(4)
 Sof(Br5)=Sof(H31A)=Sof(H31B)=FVAR(4)
4.a Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C45(H45A,H45B), C23(H23A,H23B), C12(H12A,H12B), C1(H1A,H1B),
 C30(H30A,H30B), C01P(H01A,H01B), C8(H8A,H8B), C10(H10A,H10B), C01X(H01C,H01D),
 C31(H31A,H31B), C31(H31C,H31D), C32(H32A,H32B), C21(H21A,H21B), C19(H19A,H19B),
  C9(H9A,H9B), C41(H41A,H41B), C22(H22A,H22B), C22(H22C,H22D), C11(H11A,H11B),
 C43(H43A,H43B), C43(H43C,H43D), C33(H33A,H33B), C33(H33C,H33D), C20(H20A,H20B),
  C02A(H02A,H02B), C42(H42A,H42B), C1AA(H1AA,H1AB), C44(H44A,H44B), C44A(H44C,
 H44D)
4.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C28(H28), C14(H14), C3(H3), C25(H25), C016(H016), C36(H36),
 C39(H39), C6(H6), C01M(H01M), C50(H50), C46(H46), C47(H47), C49(H49)
4.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C51(H51A,H51B,H51C)
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_shelx_res_checksum              88573
_olex2_submission_special_instructions 'No special instructions were received'