Oxacalix[4]arene-bridged pillar[5]arene dimers: syntheses, planar chirality and construction of chiral rotaxanes.
Wan, Kang; Gao, Shi-Chang; Fang, Xu; Xu, Meng-Yu; Yang, Yong; Xue, Min; Chemical communications (Cambridge, England) 56 (2020) 10155–10158; doi:10.1039/d0cc04375c

data_7126957
_publ_section_title
;
 Oxacalix[4]arene-bridged pillar[5]arene dimers: syntheses, planar
 chirality and construction of chiral rotaxanes.
;
_journal_issue                   70
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10155
_journal_page_last               10158
_journal_paper_doi               10.1039/d0cc04375c
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         '2(C H Cl3), C130 H156 N4 O28'
_chemical_formula_sum            'C132 H158 Cl6 N4 O28'
_chemical_formula_weight         2461.31
_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             2019-05-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-16 deposited with the CCDC.	2020-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                85.199(2)
_cell_angle_beta                 74.810(2)
_cell_angle_gamma                83.340(2)
_cell_formula_units_Z            2
_cell_length_a                   14.4932(11)
_cell_length_b                   21.9303(16)
_cell_length_c                   24.2711(18)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.28
_cell_volume                     7383.1(10)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_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  0.0541
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            106381
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.472
_diffrn_reflns_theta_min         2.145
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0796 before and 0.0539 after correction.
The Ratio of minimum to maximum transmission is 0.8579.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_description       needle
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.103
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1546
_refine_ls_number_reflns         30148
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.0898
_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^)+(0.1659P)^2^+4.6640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2653
_refine_ls_wR_factor_ref         0.3010
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17689
_reflns_number_total             30148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04375c2.cif
_cod_data_source_block           190513_wk_005_2_0m_sq
_cod_depositor_comments
'Adding full bibliography for 7126956--7126957.cif.'
_cod_database_code               7126957
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.946
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C89-C90
 1.55 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C131(H131), C132(H132)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B),
 C14(H14A,H14B), C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B), C25(H25A,H25B),
  C27(H27A,H27B), C34(H34A,H34B), C35(H35A,H35B), C38(H38A,H38B), C40(H40A,
 H40B), C47(H47A,H47B), C48(H48A,H48B), C50(H50A,H50B), C51(H51A,H51B),
 C53(H53A,H53B), C78(H78A,H78B), C85(H85A,H85B), C86(H86A,H86B), C88(H88A,H88B),
  C89(H89A,H89B), C91(H91A,H91B), C98(H98A,H98B), C99(H99A,H99B), C101(H10G,
 H10H), C102(H10I,H10J), C104(H10N,H10O), C111(H11C,H11D), C112(H11E,H11F),
 C114(H11J,H11K), C115(H11L,H11M), C117(H11Q,H11R), C124(H12C,H12D), C125(H12E,
 H12F), C127(H12J,H12K), C128(H12L,H12M), C130(H13D,H13E)
3.c Me refined with riding coordinates:
 C23(H23A,H23B,H23C)
3.d Aromatic/amide H refined with riding coordinates:
 O25(H25), C3(H3), C6(H6), C16(H16), C19(H19), C29(H29), C32(H32), C37(H37),
 C42(H42), C45(H45), C55(H55), C58(H58), C62(H62), C65(H65), C67(H67), C70(H70),
  C73(H73), C76(H76), C81(H81), C84(H84), C94(H94), C97(H97), C107(H107),
 C110(H110), C120(H120), C123(H123)
3.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C26(H26A,H26B,H26C), C36(H36A,H36B,
 H36C), C39(H39A,H39B,H39C), C49(H49A,H49B,H49C), C52(H52A,H52B,H52C), C87(H87A,
 H87B,H87C), C90(H90A,H90B,H90C), C100(H10D,H10E,H10F), C103(H10K,H10L,H10M),
 C113(H11G,H11H,H11I), C116(H11N,H11O,H11P), C126(H12G,H12H,H12I), C129(H12N,
 H12O,H12P)
;
_shelx_res_checksum              24337
_shelx_hkl_checksum              82264
_shelx_fab_checksum              92753
_olex2_submission_special_instructions 'No special instructions were received'