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_7126956
_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         'C H Cl3, C130 H156 N4 O28, 2(C24 H26 N4 O12)'
_chemical_formula_sum            'C179 H209 Cl3 N12 O52'
_chemical_formula_weight         3466.92
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-23
_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                90
_cell_angle_beta                 101.290(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.5752(15)
_cell_length_b                   33.8217(17)
_cell_length_c                   22.6177(14)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.03
_cell_measurement_theta_min      2.46
_cell_volume                     17685.3(18)
_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 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0667
_diffrn_reflns_av_unetI/netI     0.0660
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            152230
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.391
_diffrn_reflns_theta_min         2.223
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1553 before and 0.0612 after correction.
The Ratio of minimum to maximum transmission is 0.9345.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       needle
_exptl_crystal_F_000             7336
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.135
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.072
_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     2231
_refine_ls_number_reflns         36072
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1179
_refine_ls_R_factor_gt           0.0756
_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^)+(0.1142P)^2^+15.5774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2027
_refine_ls_wR_factor_ref         0.2322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23062
_reflns_number_total             36072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04375c2.cif
_cod_data_source_block           190419_wk_r2_0ma
_cod_depositor_comments
'Adding full bibliography for 7126956--7126957.cif.'
_cod_database_code               7126956
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.936
_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. Rigid bond restraints
 O21, C85
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O26, C114, C115, C116
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O21 \\sim C85: within 3.8A with sigma of 0.002 and sigma for terminal atoms of
0.004
O26 \\sim C114 \\sim C115 \\sim C116: within 3.8A with sigma of 0.002 and sigma
for terminal atoms of 0.004
C32 \\sim C33: within 3.8A with sigma of 0.002 and sigma for terminal atoms of
0.004
C164 \\sim C165: within 3.8A with sigma of 0.002 and sigma for terminal atoms
of 0.004
4.a Ternary CH refined with riding coordinates:
 C179(H179)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B), C18(H18A,H18B),
 C19(H19A,H19B), C21(H21A,H21B), C28(H28A,H28B), C29(H29A,H29B), C31(H31A,H31B),
  C32(H32A,H32B), C34(H34A,H34B), C41(H41A,H41B), C42(H42A,H42B), C44(H44A,
 H44B), C45(H45A,H45B), C47(H47A,H47B), C54(H54A,H54B), C55(H55A,H55B),
 C57(H57A,H57B), C58(H58A,H58B), 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(H10D,H10E), C102(H10F,H10G), C104(H10K,H10L), C111(H11A,H11B),
 C112(H11C,H11D), C114(H11H,H11I), C115(H11J,H11K), C117(H11O,H11P), C124(H12A,
 H12B), C125(H12C,H12D), C127(H12H,H12I), C128(H12J,H12K), C130(H13A,H13B),
 C138(H13C,H13D), C139(H13E,H13F), C140(H14A,H14B), C141(H14C,H14D), C142(H14E,
 H14F), C143(H14G,H14H), C144(H14I,H14J), C145(H14K,H14L), C146(H14M,H14N),
 C147(H14O,H14P), C162(H16C,H16D), C163(H16E,H16F), C164(H16G,H16H), C165(H16I,
 H16J), C166(H16K,H16L), C167(H16M,H16N), C168(H16O,H16P), C169(H16Q,H16R),
 C170(H17D,H17E), C171(H17F,H17G)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C10(H10), C13(H13), C23(H23), C26(H26), C36(H36), C39(H39),
 C49(H49), C52(H52), C62(H62), C65(H65), C67(H67), C70(H70), C74(H74), C77(H77),
  C80(H80), C83(H83), C93(H93), C96(H96), C106(H106), C109(H109), C119(H119),
 C122(H122), C131(H131), C133(H133), C135(H135), C150(H150), C152(H152),
 C154(H154), C155(H155), C157(H157), C159(H159), C178(H178), C176(H176),
 C174(H174)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C30(H30A,H30B,H30C), C33(H33A,H33B,
 H33C), C43(H43A,H43B,H43C), C46(H46A,H46B,H46C), C56(H56A,H56B,H56C), C59(H59A,
 H59B,H59C), C87(H87A,H87B,H87C), C90(H90A,H90B,H90C), C100(H10A,H10B,H10C),
 C103(H10H,H10I,H10J), C113(H11E,H11F,H11G), C116(H11L,H11M,H11N), C126(H12E,
 H12F,H12G), C129(H12L,H12M,H12N)
;
_shelx_res_checksum              1576
_shelx_hkl_checksum              28774
_olex2_submission_special_instructions 'No special instructions were received'