Construction of pillar[4]arene[1]quinone–1,10-dibromodecane pseudorotaxanes in solution and in the solid state
Sheng, Xinru; Li, Errui; Huang, Feihe; Beilstein Journal of Organic Chemistry 16 (2020) 2954–2959; doi:10.3762/bjoc.16.245

data_4038939
_publ_section_title
;
 Construction of pillar[4]arene[1]quinone--1,10-dibromodecane
 pseudorotaxanes in solution and in the solid state
;
_journal_name_full               'Beilstein Journal of Organic Chemistry'
_journal_page_first              2954
_journal_page_last               2959
_journal_paper_doi               10.3762/bjoc.16.245
_journal_volume                  16
_journal_year                    2020
_chemical_formula_moiety         'C5 H10 Br, C51 H60 O10'
_chemical_formula_sum            'C56 H70 Br O10'
_chemical_formula_weight         983.03
_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             2018-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.8000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4426(6)
_cell_length_b                   19.3528(8)
_cell_length_c                   15.3931(4)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.35
_cell_volume                     5159.6(3)
_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 0.997
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41520
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_min         2.352
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0672 before and 0.0511 after correction.
The Ratio of minimum to maximum transmission is 0.9198.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       block
_exptl_crystal_F_000             2084
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         11778
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0638P)^2^+1.6502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1350
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8600
_reflns_number_total             11778
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1860-5397-16-245-S2.cif
_cod_data_source_block           181205_p5q_10br_0ma
_cod_database_code               4038939
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.762
_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.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,
 H56B), C1(H1A,H1B), C8(H8A,H8B), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,
 H19B), C26(H26A,H26B), C28(H28A,H28B), C30(H30A,H30B), C37(H37A,H37B),
 C39(H39A,H39B), C41(H41A,H41B), C48(H48A,H48B), C50(H50A,H50B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C10(H10), C13(H13), C21(H21), C24(H24), C32(H32), C35(H35),
 C43(H43), C46(H46)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C29(H29A,H29B,
 H29C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C49(H49A,H49B,H49C), C51(H51A,
 H51B,H51C)
;
_shelx_res_checksum              77300
_shelx_hkl_checksum              63852
_olex2_submission_special_instructions 'No special instructions were received'