Molecular Entrapment of Polymers by Pyrogallol[4]arenes.
Shao, Li; Zhang, Hanwen; He, Xiaoqing; Hua, Bin; Hu, Xiangquan; Wan, Caixia; Kelley, Steven P.; Atwood, Jerry L.; Journal of the American Chemical Society 143 (2021) 693–698; doi:10.1021/jacs.0c12685

data_4135559
_publ_section_title
;
 Molecular Entrapment of Polymers by Pyrogallol[4]arenes.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              693
_journal_page_last               698
_journal_paper_doi               10.1021/jacs.0c12685
_journal_volume                  143
_journal_year                    2021
_chemical_formula_moiety         'C40 H48 O12, 2(C2 H6 O2), H O0.5'
_chemical_formula_sum            'C44 H61 O16.5'
_chemical_formula_weight         853.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-06-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 119.415(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   45.4178(15)
_cell_length_b                   9.3163(3)
_cell_length_c                   23.3301(9)
_cell_measurement_reflns_used    9766
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      73.86
_cell_measurement_theta_min      3.79
_cell_volume                     8599.0(5)
_computing_cell_refinement       'Bruker Apex3 V.2018.1-0/SAINT V8.38A'
_computing_data_collection       'Bruker Apex3 V.2018.1-0'
_computing_data_reduction        'Bruker Apex3 V.2018.1-0/SAINT V8.38A'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            105124
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.310
_diffrn_reflns_theta_min         3.790
_diffrn_source                   'Incoatec IMuS microfocus Cu tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.838
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.6718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       block
_exptl_crystal_F_000             3656
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         8569
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0681
_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^)+(0.0812P)^2^+34.5063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1793
_refine_ls_wR_factor_ref         0.1827
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7829
_reflns_number_total             8569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c12685_si_002.cif
_cod_data_source_block           s1
_cod_original_formula_sum        'C44 H61 O16.50'
_cod_database_code               4135559
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.793
_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, All O(H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C28(H28), C21(H21), C14(H14), C7(H7A)
2.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C38(H38A,H38B), C32(H32A,H32B), C35(H35A,H35B), C39(H39A,
 H39B), C4S(H4SA,H4SB), C30(H30A,H30B), C36(H36A,H36B), C33(H33A,H33B),
 C3S(H3SA,H3SB), C2S(H2SA,H2SB), C1S(H1SA,H1SB)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5A), C20(H20), C13(H13), C27(H27)
2.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C37(H37A,H37B,H37C), C40(H40A,H40B,H40C), C31(H31A,H31B,
 H31C)
;
_shelx_res_checksum              27158
_shelx_hkl_checksum              86919
_olex2_submission_special_instructions 'No special instructions were received'