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_4135557
_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(C6 H14 O4)'
_chemical_formula_sum            'C52 H76 O20'
_chemical_formula_weight         1021.12
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-03-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                103.460(2)
_cell_angle_beta                 101.469(2)
_cell_angle_gamma                91.663(2)
_cell_formula_units_Z            4
_cell_length_a                   13.0619(12)
_cell_length_b                   17.9017(17)
_cell_length_c                   22.873(2)
_cell_measurement_reflns_used    9652
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      31.72
_cell_measurement_theta_min      2.31
_cell_volume                     5081.7(8)
_computing_cell_refinement       'Bruker Apex3 V.2016.9-0/SAINT V8.37A'
_computing_data_collection       'Bruker Apex3 V.2016.9-0'
_computing_data_reduction        'Bruker Apex3 V.2016.9-0/SAINT V8.37A'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            227305
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.823
_diffrn_reflns_theta_min         1.173
_diffrn_source                   'Sealed Source Mo with TRIUMPH optics'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.7159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1433
_refine_ls_number_reflns         34510
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0808P)^2^+3.6549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25749
_reflns_number_total             34510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c12685_si_003.cif
_cod_data_source_block           s1
_cod_original_cell_volume        5081.6(8)
_cod_database_code               4135557
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.953
_olex2_refinement_description
;
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, All O(H) groups
2. Restrained distances
 O4C-H4C
 0.98 with sigma of 0.02
 H4C-O3F
 1.78 with sigma of 0.02
 C1-C3
 1.54 with sigma of 0.02
 C35A-C3
 1.54 with sigma of 0.02
3. Others
 Fixed Sof: O1F(0.6) O1F'(0.4) O2F(0.6) O2F'(0.4) O4F(0.667) O4F'(0.333)
 H1FA(0.6) H1FB(0.6) H1FC(0.4) H1FD(0.4) C2F(0.6) H2FA(0.6) H2FB(0.6) C2F'(0.4)
 H2FC(0.4) H2FD(0.4) H3FA(0.6) H3FB(0.6) H3FC(0.4) H3FD(0.4) H5FA(0.667)
 H5FB(0.667) H5FC(0.333) H5FD(0.333) C6F(0.667) H6FA(0.667) H6FB(0.667)
 C6F'(0.333) H6FC(0.333) H6FD(0.333) H30C(0.667) H30D(0.667) H30E(0.333)
 H30F(0.333) C31'(0.333) H31D(0.333) H31E(0.333) H31F(0.333) C31B(0.667)
 H31G(0.667) H31H(0.667) H31I(0.667) H35A(0.85) H35B(0.85) H35C(0.15)
 H35D(0.15) C36A(0.85) H36A(0.85) H36B(0.85) C37A(0.85) H37A(0.85) H37B(0.85)
 H37C(0.85) C1(0.15) H1B(0.15) H1C(0.15) H1D(0.15) C3(0.15) H3B(0.15) H3C(0.15)
4.a Ternary CH refined with riding coordinates:
 C7A(H7AA), C7B(H7BA), C14A(H14A), C14B(H14B), C21A(H21A), C21B(H21B),
 C28A(H28A), C28B(H28B)
4.b Secondary CH2 refined with riding coordinates:
 C1C(H1CB,H1CC), C1D(H1DB,H1DC), C1E(H1EA,H1EB), C1F(H1FA,H1FB), C1F(H1FC,
 H1FD), C2C(H2CA,H2CB), C2D(H2DA,H2DB), C2E(H2EA,H2EB), C2F(H2FA,H2FB),
 C2F'(H2FC,H2FD), C3C(H3CA,H3CB), C3D(H3DA,H3DB), C3E(H3EA,H3EB), C3F(H3FA,
 H3FB), C3F(H3FC,H3FD), C4C(H4CA,H4CB), C4D(H4DA,H4DB), C4E(H4EA,H4EB),
 C4F(H4FA,H4FB), C5C(H5CA,H5CB), C5D(H5DA,H5DB), C5E(H5EA,H5EB), C5F(H5FA,H5FB),
  C5F(H5FC,H5FD), C6C(H6CA,H6CB), C6D(H6DA,H6DB), C6E(H6EA,H6EB), C6F(H6FA,
 H6FB), C6F'(H6FC,H6FD), C29A(H29A,H29B), C29B(H29C,H29D), C30A(H30A,H30B),
 C30B(H30C,H30D), C30B(H30E,H30F), C32A(H32A,H32B), C32B(H32C,H32D), C33A(H33A,
 H33B), C33B(H33C,H33D), C35A(H35A,H35B), C35A(H35C,H35D), C35B(H35E,H35F),
 C36A(H36A,H36B), C36B(H36C,H36D), C38A(H38A,H38B), C38B(H38C,H38D), C39A(H39A,
 H39B), C39B(H39C,H39D), C3(H3B,H3C)
4.c Me refined with riding coordinates:
 C1(H1B,H1C,H1D)
4.d Aromatic/amide H refined with riding coordinates:
 C5A(H5AA), C5B(H5BA), C13A(H13A), C13B(H13B), C20A(H20A), C20B(H20B),
 C27A(H27A), C27B(H27B)
4.e Idealised Me refined as rotating group:
 C31'(H31D,H31E,H31F), C31A(H31A,H31B,H31C), C31B(H31G,H31H,H31I), C34A(H34A,
 H34B,H34C), C34B(H34D,H34E,H34F), C37A(H37A,H37B,H37C), C37B(H37D,H37E,H37F),
 C40A(H40A,H40B,H40C), C40B(H40D,H40E,H40F)
;
_shelx_res_checksum              69228
_shelx_hkl_checksum              954
_olex2_submission_special_instructions 'No special instructions were received'