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_4135558
_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
'2(C40 H48 O12), C8 H18 O5, 2.5(H2 O), C2 H3 N'
_chemical_formula_sum            'C90 H122 N O31.5'
_chemical_formula_weight         1721.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.637(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6204(7)
_cell_length_b                   23.4636(12)
_cell_length_c                   35.458(2)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      26.850
_cell_measurement_theta_min      2.175
_cell_volume                     9603.1(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      298.15
_diffrn_measured_fraction_theta_full 0.999
_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  0.0957
_diffrn_reflns_av_unetI/netI     0.0963
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            89847
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.527
_diffrn_reflns_theta_min         1.966
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1285 before and 0.0688 after correction. The Ratio of minimum to maximum transmission is 0.9065. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       block
_exptl_crystal_F_000             3684
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.099
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1215
_refine_ls_number_reflns         22028
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1583
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1151P)^2^+8.5242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2160
_refine_ls_wR_factor_ref         0.2659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11255
_reflns_number_total             22028
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c12685_si_004.cif
_cod_data_source_block           20191224hb1_sq
_cod_original_cell_volume        9603.0(10)
_cod_original_formula_sum        'C90 H122 N O31.50'
_cod_database_code               4135558
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.989
_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, All O(H,H) groups
2. Restrained distances
 C89-C78 = C85-C78 = C86-C83 = C93-C90 = C92-C91 = C88-C84
 1.54 with sigma of 0.01
 O30-C85 = O29-C89 = O30-C86 = O29-C93 = O27-C83 = O32-C90 = O32-C91 = O27-C84
 = O28-C92 = O31-C88
 1.43 with sigma of 0.01
 C85-C86 \\sim C89-C93
 with sigma of 0.02
 O30-C83 \\sim O29-C90
 with sigma of 0.02
 C86-O27 \\sim C93-O32
 with sigma of 0.02
 C83-C91 \\sim C90-C84
 with sigma of 0.02
 O32-C92 \\sim O27-C88
 with sigma of 0.02
 C91-O28 \\sim C84-O31
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C88) = Uanis(C92)
Uanis(O31) = Uanis(O28)
4. Rigid body (RIGU) restrains
 O26, O23, C78, C80, C89, C81, O29, C93, C90, O32, C91, C92, O28
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C68, C82, C87
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C68, C94, C95
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O26, O23, C78, C80, C85, C81, O30, C86, C83, O27, C84, C88, O31
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(H68C)=Sof(H68D)=Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(C95)=Sof(H95A)=Sof(H95B)=
 Sof(H95C)=Sof(O27)=Sof(O30)=Sof(O31)=Sof(H31)=Sof(H78C)=Sof(H78D)=Sof(C83)=
 Sof(H83A)=Sof(H83B)=Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(C85)=Sof(H85A)=Sof(H85B)=
 Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(C88)=Sof(H88A)=Sof(H88B)=1-FVAR(1)
 Sof(H68A)=Sof(H68B)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(C87)=Sof(H87A)=Sof(H87B)=
 Sof(H87C)=Sof(O28)=Sof(H28)=Sof(O29)=Sof(O32)=Sof(H78A)=Sof(H78B)=Sof(C89)=
 Sof(H89A)=Sof(H89B)=Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(C91)=Sof(H91A)=Sof(H91B)=
 Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(C93)=Sof(H93A)=Sof(H93B)=FVAR(1)
 Fixed Sof: O0AA(0.5) H0AA(0.5) H0AB(0.5)
6.a Riding coordinates:
 O1(H1), O6(H6), O14(H14), O19(H19A), O20(H20), O3(H3), O5(H5), O9(H9),
 O31(H31), O33(H33C,H33D), O34(H34A,H34B), O0AA(H0AA,H0AB)
6.b Ternary CH refined with riding coordinates:
 C9(H9A), C35(H35), C42(H42), C61(H61), C19(H19), C34(H34), C43(H43), C45(H45)
6.c Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C33(H33A,H33B), C48(H48A,H48B), C52(H52A,H52B), C57(H57A,
 H57B), C58(H58A,H58B), C67(H67A,H67B), C75(H75A,H75B), C32(H32A,H32B),
 C46(H46A,H46B), C49(H49A,H49B), C53(H53A,H53B), C60(H60A,H60B), C65(H65A,H65B),
  C68(H68A,H68B), C68(H68C,H68D), C82(H82A,H82B), C94(H94A,H94B), C78(H78C,
 H78D), C78(H78A,H78B), C80(H80A,H80B), C81(H81A,H81B), C83(H83A,H83B),
 C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C88(H88A,H88B), C89(H89A,H89B),
  C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B), C93(H93A,H93B)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3A), C24(H24A), C40(H40), C50(H50), C5(H5A), C10(H10), C12(H12A), C26(H26)
6.e Idealised Me refined as rotating group:
 C69(H69A,H69B,H69C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C79(H79A,H79B,
 H79C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C87(H87A,
 H87B,H87C), C95(H95A,H95B,H95C), C97(H97A,H97B,H97C)
6.f Idealised tetrahedral OH refined as rotating group:
 O8(H8), O10(H10A), O18(H18), O21(H21), O22(H22), O24(H24), O25(H25), O2(H2),
 O4(H4), O7(H7), O11(H11), O12(H12), O13(H13), O15(H15), O16(H16), O17(H17),
 O26(H26A), O28(H28)
;
_shelx_res_checksum              12031
_shelx_hkl_checksum              64282
_shelx_fab_checksum              73254
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'