Assembly of a Porous Supramolecular Polyknot from Rigid Trigonal Prismatic Building Blocks.
Li, Penghao; Chen, Zhijie; Ryder, Matthew R.; Stern, Charlotte L.; Guo, Qing-Hui; Wang, Xingjie; Farha, Omar K.; Stoddart, J. Fraser; Journal of the American Chemical Society 141 (2019) 12998–13002; doi:10.1021/jacs.9b06445

data_4127833
_publ_section_title
;
 Assembly of a Porous Supramolecular Polyknot from Rigid Trigonal
 Prismatic Building Blocks.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12998
_journal_page_last               13002
_journal_paper_doi               10.1021/jacs.9b06445
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C110 H62 O12'
_chemical_formula_sum            'C110 H62 O12'
_chemical_formula_weight         1575.59
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_space_group_name_H-M_alt        'P -6 2 c'
_symmetry_space_group_name_Hall  'P -6c -2c'
_symmetry_space_group_name_H-M   'P -6 2 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   37.888(2)
_cell_length_b                   37.888(2)
_cell_length_c                   54.616(4)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      48.459
_cell_measurement_theta_min      2.693
_cell_volume                     67898(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      250.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.586
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_Laue_measured_fraction_full 0.586
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            101532
_diffrn_reflns_point_group_measured_fraction_full 0.580
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         50.485
_diffrn_reflns_theta_min         1.346
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.6592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1167 before and 0.0551 after correction. The Ratio of minimum to maximum transmission is 0.8789. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.231
_exptl_crystal_description       prism
_exptl_crystal_F_000             4908
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.182
_refine_diff_density_max         0.064
_refine_diff_density_min         -0.099
_refine_diff_density_rms         0.006
_refine_ls_abs_structure_details
;
 Flack x determined using 5322 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.28(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.641
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         24039
_refine_ls_number_restraints     1246
_refine_ls_restrained_S_all      0.684
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1141P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1319
_reflns_Friedel_coverage         0.886
_reflns_Friedel_fraction_full    0.573
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                15079
_reflns_number_total             24039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06445_si_001.cif
_cod_data_source_block           cx1421
_cod_original_cell_volume        67899(10)
_cod_database_code               4127833
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.947
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O8-C74 = O7-C74 = O6-C59 = O5-C59 = O2-C29 = O1-C29 = O3-C44 = O4-C44
 1.2 with sigma of 0.01
 O4-O3 = O6-O5 = O7-O8 = O1-O2
 2.2 with sigma of 0.01
3. Restrained planarity
 O3, C38, C39, C40, C41, C42, C43, C44, C36, C37, O4
 with sigma of 0.01
 O5, O6, C51, C52, C53, C54, C55, C56, C57, C58, C59
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: O5(0.5) O6(0.5) H6(0.5) O7(0.5) O8(0.5) H8(0.5) C45(0.5) C46(0.5)
 H46(0.5) C47(0.5) H47(0.5) C48(0.5) C49(0.5) H49(0.5) C50(0.5) H50(0.5)
 C51(0.5) C52(0.5) C53(0.5) C54(0.5) H54(0.5) C55(0.5) H55(0.5) C56(0.5)
 C57(0.5) H57(0.5) C58(0.5) H58(0.5) C59(0.5) C60(0.5) C61(0.5) H61(0.5)
 C62(0.5) H62(0.5) C63(0.5) C64(0.5) H64(0.5) C65(0.5) H65(0.5) C66(0.5)
 C67(0.5) C68(0.5) C69(0.5) H69(0.5) C70(0.5) H70(0.5) C71(0.5) C72(0.5)
 H72(0.5) C73(0.5) H73(0.5) C74(0.5)
7.a Ternary CH refined with riding coordinates:
 C1(H1), C8(H8A)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6A), C10(H10), C13(H13), C16(H16), C17(H17), C19(H19), C20(H20),
 C24(H24), C25(H25), C27(H27), C28(H28), C31(H31), C32(H32), C34(H34), C35(H35),
  C39(H39), C40(H40), C42(H42), C43(H43), C46(H46), C47(H47), C49(H49),
 C50(H50), C54(H54), C55(H55), C57(H57), C58(H58), C61(H61), C62(H62), C64(H64),
  C65(H65), C69(H69), C70(H70), C72(H72), C73(H73)
7.c Fitted hexagon refined as free rotating group:
 C45(C46,C47,C48,C49,C50)
7.d Tetrahedral OH refined with riding coordinates:
 O4(H4), O6(H6), O8(H8)
7.e Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              15022
_shelx_hkl_checksum              13438
_shelx_fab_checksum              27155
_olex2_date_sample_data_collection 2018-10-18
_olex2_date_sample_submission    2018-10-17
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone'
_olex2_submission_original_sample_id cx1421
_olex2_submission_special_instructions 'No special instructions were received'