High compression strength single network hydrogels with pillar[5]arene junction points
Xu, Xiaowen; Jerca, Florica Adriana; Van Hecke, Kristof; Jerca, Valentin Victor; Hoogenboom, Richard; Materials Horizons 7 (2020) 566–573; doi:10.1039/C9MH01401B

data_1552477
_publ_section_title
;
 High compression strength single network hydrogels with pillar[5]arene
 junction points
;
_journal_issue                   2
_journal_name_full               'Materials Horizons'
_journal_page_first              566
_journal_page_last               573
_journal_paper_doi               10.1039/C9MH01401B
_journal_volume                  7
_journal_year                    2020
_chemical_formula_moiety         'C51 H58 O14'
_chemical_formula_sum            'C51 H58 O14'
_chemical_formula_weight         894.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-01-25
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-15 deposited with the CCDC.    2019-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                93.6475(17)
_cell_angle_beta                 99.9526(19)
_cell_angle_gamma                92.348(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6444(3)
_cell_length_b                   12.2441(3)
_cell_length_c                   19.4216(4)
_cell_measurement_reflns_used    18519
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      75.2540
_cell_measurement_theta_min      3.6190
_cell_volume                     2251.20(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -70.00  31.00   1.00    1.00    --  -41.80  57.00   0.00  101
  2  \w    -74.00  34.00   1.00    1.00    --  -41.80  77.00  90.00  108
  3  \w    -74.00  34.00   1.00    1.00    --  -41.80  77.00-150.00  108
  4  \w    -70.00  31.00   1.00    1.00    --  -41.80  57.00-120.00  101
  5  \w     83.00 178.00   1.00    6.00    --  109.13  45.00   0.00   95
  6  \w     26.00 110.00   1.00    6.00    --  109.13 -94.00  30.00   84
  7  \w     37.00 138.00   1.00    6.00    --  109.13 -61.00 150.00  101
  8  \w     37.00 123.00   1.00    6.00    --  109.13-133.00-152.00   86
  9  \w     81.00 178.00   1.00    6.00    --  109.13  30.00 120.00   97
 10  \w     83.00 178.00   1.00    6.00    --  109.13  45.00  60.00   95
 11  \w     36.00 117.00   1.00    6.00    --  109.13-125.00 -60.00   81
 12  \w     83.00 178.00   1.00    6.00    --  109.13  45.00-150.00   95
 13  \w     37.00 138.00   1.00    6.00    --  109.13 -61.00  30.00  101
 14  \w     36.00 117.00   1.00    6.00    --  109.13-125.00   0.00   81
 15  \w   -118.00  -9.00   1.00    1.00    --  -41.80 -77.00 120.00  109
 16  \w   -118.00  -9.00   1.00    1.00    --  -41.80 -77.00  30.00  109
 17  \w   -114.00 -14.00   1.00    1.00    --  -41.80 -57.00 -60.00  100
 18  \w   -114.00 -14.00   1.00    1.00    --  -41.80 -57.00-150.00  100
 19  \w     80.00 178.00   1.00    6.00    --  109.13  61.00  60.00   98
 20  \w     80.00 178.00   1.00    6.00    --  109.13  61.00-120.00   98
 21  \w     80.00 178.00   1.00    6.00    --  109.13  61.00 150.00   98
 22  \w     80.00 178.00   1.00    6.00    --  109.13  61.00 120.00   98
 23  \w     81.00 178.00   1.00    6.00    --  109.13  30.00 -60.00   97
 24  \w     80.00 178.00   1.00    6.00    --  109.13  61.00-180.00   98
 25  \w     83.00 178.00   1.00    6.00    --  109.13  45.00  30.00   95
 26  \w     83.00 178.00   1.00    6.00    --  109.13  45.00 -30.00   95
 27  \w   -118.00  -9.00   1.00    1.00    --  -41.80 -77.00-150.00  109
 28  \w   -118.00  -9.00   1.00    1.00    --  -41.80 -77.00 -60.00  109
 29  \w   -116.00 -17.00   1.00    1.00    --  -41.80 -38.00 -60.00   99
 30  \w     17.00 116.00   1.00    1.00    --   41.80  38.00   0.00   99
 31  \w     80.00 148.00   1.00    6.00    --  109.13  61.00-150.00   68
 32  \w     83.00 178.00   1.00    6.00    --  109.13  45.00 -60.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1278000000
_diffrn_orient_matrix_UB_12      -0.0045888000
_diffrn_orient_matrix_UB_13      -0.0377681000
_diffrn_orient_matrix_UB_21      -0.1000562000
_diffrn_orient_matrix_UB_22      -0.0096689000
_diffrn_orient_matrix_UB_23      -0.0713572000
_diffrn_orient_matrix_UB_31      0.0055875000
_diffrn_orient_matrix_UB_32      0.1257987000
_diffrn_orient_matrix_UB_33      -0.0010407000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42196
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.444
_diffrn_reflns_theta_min         3.622
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         9132
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0639P)^2^+0.5488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7752
_reflns_number_total             9132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9mh01401b2.cif
_cod_data_source_block           rh083
_cod_depositor_comments
;Adding full bibliography for 1552477.cif.

 Adding full bibliography for 1552477.cif.
;
_cod_database_code               1552477
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C51 H58 O14'
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.819
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 C12-O6
 1.33 with sigma of 0.01
 O6-C13A = O6-C13B
 1.46 with sigma of 0.01
 C13A-C14A = C13B-C14B
 1.49 with sigma of 0.01
 C12-C13A = C12-C13B
 2.37 with sigma of 0.02
 O6-C14A = O6-C14B
 2.38 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C14A) = Uanis(C14B)
Uanis(C13A) = Uanis(C13B)
4. Others
 Sof(C13B)=Sof(H13C)=Sof(H13D)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(1)
 Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C11(H11A,H11B), C15(H15A,H15B), C24(H24A,H24B),
 C33(H33A,H33B), C42(H42A,H42B), C51(H51A,H51B), C13A(H13A,H13B), C13B(H13C,
 H13D)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C17(H17), C20(H20), C26(H26), C29(H29), C35(H35), C38(H38),
 C44(H44), C47(H47)
5.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C49(H49A,
 H49B,H49C), C50(H50A,H50B,H50C), C14A(H14A,H14B,H14C), C14B(H14D,H14E,H14F)
;
_shelx_res_checksum              2503
_shelx_hkl_checksum              71647
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.925
_oxdiff_exptl_absorpt_empirical_full_min 0.750