Rim-differentiated Co-pillar[4+1]arenes.
Zhao, Jianyi; Yang, Weiwei; Liang, Chuanyun; Gao, Liya; Xu, Jun; Sue, Andrew C.-H.; Zhao, Hongxia; Chemical communications (Cambridge, England) 57 (2021) 11193–11196; doi:10.1039/d1cc04840f

data_7129065
_publ_section_title
;
 Rim-differentiated Co-pillar[4+1]arenes.
;
_journal_issue                   85
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11193
_journal_page_last               11196
_journal_paper_doi               10.1039/d1cc04840f
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C61 H53 O10'
_chemical_formula_sum            'C61 H53 O10'
_chemical_formula_weight         946.03
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-08-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-28 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                88.492(4)
_cell_angle_beta                 81.618(4)
_cell_angle_gamma                77.710(4)
_cell_formula_units_Z            2
_cell_length_a                   12.0930(6)
_cell_length_b                   13.4589(8)
_cell_length_c                   17.0755(7)
_cell_measurement_reflns_used    5734
_cell_measurement_temperature    100.01(12)
_cell_measurement_theta_max      28.0100
_cell_measurement_theta_min      1.9800
_cell_volume                     2686.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(12)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.789
_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     12.00  39.00   0.50   20.00    --    5.89 -95.00 -29.00   54
  2  \w    -11.00  31.00   0.50   20.00    --   -7.61 -99.00  30.00   84
  3  \w    -22.00   3.00   0.50   20.00    --    5.89 -95.00 -29.00   50
  4  \w    -66.00  35.00   0.50   20.00    --    5.89 -77.00 -90.00  202
  5  \w    -21.00  25.00   0.50   20.00    --   -7.61 -99.00 120.00   92
  6  \w    -75.00   4.00   0.50   20.00    --    5.89 -19.00 -30.00  158
  7  \w    -30.00  30.00   0.50   20.00    --    5.89  95.00  79.00  120
  8  \w    -23.00   5.00   0.50   20.00    --   -7.61  95.00  79.00   56
  9  \w    -85.00   4.00   0.50   20.00    --   -7.61 -19.00-150.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0362691000
_diffrn_orient_matrix_UB_12      -0.0180923000
_diffrn_orient_matrix_UB_13      -0.0354572000
_diffrn_orient_matrix_UB_21      -0.0129848000
_diffrn_orient_matrix_UB_22      0.0491567000
_diffrn_orient_matrix_UB_23      -0.0167531000
_diffrn_orient_matrix_UB_31      0.0468536000
_diffrn_orient_matrix_UB_32      0.0128690000
_diffrn_orient_matrix_UB_33      0.0150036000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_unetI/netI     0.1294
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.789
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37326
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.789
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.485
_diffrn_reflns_theta_min         1.958
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       plate
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.0058(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         11810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1692
_refine_ls_R_factor_gt           0.0859
_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^)+(0.1443P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2225
_refine_ls_wR_factor_ref         0.2662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5543
_reflns_number_total             11810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04840f2.cif
_cod_data_source_block           exp_66
_cod_depositor_comments
'Adding full bibliography for 7129065--7129066.cif.'
_cod_database_code               7129065
_shelx_shelxl_version_number     2014/7
_diffrn_oxdiff_digest_frames
;
014d5af3fd8f479440de39e54b05314406000256c58
;
_diffrn_oxdiff_digest_hkl
;
01d603b56dd1647980c0be4b94f4e2da4840d4
;
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C36(H36A,H36B), C61(H61A,H61B), C50(H50A,H50B), C22(H22A,
 H22B), C53(H53A,H53B), C11(H11A,H11B), C43(H43A,H43B), C14(H14A,H14B),
 C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C38(H38), C41(H41), C31(H31), C28(H28), C59(H59), C17(H17), C8(H8), C56(H56),
 C20(H20), C5(H5), C3(H3), C48(H48), C45(H45), C47(H47), C49(H49), C46(H46)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C32(H32A,H32B,H32C), C60(H60A,H60B,H60C), C10(H10A,H10B,
 H10C)
2.d :
 C51(H51), C34(H34), C12(H12), C23(H23), C1(H1)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              80720
_shelx_fab_checksum              9429
_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 1.539
_oxdiff_exptl_absorpt_empirical_full_min 0.844