A calix[3]carbazole-based cavitand: synthesis, structure and its complexation with fullerenes.
Zhang, Fan; Du, Xu-Sheng; Song, Kui-Zhu; Han, Ying; Lu, Hai-Yan; Chen, Chuan-Feng; Chemical communications (Cambridge, England) 60 (2024) 4962–4965; doi:10.1039/d4cc00928b

data_7132945
_publ_section_title
;
 A calix[3]carbazole-based cavitand: synthesis, structure and its
 complexation with fullerenes.
;
_journal_issue                   37
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4962
_journal_page_last               4965
_journal_paper_doi               10.1039/d4cc00928b
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C40.5 H19.5 N4.5 O3'
_chemical_formula_sum            'C41.5 H21.5 Cl0.25 N5 O5.5'
_chemical_formula_weight         687.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-10-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-11-04 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.643(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7611(3)
_cell_length_b                   18.5038(3)
_cell_length_c                   14.1018(3)
_cell_measurement_reflns_used    10098
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      75.2460
_cell_measurement_theta_min      3.1900
_cell_volume                     3272.56(12)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.959
_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   -111.00 -36.00   0.50    3.00    --  -47.19 -21.00  77.00  150
  2  \w    -22.00   4.00   0.50    3.00    --  -47.19  21.00-116.00   52
  3  \w     -3.00  24.00   0.50    3.00    --   47.19 -21.00  77.00   54
  4  \w     41.00 123.00   0.50    3.00    --   47.19  21.00-116.00  164
  5  \w     91.00 178.00   0.50   15.00    --  103.25  21.00-116.00  174
  6  \w   -122.00 -96.00   0.50   15.00    -- -104.50 -21.00  77.00   52
  7  \w    -21.00  26.00   0.50    3.00    --  -47.19  19.00  30.00   94
  8  \w     68.00  93.00   0.50    3.00    --   47.19-125.00-150.00   50
  9  \w    -26.00  45.00   0.50    3.00    --   47.19 -38.00 -60.00  142
 10  \w     31.00  56.00   0.50   15.00    --  103.25 -61.00 150.00   50
 11  \w     43.00  74.00   0.50   15.00    --  103.25 -61.00  90.00   62
 12  \w     57.00 108.00   0.50   15.00    --  103.25-125.00   0.00  102
 13  \w     32.00 105.00   0.50   15.00    --  103.25 -77.00-180.00  146
 14  \w     33.00  74.00   0.50   15.00    --  103.25 -61.00 -30.00   82
 15  \w     37.00 106.00   0.50   15.00    --  103.25-125.00  90.00  138
 16  \w     56.00 100.00   0.50   15.00    --  103.25 -94.00-120.00   88
 17  \w     36.00  62.00   0.50   15.00    --  103.25 -61.00-120.00   52
 18  \w     33.00  60.00   0.50   15.00    --  103.25 -61.00 120.00   54
 19  \w     33.00  75.00   0.50   15.00    --  103.25 -61.00 -90.00   84
 20  \w     35.00  61.00   0.50   15.00    --  103.25 -61.00  60.00   52
 21  \w   -164.00 -96.00   0.50   15.00    -- -104.50 -61.00  30.00  136
 22  \w   -127.00 -92.00   0.50   15.00    -- -104.50 -61.00   0.00   70
 23  \w   -173.00-131.00   0.50   15.00    -- -104.50 -61.00   0.00   84
 24  \w    -89.00 -61.00   0.50   15.00    -- -104.50  77.00   0.00   56
 25  \w   -174.00-104.00   0.50   15.00    -- -104.50 -45.00 -30.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0907536000
_diffrn_orient_matrix_UB_12      0.0214805000
_diffrn_orient_matrix_UB_13      -0.0831635000
_diffrn_orient_matrix_UB_21      -0.0810476000
_diffrn_orient_matrix_UB_22      -0.0077581000
_diffrn_orient_matrix_UB_23      0.0679011000
_diffrn_orient_matrix_UB_31      0.0167096000
_diffrn_orient_matrix_UB_32      0.0800519000
_diffrn_orient_matrix_UB_33      0.0289534000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25286
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.551
_diffrn_reflns_theta_min         3.189
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       cube
_exptl_crystal_F_000             1415
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         6729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0692P)^2^+0.6289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1341
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5099
_reflns_number_total             6729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00928b2.cif
_cod_data_source_block           tx12699_auto_sq
_cod_depositor_comments
'Adding full bibliography for 7132945--7132948.cif.'
_cod_original_formula_sum        'C41.50 H21.50 Cl0.25 N5 O5.50'
_cod_database_code               7132945
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOCl
_chemical_oxdiff_usercomment     CHNOCl
_diffrn_oxdiff_digest_frames
;
017b0f4b2f5553bf444cdc35b31812ab5a000277a2f
;
_diffrn_oxdiff_digest_hkl
;
01ad270ab8a439514438a201a255dda27fa7d9
;
_reflns_odcompleteness_completeness 99.95
_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
2.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C51(H51), C42(H42), C14(H14), C39(H39), C21(H21), C8(H8), C30(H30),
 C45(H45), C18(H18), C32(H32), C28(H28), C38(H38), C34(H34), C31(H31), C37(H37),
  C35(H35), C36(H36), C29(H29)
;
_shelx_res_checksum              5762
_shelx_hkl_checksum              3254
_shelx_fab_checksum              68525
_platon_squeeze_void_probe_radius 1.20
_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 1.473
_oxdiff_exptl_absorpt_empirical_full_min 0.690