Conformational switch in the crystal states of a calix[4]arene
Mirzaei, Saber; Lindeman, Sergey V.; Wang, Denan; Mirzaei, M. Saeed; Timerghazin, Qadir K.; CrystEngComm 23 (2021) 1906–1911; doi:10.1039/D0CE01704C

data_7242126
_publ_section_title
;
 Conformational switch in the crystal states of a calix[4]arene
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1906
_journal_page_last               1911
_journal_paper_doi               10.1039/D0CE01704C
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C56 H80 O8'
_chemical_formula_sum            'C56 H80 O8'
_chemical_formula_weight         881.20
_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     direct
_audit_creation_date             2019-01-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-09 deposited with the CCDC.	2021-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                95.6026(16)
_cell_angle_beta                 92.8626(16)
_cell_angle_gamma                94.0129(16)
_cell_formula_units_Z            2
_cell_length_a                   12.9716(3)
_cell_length_b                   13.0379(3)
_cell_length_c                   14.9706(3)
_cell_measurement_reflns_used    21344
_cell_measurement_temperature    99.8(4)
_cell_measurement_theta_max      70.4960
_cell_measurement_theta_min      4.2680
_cell_volume                     2509.48(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      99.8(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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    -67.00  32.00   1.00    1.00    --  -42.46  37.00-150.00   99
  2  \w    -71.00  31.00   1.00    1.00    --  -42.46  57.00 -60.00  102
  3  \w   -117.00 -18.00   1.00    1.00    --  -42.46 -37.00  30.00   99
  4  \w      1.00  83.00   1.00    1.00    --   42.46 -99.00 -60.00   82
  5  \w     28.00 129.00   1.00    4.00    --  100.00 -61.00 -90.00  101
  6  \w     94.00 173.00   1.00    4.00    --  100.00 125.00-150.00   79
  7  \w     17.00 110.00   1.00    4.00    --  100.00 -94.00-180.00   93
  8  \w     17.00 110.00   1.00    4.00    --  100.00 -94.00-120.00   93
  9  \w     72.00 176.00   1.00    4.00    --  100.00  30.00   0.00  104
 10  \w     72.00 176.00   1.00    4.00    --  100.00  30.00  90.00  104
 11  \w     94.00 173.00   1.00    4.00    --  100.00 125.00-180.00   79
 12  \w     27.00 118.00   1.00    4.00    --  100.00-125.00-180.00   91
 13  \w     27.00 118.00   1.00    4.00    --  100.00-125.00  60.00   91
 14  \w     17.00 110.00   1.00    4.00    --  100.00 -94.00 -90.00   93
 15  \w     71.00 172.00   1.00    4.00    --  100.00  61.00 120.00  101
 16  \w     24.00 128.00   1.00    4.00    --  100.00 -30.00 150.00  104
 17  \w   -115.00 -14.00   1.00    1.00    --  -42.46 -57.00 150.00  101
 18  \w    -92.00  -2.00   1.00    1.00    --  -42.46 125.00  30.00   90
 19  \w   -117.00 -18.00   1.00    1.00    --  -42.46 -37.00-150.00   99
 20  \w   -119.00 -10.00   1.00    1.00    --  -42.46 -77.00 -30.00  109
 21  \w     67.00 144.00   1.00    4.00    --  100.00  77.00 -30.00   77
 22  \w     67.00 176.00   1.00    4.00    --  100.00  77.00 -90.00  109
 23  \w     67.00 176.00   1.00    4.00    --  100.00  77.00 150.00  109
 24  \w     71.00 172.00   1.00    4.00    --  100.00  61.00  90.00  101
 25  \w     47.00 178.00   1.00    4.00    --  100.00  15.00 -90.00  131
 26  \w     67.00 176.00   1.00    4.00    --  100.00  77.00-180.00  109
 27  \w     67.00 176.00   1.00    4.00    --  100.00  77.00-134.00  109
 28  \w     67.00 176.00   1.00    4.00    --  100.00  77.00   0.00  109
;
_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      -0.0709360000
_diffrn_orient_matrix_UB_12      0.0130444000
_diffrn_orient_matrix_UB_13      -0.0831320000
_diffrn_orient_matrix_UB_21      0.0065325000
_diffrn_orient_matrix_UB_22      0.1176524000
_diffrn_orient_matrix_UB_23      0.0259628000
_diffrn_orient_matrix_UB_31      0.0956358000
_diffrn_orient_matrix_UB_32      0.0128199000
_diffrn_orient_matrix_UB_33      -0.0560497000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            45942
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        70.613
_diffrn_reflns_theta_max         70.613
_diffrn_reflns_theta_min         3.416
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.518
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.332
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.093
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         9537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+0.7035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8418
_reflns_number_total             9537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01704c2.cif
_cod_data_source_block           kad1ix
_cod_depositor_comments
'Adding full bibliography for 7242124--7242127.cif.'
_cod_original_cell_volume        2509.49(9)
_cod_database_code               7242126
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C56 H80 O8'
_reflns_odcompleteness_completeness 99.98
_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.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B), C33(H33A,H33B), C34(H34A,H34B), C36(H36A,H36B), C37(H37A,H37B),
  C40(H40A,H40B), C41(H41A,H41B), C43(H43A,H43B), C44(H44A,H44B), C47(H47A,
 H47B), C48(H48A,H48B), C50(H50A,H50B), C51(H51A,H51B), C54(H54A,H54B),
 C55(H55A,H55B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8), C15(H15), C22(H22)
2.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C42(H42A,H42B,H42C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C49(H49A,H49B,H49C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C56(H56A,H56B,H56C)
;
_olex2_date_sample_data_collection 2019-01-03
_olex2_date_sample_submission    2019-01-02
_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 1.606
_oxdiff_exptl_absorpt_empirical_full_min 0.868