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_7242125
_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             2019-03-14
_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                104.555(4)
_cell_angle_beta                 99.233(3)
_cell_angle_gamma                98.058(4)
_cell_formula_units_Z            1
_cell_length_a                   6.8417(3)
_cell_length_b                   12.7268(6)
_cell_length_c                   15.2879(6)
_cell_measurement_reflns_used    6187
_cell_measurement_temperature    100.05(10)
_cell_measurement_theta_max      70.3740
_cell_measurement_theta_min      4.0210
_cell_volume                     1248.84(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      100.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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   10.00    --  -42.46  37.00  30.00   99
  2  \w    -67.00  32.00   1.00   10.00    --  -42.46  37.00-180.00   99
  3  \w   -117.00 -18.00   1.00   10.00    --  -42.46 -37.00-150.00   99
  4  \w      1.00  83.00   1.00   10.00    --   42.46 -99.00 120.00   82
  5  \w     28.00 129.00   1.00   40.00    --  100.00 -61.00 150.00  101
  6  \w     72.00 176.00   1.00   40.00    --  100.00  30.00 -30.00  104
  7  \w     72.00 176.00   1.00   40.00    --  100.00  30.00-120.00  104
  8  \w     27.00 118.00   1.00   40.00    --  100.00-125.00  90.00   91
  9  \w     27.00 118.00   1.00   40.00    --  100.00-125.00 150.00   91
 10  \w     27.00 126.00   1.00   40.00    --  100.00 -45.00 -30.00   99
 11  \w     24.00 128.00   1.00   40.00    --  100.00 -30.00 -90.00  104
 12  \w     74.00 173.00   1.00   40.00    --  100.00  45.00 -60.00   99
 13  \w     27.00 118.00   1.00   40.00    --  100.00-125.00 -60.00   91
 14  \w     24.00 133.00   1.00   40.00    --  100.00 -77.00 -60.00  109
 15  \w     17.00 110.00   1.00   40.00    --  100.00 -94.00 150.00   93
 16  \w   -115.00 -14.00   1.00   10.00    --  -42.46 -57.00 150.00  101
 17  \w    -67.00  32.00   1.00   10.00    --  -42.46  37.00 -60.00   99
 18  \w   -115.00 -14.00   1.00   10.00    --  -42.46 -57.00  60.00  101
 19  \w   -119.00 -10.00   1.00   10.00    --  -42.46 -77.00   0.00  109
 20  \w     71.00 172.00   1.00   40.00    --  100.00  61.00 -30.00  101
 21  \w     71.00 172.00   1.00   40.00    --  100.00  61.00 150.00  101
 22  \w     71.00 172.00   1.00   40.00    --  100.00  61.00   0.00  101
 23  \w     71.00 172.00   1.00   40.00    --  100.00  61.00  30.00  101
 24  \w     72.00 176.00   1.00   40.00    --  100.00  30.00  90.00  104
 25  \w     71.00  95.00   1.00   40.00    --  100.00  61.00-180.00   24
;
_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      0.0491180000
_diffrn_orient_matrix_UB_12      0.0278448000
_diffrn_orient_matrix_UB_13      0.1061222000
_diffrn_orient_matrix_UB_21      0.1040403000
_diffrn_orient_matrix_UB_22      0.1177379000
_diffrn_orient_matrix_UB_23      0.0058355000
_diffrn_orient_matrix_UB_31      -0.2018226000
_diffrn_orient_matrix_UB_32      0.0397745000
_diffrn_orient_matrix_UB_33      0.0038396000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_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            19839
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        70.632
_diffrn_reflns_theta_max         70.632
_diffrn_reflns_theta_min         3.654
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.698
_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    1.172
_exptl_crystal_description       needle
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.384
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.014
_refine_diff_density_max         0.205
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       0.0017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0477P)^2^+0.3276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3946
_reflns_number_total             4745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01704c2.cif
_cod_data_source_block           kad1r
_cod_depositor_comments
'Adding full bibliography for 7242124--7242127.cif.'
_cod_original_cell_volume        1248.84(9)
_cod_database_code               7242125
_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, All C(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C19(H19A,H19B),
 C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C26(H26A,H26B), C27(H27A,H27B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8)
3.c Disordered Me refined as rotating group:
 C25(H25A,H25B,H25C,H25D,H25E,H25F)
3.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C24(H24A,H24B,
 H24C), C28(H28A,H28B,H28C)
;
_olex2_date_sample_data_collection 2019-03-13
_olex2_date_sample_submission    2019-03-07
_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 2.019
_oxdiff_exptl_absorpt_empirical_full_min 0.793