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_7242127
_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             2019-01-07
_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                104.714(2)
_cell_angle_beta                 96.728(2)
_cell_angle_gamma                99.499(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6612(4)
_cell_length_b                   14.1198(3)
_cell_length_c                   15.7544(4)
_cell_measurement_reflns_used    17924
_cell_measurement_temperature    250.00(14)
_cell_measurement_theta_max      70.4950
_cell_measurement_theta_min      4.3370
_cell_volume                     2649.14(13)
_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      250.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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    -71.00  31.00   1.00    4.00    --  -42.46  57.00-150.00  102
  2  \w   -115.00 -14.00   1.00    4.00    --  -42.46 -57.00  60.00  101
  3  \w    -30.00  71.00   1.00    4.00    --   42.46 -57.00 -60.00  101
  4  \w     18.00 117.00   1.00    4.00    --   42.46  37.00-180.00   99
  5  \w      1.00  83.00   1.00    4.00    --   42.46 -99.00 -90.00   82
  6  \w     17.00 110.00   1.00   16.00    --  100.00 -94.00-180.00   93
  7  \w     17.00 110.00   1.00   16.00    --  100.00 -94.00   0.00   93
  8  \w     27.00 126.00   1.00   16.00    --  100.00 -45.00 -30.00   99
  9  \w     28.00 129.00   1.00   16.00    --  100.00 -61.00-150.00  101
 10  \w     18.00 153.00   1.00   16.00    --  100.00 -15.00-180.00  135
 11  \w     27.00 118.00   1.00   16.00    --  100.00-125.00 120.00   91
 12  \w     72.00 176.00   1.00   16.00    --  100.00  30.00-150.00  104
 13  \w     72.00 176.00   1.00   16.00    --  100.00  30.00-180.00  104
 14  \w     17.00 110.00   1.00   16.00    --  100.00 -94.00 120.00   93
 15  \w     94.00 173.00   1.00   16.00    --  100.00 125.00-120.00   79
 16  \w     27.00 118.00   1.00   16.00    --  100.00-125.00 -30.00   91
 17  \w     27.00 126.00   1.00   16.00    --  100.00 -45.00  90.00   99
 18  \w   -119.00 -10.00   1.00    4.00    --  -42.46 -77.00-120.00  109
 19  \w   -119.00 -10.00   1.00    4.00    --  -42.46 -77.00 150.00  109
 20  \w   -115.00 -14.00   1.00    4.00    --  -42.46 -57.00 -60.00  101
 21  \w   -119.00 -10.00   1.00    4.00    --  -42.46 -77.00  30.00  109
 22  \w     23.00  98.00   1.00    4.00    --   42.46-125.00  90.00   75
 23  \w     71.00 172.00   1.00   16.00    --  100.00  61.00  30.00  101
 24  \w     67.00 115.00   1.00   16.00    --  100.00  77.00 120.00   48
 25  \w     74.00 173.00   1.00   16.00    --  100.00  45.00 -30.00   99
 26  \w     71.00 172.00   1.00   16.00    --  100.00  61.00-150.00  101
 27  \w     71.00 172.00   1.00   16.00    --  100.00  61.00   0.00  101
 28  \w     71.00 172.00   1.00   16.00    --  100.00  61.00  90.00  101
 29  \w     74.00 173.00   1.00   16.00    --  100.00  45.00 -90.00   99
;
_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      -0.0205813000
_diffrn_orient_matrix_UB_12      -0.1128979000
_diffrn_orient_matrix_UB_13      -0.0084912000
_diffrn_orient_matrix_UB_21      -0.1069777000
_diffrn_orient_matrix_UB_22      0.0069559000
_diffrn_orient_matrix_UB_23      0.0365325000
_diffrn_orient_matrix_UB_31      -0.0615396000
_diffrn_orient_matrix_UB_32      -0.0218321000
_diffrn_orient_matrix_UB_33      -0.0954315000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_unetI/netI     0.0116
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            48412
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        70.596
_diffrn_reflns_theta_max         70.596
_diffrn_reflns_theta_min         3.590
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.257
_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    1.105
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.463
_exptl_crystal_size_mid          0.398
_exptl_crystal_size_min          0.177
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.0019(5)
_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   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         10031
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0748
_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^)+(0.1570P)^2^+0.2860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2460
_refine_ls_wR_factor_ref         0.2636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7913
_reflns_number_total             10031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01704c2.cif
_cod_data_source_block           kad1j
_cod_depositor_comments
'Adding full bibliography for 7242124--7242127.cif.'
_cod_original_cell_volume        2649.12(12)
_cod_database_code               7242127
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C56 H80 O8'
_reflns_odcompleteness_completeness 99.97
_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) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C54-C55 = C55-C56 = C54A-C55A = C55A-C56A
 1.54 with sigma of 0.02
 C54-C56 = C54A-C56A
 2.5 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C51) = Uanis(C51A)
Uanis(C52) = Uanis(C52A)
Uanis(C37) = Uanis(C37A)
Uanis(C38) = Uanis(C38A)
Uanis(C40) = Uanis(C40A)
Uanis(C41) = Uanis(C41A)
Uanis(C42) = Uanis(C42A)
Uanis(C34) = Uanis(C34A)
Uanis(C35) = Uanis(C35A)
Uanis(C54) = Uanis(C54A)
Uanis(C55) = Uanis(C55A)
4. Others
 Sof(H50C)=Sof(H50D)=Sof(C51A)=Sof(H51C)=Sof(H51D)=Sof(C52A)=Sof(H52D)=
 Sof(H52E)=Sof(H52F)=1-FVAR(1)
 Sof(H50A)=Sof(H50B)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=
 Sof(H52C)=FVAR(1)
 Sof(H36C)=Sof(H36D)=Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(C38A)=Sof(H38D)=
 Sof(H38E)=Sof(H38F)=1-FVAR(2)
 Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(H38C)=FVAR(2)
 Sof(C40A)=Sof(H40C)=Sof(H40D)=Sof(C41A)=Sof(H41C)=Sof(H41D)=Sof(C42A)=
 Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(3)
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=
 Sof(H42B)=Sof(H42C)=FVAR(3)
 Sof(H33C)=Sof(H33D)=Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C35A)=Sof(H35D)=
 Sof(H35E)=Sof(H35F)=1-FVAR(4)
 Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35A)=Sof(H35B)=
 Sof(H35C)=FVAR(4)
 Sof(C54A)=Sof(H54C)=Sof(H54D)=Sof(C55A)=Sof(H55C)=Sof(H55D)=Sof(C56A)=
 Sof(H56D)=Sof(H56E)=Sof(H56F)=1-FVAR(5)
 Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(C56)=Sof(H56A)=
 Sof(H56B)=Sof(H56C)=FVAR(5)
5.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), C33(H33C,H33D), C34(H34A,H34B), C34A(H34C,
 H34D), C36(H36A,H36B), C36(H36C,H36D), C37(H37A,H37B), C37A(H37C,H37D),
 C40(H40A,H40B), C40A(H40C,H40D), C41(H41A,H41B), C41A(H41C,H41D), C43(H43A,
 H43B), C44(H44A,H44B), C47(H47A,H47B), C48(H48A,H48B), C50(H50A,H50B),
 C50(H50C,H50D), C51(H51A,H51B), C51A(H51C,H51D), C54(H54A,H54B), C54A(H54C,
 H54D), C55(H55A,H55B), C55A(H55C,H55D)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8), C15(H15), C22(H22)
5.c Idealised Me refined with riding coordinates:
 C35(H35A,H35B,H35C), C35A(H35D,H35E,H35F), C38(H38A,H38B,H38C), C38A(H38D,
 H38E,H38F), C56(H56A,H56B,H56C), C56A(H56D,H56E,H56F)
5.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C39(H39A,H39B,H39C), C42(H42A,H42B,
 H42C), C42A(H42D,H42E,H42F), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C),
 C49(H49A,H49B,H49C), C52(H52A,H52B,H52C), C52A(H52D,H52E,H52F), C53(H53A,H53B,
 H53C)
;
_olex2_date_sample_data_collection 2019-01-11
_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 1.205
_oxdiff_exptl_absorpt_empirical_full_min 0.832