Rigid tetraarylene-bridged cavitands from reduced-symmetry resorcin[4]arene derivatives.
Smith, Jordan N.; Lucas, Nigel T.; Chemical communications (Cambridge, England) 54 (2018) 4716–4719; doi:10.1039/c8cc01903g

data_7121545
_publ_section_title
;
 Rigid tetraarylene-bridged cavitands from reduced-symmetry
 resorcin[4]arene derivatives.
;
_journal_issue                   37
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4716
_journal_page_last               4719
_journal_paper_doi               10.1039/c8cc01903g
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C68 H64 O8, 3.5(C8 H10)'
_chemical_formula_sum            'C96 H99 O8'
_chemical_formula_weight         1380.75
_chemical_name_systematic
'1^4^,7^4^:1^6^,3^6^:3^4^,5^6^:5^4^,7^6^-Tetrakis(4,5-dimethoxy[1,2]benzeno)-2,4,6,8-tetraethyl-1,3,5,7(1,3)-tetrabenzenacyclooctaphane ethylbenzene solvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_code                ntl1814_JNS_646
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-04-05 deposited with the CCDC.
2018-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                101.4820(10)
_cell_angle_beta                 91.2600(10)
_cell_angle_gamma                95.4360(10)
_cell_formula_units_Z            2
_cell_length_a                   14.2685(3)
_cell_length_b                   14.5929(2)
_cell_length_c                   19.2492(3)
_cell_measurement_reflns_used    36831
_cell_measurement_temperature    99.9(9)
_cell_measurement_theta_max      74.8840
_cell_measurement_theta_min      3.7930
_cell_volume                     3906.74(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2014)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2014)'
_computing_molecular_graphics    'Mercury CSD 3.9 (CCDC, 2016)'
_computing_publication_material  'enCIFer 1.6 (CCDC, 2016)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXt-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.9(9)
_diffrn_crystal_treatment
; 
Crystal was attached with Paratone N oil to a 0.3 mm CryoLoop supported 
in a copper mounting pin, then quenched in a cold nitrogen gas stream
from an Oxford Cryosystems Cryostream.
;
_diffrn_detector_area_resol_mean 5.1725
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            73852
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         75.130
_diffrn_reflns_theta_min         3.494
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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_density_diffrn    1.174
_exptl_crystal_description       plate
_exptl_crystal_F_000             1478
_exptl_crystal_preparation
;
Crystals were grown by evaporation of an ethylbenzene solution.
;
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethylbenzene'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     998
_refine_ls_number_reflns         15664
_refine_ls_number_restraints     315
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0885
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1739P)^2^+3.9285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2570
_refine_ls_wR_factor_ref         0.2685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13432
_reflns_number_total             15664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01903g2.cif
_cod_data_source_block           4-EtPh
_cod_depositor_comments
'Adding full bibliography for 7121542--7121547.cif.'
_cod_database_code               7121545
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.871
_shelx_estimated_absorpt_t_max   0.972
_shelx_res_checksum              79267