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_7121544
_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         '2(C68 H68 O8), 3(C H Cl3)'
_chemical_formula_sum            'C139 H139 Cl9 O16'
_chemical_formula_weight         2384.54
_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)-1^6^,5^4^-bis(3,4-dimethoxyphenyl)-2,4,6,8-tetraethyl-1,3,5,7(1,3)-tetrabenzenacyclooctaphane
_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                ntl1726_JNS_467
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-02-28 deposited with the CCDC.
2018-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                72.549(2)
_cell_angle_beta                 80.550(2)
_cell_angle_gamma                75.159(2)
_cell_formula_units_Z            2
_cell_length_a                   14.3309(4)
_cell_length_b                   18.0783(5)
_cell_length_c                   24.9943(5)
_cell_measurement_reflns_used    16856
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      74.072
_cell_measurement_theta_min      3.690
_cell_volume                     5944.5(3)
_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    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0(1)
_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 0.967
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            45719
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         74.266
_diffrn_reflns_theta_min         3.551
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.477
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.461
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2014)
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            'pale yellow'
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2508
_exptl_crystal_preparation
;
Crystals were grown by diffusion of methanol into a chloroform solution at 
room temperature.
;
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform, methanol'
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.537
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.248
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1632
_refine_ls_number_reflns         23441
_refine_ls_number_restraints     348
_refine_ls_restrained_S_all      2.789
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.0984
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2920
_refine_ls_wR_factor_ref         0.3244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17397
_reflns_number_total             23441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01903g2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7121542--7121547.cif.'
_cod_database_code               7121544
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.514
_shelx_estimated_absorpt_t_max   0.826
_shelx_res_checksum              28929