Design and Synthesis of Open-Chain Hosts Having a Partial Structure of p-tert-Butylthiacalixarene.
Morohashi, Naoya; Nanbu, Kazuki; Sonehara, Hayato; Ogihara, Jun; Shimazaki, Takanori; Hattori, Tetsutaro; The Journal of organic chemistry 83 (2018) 2235–2243; doi:10.1021/acs.joc.7b03137

data_4035008
_publ_section_title
;
 Design and Synthesis of Open-Chain Hosts Having a Partial Structure of
 p-tert-Butylthiacalixarene.
;
_journal_issue                   4
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              2235
_journal_page_last               2243
_journal_paper_doi               10.1021/acs.joc.7b03137
_journal_volume                  83
_journal_year                    2018
_chemical_formula_sum            'C34.5 H43.5 N1.5 O6 S'
_chemical_formula_weight         607.27
_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_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                73.209(3)
_cell_angle_beta                 88.784(3)
_cell_angle_gamma                88.223(3)
_cell_formula_units_Z            4
_cell_length_a                   9.6064(19)
_cell_length_b                   18.787(4)
_cell_length_c                   19.001(4)
_cell_measurement_reflns_used    7034
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.22
_cell_volume                     3281.2(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayered confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15464
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.343
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6205
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       prism
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     914
_refine_ls_number_reflns         11248
_refine_ls_number_restraints     257
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0703
_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^)+(0.1019P)^2^+6.0038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1876
_refine_ls_wR_factor_ref         0.1987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9187
_reflns_number_total             11248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b03137_si_004.cif
_cod_data_source_block           4-pToluidine-oToluidine
_cod_original_cell_volume        3281.2(11)
_cod_original_formula_sum        'C34.50 H43.50 N1.50 O6 S'
_cod_database_code               4035008
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              49988
_shelx_hkl_checksum              42703