Calix[4, 5]tetrolarenes: A New Family of Macrocycles.
Zafrani, Yossi; Cohen, Yoram; Organic letters 19 (2017) 3719–3722; doi:10.1021/acs.orglett.7b01511

data_1546431
_publ_section_title
;
 Calix[4, 5]tetrolarenes: A New Family of Macrocycles.
;
_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3719
_journal_page_last               3722
_journal_paper_doi               10.1021/acs.orglett.7b01511
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C40 H48 O16'
_chemical_formula_sum            'C40 H48 O16'
_chemical_formula_weight         784.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 113.800(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.1484(7)
_cell_length_b                   23.5395(7)
_cell_length_c                   16.3621(5)
_cell_measurement_reflns_used    6377
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.389
_cell_measurement_theta_min      1.403
_cell_volume                     7100.3(4)
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_collection       'Apex2, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 1.75
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. \f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37388
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.389
_diffrn_reflns_theta_min         1.403
_diffrn_source                   'ImuS micro-focus'
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       hexagone
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         8859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.001
_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^+8.2991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1206
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6377
_reflns_number_total             8859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b01511_si_002.cif
_cod_data_source_block           yco1
_cod_depositor_comments          'Adding full bibliography for 1546431.cif.'
_cod_database_code               1546431
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              17929
_shelx_hkl_checksum              80185