Inherently Chiral Upper-Rim-Bridged Calix[4]arenes Possessing a Seven Membered Ring.
Tlustý, Martin; Slavík, Petr; Kohout, Michal; Eigner, Václav; Lhoták, Pavel; Organic letters  (2017) –; doi:10.1021/acs.orglett.7b01170

data_1546095
_publ_section_title
;
 Inherently Chiral Upper-Rim-Bridged Calix[4]arenes Possessing a Seven
 Membered Ring.
;
_journal_name_full               'Organic letters'
_journal_paper_doi               10.1021/acs.orglett.7b01170
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C42 H49 N O4'
_chemical_formula_sum            'C42 H49 N O4'
_chemical_formula_weight         631.86
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 101.3003(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9619(4)
_cell_length_b                   24.0179(10)
_cell_length_c                   15.5925(6)
_cell_measurement_reflns_used    120
_cell_measurement_temperature    180
_cell_measurement_theta_max      57
_cell_measurement_theta_min      6
_cell_volume                     3658.4(3)
_computing_cell_refinement       'Apex3 (Bruker AXS, 2015)'
_computing_data_collection       'Apex3 (Bruker AXS, 2015)'
_computing_data_reduction        'Apex3 (Bruker AXS, 2015)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex3'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            55327
_diffrn_reflns_theta_full        68.246
_diffrn_reflns_theta_max         68.246
_diffrn_reflns_theta_min         2.890
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1360.000
_exptl_crystal_size_max          0.523
_exptl_crystal_size_mid          0.263
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.20
_refine_ls_abs_structure_details 'Flack (1983), 6453 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.01(11)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8561
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     932
_refine_ls_number_reflns         13298
_refine_ls_number_restraints     142
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.0022235
_refine_ls_shift/su_mean         0.0001513
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 7.30 11.5 6.09 2.06 0.310 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0896
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0896
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              28
_reflns_limit_k_min              -28
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                13082
_reflns_number_total             13302
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.61
_oxford_diffrn_Wilson_scale      38.52
_oxford_refine_ls_r_factor_ref   0.0383
_oxford_refine_ls_scale          0.18826(6)
_oxford_reflns_number_all        13301
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            ol7b01170_si_002.cif
_cod_data_source_block           6a_1_MT86
_cod_original_sg_symbol_Hall     'P 2yb '
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_database_code               1546095