Synthesis of inherently chiral calix[4]arenes: stereocontrol through ligand choice.
Herbert, Simon A.; Arnott, Gareth E.; Organic letters 12 (2010) 4600–4603; doi:10.1021/ol101909f

data_1503234
_publ_section_title
;
 Synthesis of inherently chiral calix[4]arenes: stereocontrol through
 ligand choice.
;
_journal_issue                   20
_journal_name_full               'Organic letters'
_journal_page_first              4600
_journal_page_last               4603
_journal_paper_doi               10.1021/ol101909f
_journal_volume                  12
_journal_year                    2010
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C232 H264 N4 O27 P4'
_chemical_formula_sum            'C232 H264 N4 O27 P4'
_chemical_formula_weight         3664.35
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.45(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   9.5900(19)
_cell_length_b                   16.381(3)
_cell_length_c                   32.198(6)
_cell_measurement_reflns_used    6655
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.3
_cell_measurement_theta_min      2.3
_cell_volume                     5026.1(17)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'X-Seed (Barbour 2001)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0680
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            30595
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.9893
_exptl_absorpt_correction_T_min  0.9809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), 9418 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.06(10)
_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     1674
_refine_ls_number_reflns         20808
_refine_ls_number_restraints     526
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+1.5440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1339
_reflns_number_gt                15689
_reflns_number_total             20808
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol101909f_si_002.cif
_cod_data_source_block           c:\tia\sh2\finalr~1\sh2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1503234