Inherently Chiral Iminoresorcinarenes through Regioselective Unidirectional Tautomerization
Marcin Grajda; Michał Wierzbicki; Piotr Cmoch; Agnieszka Szumna; Journal of Organic Chemistry 78 (2013) 11597–11601; doi:10.1021/jo4019182

data_4028754
_publ_section_title
;
 Inherently Chiral Iminoresorcinarenes through Regioselective
 Unidirectional Tautomerization
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              11597
_journal_page_last               11601
_journal_paper_doi               10.1021/jo4019182
_journal_volume                  78
_journal_year                    2013
_chemical_formula_sum            'C95.5 H110 N4 O9'
_chemical_formula_weight         1457.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.136(2)
_cell_angle_beta                 80.277(2)
_cell_angle_gamma                86.364(2)
_cell_formula_units_Z            2
_cell_length_a                   15.3492(3)
_cell_length_b                   15.6210(4)
_cell_length_c                   17.0234(2)
_cell_measurement_reflns_used    29631
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      71.4855
_cell_measurement_theta_min      3.5904
_cell_volume                     4014.93(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 16.2974
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) x-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            63014
_diffrn_reflns_theta_full        71.62
_diffrn_reflns_theta_max         71.62
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67343
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       prism
_exptl_crystal_F_000             1566
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         15485
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0840
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1794P)^2^+1.9418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2447
_refine_ls_wR_factor_ref         0.2527
_reflns_number_gt                13942
_reflns_number_total             15485
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo4019182_si_001.cif
_cod_data_source_block           mw200_a
_cod_original_formula_sum        'C95.50 H110 N4 O9'
_cod_database_code               4028754