A Combined Experimental and Theoretical Study on the Circular Dichroism of Staggered and Eclipsed Forms of Dimethoxy[2.2]-, [3.2]-, and [3.3]Pyridinophanes and Their Protonated Forms.
Shimizu, Akinori; Inoue, Yoshihisa; Mori, Tadashi; The journal of physical chemistry. A 121 (2017) 8389–8398; doi:10.1021/acs.jpca.7b08623

data_1547778
_publ_section_title
;
 A Combined Experimental and Theoretical Study on the Circular Dichroism
 of Staggered and Eclipsed Forms of Dimethoxy[2.2]-, [3.2]-, and
 [3.3]Pyridinophanes and Their Protonated Forms.
;
_journal_issue                   44
_journal_name_full               'The journal of physical chemistry. A'
_journal_page_first              8389
_journal_page_last               8398
_journal_paper_doi               10.1021/acs.jpca.7b08623
_journal_volume                  121
_journal_year                    2017
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C17 H20 Br N O2 S2'
_chemical_formula_sum            'C17 H20 Br N O2 S2'
_chemical_formula_weight         414.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.5091(5)
_cell_length_b                   15.7579(6)
_cell_length_c                   7.3886(3)
_cell_measurement_reflns_used    12394
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.04
_cell_volume                     1805.71(12)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0964
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4132
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.045
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.522
_exptl_absorpt_correction_T_max  0.777
_exptl_absorpt_correction_T_min  0.238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             848.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
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_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1763 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.003(19)
_refine_ls_extinction_coef       84(23)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3397
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    56.7325    40.0699    37.8806
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0660
_reflns_number_gt                3397
_reflns_number_total             4132
_reflns_threshold_expression     F>2.0\s(F)
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_cod_data_source_block           PyP-OMe-ec-H+
_cod_depositor_comments
'Adding full bibliography for 1547777--1547780.cif.'
_cod_database_code               1547778