#------------------------------------------------------------------------------
#$Date: 2017-12-05 15:19:23 +0200 (Tue, 05 Dec 2017) $
#$Revision: 203991 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/77/1547777.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1547777
loop_
_publ_author_name
'Shimizu, Akinori'
'Inoue, Yoshihisa'
'Mori, Tadashi'
_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 H19 N O2 S2'
_chemical_formula_sum            'C17 H19 N O2 S2'
_chemical_formula_weight         333.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 100.2740(17)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   7.6012(6)
_cell_length_b                   10.7068(9)
_cell_length_c                   9.9472(7)
_cell_measurement_reflns_used    6703
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      3.12
_cell_volume                     796.57(11)
_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      296
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7738
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         4.164
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(Walker & Stuart, 1983)'
_exptl_crystal_colour            unknown
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       unknown
_exptl_crystal_F_000             352.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.810
_refine_diff_density_min         -0.761
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1661 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.61200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.271
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2950
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo² + 1.0000σ(Fo²)]/(4Fo²)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1408
_reflns_number_gt                2950
_reflns_number_total             3559
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            jp7b08623_si_002.cif
_cod_data_source_block           PyP-OMe-st
_cod_depositor_comments
'Adding full bibliography for 1547777--1547780.cif.'
_cod_original_cell_volume        796.57(10)
_cod_database_code               1547777
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,-Z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
S(1) S 0.02718(12) 0.06526(12) 1.04326(8) 0.0413(3) Uani 1 2 d .
S(2) S 0.30976(11) 0.03799(13) 0.41245(8) 0.0401(3) Uani 1 2 d .
O(1) O 0.3259(4) 0.3609(3) 0.8943(3) 0.0436(8) Uani 1 2 d .
O(2) O 0.4496(4) -0.1113(3) 0.7095(3) 0.0511(9) Uani 1 2 d .
N(1) N 0.0136(4) 0.2535(4) 0.5979(3) 0.0439(9) Uani 1 2 d .
C(1) C 0.0438(4) 0.1450(4) 0.5390(3) 0.0330(9) Uani 1 2 d .
C(2) C -0.0578(5) 0.2468(5) 0.7128(4) 0.0439(11) Uani 1 2 d .
C(3) C -0.0939(4) 0.1379(5) 0.7739(3) 0.0404(10) Uani 1 2 d .
C(4) C -0.0752(4) 0.0288(4) 0.7057(3) 0.0395(10) Uani 1 2 d .
C(5) C -0.0062(4) 0.0321(4) 0.5847(3) 0.0374(9) Uani 1 2 d .
C(6) C 0.4519(4) 0.1072(4) 0.6813(3) 0.0362(10) Uani 1 2 d .
C(7) C 0.4290(5) 0.2257(4) 0.7279(3) 0.0355(10) Uani 1 2 d .
C(8) C 0.3598(4) 0.2450(4) 0.8483(3) 0.0334(9) Uani 1 2 d .
C(9) C 0.3156(4) 0.1436(4) 0.9202(3) 0.0319(9) Uani 1 2 d .
C(10) C 0.3502(4) 0.0244(4) 0.8790(3) 0.0364(9) Uani 1 2 d .
C(11) C 0.4192(5) 0.0070(4) 0.7583(4) 0.0400(10) Uani 1 2 d .
C(12) C 0.3453(7) 0.4638(4) 0.8077(5) 0.0550(14) Uani 1 2 d .
C(13) C 0.3659(7) -0.2135(5) 0.7612(4) 0.0573(14) Uani 1 2 d .
C(14) C 0.1424(5) 0.1553(4) 0.4192(3) 0.0419(11) Uani 1 2 d .
C(15) C 0.4965(5) 0.0906(4) 0.5393(3) 0.0414(11) Uani 1 2 d .
C(16) C 0.2203(5) 0.1647(4) 1.0407(3) 0.0368(10) Uani 1 2 d .
C(17) C -0.1426(5) 0.1381(5) 0.9162(3) 0.0530(12) Uani 1 2 d .
H(1) H -0.08153 0.32145 0.75387 0.0524 Uiso 1 2 calc R
H(2) H -0.10678 -0.04692 0.74071 0.0473 Uiso 1 2 calc R
H(3) H 0.00524 -0.04002 0.5349 0.0443 Uiso 1 2 calc R
H(4) H 0.45903 0.29377 0.67854 0.0426 Uiso 1 2 calc R
H(5) H 0.32807 -0.04405 0.931 0.0428 Uiso 1 2 calc R
H(6) H 0.18528 0.24061 0.43144 0.0510 Uiso 1 2 calc R
H(7) H 0.04211 0.15641 0.34362 0.0507 Uiso 1 2 calc R
H(8) H 0.59745 0.03403 0.56012 0.0512 Uiso 1 2 calc R
H(9) H 0.54549 0.17221 0.52525 0.0508 Uiso 1 2 calc R
H(10) H 0.19774 0.25372 1.03186 0.0444 Uiso 1 2 calc R
H(11) H 0.31995 0.15423 1.11566 0.0449 Uiso 1 2 calc R
H(12) H -0.26032 0.10024 0.89747 0.0639 Uiso 1 2 calc R
H(13) H -0.16184 0.22693 0.9261 0.0637 Uiso 1 2 calc R
H(14) H 0.2652 0.4537 0.72216 0.0702 Uiso 1 2 calc R
H(15) H 0.31802 0.54014 0.85018 0.0701 Uiso 1 2 calc R
H(16) H 0.46621 0.46666 0.79189 0.0700 Uiso 1 2 calc R
H(17) H 0.2388 -0.20204 0.73832 0.0680 Uiso 1 2 calc R
H(18) H 0.39844 -0.28954 0.72071 0.0679 Uiso 1 2 calc R
H(19) H 0.40099 -0.21825 0.85867 0.0680 Uiso 1 2 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
C C 0.0033 0.0016
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
C(16) S(1) C(17) 102.4(2) yes
C(14) S(2) C(15) 103.23(19) yes
C(8) O(1) C(12) 117.1(3) yes
C(11) O(2) C(13) 117.8(3) yes
C(1) N(1) C(2) 116.7(4) yes
N(1) C(1) C(5) 122.8(3) yes
N(1) C(1) C(14) 115.3(4) yes
C(5) C(1) C(14) 121.9(4) yes
N(1) C(2) C(3) 124.4(4) yes
C(2) C(3) C(4) 117.4(3) yes
C(2) C(3) C(17) 120.9(4) yes
C(4) C(3) C(17) 121.6(4) yes
C(3) C(4) C(5) 119.5(4) yes
C(1) C(5) C(4) 118.5(4) yes
C(7) C(6) C(11) 119.3(3) yes
C(7) C(6) C(15) 119.0(3) yes
C(11) C(6) C(15) 121.5(4) yes
C(6) C(7) C(8) 120.9(4) yes
O(1) C(8) C(7) 122.8(3) yes
O(1) C(8) C(9) 117.8(3) yes
C(7) C(8) C(9) 119.3(4) yes
C(8) C(9) C(10) 119.9(3) yes
C(8) C(9) C(16) 119.1(4) yes
C(10) C(9) C(16) 120.9(3) yes
C(9) C(10) C(11) 119.8(4) yes
O(2) C(11) C(6) 117.4(3) yes
O(2) C(11) C(10) 122.0(4) yes
C(6) C(11) C(10) 120.5(4) yes
S(2) C(14) C(1) 115.4(3) yes
S(2) C(15) C(6) 114.0(3) yes
S(1) C(16) C(9) 115.0(3) yes
S(1) C(17) C(3) 112.7(3) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
S(1) C(16) 1.817(4) yes
S(1) C(17) 1.813(4) yes
S(2) C(14) 1.798(4) yes
S(2) C(15) 1.813(3) yes
O(1) C(8) 1.363(5) yes
O(1) C(12) 1.422(6) yes
O(2) C(11) 1.391(5) yes
O(2) C(13) 1.408(6) yes
N(1) C(1) 1.338(5) yes
N(1) C(2) 1.352(5) yes
C(1) C(5) 1.368(6) yes
C(1) C(14) 1.521(5) yes
C(2) C(3) 1.365(6) yes
C(3) C(4) 1.372(6) yes
C(3) C(17) 1.525(5) yes
C(4) C(5) 1.397(5) yes
C(6) C(7) 1.373(6) yes
C(6) C(11) 1.366(6) yes
C(6) C(15) 1.521(5) yes
C(7) C(8) 1.406(5) yes
C(8) C(9) 1.375(5) yes
C(9) C(10) 1.379(6) yes
C(9) C(16) 1.524(5) yes
C(10) C(11) 1.405(5) yes
