#------------------------------------------------------------------------------
#$Date: 2016-06-11 05:14:50 +0300 (Sat, 11 Jun 2016) $
#$Revision: 183354 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/34/1543414.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_1543414
loop_
_publ_author_name
'Kitagawa, Hakuba'
'Ohtsu, Hiroyoshi'
'Cruz-Cabeza, Aurora J.'
'Kawano, Masaki'
_publ_section_title
;
 Isolation and evolution of labile sulfur allotropesviakinetic
 encapsulation in interactive porous networks
;
_journal_issue                   4
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252516008423
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety
'(CuI)1.88 (N1C5H4C6H4)4C (cycro-S3)0.62 (bent-S3)0.39'
_chemical_formula_sum            'C45 H32 Cu1.88 I1.88 N4 S3.01'
_chemical_formula_weight         1083.34
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.8758(4)
_cell_length_b                   26.8758(4)
_cell_length_c                   7.1689(1)
_cell_measurement_reflns_used    52191
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      28.077
_cell_measurement_theta_min      2.698
_cell_volume                     5178.16(13)
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.800
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_Laue_measured_fraction_full 0.936
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            52191
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        28.685
_diffrn_reflns_theta_max         28.077
_diffrn_reflns_theta_min         2.698
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    2.715
_exptl_absorpt_correction_T_max  0.6195
_exptl_absorpt_correction_T_min  0.5871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            'brownish yellow'
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2141
_exptl_crystal_size_max          0.760
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 1625 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.430(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         4353
_refine_ls_number_restraints     397
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.086
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0908P)²+0.1257P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1182
_reflns_Friedel_coverage         0.833
_reflns_Friedel_fraction_full    0.930
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                3852
_reflns_number_total             4353
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ed5008.cif
_cod_data_source_block           300K_S_helical
_cod_original_cell_volume        5178.1(2)
_cod_database_code               1543414
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.232
_shelx_estimated_absorpt_t_max   0.876
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
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_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1X S 0.3957(8) 0.239(2) 0.660(10) 0.30(4) Uani 0.166(12) 1 d D U P A 1
S2X S 0.457(3) 0.284(3) 0.622(17) 0.47(5) Uani 0.166(12) 1 d D U P A 1
S3X S 0.4598(11) 0.2278(15) 0.818(7) 0.187(17) Uani 0.166(12) 1 d D U P A 1
S1B S 0.479(3) 0.250(2) 0.417(19) 0.47(5) Uani 0.193(12) 1 d D U P B 3
S2B S 0.480(2) 0.255(3) 0.152(19) 0.47(4) Uani 0.193(12) 1 d D U P B 3
S3B S 0.419(2) 0.247(3) 0.022(18) 0.49(5) Uani 0.193(12) 1 d D U P B 3
S1A S 0.485(4) 0.228(3) 0.65(2) 0.47(5) Uani 0.143(13) 1 d D U P C 4
S2A S 0.435(3) 0.220(3) 0.42(2) 0.46(5) Uani 0.143(13) 1 d D U P C 4
S3A S 0.489(4) 0.278(4) 0.41(2) 0.46(5) Uani 0.143(13) 1 d D U P C 4
I1 I 0.30489(3) 0.24567(4) 0.61605(13) 0.1105(3) Uani 0.940(9) 1 d . . P . .
Cu1 Cu 0.25078(6) 0.29817(5) 0.3765(2) 0.1081(4) Uani 0.940(9) 1 d . . P A .
C1 C 0.0000 0.5000 1.2500 0.081(4) Uani 1 4 d S TU P . .
C2 C 0.5000 0.5000 -0.5000 0.092(5) Uani 1 4 d S TU P . .
N1A N 0.2026(4) 0.3409(4) 0.5329(13) 0.109(3) Uani 1 1 d D . . A 1
C2A C 0.1585(7) 0.3554(8) 0.470(2) 0.151(7) Uani 1 1 d D U . A 1
H2AA H 0.1490 0.3458 0.3503 0.181 Uiso 1 1 calc R U . A 1
C3A C 0.1263(5) 0.3842(6) 0.5738(16) 0.123(4) Uani 1 1 d D U . A 1
H3AA H 0.0971 0.3963 0.5210 0.147 Uiso 1 1 calc R U . A 1
C4A C 0.1378(4) 0.3949(4) 0.7562(14) 0.093(3) Uani 1 1 d D U . A 1
C5A C 0.1819(5) 0.3770(6) 0.8207(18) 0.129(5) Uani 1 1 d D U . A 1
H5AA H 0.1906 0.3827 0.9444 0.154 Uiso 1 1 calc R U . A 1
C6A C 0.2141(5) 0.3507(7) 0.7084(17) 0.135(6) Uani 1 1 d D U . A 1
H6AA H 0.2443 0.3398 0.7566 0.162 Uiso 1 1 calc R U . A 1
C7A C 0.1044(3) 0.4239(3) 0.8815(13) 0.087(2) Uani 1 1 d D U . A 1
C8A C 0.1218(4) 0.4546(4) 1.0209(14) 0.095(3) Uani 1 1 d D U . A 1
H8AA H 0.1559 0.4590 1.0346 0.115 Uiso 1 1 calc R U . A 1
C9A C 0.0894(3) 0.4796(4) 1.1428(13) 0.091(2) Uani 1 1 d D U . A 1
H9AA H 0.1022 0.4998 1.2364 0.109 Uiso 1 1 calc R U . A 1
C10A C 0.0385(3) 0.4741(3) 1.1240(13) 0.083(2) Uani 1 1 d D U . A 1
C11A C 0.0211(4) 0.4434(4) 0.9792(13) 0.088(2) Uani 1 1 d D U . A 1
H11A H -0.0130 0.4395 0.9644 0.105 Uiso 1 1 calc R U . A 1
C12A C 0.0527(4) 0.4186(4) 0.8573(13) 0.095(2) Uani 1 1 d D U . A 1
H12A H 0.0400 0.3989 0.7619 0.114 Uiso 1 1 calc R U . A 1
N1B N 0.3031(5) 0.3376(4) 0.2311(13) 0.110(3) Uani 0.651(18) 1 d D . P A 1
C2B C 0.3159(10) 0.3202(8) 0.069(3) 0.128(7) Uani 0.651(18) 1 d D U P A 1
H2BA H 0.3025 0.2900 0.0304 0.153 Uiso 0.651(18) 1 calc R U P A 1
C3B C 0.3488(10) 0.3449(7) -0.048(3) 0.113(6) Uani 0.651(18) 1 d D U P A 1
H3BA H 0.3584 0.3302 -0.1598 0.135 Uiso 0.651(18) 1 calc R U P A 1
C4B C 0.3672(4) 0.3902(5) -0.0014(17) 0.104(3) Uani 0.651(18) 1 d D U P A 1
C5B C 0.3607(10) 0.4034(9) 0.184(2) 0.125(7) Uani 0.651(18) 1 d D U P A 1
H5BA H 0.3788 0.4295 0.2361 0.150 Uiso 0.651(18) 1 calc R U P A 1
C6B C 0.3272(9) 0.3773(8) 0.290(3) 0.123(7) Uani 0.651(18) 1 d D U P A 1
H6BA H 0.3210 0.3883 0.4106 0.148 Uiso 0.651(18) 1 calc R U P A 1
C7B C 0.4023(4) 0.4170(4) -0.1266(16) 0.098(3) Uani 1 1 d D U . A 1
C8B C 0.4083(4) 0.4682(4) -0.1078(16) 0.103(3) Uani 1 1 d D U . A 1
H8BA H 0.3911 0.4855 -0.0155 0.124 Uiso 1 1 calc R U . A 1
C9B C 0.4402(4) 0.4934(4) -0.2286(14) 0.098(3) Uani 1 1 d D U . A 1
H9BA H 0.4445 0.5275 -0.2139 0.117 Uiso 1 1 calc R U . A 1
C10B C 0.4658(4) 0.4691(4) -0.3703(13) 0.094(2) Uani 1 1 d D U . A 1
C11B C 0.4595(4) 0.4179(4) -0.3882(18) 0.107(3) Uani 1 1 d D U . A 1
H11B H 0.4770 0.4002 -0.4782 0.129 Uiso 1 1 calc R U . A 1
C12B C 0.4269(5) 0.3941(5) -0.2695(18) 0.116(4) Uani 1 1 d D U . A 1
H12B H 0.4212 0.3603 -0.2881 0.139 Uiso 1 1 calc R U . A 1
N1Y N 0.3031(5) 0.3376(4) 0.2311(13) 0.110(3) Uani 0.349(18) 1 d D . P A 2
C2Y C 0.3427(13) 0.3167(11) 0.161(6) 0.131(11) Uani 0.349(18) 1 d D U P A 2
H2YA H 0.3501 0.2843 0.1972 0.158 Uiso 0.349(18) 1 calc R U P A 2
C3Y C 0.3744(13) 0.3397(9) 0.036(6) 0.111(8) Uani 0.349(18) 1 d D U P A 2
H3YA H 0.3998 0.3221 -0.0217 0.133 Uiso 0.349(18) 1 calc R U P A 2
C4Y C 0.3672(4) 0.3902(5) -0.0014(17) 0.104(3) Uani 0.349(18) 1 d D U P A 2
C5Y C 0.3267(11) 0.4107(10) 0.082(5) 0.112(9) Uani 0.349(18) 1 d D U P A 2
H5YA H 0.3209 0.4446 0.0661 0.134 Uiso 0.349(18) 1 calc R U P A 2
C6Y C 0.2939(11) 0.3836(10) 0.188(5) 0.115(9) Uani 0.349(18) 1 d D U P A 2
H6YA H 0.2647 0.3984 0.2298 0.138 Uiso 0.349(18) 1 calc R U P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0043 0.0021 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2655 1.5610 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.2698 2.2366 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0082 0.0043 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1506 0.1570 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 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_site_symmetry_1
_geom_angle_site_symmetry_3
S2X S1X S3X 59.8(8) . .
S2X S1X I1 137(3) . .
S3X S1X I1 154(4) . .
S3X S2X S1X 60.2(8) . .
S2X S3X S1X 60.0(8) . .
S1B S2B S3B 117(2) . .
S2A S1A S3A 59.7(8) . .
S3A S2A S1A 60.1(8) . .
S2A S3A S1A 60.2(8) . .
S1X I1 Cu1 131.7(15) . .
S1X I1 Cu1 115.5(16) . 6
Cu1 I1 Cu1 112.35(3) . 6
N1B Cu1 N1A 114.9(4) . .
N1B Cu1 I1 103.2(3) . .
N1A Cu1 I1 106.7(3) . .
N1B Cu1 I1 104.9(3) . 6_554
N1A Cu1 I1 105.9(3) . 6_554
I1 Cu1 I1 121.67(5) . 6_554
C10A C1 C10A 110.1(4) . 8_557
C10A C1 C10A 108.1(7) . 2_565
C10A C1 C10A 110.1(4) 8_557 2_565
C10A C1 C10A 110.1(4) . 7_457
C10A C1 C10A 108.1(7) 8_557 7_457
C10A C1 C10A 110.1(4) 2_565 7_457
C10B C2 C10B 111.1(4) 2_665 4_654
C10B C2 C10B 111.1(4) 2_665 3_564
C10B C2 C10B 106.2(8) 4_654 3_564
C10B C2 C10B 106.2(8) 2_665 .
C10B C2 C10B 111.1(4) 4_654 .
C10B C2 C10B 111.1(4) 3_564 .
C6A N1A C2A 118.4(11) . .
C6A N1A Cu1 118.8(9) . .
C2A N1A Cu1 122.6(9) . .
N1A C2A C3A 122.6(13) . .
C4A C3A C2A 119.4(12) . .
C5A C4A C3A 116.5(11) . .
C5A C4A C7A 120.3(9) . .
C3A C4A C7A 123.2(10) . .
C4A C5A C6A 122.0(11) . .
N1A C6A C5A 120.7(13) . .
C8A C7A C12A 118.9(8) . .
C8A C7A C4A 123.2(9) . .
C12A C7A C4A 117.9(9) . .
C7A C8A C9A 121.8(9) . .
C10A C9A C8A 120.2(9) . .
C9A C10A C11A 117.5(9) . .
C9A C10A C1 124.0(7) . .
C11A C10A C1 118.5(7) . .
C12A C11A C10A 123.0(9) . .
C11A C12A C7A 118.5(9) . .
C2B N1B C6B 116.6(13) . .
C2B N1B Cu1 116.8(11) . .
C6B N1B Cu1 126.5(9) . .
N1B C2B C3B 122.5(15) . .
C4B C3B C2B 120.8(13) . .
C3B C4B C5B 114.9(13) . .
C3B C4B C7B 121.1(11) . .
C5B C4B C7B 122.2(12) . .
C6B C5B C4B 118.6(17) . .
N1B C6B C5B 124.2(16) . .
C12B C7B C8B 117.6(10) . .
C12B C7B C4B 122.7(11) . .
C8B C7B C4B 119.6(9) . .
C7B C8B C9B 119.4(10) . .
C10B C9B C8B 122.0(11) . .
C9B C10B C11B 118.2(10) . .
C9B C10B C2 118.7(9) . .
C11B C10B C2 123.1(8) . .
C12B C11B C10B 118.6(10) . .
C7B C12B C11B 124.1(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1X S2X 2.08(5) .
S1X S3X 2.08(4) .
S1X I1 2.47(2) .
S2X S3X 2.07(5) .
S1B S2B 1.91(3) .
S2B S3B 1.91(3) .
S1A S2A 2.15(10) .
S1A S3A 2.15(10) .
S2A S3A 2.14(10) .
I1 Cu1 2.6563(17) .
I1 Cu1 2.6669(18) 6
Cu1 N1B 2.046(11) .
Cu1 N1A 2.062(9) .
Cu1 I1 2.6669(18) 6_554
C1 C10A 1.539(9) .
C1 C10A 1.539(9) 8_557
C1 C10A 1.539(9) 2_565
C1 C10A 1.539(9) 7_457
C2 C10B 1.549(10) 2_665
C2 C10B 1.549(10) 4_654
C2 C10B 1.549(10) 3_564
C2 C10B 1.549(10) .
N1A C6A 1.322(15) .
N1A C2A 1.327(17) .
C2A C3A 1.381(17) .
C3A C4A 1.373(15) .
C4A C5A 1.359(15) .
C4A C7A 1.490(13) .
C5A C6A 1.377(16) .
C7A C8A 1.379(14) .
C7A C12A 1.407(13) .
C8A C9A 1.404(13) .
C9A C10A 1.383(12) .
C10A C11A 1.406(13) .
C11A C12A 1.389(13) .
N1B C2B 1.296(18) .
N1B C6B 1.317(18) .
C2B C3B 1.391(19) .
C3B C4B 1.355(19) .
C4B C5B 1.389(18) .
C4B C7B 1.489(15) .
C5B C6B 1.37(2) .
C7B C12B 1.365(14) .
C7B C8B 1.393(14) .
C8B C9B 1.394(14) .
C9B C10B 1.390(13) .
C10B C11B 1.391(15) .
C11B C12B 1.381(15) .
C2Y C3Y 1.38(2) .
C5Y C6Y 1.37(2) .
