#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:55:43 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179084 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/46/4304629.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_4304629
loop_
_publ_author_name
'Huaze Dong'
'Juan Yang'
'Xia Liu'
'Shaohua Gou'
_publ_section_title
;
Anion-Modulated Reversible Conversion of Molecular Assembly between a
Macrocycle and a Linear Chain
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2913
_journal_page_last               2915
_journal_paper_doi               10.1021/ic702157r
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C20 H16 N6 S2 Hg I2 '
_chemical_formula_sum            'C20 H16 Hg I2 N6 S2'
_chemical_formula_weight         858.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 103.066(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.447(2)
_cell_length_b                   6.8547(8)
_cell_length_c                   22.978(3)
_cell_measurement_reflns_used    1188
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      21.941
_cell_measurement_theta_min      2.547
_cell_volume                     2523.5(5)
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXTL (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker CCD area detector'
_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  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0831
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            6531
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    8.731
_exptl_absorpt_correction_T_max  0.4555
_exptl_absorpt_correction_T_min  0.3741
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.296
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0162P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0732
_reflns_number_gt                1814
_reflns_number_total             2477
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702157r-file002_1.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4304629
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Hg1 Hg 0.0000 0.09981(7) 0.2500 0.04812(17) Uani 1 2 d S . .
I1 I 0.03796(4) -0.03690(10) 0.15224(3) 0.0719(2) Uani 1 1 d . . .
N3 N 0.1020(4) 0.3477(9) 0.2857(3) 0.0508(19) Uani 1 1 d . . .
C9 C 0.1304(5) 0.3664(11) 0.3440(4) 0.048(2) Uani 1 1 d . . .
H9 H 0.1072 0.2882 0.3690 0.058 Uiso 1 1 calc R . .
C7 C 0.1926(6) 0.6025(13) 0.2722(4) 0.067(3) Uani 1 1 d . . .
H7 H 0.2109 0.6880 0.2464 0.080 Uiso 1 1 calc R . .
C8 C 0.1326(6) 0.4657(13) 0.2504(4) 0.061(3) Uani 1 1 d . . .
H8 H 0.1127 0.4554 0.2093 0.073 Uiso 1 1 calc R . .
N1 N 0.1623(4) 0.4706(8) 0.4662(3) 0.0369(16) Uani 1 1 d . . .
C5 C 0.1928(5) 0.4955(11) 0.3699(4) 0.037(2) Uani 1 1 d . . .
C4 C 0.2221(5) 0.5022(10) 0.4359(4) 0.040(2) Uani 1 1 d . . .
C1 C 0.1882(6) 0.4739(10) 0.5253(4) 0.042(2) Uani 1 1 d . . .
C3 C 0.3045(5) 0.5349(10) 0.4645(4) 0.043(2) Uani 1 1 d . . .
H3 H 0.3457 0.5562 0.4434 0.052 Uiso 1 1 calc R . .
C6 C 0.2246(5) 0.6111(11) 0.3314(4) 0.054(2) Uani 1 1 d . . .
H6 H 0.2685 0.6957 0.3464 0.065 Uiso 1 1 calc R . .
S1 S 0.11508(15) 0.4447(3) 0.56976(10) 0.0563(6) Uani 1 1 d . . .
N2 N 0.2652(5) 0.5047(9) 0.5575(3) 0.0485(19) Uani 1 1 d . . .
C2 C 0.3221(6) 0.5341(10) 0.5260(4) 0.052(2) Uani 1 1 d . . .
H2 H 0.3769 0.5554 0.5464 0.062 Uiso 1 1 calc R . .
C10 C 0.0178(5) 0.4085(10) 0.5147(4) 0.053(2) Uani 1 1 d . . .
H10A H 0.0276 0.3185 0.4844 0.063 Uiso 1 1 calc R . .
H10B H -0.0226 0.3490 0.5341 0.063 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 '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
_geom_angle_publ_flag
N3 Hg1 N3 89.8(3) . 2 ?
N3 Hg1 I1 105.17(16) . . ?
N3 Hg1 I1 104.02(16) 2 . ?
N3 Hg1 I1 104.02(16) . 2 ?
N3 Hg1 I1 105.17(16) 2 2 ?
I1 Hg1 I1 138.35(4) . 2 ?
C9 N3 C8 117.7(7) . . ?
C9 N3 Hg1 118.4(5) . . ?
C8 N3 Hg1 123.9(6) . . ?
N3 C9 C5 123.9(7) . . ?
N3 C9 H9 118.1 . . ?
C5 C9 H9 118.1 . . ?
C6 C7 C8 118.9(8) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
N3 C8 C7 122.5(9) . . ?
N3 C8 H8 118.7 . . ?
C7 C8 H8 118.7 . . ?
C1 N1 C4 115.1(7) . . ?
C6 C5 C9 116.3(8) . . ?
C6 C5 C4 123.8(7) . . ?
C9 C5 C4 119.9(7) . . ?
N1 C4 C3 122.2(8) . . ?
N1 C4 C5 114.7(7) . . ?
C3 C4 C5 123.1(8) . . ?
N1 C1 N2 128.0(8) . . ?
N1 C1 S1 119.3(7) . . ?
N2 C1 S1 112.7(7) . . ?
C2 C3 C4 116.2(8) . . ?
C2 C3 H3 121.9 . . ?
C4 C3 H3 121.9 . . ?
C7 C6 C5 120.5(8) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C1 S1 C10 102.8(4) . . ?
C2 N2 C1 114.9(8) . . ?
N2 C2 C3 123.6(9) . . ?
N2 C2 H2 118.2 . . ?
C3 C2 H2 118.2 . . ?
C10 C10 S1 113.4(8) 5_566 . ?
C10 C10 H10A 108.9 5_566 . ?
S1 C10 H10A 108.9 . . ?
C10 C10 H10B 108.9 5_566 . ?
S1 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hg1 N3 2.398(6) . ?
Hg1 N3 2.398(6) 2 ?
Hg1 I1 2.6358(7) . ?
Hg1 I1 2.6358(7) 2 ?
N3 C9 1.320(9) . ?
N3 C8 1.323(9) . ?
C9 C5 1.383(10) . ?
C9 H9 0.9300 . ?
C7 C6 1.345(11) . ?
C7 C8 1.371(11) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
N1 C1 1.328(9) . ?
N1 C4 1.344(9) . ?
C5 C6 1.376(10) . ?
C5 C4 1.485(10) . ?
C4 C3 1.385(10) . ?
C1 N2 1.331(9) . ?
C1 S1 1.756(8) . ?
C3 C2 1.376(11) . ?
C3 H3 0.9300 . ?
C6 H6 0.9300 . ?
S1 C10 1.818(9) . ?
N2 C2 1.322(10) . ?
C2 H2 0.9300 . ?
C10 C10 1.482(13) 5_566 ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
