#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/54/4325442.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_4325442
loop_
_publ_author_name
'Eunji Lee'
'Shim Sung Lee'
_publ_section_title
;
 Rational Approach to Endo/Exocoordinated Heteronuclear Macrocyclic
 network: Supramolecular Hg(ll), Cu(ll), and Hg(ll)/Cu(ll) Complexes of a
 NS4 Macrocycle
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5803
_journal_page_last               5807
_journal_paper_doi               10.1021/ic200684x
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C19 H23 n S4'
_chemical_formula_sum            'C19 H23 S4 n'
_chemical_formula_weight         393.62
_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                 97.035(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.93(3)
_cell_length_b                   5.602(6)
_cell_length_c                   22.55(2)
_cell_measurement_reflns_used    3411
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.56
_cell_measurement_theta_min      2.35
_cell_volume                     4003(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0923
_diffrn_reflns_av_sigmaI/netI    0.0790
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15256
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.476
_exptl_absorpt_correction_T_max  0.9235
_exptl_absorpt_correction_T_min  0.8985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0585
_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)+(0.0761P)²+10.4031P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1804
_reflns_number_gt                2477
_reflns_number_total             3911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200684x_si_002_1.cif
_cod_data_source_block           L
_cod_original_cell_volume        4005(7)
_cod_original_formula_sum        'C19 H23 n S4'
_cod_database_code               4325442
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
S1 S 0.37983(4) 0.3766(3) 0.23801(5) 0.0482(4) Uani 1 1 d .
S2 S 0.43596(4) -0.0929(3) 0.38703(6) 0.0516(4) Uani 1 1 d .
S3 S 0.21667(3) 0.5601(2) 0.19001(5) 0.0362(3) Uani 1 1 d .
S4 S 0.15544(3) 0.0363(2) 0.05817(4) 0.0337(3) Uani 1 1 d .
C1 C 0.46994(12) 0.1576(8) 0.17126(17) 0.0380(10) Uani 0.50 1 d P
H1A H 0.4835 0.1391 0.2109 0.046 Uiso 0.50 1 calc PR
N1 n 0.46994(12) 0.1576(8) 0.17126(17) 0.0380(10) Uani 0.50 1 d P
C2 C 0.48034(13) 0.0117(9) 0.12659(19) 0.0403(11) Uani 1 1 d .
C3 C 0.46063(14) 0.0390(11) 0.0680(2) 0.0528(14) Uani 1 1 d .
H3A H 0.4679 -0.0633 0.0373 0.063 Uiso 1 1 calc R
C4 C 0.43061(15) 0.2155(11) 0.0551(2) 0.0588(16) Uani 1 1 d .
H4A H 0.4172 0.2353 0.0154 0.071 Uiso 1 1 calc R
C5 C 0.42013(14) 0.3638(10) 0.1005(2) 0.0498(13) Uani 1 1 d .
H5A H 0.3998 0.4866 0.0920 0.060 Uiso 1 1 calc R
C6 C 0.43975(13) 0.3308(9) 0.15857(19) 0.0393(11) Uani 1 1 d .
C7 C 0.42758(15) 0.4840(9) 0.2093(2) 0.0475(12) Uani 1 1 d .
H7A H 0.4230 0.6501 0.1950 0.057 Uiso 1 1 calc R
H7B H 0.4512 0.4853 0.2422 0.057 Uiso 1 1 calc R
C8 C 0.39974(14) 0.1156(9) 0.28012(19) 0.0417(11) Uani 1 1 d .
H8A H 0.3761 0.0042 0.2833 0.050 Uiso 1 1 calc R
H8B H 0.4204 0.0330 0.2579 0.050 Uiso 1 1 calc R
C9 C 0.42091(14) 0.1746(9) 0.34296(19) 0.0405(11) Uani 1 1 d .
H9A H 0.4013 0.2711 0.3639 0.049 Uiso 1 1 calc R
H9B H 0.4464 0.2721 0.3398 0.049 Uiso 1 1 calc R
C10 C 0.48550(14) -0.1728(10) 0.3589(2) 0.0494(13) Uani 1 1 d .
H10A H 0.4955 -0.3277 0.3765 0.059 Uiso 1 1 calc R
H10B H 0.4802 -0.1932 0.3151 0.059 Uiso 1 1 calc R
N11 n 0.28702(11) 0.5063(7) 0.08060(15) 0.0296(9) Uani 0.50 1 d P
C11 C 0.28702(11) 0.5063(7) 0.08060(15) 0.0296(9) Uani 0.50 1 d P
H11A H 0.2729 0.3584 0.0726 0.036 Uiso 0.50 1 calc PR
C12 C 0.30345(12) 0.6288(8) 0.03487(18) 0.0310(10) Uani 1 1 d .
C13 C 0.32518(13) 0.8393(8) 0.04681(18) 0.0338(10) Uani 1 1 d .
H13A H 0.3369 0.9206 0.0157 0.041 Uiso 1 1 calc R
C14 C 0.33002(14) 0.9329(8) 0.10439(19) 0.0393(11) Uani 1 1 d .
H14A H 0.3451 1.0776 0.1127 0.047 Uiso 1 1 calc R
C15 C 0.31254(13) 0.8130(8) 0.15012(18) 0.0351(10) Uani 1 1 d .
H15A H 0.3152 0.8772 0.1894 0.042 Uiso 1 1 calc R
C16 C 0.29129(12) 0.5999(8) 0.13744(17) 0.0302(10) Uani 1 1 d .
C17 C 0.27134(13) 0.4672(9) 0.18505(18) 0.0367(10) Uani 1 1 d .
H17A H 0.2884 0.4941 0.2242 0.044 Uiso 1 1 calc R
H17B H 0.2718 0.2940 0.1764 0.044 Uiso 1 1 calc R
C18 C 0.18907(13) 0.4300(8) 0.12202(17) 0.0308(9) Uani 1 1 d .
H18A H 0.1628 0.5211 0.1103 0.037 Uiso 1 1 calc R
H18B H 0.2070 0.4452 0.0894 0.037 Uiso 1 1 calc R
C19 C 0.17805(13) 0.1690(8) 0.12926(17) 0.0341(10) Uani 1 1 d .
H19A H 0.1575 0.1548 0.1586 0.041 Uiso 1 1 calc R
H19B H 0.2038 0.0800 0.1450 0.041 Uiso 1 1 calc R
C20 C 0.20459(12) -0.0240(9) 0.02745(18) 0.0369(11) Uani 1 1 d .
H20A H 0.2208 0.1263 0.0261 0.044 Uiso 1 1 calc R
H20B H 0.2218 -0.1369 0.0539 0.044 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'
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
C8 S1 C7 101.3(2) . .
C9 S2 C10 101.1(2) . .
C18 S3 C17 101.57(19) . .
C20 S4 C19 98.2(2) . .
C2 C1 C6 119.7(4) . .
C1 C2 C3 120.5(4) . .
C1 C2 C10 118.9(4) . 2_655
C3 C2 C10 120.5(4) . 2_655
C4 C3 C2 119.8(5) . .
C3 C4 C5 119.6(4) . .
C4 C5 C6 119.5(5) . .
C1 C6 C5 120.9(4) . .
C1 C6 C7 118.7(4) . .
C5 C6 C7 120.4(4) . .
C6 C7 S1 112.5(3) . .
C9 C8 S1 113.4(3) . .
C8 C9 S2 112.5(3) . .
C2 C10 S2 113.0(4) 2_655 .
C16 n11 C12 119.9(4) . .
C13 C12 n11 120.2(4) . .
C13 C12 C20 122.5(4) . 7
N11 C12 C20 117.3(4) . 7
C12 C13 C14 120.0(4) . .
C13 C14 C15 119.8(4) . .
C16 C15 C14 119.3(4) . .
N11 C16 C15 120.7(4) . .
N11 C16 C17 118.2(4) . .
C15 C16 C17 121.1(4) . .
C16 C17 S3 113.0(3) . .
C19 C18 S3 112.9(3) . .
C18 C19 S4 111.6(3) . .
C12 C20 S4 111.6(3) 7 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 C8 1.816(5) .
S1 C7 1.830(5) .
S2 C9 1.830(5) .
S2 C10 1.830(5) .
S3 C18 1.824(4) .
S3 C17 1.838(5) .
S4 C20 1.823(4) .
S4 C19 1.833(4) .
C1 C2 1.370(6) .
C1 C6 1.373(6) .
C2 C3 1.400(6) .
C2 C10 1.509(7) 2_655
C3 C4 1.383(7) .
C4 C5 1.391(7) .
C5 C6 1.393(6) .
C6 C7 1.518(6) .
C8 C9 1.530(6) .
C10 C2 1.509(7) 2_655
N11 C16 1.376(5) .
N11 C12 1.394(5) .
C12 C13 1.378(6) .
C12 C20 1.516(6) 7
C13 C14 1.391(6) .
C14 C15 1.403(6) .
C15 C16 1.385(6) .
C16 C17 1.510(6) .
C18 C19 1.518(6) .
C20 C12 1.516(6) 7
