#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:17:34 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179622 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/86/4508677.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_4508677
loop_
_publ_author_name
'Zhang, Xuanjun'
'Zhou, Xiao-Ping'
'Li, Dan'
_publ_section_title
;
 Anion-Directed Assembly of Macrocycle and Helix
;
_journal_issue                   6
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1440
_journal_paper_doi               10.1021/cg060076s
_journal_volume                  6
_journal_year                    2006
_chemical_formula_sum            'C28 H36 Cd Cl2 N8 O2 S2'
_chemical_formula_weight         764.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 105.951(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.428(4)
_cell_length_b                   22.396(9)
_cell_length_c                   7.908(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1605.5(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4842
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    1.017
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.65
_exptl_crystal_size_min          0.60
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0340
_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)+(0.0666P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                1715
_reflns_number_total             1861
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg060076ssup3.cif
_cod_data_source_block           0713am
_cod_original_cell_volume        1605.5(12)
_cod_database_code               4508677
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cd1 Cd 1.0000 1.0000 0.5000 0.02777(16) Uani 1 4 d S
Cl1 Cl 0.84181(11) 1.0000 0.17362(12) 0.0359(2) Uani 1 2 d S
N1 N 0.8551(2) 0.92098(10) 0.5721(3) 0.0332(5) Uani 1 1 d .
N2 N 0.6146(3) 0.87893(12) 0.9822(4) 0.0399(6) Uani 1 1 d .
S1 S 0.5000 0.77157(5) 1.0000 0.0461(3) Uani 1 2 d S
C1 C 0.7899(4) 0.88205(14) 0.4469(4) 0.0424(7) Uani 1 1 d .
H1 H 0.7974 0.8882 0.3334 0.051 Uiso 1 1 calc R
C2 C 0.7126(4) 0.83362(15) 0.4776(4) 0.0487(8) Uani 1 1 d .
H2 H 0.6690 0.8075 0.3868 0.058 Uiso 1 1 calc R
C3 C 0.7002(4) 0.82393(14) 0.6456(4) 0.0436(7) Uani 1 1 d .
H3 H 0.6482 0.7911 0.6690 0.052 Uiso 1 1 calc R
C4 C 0.7654(3) 0.86323(12) 0.7778(3) 0.0306(5) Uani 1 1 d .
C5 C 0.8418(3) 0.91080(12) 0.7346(3) 0.0308(5) Uani 1 1 d .
H5 H 0.8868 0.9374 0.8233 0.037 Uiso 1 1 calc R
C6 C 0.7529(3) 0.85593(14) 0.9621(4) 0.0359(6) Uani 1 1 d .
H6A H 0.7609 0.8139 0.9930 0.043 Uiso 1 1 calc R
H6B H 0.8340 0.8767 1.0428 0.043 Uiso 1 1 calc R
C7 C 0.5000 0.84650(16) 1.0000 0.0292(7) Uani 1 2 d S
O1 O 0.4910(6) 0.0000 0.8153(9) 0.1035(19) Uani 1 2 d S
H1A H 0.4091 0.0119 0.8167 0.155 Uiso 0.50 1 calc PR
C8 C 0.5017(17) 0.0000 0.640(2) 0.301(12) Uani 1 2 d S
H8A H 0.5753 -0.0283 0.6296 0.452 Uiso 0.50 1 calc PR
H8B H 0.5290 0.0391 0.6108 0.452 Uiso 0.50 1 calc PR
H8C H 0.4082 -0.0109 0.5617 0.452 Uiso 0.50 1 calc PR
H1N H 0.605(4) 0.9137(16) 0.972(4) 0.043(9) Uiso 1 1 d .
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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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
N1 Cd1 N1 95.12(11) 5_776 2_756
N1 Cd1 N1 180.0 5_776 .
N1 Cd1 N1 84.88(11) 2_756 .
N1 Cd1 N1 84.88(11) 5_776 6_575
N1 Cd1 N1 180.000(1) 2_756 6_575
N1 Cd1 N1 95.12(11) . 6_575
N1 Cd1 Cl1 91.56(6) 5_776 5_776
N1 Cd1 Cl1 91.56(6) 2_756 5_776
N1 Cd1 Cl1 88.44(6) . 5_776
N1 Cd1 Cl1 88.44(6) 6_575 5_776
N1 Cd1 Cl1 88.44(6) 5_776 .
N1 Cd1 Cl1 88.44(6) 2_756 .
N1 Cd1 Cl1 91.56(6) . .
N1 Cd1 Cl1 91.56(6) 6_575 .
Cl1 Cd1 Cl1 180.0 5_776 .
C1 N1 C5 116.9(2) . .
C1 N1 Cd1 118.82(18) . .
C5 N1 Cd1 124.16(17) . .
C7 N2 C6 126.4(3) . .
C7 N2 H1N 118(3) . .
C6 N2 H1N 115(3) . .
N1 C1 C2 123.1(3) . .
N1 C1 H1 118.4 . .
C2 C1 H1 118.4 . .
C1 C2 C3 119.1(3) . .
C1 C2 H2 120.5 . .
C3 C2 H2 120.5 . .
C4 C3 C2 119.5(3) . .
C4 C3 H3 120.3 . .
C2 C3 H3 120.3 . .
C3 C4 C5 117.4(3) . .
C3 C4 C6 122.0(3) . .
C5 C4 C6 120.6(2) . .
N1 C5 C4 124.0(2) . .
N1 C5 H5 118.0 . .
C4 C5 H5 118.0 . .
N2 C6 C4 112.3(2) . .
N2 C6 H6A 109.1 . .
C4 C6 H6A 109.1 . .
N2 C6 H6B 109.1 . .
C4 C6 H6B 109.1 . .
H6A C6 H6B 107.9 . .
N2 C7 N2 114.4(4) . 2_657
N2 C7 S1 122.79(18) . .
N2 C7 S1 122.79(18) 2_657 .
C8 O1 H1A 109.5 . .
O1 C8 H8A 109.5 . .
O1 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
O1 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 N1 2.398(2) 5_776
Cd1 N1 2.398(2) 2_756
Cd1 N1 2.398(2) .
Cd1 N1 2.398(2) 6_575
Cd1 Cl1 2.6021(13) 5_776
Cd1 Cl1 2.6021(13) .
N1 C1 1.336(4) .
N1 C5 1.344(3) .
N2 C7 1.341(3) .
N2 C6 1.450(4) .
N2 H1N 0.79(4) .
S1 C7 1.678(4) .
C1 C2 1.365(4) .
C1 H1 0.9300 .
C2 C3 1.382(4) .
C2 H2 0.9300 .
C3 C4 1.376(4) .
C3 H3 0.9300 .
C4 C5 1.381(4) .
C4 C6 1.503(3) .
C5 H5 0.9300 .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 N2 1.341(3) 2_657
O1 C8 1.416(12) .
O1 H1A 0.8200 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1 Cd1 N1 C1 43(100) 5_776 .
N1 Cd1 N1 C1 -59.8(2) 2_756 .
N1 Cd1 N1 C1 120.2(2) 6_575 .
Cl1 Cd1 N1 C1 -151.6(2) 5_776 .
Cl1 Cd1 N1 C1 28.4(2) . .
N1 Cd1 N1 C5 -141(100) 5_776 .
N1 Cd1 N1 C5 116.0(2) 2_756 .
N1 Cd1 N1 C5 -64.0(2) 6_575 .
Cl1 Cd1 N1 C5 24.3(2) 5_776 .
Cl1 Cd1 N1 C5 -155.7(2) . .
C5 N1 C1 C2 -0.2(5) . .
Cd1 N1 C1 C2 176.0(3) . .
N1 C1 C2 C3 0.2(6) . .
C1 C2 C3 C4 0.2(5) . .
C2 C3 C4 C5 -0.4(5) . .
C2 C3 C4 C6 178.6(3) . .
C1 N1 C5 C4 -0.2(4) . .
Cd1 N1 C5 C4 -176.07(19) . .
C3 C4 C5 N1 0.5(4) . .
C6 C4 C5 N1 -178.6(3) . .
C7 N2 C6 C4 106.8(3) . .
C3 C4 C6 N2 -81.4(4) . .
C5 C4 C6 N2 97.6(3) . .
C6 N2 C7 N2 179.5(3) . 2_657
C6 N2 C7 S1 -0.5(3) . .
