#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:02:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179464 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/61/4336100.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_4336100
loop_
_publ_author_name
'Li Yu'
'Mian Li'
'Xiao-Ping Zhou'
'Dan Li'
_publ_section_title
;
 Hybrid Inorganic-Organic Polyrotaxane, Pseudorotaxane, and Sandwich
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10232
_journal_page_last               10234
_journal_paper_doi               10.1021/ic401722c
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C22 H16 Cu2 N6 S4'
_chemical_formula_weight         619.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                112.967(7)
_cell_angle_beta                 101.238(8)
_cell_angle_gamma                96.815(9)
_cell_formula_units_Z            2
_cell_length_a                   9.7147(11)
_cell_length_b                   11.6888(11)
_cell_length_c                   12.1026(6)
_cell_measurement_temperature    293(2)
_cell_volume                     1211.9(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9723
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    2.124
_exptl_absorpt_correction_T_max  0.346
_exptl_absorpt_correction_T_min  0.117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0612P)²+0.4635P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1386
_reflns_number_gt                3662
_reflns_number_total             5348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401722c_si_001_1.cif
_cod_data_source_block           complex_3
_cod_original_cell_volume        1211.90(19)
_cod_database_code               4336100
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C -0.4140(4) 0.8004(4) -0.0339(3) 0.0485(8) Uani 1 1 d .
H1A H -0.5089 0.7883 -0.0205 0.058 Uiso 1 1 calc R
H1B H -0.3951 0.8806 -0.0404 0.058 Uiso 1 1 calc R
C2 C -0.3207(4) 0.7084(4) 0.1078(3) 0.0467(8) Uani 1 1 d .
H2 H -0.4063 0.6476 0.0724 0.056 Uiso 1 1 calc R
C3 C -0.2132(4) 0.6987(4) 0.1934(3) 0.0459(8) Uani 1 1 d .
H3 H -0.2261 0.6309 0.2153 0.055 Uiso 1 1 calc R
C4 C -0.0851(3) 0.7893(3) 0.2477(3) 0.0397(7) Uani 1 1 d .
C5 C -0.0761(4) 0.8935(4) 0.2193(3) 0.0484(8) Uani 1 1 d .
H5 H 0.0042 0.9602 0.2595 0.058 Uiso 1 1 calc R
C6 C -0.1863(4) 0.8978(4) 0.1315(3) 0.0482(8) Uani 1 1 d .
H6 H -0.1788 0.9671 0.1115 0.058 Uiso 1 1 calc R
C7 C 0.0388(3) 0.7654(3) 0.3227(3) 0.0399(7) Uani 1 1 d .
C8 C 0.0177(4) 0.6957(4) 0.3903(3) 0.0482(9) Uani 1 1 d .
H8 H -0.0728 0.6759 0.4013 0.058 Uiso 1 1 calc R
C9 C 0.1303(4) 0.6560(4) 0.4408(3) 0.0499(9) Uani 1 1 d .
H9 H 0.1149 0.6076 0.4844 0.060 Uiso 1 1 calc R
C10 C 0.2868(4) 0.7590(4) 0.3706(3) 0.0479(8) Uani 1 1 d .
H10 H 0.3799 0.7829 0.3668 0.057 Uiso 1 1 calc R
C11 C 0.1775(4) 0.8001(4) 0.3161(3) 0.0447(8) Uani 1 1 d .
H11 H 0.1963 0.8506 0.2753 0.054 Uiso 1 1 calc R
C12 C 0.3791(4) 0.6269(4) 0.4722(3) 0.0496(9) Uani 1 1 d .
H12A H 0.4694 0.6891 0.5090 0.060 Uiso 1 1 calc R
H12B H 0.3566 0.6018 0.5353 0.060 Uiso 1 1 calc R
C13 C 0.3933(3) 0.5127(4) 0.3645(3) 0.0426(8) Uani 1 1 d .
C14 C 0.3029(4) 0.3948(4) 0.3217(3) 0.0507(9) Uani 1 1 d .
H14 H 0.2359 0.3839 0.3641 0.061 Uiso 1 1 calc R
C15 C 0.3106(4) 0.2931(4) 0.2173(3) 0.0483(8) Uani 1 1 d .
H15 H 0.2486 0.2148 0.1900 0.058 Uiso 1 1 calc R
C16 C 0.4098(3) 0.3066(4) 0.1527(3) 0.0423(8) Uani 1 1 d .
C17 C 0.5032(3) 0.4230(4) 0.1983(3) 0.0486(9) Uani 1 1 d .
H17 H 0.5732 0.4327 0.1581 0.058 Uiso 1 1 calc R
C18 C 0.4950(4) 0.5250(4) 0.3019(3) 0.0511(9) Uani 1 1 d .
H18 H 0.5583 0.6028 0.3300 0.061 Uiso 1 1 calc R
C19 C 0.3184(5) 1.0850(4) 0.5511(4) 0.0641(11) Uani 1 1 d .
C20 C 0.2329(4) 0.7435(4) 0.7362(3) 0.0538(9) Uani 1 1 d .
C21 C 0.2735(6) 0.9275(4) 1.0940(4) 0.0626(11) Uani 1 1 d .
C22 C 0.1683(3) 0.5135(4) 1.0736(3) 0.0430(8) Uani 1 1 d .
Cu1 Cu 0.42352(7) 0.96751(6) 0.72715(5) 0.0757(2) Uani 1 1 d .
Cu2 Cu 0.08773(5) 0.66081(5) 0.91901(5) 0.06055(19) Uani 1 1 d .
N1 N -0.3035(3) 0.8047(3) 0.0747(2) 0.0414(6) Uani 1 1 d .
N2 N 0.2620(3) 0.6852(3) 0.4289(2) 0.0429(7) Uani 1 1 d .
N3 N 0.3609(4) 1.0409(4) 0.6169(4) 0.0767(11) Uani 1 1 d .
N4 N 0.3076(4) 0.8314(4) 0.7412(3) 0.0670(9) Uani 1 1 d .
N5 N 0.3900(5) 0.9620(4) 1.1562(4) 0.0776(11) Uani 1 1 d .
N6 N 0.0908(3) 0.4457(4) 1.0922(3) 0.0597(9) Uani 1 1 d .
S1 S 0.26005(15) 1.15038(13) 0.45865(12) 0.0847(4) Uani 1 1 d .
S2 S 0.12697(12) 0.61484(12) 0.71952(10) 0.0683(3) Uani 1 1 d .
S3 S 0.10925(13) 0.88179(13) 1.00676(13) 0.0761(4) Uani 1 1 d .
S4 S 0.27595(9) 0.61439(10) 1.04653(8) 0.0478(2) Uani 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'
Cu Cu 0.3201 1.2651 '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
C16 C1 N1 110.4(3) 2_565 .
C16 C1 H1A 109.6 2_565 .
N1 C1 H1A 109.6 . .
C16 C1 H1B 109.6 2_565 .
N1 C1 H1B 109.6 . .
H1A C1 H1B 108.1 . .
N1 C2 C3 120.6(3) . .
N1 C2 H2 119.7 . .
C3 C2 H2 119.7 . .
C2 C3 C4 120.4(3) . .
C2 C3 H3 119.8 . .
C4 C3 H3 119.8 . .
C5 C4 C3 117.4(3) . .
C5 C4 C7 123.0(3) . .
C3 C4 C7 119.4(3) . .
C6 C5 C4 119.7(3) . .
C6 C5 H5 120.1 . .
C4 C5 H5 120.1 . .
N1 C6 C5 121.2(3) . .
N1 C6 H6 119.4 . .
C5 C6 H6 119.4 . .
C8 C7 C11 118.0(3) . .
C8 C7 C4 120.8(3) . .
C11 C7 C4 120.7(3) . .
C9 C8 C7 119.8(3) . .
C9 C8 H8 120.1 . .
C7 C8 H8 120.1 . .
N2 C9 C8 121.4(3) . .
N2 C9 H9 119.3 . .
C8 C9 H9 119.3 . .
N2 C10 C11 121.3(3) . .
N2 C10 H10 119.3 . .
C11 C10 H10 119.3 . .
C10 C11 C7 119.4(3) . .
C10 C11 H11 120.3 . .
C7 C11 H11 120.3 . .
C13 C12 N2 110.1(2) . .
C13 C12 H12A 109.6 . .
N2 C12 H12A 109.6 . .
C13 C12 H12B 109.6 . .
N2 C12 H12B 109.6 . .
H12A C12 H12B 108.2 . .
C18 C13 C14 118.2(4) . .
C18 C13 C12 119.9(3) . .
C14 C13 C12 121.9(3) . .
C15 C14 C13 121.2(3) . .
C15 C14 H14 119.4 . .
C13 C14 H14 119.4 . .
C14 C15 C16 120.6(4) . .
C14 C15 H15 119.7 . .
C16 C15 H15 119.7 . .
C17 C16 C15 118.1(3) . .
C17 C16 C1 120.3(3) . 2_565
C15 C16 C1 121.6(3) . 2_565
C18 C17 C16 121.5(3) . .
C18 C17 H17 119.3 . .
C16 C17 H17 119.3 . .
C17 C18 C13 120.5(4) . .
C17 C18 H18 119.8 . .
C13 C18 H18 119.8 . .
N3 C19 S1 179.0(4) . .
N4 C20 S2 176.3(4) . .
N5 C21 S3 178.9(4) . .
N6 C22 S4 178.0(3) . .
N3 Cu1 N4 124.57(17) . .
N3 Cu1 N5 119.79(17) . 2_677
N4 Cu1 N5 115.48(16) . 2_677
N6 Cu2 S3 117.82(12) 2_567 .
N6 Cu2 S2 111.75(11) 2_567 .
S3 Cu2 S2 103.49(5) . .
N6 Cu2 S4 105.41(9) 2_567 .
S3 Cu2 S4 107.51(5) . .
S2 Cu2 S4 110.83(4) . .
C6 N1 C2 120.4(3) . .
C6 N1 C1 120.9(3) . .
C2 N1 C1 118.6(3) . .
C9 N2 C10 119.9(3) . .
C9 N2 C12 119.8(3) . .
C10 N2 C12 120.2(3) . .
C19 N3 Cu1 177.6(4) . .
C20 N4 Cu1 172.8(3) . .
C21 N5 Cu1 173.9(4) . 2_677
C22 N6 Cu2 160.3(3) . 2_567
C20 S2 Cu2 105.24(14) . .
C21 S3 Cu2 100.17(16) . .
C22 S4 Cu2 95.74(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C16 1.505(5) 2_565
C1 N1 1.506(4) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 N1 1.338(4) .
C2 C3 1.369(5) .
C2 H2 0.9300 .
C3 C4 1.388(5) .
C3 H3 0.9300 .
C4 C5 1.386(5) .
C4 C7 1.484(5) .
C5 C6 1.374(5) .
C5 H5 0.9300 .
C6 N1 1.330(4) .
C6 H6 0.9300 .
C7 C8 1.387(5) .
C7 C11 1.387(5) .
C8 C9 1.366(5) .
C8 H8 0.9300 .
C9 N2 1.334(4) .
C9 H9 0.9300 .
C10 N2 1.339(4) .
C10 C11 1.374(5) .
C10 H10 0.9300 .
C11 H11 0.9300 .
C12 C13 1.502(5) .
C12 N2 1.505(4) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 C18 1.384(5) .
C13 C14 1.384(5) .
C14 C15 1.378(5) .
C14 H14 0.9300 .
C15 C16 1.386(5) .
C15 H15 0.9300 .
C16 C17 1.380(5) .
C16 C1 1.505(5) 2_565
C17 C18 1.377(5) .
C17 H17 0.9300 .
C18 H18 0.9300 .
C19 N3 1.147(6) .
C19 S1 1.637(5) .
C20 N4 1.158(5) .
C20 S2 1.636(4) .
C21 N5 1.155(6) .
C21 S3 1.627(6) .
C22 N6 1.144(4) .
C22 S4 1.653(4) .
Cu1 N3 1.893(4) .
Cu1 N4 1.921(4) .
Cu1 N5 1.922(5) 2_677
Cu2 N6 1.960(3) 2_567
Cu2 S3 2.3426(15) .
Cu2 S2 2.3787(11) .
Cu2 S4 2.4101(10) .
N5 Cu1 1.922(5) 2_677
N6 Cu2 1.960(3) 2_567
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 C2 C3 C4 0.5(6) . .
C2 C3 C4 C5 5.1(5) . .
C2 C3 C4 C7 -169.3(3) . .
C3 C4 C5 C6 -5.9(5) . .
C7 C4 C5 C6 168.2(3) . .
C4 C5 C6 N1 1.4(6) . .
C5 C4 C7 C8 153.9(4) . .
C3 C4 C7 C8 -32.0(5) . .
C5 C4 C7 C11 -33.3(5) . .
C3 C4 C7 C11 140.8(3) . .
C11 C7 C8 C9 -4.4(5) . .
C4 C7 C8 C9 168.6(3) . .
C7 C8 C9 N2 1.5(6) . .
N2 C10 C11 C7 0.6(5) . .
C8 C7 C11 C10 3.4(5) . .
C4 C7 C11 C10 -169.6(3) . .
N2 C12 C13 C18 95.7(4) . .
N2 C12 C13 C14 -81.5(4) . .
C18 C13 C14 C15 -2.0(5) . .
C12 C13 C14 C15 175.3(3) . .
C13 C14 C15 C16 0.3(5) . .
C14 C15 C16 C17 2.1(5) . .
C14 C15 C16 C1 -176.0(3) . 2_565
C15 C16 C17 C18 -2.7(5) . .
C1 C16 C17 C18 175.4(3) 2_565 .
C16 C17 C18 C13 1.0(5) . .
C14 C13 C18 C17 1.4(5) . .
C12 C13 C18 C17 -175.9(3) . .
C5 C6 N1 C2 4.4(5) . .
C5 C6 N1 C1 -171.2(3) . .
C3 C2 N1 C6 -5.3(5) . .
C3 C2 N1 C1 170.4(3) . .
C16 C1 N1 C6 108.9(4) 2_565 .
C16 C1 N1 C2 -66.7(4) 2_565 .
C8 C9 N2 C10 2.6(5) . .
C8 C9 N2 C12 -172.6(3) . .
C11 C10 N2 C9 -3.6(5) . .
C11 C10 N2 C12 171.6(3) . .
C13 C12 N2 C9 96.7(4) . .
C13 C12 N2 C10 -78.5(4) . .
S1 C19 N3 Cu1 119(24) . .
N4 Cu1 N3 C19 40(10) . .
N5 Cu1 N3 C19 -135(10) 2_677 .
S2 C20 N4 Cu1 16(9) . .
N3 Cu1 N4 C20 42(3) . .
N5 Cu1 N4 C20 -142(3) 2_677 .
S3 C21 N5 Cu1 53(23) . 2_677
S4 C22 N6 Cu2 41(11) . 2_567
N4 C20 S2 Cu2 -179(100) . .
N6 Cu2 S2 C20 156.63(19) 2_567 .
S3 Cu2 S2 C20 28.86(16) . .
S4 Cu2 S2 C20 -86.12(16) . .
N5 C21 S3 Cu2 167(21) . .
N6 Cu2 S3 C21 136.89(17) 2_567 .
S2 Cu2 S3 C21 -99.24(15) . .
S4 Cu2 S3 C21 18.09(15) . .
N6 C22 S4 Cu2 -32(10) . .
N6 Cu2 S4 C22 -1.85(18) 2_567 .
S3 Cu2 S4 C22 124.63(14) . .
S2 Cu2 S4 C22 -122.92(14) . .
