#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:02:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179464 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/61/4336103.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_4336103
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_moiety         'C48 H40 Cu2 I6 N4'
_chemical_formula_sum            'C48 H40 Cu2 I6 N4'
_chemical_formula_weight         1561.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 99.328(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7853(3)
_cell_length_b                   12.7446(5)
_cell_length_c                   18.3024(7)
_cell_measurement_temperature    293(2)
_cell_volume                     2482.48(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0683
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13067
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    4.624
_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    2.089
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.218
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.0596
_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)+(0.0627P)²+4.9699P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1512
_reflns_number_gt                3225
_reflns_number_total             5532
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401722c_si_001_4.cif
_cod_data_source_block           complex_6
_cod_original_cell_volume        2482.47(15)
_cod_database_code               4336103
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C1 C 1.0378(8) 0.4275(7) 0.2829(5) 0.054(2) Uani 1 1 d .
H1 H 1.1034 0.4751 0.2948 0.065 Uiso 1 1 calc R
C2 C 0.9298(8) 0.4407(7) 0.3117(6) 0.057(2) Uani 1 1 d .
H2 H 0.9210 0.4985 0.3414 0.068 Uiso 1 1 calc R
C3 C 0.8333(7) 0.3680(7) 0.2968(5) 0.042(2) Uani 1 1 d .
C4 C 0.8458(8) 0.2914(7) 0.2454(5) 0.048(2) Uani 1 1 d .
H4 H 0.7800 0.2449 0.2306 0.058 Uiso 1 1 calc R
C5 C 0.9535(8) 0.2829(7) 0.2161(5) 0.051(2) Uani 1 1 d .
H5 H 0.9592 0.2317 0.1806 0.061 Uiso 1 1 calc R
C6 C 1.1745(7) 0.3192(7) 0.2173(5) 0.043(2) Uani 1 1 d .
H6A H 1.2308 0.3787 0.2271 0.051 Uiso 1 1 calc R
H6B H 1.1649 0.3029 0.1650 0.051 Uiso 1 1 calc R
C7 C 1.2295(7) 0.2262(7) 0.2619(4) 0.042(2) Uani 1 1 d .
C8 C 1.1993(8) 0.2032(7) 0.3313(5) 0.050(2) Uani 1 1 d .
H8 H 1.1421 0.2453 0.3506 0.060 Uiso 1 1 calc R
C9 C 1.2534(7) 0.1185(7) 0.3719(4) 0.045(2) Uani 1 1 d .
H9 H 1.2325 0.1055 0.4184 0.054 Uiso 1 1 calc R
C10 C 1.3386(7) 0.0518(6) 0.3448(4) 0.0396(19) Uani 1 1 d .
C11 C 1.3698(7) 0.0790(7) 0.2761(4) 0.0410(19) Uani 1 1 d .
H11 H 1.4300 0.0392 0.2575 0.049 Uiso 1 1 calc R
C12 C 1.3159(7) 0.1618(6) 0.2346(4) 0.0407(19) Uani 1 1 d .
H12 H 1.3370 0.1749 0.1882 0.049 Uiso 1 1 calc R
C13 C 1.3895(7) -0.0392(6) 0.3868(4) 0.0380(18) Uani 1 1 d .
C14 C 1.3143(8) -0.0958(8) 0.4267(5) 0.055(2) Uani 1 1 d .
H14 H 1.2314 -0.0749 0.4257 0.066 Uiso 1 1 calc R
C15 C 1.3583(8) -0.1821(8) 0.4679(6) 0.059(3) Uani 1 1 d .
H15 H 1.3044 -0.2190 0.4934 0.071 Uiso 1 1 calc R
C16 C 1.4805(7) -0.2150(6) 0.4719(4) 0.0403(19) Uani 1 1 d .
C17 C 1.5580(7) -0.1587(7) 0.4332(5) 0.047(2) Uani 1 1 d .
H17 H 1.6415 -0.1787 0.4357 0.056 Uiso 1 1 calc R
C18 C 1.5127(7) -0.0727(7) 0.3906(5) 0.047(2) Uani 1 1 d .
H18 H 1.5660 -0.0368 0.3641 0.057 Uiso 1 1 calc R
C19 C 1.5295(7) -0.3121(7) 0.5127(5) 0.049(2) Uani 1 1 d .
H19A H 1.5313 -0.3693 0.4779 0.058 Uiso 1 1 calc R
H19B H 1.6146 -0.3001 0.5378 0.058 Uiso 1 1 calc R
C20 C 1.4616(8) -0.2924(7) 0.6339(5) 0.052(2) Uani 1 1 d .
H20 H 1.5311 -0.2495 0.6479 0.062 Uiso 1 1 calc R
C21 C 1.3758(7) -0.3043(7) 0.6809(5) 0.048(2) Uani 1 1 d .
H21 H 1.3879 -0.2704 0.7265 0.058 Uiso 1 1 calc R
C22 C 1.2721(7) -0.3662(6) 0.6604(4) 0.0380(18) Uani 1 1 d .
C23 C 1.2639(8) -0.4206(7) 0.5936(5) 0.048(2) Uani 1 1 d .
H23 H 1.1975 -0.4666 0.5794 0.058 Uiso 1 1 calc R
C24 C 1.3513(8) -0.4070(7) 0.5492(5) 0.048(2) Uani 1 1 d .
H24 H 1.3443 -0.4441 0.5050 0.058 Uiso 1 1 calc R
Cu1 Cu 0.96989(11) -0.10933(10) 0.48582(7) 0.0664(4) Uani 1 1 d .
I1 I 0.93405(7) -0.30618(5) 0.47702(4) 0.0696(2) Uani 1 1 d .
I2 I 0.87953(7) 0.04277(6) 0.40015(4) 0.0727(2) Uani 1 1 d .
I3 I 0.64069(5) 0.05019(5) 0.16179(3) 0.0511(2) Uani 1 1 d .
N1 N 1.0508(6) 0.3461(5) 0.2371(4) 0.0418(16) Uani 1 1 d .
N2 N 1.4479(6) -0.3412(5) 0.5679(4) 0.0400(16) 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'
I I -0.4742 1.8119 '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 C1 C2 120.9(8) . .
C1 C2 C3 120.2(8) . .
C4 C3 C2 117.0(8) . .
C4 C3 C22 121.2(7) . 3_756
C2 C3 C22 121.5(8) . 3_756
C5 C4 C3 120.6(8) . .
N1 C5 C4 121.5(8) . .
N1 C6 C7 110.0(6) . .
C8 C7 C12 118.1(7) . .
C8 C7 C6 122.0(7) . .
C12 C7 C6 119.9(7) . .
C9 C8 C7 120.9(8) . .
C8 C9 C10 121.7(8) . .
C11 C10 C9 115.9(7) . .
C11 C10 C13 123.4(7) . .
C9 C10 C13 120.7(7) . .
C12 C11 C10 123.1(8) . .
C11 C12 C7 120.3(7) . .
C14 C13 C18 117.0(8) . .
C14 C13 C10 119.7(7) . .
C18 C13 C10 123.3(7) . .
C15 C14 C13 121.9(8) . .
C16 C15 C14 121.2(8) . .
C15 C16 C17 117.9(8) . .
C15 C16 C19 122.5(8) . .
C17 C16 C19 119.4(7) . .
C16 C17 C18 120.8(7) . .
C17 C18 C13 121.2(8) . .
N2 C19 C16 110.1(6) . .
N2 C20 C21 121.7(7) . .
C20 C21 C22 119.7(8) . .
C21 C22 C23 117.3(7) . .
C21 C22 C3 121.8(7) . 3_756
C23 C22 C3 120.7(7) . 3_756
C24 C23 C22 120.8(8) . .
N2 C24 C23 121.1(8) . .
I1 Cu1 I2 116.55(6) . 3_756
I1 Cu1 I2 131.63(5) . .
I2 Cu1 I2 111.82(5) 3_756 .
I1 Cu1 Cu1 172.62(8) . 3_756
I2 Cu1 Cu1 56.09(4) 3_756 3_756
I2 Cu1 Cu1 55.73(5) . 3_756
Cu1 I2 Cu1 68.18(5) 3_756 .
C5 N1 C1 119.2(7) . .
C5 N1 C6 119.3(7) . .
C1 N1 C6 121.1(7) . .
C24 N2 C20 119.2(7) . .
C24 N2 C19 120.2(7) . .
C20 N2 C19 120.2(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.355(11) .
C1 C2 1.364(13) .
C2 C3 1.387(11) .
C3 C4 1.378(12) .
C3 C22 1.482(11) 3_756
C4 C5 1.360(12) .
C5 N1 1.329(10) .
C6 N1 1.478(10) .
C6 C7 1.504(11) .
C7 C8 1.393(11) .
C7 C12 1.393(11) .
C8 C9 1.385(12) .
C9 C10 1.401(11) .
C10 C11 1.397(11) .
C10 C13 1.450(11) .
C11 C12 1.372(11) .
C13 C14 1.379(11) .
C13 C18 1.387(11) .
C14 C15 1.374(12) .
C15 C16 1.373(11) .
C16 C17 1.381(11) .
C16 C19 1.497(11) .
C17 C18 1.387(12) .
C19 N2 1.491(10) .
C20 N2 1.344(11) .
C20 C21 1.370(12) .
C21 C22 1.370(11) .
C22 C23 1.396(11) .
C22 C3 1.482(11) 3_756
C23 C24 1.351(12) .
C24 N2 1.338(10) .
Cu1 I1 2.5395(15) .
Cu1 I2 2.5718(14) 3_756
Cu1 I2 2.5827(16) .
Cu1 Cu1 2.889(3) 3_756
I2 Cu1 2.5718(14) 3_756
