#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:40:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179388 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/85/4328560.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_4328560
loop_
_publ_author_name
'Isurika R. Fernando'
'Gellert Mezei'
_publ_section_title
;
 Blue-Colored, Linear Rigid-Axle [2]Pseudorotaxanes: Metal-Binding
 Properties, Crystal Structures, and Blue/Red Dichroism
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3156
_journal_page_last               3160
_journal_paper_doi               10.1021/ic2026329
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C52 H52 Cl6 Hg2 N4 O8'
_chemical_formula_weight         1474.86
_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                98.5500(10)
_cell_angle_beta                 103.9650(10)
_cell_angle_gamma                101.3510(10)
_cell_formula_units_Z            1
_cell_length_a                   9.7025(2)
_cell_length_b                   11.5838(3)
_cell_length_c                   12.6269(3)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.04
_cell_measurement_theta_min      2.23
_cell_volume                     1321.26(5)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0745
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            57649
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    6.164
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5757
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_description       block
_exptl_crystal_F_000             718
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.296
_refine_diff_density_min         -1.674
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         7696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0426
_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)+(0.0633P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1083
_reflns_number_gt                6137
_reflns_number_total             7696
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2026329_si_003_2.cif
_cod_data_source_block           1[Hg2Cl6]
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4328560
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
Hg1 Hg 0.56784(2) 0.659409(17) 0.580721(15) 0.02871(7) Uani 1 1 d .
Cl1 Cl 0.43178(14) 0.46099(11) 0.61901(10) 0.0309(3) Uani 1 1 d .
Cl2 Cl 0.81394(14) 0.68854(13) 0.69223(10) 0.0350(3) Uani 1 1 d .
Cl3 Cl 0.40842(17) 0.78684(14) 0.53602(12) 0.0436(3) Uani 1 1 d .
O1 O 0.1239(4) 0.5520(3) 0.7863(3) 0.0304(7) Uani 1 1 d .
O2 O 0.0670(4) 0.3226(4) 0.6260(3) 0.0395(9) Uani 1 1 d .
O3 O 0.8388(4) 0.8998(4) 1.3697(3) 0.0355(8) Uani 1 1 d .
O4 O 0.5416(4) 0.8544(4) 1.2058(3) 0.0361(8) Uani 1 1 d .
N1 N -0.2046(5) -0.0050(4) 0.8858(4) 0.0387(11) Uani 1 1 d .
N2 N 0.1855(5) 0.2656(4) 0.9481(3) 0.0263(8) Uani 1 1 d .
C1 C -0.1511(6) 0.0774(5) 0.9812(5) 0.0359(12) Uani 1 1 d .
H1 H -0.2020 0.0733 1.0347 0.043 Uiso 1 1 calc R
C2 C -0.0252(5) 0.1682(5) 1.0054(4) 0.0312(11) Uani 1 1 d .
H2 H 0.0064 0.2244 1.0724 0.037 Uiso 1 1 calc R
C3 C 0.0518(5) 0.1728(4) 0.9270(4) 0.0282(10) Uani 1 1 d .
C4 C 0.0007(6) 0.0890(4) 0.8274(4) 0.0307(11) Uani 1 1 d .
H4 H 0.0511 0.0899 0.7735 0.037 Uiso 1 1 calc R
C5 C -0.1292(7) 0.0032(5) 0.8113(5) 0.0400(13) Uani 1 1 d .
H5 H -0.1655 -0.0521 0.7437 0.048 Uiso 1 1 calc R
C6 C 0.2729(5) 0.3096(5) 1.0536(4) 0.0273(10) Uani 1 1 d .
H6 H 0.2502 0.2762 1.1117 0.033 Uiso 1 1 calc R
C7 C 0.3936(5) 0.4023(4) 1.0758(4) 0.0265(10) Uani 1 1 d .
H7 H 0.4495 0.4338 1.1492 0.032 Uiso 1 1 calc R
C8 C 0.4347(5) 0.4507(4) 0.9894(4) 0.0255(9) Uani 1 1 d .
C9 C 0.3464(6) 0.3993(4) 0.8815(4) 0.0279(10) Uani 1 1 d .
H9 H 0.3725 0.4252 0.8211 0.033 Uiso 1 1 calc R
C10 C 0.2208(6) 0.3106(4) 0.8632(4) 0.0299(10) Uani 1 1 d .
H10 H 0.1595 0.2813 0.7911 0.036 Uiso 1 1 calc R
C11 C 0.2353(6) 0.6506(5) 0.8439(4) 0.0295(10) Uani 1 1 d .
C12 C 0.3165(6) 0.7283(5) 0.7971(5) 0.0344(11) Uani 1 1 d .
H12 H 0.2938 0.7197 0.7200 0.041 Uiso 1 1 calc R
C13 C 0.4348(6) 0.8216(5) 0.8666(5) 0.0322(11) Uani 1 1 d .
H13 H 0.4892 0.8739 0.8342 0.039 Uiso 1 1 calc R
C14 C 0.4711(6) 0.8367(5) 0.9797(5) 0.0350(12) Uani 1 1 d .
H14 H 0.5510 0.8973 1.0237 0.042 Uiso 1 1 calc R
C15 C 0.3859(6) 0.7591(5) 1.0302(4) 0.0303(10) Uani 1 1 d .
C16 C 0.2649(5) 0.6664(5) 0.9618(4) 0.0294(10) Uani 1 1 d .
C17 C 0.1752(6) 0.5916(5) 1.0118(4) 0.0335(11) Uani 1 1 d .
H17 H 0.0963 0.5304 0.9673 0.040 Uiso 1 1 calc R
C18 C 0.2058(6) 0.6101(6) 1.1256(5) 0.0386(12) Uani 1 1 d .
H18 H 0.1451 0.5629 1.1577 0.046 Uiso 1 1 calc R
C19 C 0.3274(6) 0.6993(5) 1.1946(5) 0.0357(12) Uani 1 1 d .
H19 H 0.3473 0.7104 1.2717 0.043 Uiso 1 1 calc R
C20 C 0.4167(6) 0.7702(5) 1.1475(4) 0.0318(11) Uani 1 1 d .
C21 C 0.5735(7) 0.8794(6) 1.3262(5) 0.0447(14) Uani 1 1 d .
H21A H 0.5697 0.8052 1.3535 0.054 Uiso 1 1 calc R
H21B H 0.5020 0.9178 1.3490 0.054 Uiso 1 1 calc R
C22 C 0.7223(7) 0.9605(5) 1.3722(5) 0.0426(13) Uani 1 1 d .
H22A H 0.7315 1.0236 1.3299 0.051 Uiso 1 1 calc R
H22B H 0.7339 0.9983 1.4488 0.051 Uiso 1 1 calc R
C23 C 0.8801(7) 0.8504(5) 1.4656(4) 0.0393(13) Uani 1 1 d .
H23A H 0.7952 0.7958 1.4736 0.047 Uiso 1 1 calc R
H23B H 0.9173 0.9144 1.5316 0.047 Uiso 1 1 calc R
C24 C 0.0052(7) 0.2156(5) 0.5448(5) 0.0412(14) Uani 1 1 d .
H24A H -0.0373 0.2343 0.4736 0.049 Uiso 1 1 calc R
H24B H -0.0721 0.1653 0.5658 0.049 Uiso 1 1 calc R
C25 C -0.0197(6) 0.4102(5) 0.6208(5) 0.0374(12) Uani 1 1 d .
H25A H -0.0889 0.3956 0.6642 0.045 Uiso 1 1 calc R
H25B H -0.0741 0.4047 0.5442 0.045 Uiso 1 1 calc R
C26 C 0.0825(6) 0.5333(5) 0.6671(4) 0.0333(11) Uani 1 1 d .
H26A H 0.1687 0.5386 0.6403 0.040 Uiso 1 1 calc R
H26B H 0.0340 0.5945 0.6431 0.040 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'
O O 0.0106 0.0060 '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'
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_3
Cl3 Hg1 Cl2 135.06(6) .
Cl3 Hg1 Cl1 111.40(5) .
Cl2 Hg1 Cl1 103.57(5) .
Cl3 Hg1 Cl1 104.24(5) 2_666
Cl2 Hg1 Cl1 103.34(4) 2_666
Cl1 Hg1 Cl1 89.55(4) 2_666
Hg1 Cl1 Hg1 90.46(4) 2_666
C11 O1 C26 117.1(4) .
C24 O2 C25 114.7(4) .
C23 O3 C22 112.8(4) .
C20 O4 C21 117.0(4) .
C5 N1 C1 116.3(5) .
C10 N2 C6 119.8(5) .
C10 N2 C3 120.0(4) .
C6 N2 C3 120.1(4) .
N1 C1 C2 124.3(5) .
C3 C2 C1 117.8(5) .
C2 C3 C4 119.8(5) .
C2 C3 N2 120.3(5) .
C4 C3 N2 119.9(5) .
C3 C4 C5 117.4(5) .
N1 C5 C4 124.4(5) .
N2 C6 C7 120.9(5) .
C6 C7 C8 120.9(5) .
C9 C8 C7 116.6(5) .
C9 C8 C8 121.3(5) 2_667
C7 C8 C8 122.1(5) 2_667
C10 C9 C8 120.7(5) .
N2 C10 C9 121.0(5) .
C12 C11 O1 125.7(5) .
C12 C11 C16 120.6(5) .
O1 C11 C16 113.8(4) .
C11 C12 C13 119.7(5) .
C14 C13 C12 121.7(5) .
C13 C14 C15 119.6(5) .
C20 C15 C16 117.8(5) .
C20 C15 C14 122.7(5) .
C16 C15 C14 119.5(5) .
C15 C16 C11 118.8(5) .
C15 C16 C17 119.9(5) .
C11 C16 C17 121.3(5) .
C18 C17 C16 119.8(5) .
C17 C18 C19 121.1(5) .
C20 C19 C18 119.7(5) .
O4 C20 C19 124.8(5) .
O4 C20 C15 113.6(5) .
C19 C20 C15 121.6(5) .
O4 C21 C22 107.6(5) .
O3 C22 C21 113.7(5) .
O3 C23 C24 110.0(5) 2_667
O2 C24 C23 109.9(5) 2_667
O2 C25 C26 108.0(4) .
O1 C26 C25 108.3(4) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hg1 Cl3 2.3697(13) .
Hg1 Cl2 2.3910(12) .
Hg1 Cl1 2.5891(12) .
Hg1 Cl1 2.6956(12) 2_666
Cl1 Hg1 2.6955(12) 2_666
O1 C11 1.375(6) .
O1 C26 1.432(6) .
O2 C24 1.408(7) .
O2 C25 1.439(7) .
O3 C23 1.420(6) .
O3 C22 1.447(7) .
O4 C20 1.362(6) .
O4 C21 1.449(7) .
N1 C5 1.328(7) .
N1 C1 1.339(8) .
N2 C10 1.346(6) .
N2 C6 1.355(6) .
N2 C3 1.452(6) .
C1 C2 1.382(8) .
C2 C3 1.378(7) .
C3 C4 1.384(7) .
C4 C5 1.393(8) .
C6 C7 1.364(7) .
C7 C8 1.403(7) .
C8 C9 1.393(7) .
C8 C8 1.468(10) 2_667
C9 C10 1.377(7) .
C11 C12 1.373(7) .
C11 C16 1.423(7) .
C12 C13 1.414(8) .
C13 C14 1.361(8) .
C14 C15 1.425(8) .
C15 C20 1.419(7) .
C15 C16 1.420(7) .
C16 C17 1.428(7) .
C17 C18 1.369(7) .
C18 C19 1.405(8) .
C19 C20 1.375(7) .
C21 C22 1.485(8) .
C23 C24 1.488(9) 2_667
C24 C23 1.488(9) 2_667
C25 C26 1.509(8) .
