#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:40:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179388 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/85/4328562.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_4328562
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            'C78 H84 Cl12 Hg4 N8 O12'
_chemical_formula_weight         2553.29
_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                112.3730(10)
_cell_angle_beta                 100.9170(10)
_cell_angle_gamma                103.5720(10)
_cell_formula_units_Z            1
_cell_length_a                   10.88690(10)
_cell_length_b                   14.78220(10)
_cell_length_c                   15.32430(10)
_cell_measurement_reflns_used    8084
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.70
_cell_measurement_theta_min      2.63
_cell_volume                     2107.60(4)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0680
_diffrn_reflns_av_sigmaI/netI    0.0800
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            57233
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    7.707
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5630
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.012
_exptl_crystal_description       prism
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.915
_refine_diff_density_min         -1.654
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         12266
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0164P)²+4.2906P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                7828
_reflns_number_total             12266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2026329_si_003_4.cif
_cod_data_source_block           2(Hg2Cl6)2+PyBP+2CH3OH
_cod_original_cell_volume        2107.60(3)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4328562
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Hg1 Hg 0.80748(2) 0.736158(16) 0.734716(15) 0.02970(7) Uani 1 1 d . . .
Hg2 Hg 0.45713(2) 0.787072(17) 0.602751(16) 0.03321(7) Uani 1 1 d . . .
Cl1 Cl 0.94641(14) 0.91357(10) 0.79552(10) 0.0344(4) Uani 1 1 d . . .
Cl2 Cl 0.83519(15) 0.61261(11) 0.79334(11) 0.0353(3) Uani 1 1 d . . .
Cl3 Cl 0.56657(13) 0.73434(10) 0.74047(9) 0.0254(3) Uani 1 1 d . . .
Cl4 Cl 0.63385(14) 0.94221(10) 0.63458(10) 0.0304(3) Uani 1 1 d . . .
Cl5 Cl 0.38146(13) 0.64304(10) 0.43953(9) 0.0255(3) Uani 1 1 d . . .
Cl6 Cl 0.27387(17) 0.81526(15) 0.67144(12) 0.0545(5) Uani 1 1 d . . .
O1 O 0.5015(3) 0.8094(3) 0.2391(2) 0.0253(8) Uani 1 1 d . . .
O2 O 0.7522(3) 0.9324(3) 0.3992(2) 0.0251(8) Uani 1 1 d . . .
O3 O 0.9519(3) 0.8525(3) 0.3550(3) 0.0251(8) Uani 1 1 d . . .
O4 O 0.0004(4) 0.3281(3) -0.3224(3) 0.0339(10) Uani 1 1 d . . .
O5 O 0.1308(3) 0.5253(3) -0.1682(2) 0.0277(9) Uani 1 1 d . . .
O6A O 0.0329(18) 0.6917(15) 0.6701(14) 0.160(7) Uiso 0.50 1 d PD A 1
O6B O 0.108(3) 0.569(2) 0.555(2) 0.245(11) Uiso 0.50 1 d PD A 2
N1 N 0.7463(4) 0.6783(3) 0.5643(3) 0.0214(10) Uani 1 1 d . . .
N2 N 0.6094(4) 0.5842(3) 0.2580(3) 0.0173(9) Uani 1 1 d . . .
N3 N -0.1551(4) 0.7497(3) 0.0681(3) 0.0297(11) Uani 1 1 d . . .
N4 N 0.1989(4) 0.8978(3) 0.0348(3) 0.0219(10) Uani 1 1 d . . .
C1 C 0.6786(5) 0.5777(4) 0.5003(4) 0.0217(12) Uani 1 1 d . . .
H1 H 0.6620 0.5295 0.5256 0.026 Uiso 1 1 calc R . .
C2 C 0.6328(5) 0.5431(4) 0.3990(4) 0.0201(11) Uani 1 1 d . . .
H2 H 0.5866 0.4733 0.3562 0.024 Uiso 1 1 calc R . .
C3 C 0.6587(5) 0.6164(4) 0.3643(3) 0.0174(11) Uani 1 1 d . . .
C4 C 0.7289(5) 0.7197(4) 0.4277(3) 0.0178(11) Uani 1 1 d . . .
H4 H 0.7475 0.7689 0.4039 0.021 Uiso 1 1 calc R . .
C5 C 0.7703(5) 0.7472(4) 0.5277(3) 0.0205(11) Uani 1 1 d . . .
H5 H 0.8170 0.8167 0.5716 0.025 Uiso 1 1 calc R . .
C6 C 0.4886(5) 0.5107(4) 0.2030(3) 0.0177(11) Uani 1 1 d . . .
H6 H 0.4347 0.4838 0.2338 0.021 Uiso 1 1 calc R . .
C7 C 0.4447(5) 0.4756(4) 0.1017(3) 0.0183(11) Uani 1 1 d . . .
H7 H 0.3632 0.4229 0.0644 0.022 Uiso 1 1 calc R . .
C8 C 0.5214(5) 0.5181(4) 0.0543(3) 0.0168(10) Uani 1 1 d . . .
C9 C 0.6441(5) 0.5967(4) 0.1149(3) 0.0194(11) Uani 1 1 d . . .
H9 H 0.6975 0.6277 0.0862 0.023 Uiso 1 1 calc R . .
C10 C 0.6864(5) 0.6285(4) 0.2148(3) 0.0193(11) Uani 1 1 d . . .
H10 H 0.7680 0.6805 0.2535 0.023 Uiso 1 1 calc R . .
C11 C -0.0377(5) 0.7454(4) 0.1107(4) 0.0286(13) Uani 1 1 d . . .
H11 H -0.0373 0.7080 0.1477 0.034 Uiso 1 1 calc R . .
C12 C 0.0814(5) 0.7931(4) 0.1028(4) 0.0254(12) Uani 1 1 d . . .
H12 H 0.1608 0.7883 0.1328 0.031 Uiso 1 1 calc R . .
C13 C 0.0769(5) 0.8486(4) 0.0477(3) 0.0198(11) Uani 1 1 d . . .
C14 C -0.0402(5) 0.8561(4) 0.0050(4) 0.0264(12) Uani 1 1 d . . .
H14 H -0.0431 0.8941 -0.0313 0.032 Uiso 1 1 calc R . .
C15 C -0.1537(5) 0.8052(4) 0.0177(4) 0.0275(13) Uani 1 1 d . . .
H15 H -0.2337 0.8102 -0.0106 0.033 Uiso 1 1 calc R . .
C16 C 0.3061(5) 0.9640(4) 0.1140(4) 0.0321(14) Uani 1 1 d . . .
H16 H 0.2998 0.9816 0.1776 0.039 Uiso 1 1 calc R . .
C17 C 0.4244(5) 1.0057(4) 0.1019(4) 0.0319(14) Uani 1 1 d . . .
H17 H 0.4978 1.0510 0.1571 0.038 Uiso 1 1 calc R . .
C18 C 0.4347(5) 0.9802(4) 0.0071(4) 0.0231(12) Uani 1 1 d . . .
C19 C 0.3221(5) 0.9151(5) -0.0724(4) 0.0351(15) Uani 1 1 d . . .
H19 H 0.3251 0.8988 -0.1367 0.042 Uiso 1 1 calc R . .
C20 C 0.2066(5) 0.8745(5) -0.0576(4) 0.0357(15) Uani 1 1 d . . .
H20 H 0.1319 0.8299 -0.1120 0.043 Uiso 1 1 calc R . .
C21 C 0.3919(5) 0.7270(4) 0.1729(4) 0.0211(11) Uani 1 1 d . . .
C22 C 0.3005(5) 0.6683(4) 0.1981(4) 0.0235(12) Uani 1 1 d . . .
H22 H 0.3111 0.6837 0.2644 0.028 Uiso 1 1 calc R . .
C23 C 0.1907(5) 0.5846(4) 0.1230(4) 0.0235(12) Uani 1 1 d . . .
H23 H 0.1298 0.5442 0.1401 0.028 Uiso 1 1 calc R . .
C24 C 0.1726(5) 0.5621(4) 0.0251(4) 0.0232(12) Uani 1 1 d . . .
H24 H 0.0993 0.5068 -0.0237 0.028 Uiso 1 1 calc R . .
C25 C 0.2643(5) 0.6220(4) -0.0021(3) 0.0178(11) Uani 1 1 d . . .
C26 C 0.3783(5) 0.7043(4) 0.0717(3) 0.0180(11) Uani 1 1 d . . .
C27 C 0.4735(5) 0.7618(4) 0.0434(4) 0.0216(11) Uani 1 1 d . . .
H27 H 0.5497 0.8145 0.0914 0.026 Uiso 1 1 calc R . .
C28 C 0.4531(5) 0.7396(4) -0.0541(4) 0.0254(12) Uani 1 1 d . . .
H28 H 0.5173 0.7765 -0.0718 0.031 Uiso 1 1 calc R . .
C29 C 0.3375(5) 0.6623(4) -0.1290(4) 0.0248(12) Uani 1 1 d . . .
H29 H 0.3235 0.6508 -0.1947 0.030 Uiso 1 1 calc R . .
C30 C 0.2453(5) 0.6039(4) -0.1032(4) 0.0218(11) Uani 1 1 d . . .
C31 C 0.0980(5) 0.5089(4) -0.2700(4) 0.0291(13) Uani 1 1 d . . .
H31A H 0.1706 0.4975 -0.2959 0.035 Uiso 1 1 calc R . .
H31B H 0.0832 0.5695 -0.2741 0.035 Uiso 1 1 calc R . .
C32 C -0.0245(5) 0.4163(4) -0.3288(4) 0.0300(13) Uani 1 1 d . . .
H32A H -0.0971 0.4280 -0.3031 0.036 Uiso 1 1 calc R . .
H32B H -0.0494 0.4041 -0.3976 0.036 Uiso 1 1 calc R . .
C33 C 1.0916(5) 0.7670(4) 0.4021(4) 0.0296(13) Uani 1 1 d . . .
H33A H 1.1810 0.7639 0.4121 0.036 Uiso 1 1 calc R . .
H33B H 1.0696 0.7780 0.4629 0.036 Uiso 1 1 calc R . .
C34 C 1.0852(5) 0.8535(4) 0.3776(4) 0.0332(14) Uani 1 1 d . . .
H34A H 1.1419 0.9191 0.4335 0.040 Uiso 1 1 calc R . .
H34B H 1.1168 0.8465 0.3211 0.040 Uiso 1 1 calc R . .
C35 C 0.9433(5) 0.9456(4) 0.3496(4) 0.0294(13) Uani 1 1 d . . .
H35A H 0.9833 0.9553 0.3009 0.035 Uiso 1 1 calc R . .
H35B H 0.9913 1.0051 0.4135 0.035 Uiso 1 1 calc R . .
C36 C 0.8013(5) 0.9376(4) 0.3208(4) 0.0295(13) Uani 1 1 d . . .
H36A H 0.7936 0.9979 0.3120 0.035 Uiso 1 1 calc R . .
H36B H 0.7512 0.8758 0.2590 0.035 Uiso 1 1 calc R . .
C37 C 0.6278(5) 0.9502(4) 0.3960(4) 0.0260(12) Uani 1 1 d . . .
H37A H 0.6202 0.9942 0.3632 0.031 Uiso 1 1 calc R . .
H37B H 0.6269 0.9870 0.4634 0.031 Uiso 1 1 calc R . .
C38 C 0.5101(5) 0.8516(4) 0.3426(3) 0.0250(12) Uani 1 1 d . . .
H38A H 0.5216 0.8026 0.3685 0.030 Uiso 1 1 calc R . .
H38B H 0.4296 0.8660 0.3512 0.030 Uiso 1 1 calc R . .
C39 C -0.014(2) 0.5988(17) 0.5691(16) 0.277(11) Uiso 1 1 d 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'
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'
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'
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 Hg1 Cl2 116.69(11) . .
N1 Hg1 Cl1 102.37(10) . .
Cl2 Hg1 Cl1 129.01(5) . .
N1 Hg1 Cl3 92.58(11) . .
Cl2 Hg1 Cl3 101.74(5) . .
Cl1 Hg1 Cl3 108.15(5) . .
Cl5 Hg2 Cl4 117.59(4) . .
Cl5 Hg2 Cl6 112.95(5) . .
Cl4 Hg2 Cl6 116.45(6) . .
Cl5 Hg2 Cl3 110.75(4) . .
Cl4 Hg2 Cl3 101.75(4) . .
Cl6 Hg2 Cl3 93.67(5) . .
Hg1 Cl3 Hg2 109.08(4) . .
C21 O1 C38 118.1(4) . .
C36 O2 C37 114.1(4) . .
C34 O3 C35 112.1(4) . .
C32 O4 C33 111.6(4) . 2_665
C30 O5 C31 117.0(4) . .
C5 N1 C1 118.4(4) . .
C5 N1 Hg1 119.4(3) . .
C1 N1 Hg1 122.0(3) . .
C6 N2 C10 120.4(4) . .
C6 N2 C3 120.3(4) . .
C10 N2 C3 119.3(4) . .
C15 N3 C11 117.3(4) . .
C16 N4 C20 119.8(4) . .
C16 N4 C13 120.8(4) . .
C20 N4 C13 119.4(4) . .
N1 C1 C2 122.8(4) . .
C3 C2 C1 117.0(4) . .
C2 C3 C4 121.5(4) . .
C2 C3 N2 119.1(4) . .
C4 C3 N2 119.4(4) . .
C5 C4 C3 117.5(4) . .
N1 C5 C4 122.7(5) . .
N2 C6 C7 120.6(4) . .
C6 C7 C8 120.7(4) . .
C7 C8 C9 116.8(4) . .
C7 C8 C8 122.4(5) . 2_665
C9 C8 C8 120.9(5) . 2_665
C10 C9 C8 121.3(4) . .
N2 C10 C9 120.2(4) . .
N3 C11 C12 123.9(5) . .
C11 C12 C13 116.4(5) . .
C14 C13 C12 121.2(5) . .
C14 C13 N4 120.2(4) . .
C12 C13 N4 118.5(5) . .
C13 C14 C15 117.5(5) . .
N3 C15 C14 123.6(5) . .
N4 C16 C17 120.8(5) . .
C16 C17 C18 120.0(5) . .
C19 C18 C17 117.8(5) . .
C19 C18 C18 121.7(6) . 2_675
C17 C18 C18 120.5(6) . 2_675
C20 C19 C18 120.5(5) . .
N4 C20 C19 121.0(5) . .
O1 C21 C22 124.7(4) . .
O1 C21 C26 114.1(4) . .
C22 C21 C26 121.1(4) . .
C21 C22 C23 119.7(5) . .
C24 C23 C22 120.8(5) . .
C23 C24 C25 120.3(5) . .
C24 C25 C26 120.0(4) . .
C24 C25 C30 121.9(4) . .
C26 C25 C30 118.1(4) . .
C25 C26 C27 119.7(4) . .
C25 C26 C21 117.9(4) . .
C27 C26 C21 122.3(4) . .
C28 C27 C26 119.9(4) . .
C27 C28 C29 121.9(5) . .
C30 C29 C28 118.9(5) . .
O5 C30 C29 125.1(5) . .
O5 C30 C25 113.6(4) . .
C29 C30 C25 121.2(4) . .
O5 C31 C32 108.3(4) . .
O4 C32 C31 108.9(4) . .
O4 C33 C34 109.0(4) 2_665 .
O3 C34 C33 109.7(4) . .
O3 C35 C36 109.5(4) . .
O2 C36 C35 106.7(4) . .
O2 C37 C38 113.0(4) . .
O1 C38 C37 107.0(4) . .
O6B C39 O6A 106(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hg1 N1 2.317(4) .
Hg1 Cl2 2.3745(14) .
Hg1 Cl1 2.4037(13) .
Hg1 Cl3 2.6350(14) .
Hg2 Cl5 2.4105(13) .
Hg2 Cl4 2.4333(14) .
Hg2 Cl6 2.4726(17) .
Hg2 Cl3 2.6865(13) .
O1 C21 1.363(6) .
O1 C38 1.441(5) .
O2 C36 1.425(6) .
O2 C37 1.434(6) .
O3 C34 1.422(6) .
O3 C35 1.433(6) .
O4 C32 1.426(6) .
O4 C33 1.429(6) 2_665
O5 C30 1.366(5) .
O5 C31 1.442(6) .
O6A C39 1.514(16) .
O6B C39 1.517(17) .
N1 C5 1.337(6) .
N1 C1 1.349(6) .
N2 C6 1.354(6) .
N2 C10 1.361(6) .
N2 C3 1.458(6) .
N3 C15 1.324(6) .
N3 C11 1.348(7) .
N4 C16 1.347(6) .
N4 C20 1.349(6) .
N4 C13 1.445(6) .
C1 C2 1.379(7) .
C2 C3 1.375(6) .
C3 C4 1.379(6) .
C4 C5 1.376(6) .
C6 C7 1.377(6) .
C7 C8 1.396(6) .
C8 C9 1.406(6) .
C8 C8 1.478(9) 2_665
C9 C10 1.365(6) .
C11 C12 1.375(7) .
C12 C13 1.386(7) .
C13 C14 1.368(7) .
C14 C15 1.377(7) .
C16 C17 1.370(7) .
C17 C18 1.389(7) .
C18 C19 1.379(7) .
C18 C18 1.495(10) 2_675
C19 C20 1.360(7) .
C21 C22 1.373(7) .
C21 C26 1.426(6) .
C22 C23 1.409(7) .
C23 C24 1.370(7) .
C24 C25 1.406(6) .
C25 C26 1.419(6) .
C25 C30 1.432(7) .
C26 C27 1.423(6) .
C27 C28 1.362(6) .
C28 C29 1.409(7) .
C29 C30 1.383(7) .
C31 C32 1.488(7) .
C33 O4 1.429(6) 2_665
C33 C34 1.475(8) .
C35 C36 1.488(7) .
C37 C38 1.501(7) .
