#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:26:07 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180505 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/74/7217430.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_7217430
loop_
_publ_author_name
'Fernando, Isurika R.'
'Mo, Yirong'
'Mezei, Gellert'
_publ_section_title
;
 Metal-binding studies of linear rigid-axle [2]pseudorotaxanes with in
 situ generated anionic metal halide complexes
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              7320
_journal_paper_doi               10.1039/C4CE00789A
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C77 H80 Br12 Hg4 N8 O11'
_chemical_formula_weight         3054.77
_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                111.5800(10)
_cell_angle_beta                 101.9510(10)
_cell_angle_gamma                104.7280(10)
_cell_formula_units_Z            1
_cell_length_a                   10.9943(2)
_cell_length_b                   15.1689(2)
_cell_length_c                   15.5408(3)
_cell_measurement_reflns_used    3928
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.61
_cell_measurement_theta_min      2.59
_cell_volume                     2196.87(7)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1061
_diffrn_reflns_av_sigmaI/netI    0.1120
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            61152
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    12.484
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5264
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow/purple
_exptl_crystal_density_diffrn    2.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1426
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.507
_refine_diff_density_min         -2.132
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         12778
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0476
_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)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0692
_reflns_number_gt                7328
_reflns_number_total             12778
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7216366
_cod_data_source_file            c4ce00789a2.cif
_cod_data_source_block           2(Hg2Br6)2+PyBP+CH3OH
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2196.86(7)
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               7217430
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 0.18643(3) 0.25951(2) 0.269957(18) 0.02640(8) Uani 1 1 d .
Hg2 Hg 0.55276(3) 0.21314(2) 0.397926(19) 0.02912(8) Uani 1 1 d .
Br1 Br 0.02540(8) 0.07844(6) 0.20069(5) 0.0380(2) Uani 1 1 d .
Br2 Br 0.13936(7) 0.38332(6) 0.20856(5) 0.03108(18) Uani 1 1 d .
Br3 Br 0.42642(7) 0.26446(6) 0.25425(5) 0.02993(18) Uani 1 1 d .
Br4 Br 0.36367(7) 0.05505(6) 0.36719(5) 0.03269(18) Uani 1 1 d .
Br5 Br 0.62088(6) 0.36310(6) 0.56407(5) 0.02456(16) Uani 1 1 d .
Br6 Br 0.74906(7) 0.19996(7) 0.33409(5) 0.0419(2) Uani 1 1 d .
O1 O 0.8646(4) 0.4783(3) 0.1676(3) 0.0199(10) Uani 1 1 d .
O2 O 0.9937(4) 0.6745(4) 0.3216(3) 0.0296(12) Uani 1 1 d .
O3 O 0.9508(4) 0.8534(3) 0.3580(3) 0.0196(10) Uani 1 1 d .
O4 O 0.2447(4) 0.0660(4) -0.4002(3) 0.0228(11) Uani 1 1 d .
O5 O 0.4948(4) 0.1935(4) -0.2383(3) 0.0246(11) Uani 1 1 d .
O6 O 0.0913(13) 0.5424(14) 0.5401(12) 0.085(5) Uani 0.50 1 d P
N1 N 0.2486(5) 0.3179(5) 0.4400(4) 0.0213(13) Uani 1 1 d .
N2 N 0.3894(5) 0.4138(4) 0.7437(3) 0.0154(12) Uani 1 1 d .
N3 N 1.1484(5) 0.2552(4) 0.9305(4) 0.0229(13) Uani 1 1 d .
N4 N 0.7950(5) 0.1079(4) 0.9646(4) 0.0165(12) Uani 1 1 d .
C1 C 0.2262(5) 0.2504(5) 0.4769(4) 0.0160(14) Uani 1 1 d .
H1 H 0.1793 0.1820 0.4339 0.019 Uiso 1 1 calc R
C2 C 0.2703(5) 0.2791(5) 0.5768(4) 0.0174(15) Uani 1 1 d .
H2 H 0.2537 0.2313 0.6011 0.021 Uiso 1 1 calc R
C3 C 0.3394(5) 0.3803(5) 0.6384(4) 0.0132(14) Uani 1 1 d .
C4 C 0.3618(6) 0.4519(5) 0.6022(4) 0.0181(14) Uani 1 1 d .
H4 H 0.4073 0.5209 0.6437 0.022 Uiso 1 1 calc R
C5 C 0.3136(6) 0.4158(5) 0.5021(5) 0.0240(16) Uani 1 1 d .
H5 H 0.3272 0.4625 0.4762 0.029 Uiso 1 1 calc R
C6 C 0.3132(6) 0.3702(5) 0.7863(4) 0.0188(15) Uani 1 1 d .
H6 H 0.2308 0.3184 0.7478 0.023 Uiso 1 1 calc R
C7 C 0.3569(6) 0.4021(5) 0.8851(4) 0.0189(15) Uani 1 1 d .
H7 H 0.3043 0.3704 0.9127 0.023 Uiso 1 1 calc R
C8 C 0.4776(5) 0.4805(5) 0.9455(4) 0.0144(14) Uani 1 1 d .
C9 C 0.5544(6) 0.5223(5) 0.8990(4) 0.0159(14) Uani 1 1 d .
H9 H 0.6368 0.5746 0.9365 0.019 Uiso 1 1 calc R
C10 C 0.5103(6) 0.4875(5) 0.7996(4) 0.0175(14) Uani 1 1 d .
H10 H 0.5642 0.5149 0.7699 0.021 Uiso 1 1 calc R
C11 C 1.0325(6) 0.2601(5) 0.8906(5) 0.0257(17) Uani 1 1 d .
H11 H 1.0322 0.2981 0.8553 0.031 Uiso 1 1 calc R
C12 C 0.9127(6) 0.2125(5) 0.8979(4) 0.0202(15) Uani 1 1 d .
H12 H 0.8336 0.2177 0.8688 0.024 Uiso 1 1 calc R
C13 C 0.9171(6) 0.1568(5) 0.9507(4) 0.0195(15) Uani 1 1 d .
C14 C 1.0335(6) 0.1495(5) 0.9931(4) 0.0196(15) Uani 1 1 d .
H14 H 1.0368 0.1119 1.0287 0.024 Uiso 1 1 calc R
C15 C 1.1472(6) 0.2013(6) 0.9802(5) 0.0286(18) Uani 1 1 d .
H15 H 1.2277 0.1975 1.0087 0.034 Uiso 1 1 calc R
C16 C 0.6895(7) 0.0375(6) 0.8881(5) 0.043(2) Uani 1 1 d .
H16 H 0.6953 0.0166 0.8253 0.052 Uiso 1 1 calc R
C17 C 0.5720(7) -0.0048(6) 0.9004(5) 0.041(2) Uani 1 1 d .
H17 H 0.4977 -0.0515 0.8458 0.049 Uiso 1 1 calc R
C18 C 0.5638(6) 0.0217(5) 0.9928(5) 0.0201(15) Uani 1 1 d .
C19 C 0.6747(6) 0.0918(6) 1.0710(5) 0.035(2) Uani 1 1 d .
H19 H 0.6729 0.1097 1.1346 0.042 Uiso 1 1 calc R
C20 C 0.7898(6) 0.1363(6) 1.0559(5) 0.0304(19) Uani 1 1 d .
H20 H 0.8636 0.1861 1.1092 0.037 Uiso 1 1 calc R
C21 C 0.7509(6) 0.3993(5) 0.1027(4) 0.0179(14) Uani 1 1 d .
C22 C 0.6594(6) 0.3403(5) 0.1246(4) 0.0221(16) Uani 1 1 d .
H22 H 0.6730 0.3518 0.1894 0.027 Uiso 1 1 calc R
C23 C 0.5435(6) 0.2616(5) 0.0495(5) 0.0215(16) Uani 1 1 d .
H23 H 0.4792 0.2245 0.0661 0.026 Uiso 1 1 calc R
C24 C 0.5243(6) 0.2391(5) -0.0469(5) 0.0234(16) Uani 1 1 d .
H24 H 0.4491 0.1853 -0.0955 0.028 Uiso 1 1 calc R
C25 C 0.6182(6) 0.2973(5) -0.0724(4) 0.0164(14) Uani 1 1 d .
C26 C 0.7329(6) 0.3802(5) 0.0018(4) 0.0169(14) Uani 1 1 d .
C27 C 0.8246(6) 0.4402(5) -0.0240(4) 0.0195(15) Uani 1 1 d .
H27 H 0.8979 0.4958 0.0247 0.023 Uiso 1 1 calc R
C28 C 0.8061(6) 0.4169(5) -0.1210(5) 0.0220(15) Uani 1 1 d .
H28 H 0.8670 0.4574 -0.1372 0.026 Uiso 1 1 calc R
C29 C 0.6972(6) 0.3332(5) -0.1962(5) 0.0232(16) Uani 1 1 d .
H29 H 0.6879 0.3174 -0.2616 0.028 Uiso 1 1 calc R
C30 C 0.6052(6) 0.2753(5) -0.1732(4) 0.0188(15) Uani 1 1 d .
C31 C 0.4871(6) 0.1505(5) -0.3398(4) 0.0218(15) Uani 1 1 d .
H31A H 0.5685 0.1387 -0.3453 0.026 Uiso 1 1 calc R
H31B H 0.4750 0.1964 -0.3679 0.026 Uiso 1 1 calc R
C32 C 0.3701(6) 0.0519(5) -0.3925(5) 0.0252(16) Uani 1 1 d .
H32A H 0.3717 0.0150 -0.4579 0.030 Uiso 1 1 calc R
H32B H 0.3779 0.0109 -0.3578 0.030 Uiso 1 1 calc R
C33 C 0.1948(6) 0.0626(6) -0.3226(4) 0.0268(17) Uani 1 1 d .
H33A H 0.2478 0.1233 -0.2617 0.032 Uiso 1 1 calc R
H33B H 0.1992 0.0037 -0.3129 0.032 Uiso 1 1 calc R
C34 C 0.9468(6) 0.9439(6) 0.3519(5) 0.0302(18) Uani 1 1 d .
H34A H 0.9863 0.9526 0.3039 0.036 Uiso 1 1 calc R
H34B H 0.9978 1.0022 0.4150 0.036 Uiso 1 1 calc R
C35 C 1.0820(6) 0.8538(6) 0.3784(5) 0.0314(19) Uani 1 1 d .
H35A H 1.1420 0.9173 0.4343 0.038 Uiso 1 1 calc R
H35B H 1.1109 0.8484 0.3223 0.038 Uiso 1 1 calc R
C36 C 1.0867(6) 0.7662(6) 0.4003(5) 0.0283(18) Uani 1 1 d .
H36A H 1.1757 0.7639 0.4104 0.034 Uiso 1 1 calc R
H36B H 1.0660 0.7750 0.4600 0.034 Uiso 1 1 calc R
C37 C 1.0179(6) 0.5892(6) 0.3287(5) 0.0279(17) Uani 1 1 d .
H37A H 1.0425 0.6008 0.3967 0.033 Uiso 1 1 calc R
H37B H 1.0910 0.5796 0.3052 0.033 Uiso 1 1 calc R
C38 C 0.8940(6) 0.4962(6) 0.2681(4) 0.0260(17) Uani 1 1 d .
H38A H 0.9076 0.4380 0.2748 0.031 Uiso 1 1 calc R
H38B H 0.8202 0.5063 0.2902 0.031 Uiso 1 1 calc R
C39 C 0.040(3) 0.441(2) 0.4632(19) 0.104(9) Uani 0.50 1 d P
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'
Br Br -0.2901 2.4595 '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
N1 Hg1 Br2 115.40(14) .
N1 Hg1 Br1 104.41(14) .
Br2 Hg1 Br1 122.51(3) .
N1 Hg1 Br3 97.18(12) .
Br2 Hg1 Br3 103.30(2) .
Br1 Hg1 Br3 111.20(3) .
Br5 Hg2 Br4 114.92(2) .
Br5 Hg2 Br6 113.38(3) .
Br4 Hg2 Br6 121.61(3) .
Br5 Hg2 Br3 107.49(2) .
Br4 Hg2 Br3 100.17(2) .
Br6 Hg2 Br3 94.73(2) .
Hg1 Br3 Hg2 107.37(2) .
C21 O1 C38 116.2(5) .
C36 O2 C37 110.9(5) .
C35 O3 C34 110.9(5) .
C32 O4 C33 114.2(4) .
C30 O5 C31 117.5(4) .
C39 O6 C39 98.6(18) 2_566
C5 N1 C1 118.5(5) .
C5 N1 Hg1 122.1(4) .
C1 N1 Hg1 119.3(4) .
C6 N2 C10 119.7(5) .
C6 N2 C3 119.4(5) .
C10 N2 C3 120.9(5) .
C15 N3 C11 117.0(5) .
C16 N4 C20 120.2(5) .
C16 N4 C13 120.8(5) .
C20 N4 C13 119.0(5) .
N1 C1 C2 122.3(6) .
C3 C2 C1 117.6(6) .
C2 C3 C4 121.2(5) .
C2 C3 N2 119.6(5) .
C4 C3 N2 119.3(6) .
C5 C4 C3 116.7(6) .
N1 C5 C4 123.7(6) .
N2 C6 C7 120.3(6) .
C6 C7 C8 121.8(5) .
C7 C8 C9 116.3(5) .
C7 C8 C8 121.9(6) 2_667
C9 C8 C8 121.8(7) 2_667
C10 C9 C8 121.0(6) .
N2 C10 C9 120.8(5) .
N3 C11 C12 124.4(6) .
C13 C12 C11 116.2(5) .
C14 C13 C12 121.6(5) .
C14 C13 N4 119.4(5) .
C12 C13 N4 119.0(5) .
C13 C14 C15 116.4(6) .
N3 C15 C14 124.4(6) .
N4 C16 C17 121.0(6) .
C18 C17 C16 120.2(7) .
C17 C18 C19 118.0(6) .
C17 C18 C18 120.8(8) 2_657
C19 C18 C18 121.1(7) 2_657
C18 C19 C20 120.3(6) .
N4 C20 C19 120.2(6) .
C22 C21 O1 126.4(5) .
C22 C21 C26 120.2(6) .
O1 C21 C26 113.3(5) .
C21 C22 C23 120.5(6) .
C24 C23 C22 121.2(6) .
C23 C24 C25 119.8(6) .
C24 C25 C26 120.2(5) .
C24 C25 C30 122.3(6) .
C26 C25 C30 117.4(5) .
C27 C26 C25 120.0(5) .
C27 C26 C21 122.1(6) .
C25 C26 C21 117.9(5) .
C28 C27 C26 120.1(6) .
C27 C28 C29 121.4(6) .
C30 C29 C28 119.8(6) .
O5 C30 C29 125.8(5) .
O5 C30 C25 112.9(5) .
C29 C30 C25 121.3(6) .
O5 C31 C32 107.0(5) .
O4 C32 C31 112.7(6) .
O4 C33 C34 107.6(5) 2_665
O3 C34 C33 109.6(5) 2_665
O3 C35 C36 109.6(5) .
O2 C36 C35 109.7(5) .
O2 C37 C38 109.1(5) .
O1 C38 C37 108.4(5) .
O6 C39 O6 81.4(18) 2_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hg1 N1 2.336(5) .
Hg1 Br2 2.5125(7) .
Hg1 Br1 2.5300(8) .
Hg1 Br3 2.6845(7) .
Hg2 Br5 2.5327(8) .
Hg2 Br4 2.5519(8) .
Hg2 Br6 2.5772(8) .
Hg2 Br3 2.8399(7) .
O1 C21 1.357(7) .
O1 C38 1.432(6) .
O2 C36 1.408(8) .
O2 C37 1.423(8) .
O3 C35 1.410(6) .
O3 C34 1.421(7) .
O4 C32 1.435(7) .
O4 C33 1.437(6) .
O5 C30 1.356(7) .
O5 C31 1.443(7) .
O6 C39 1.43(3) .
O6 C39 1.52(2) 2_566
N1 C5 1.329(8) .
N1 C1 1.341(7) .
N2 C6 1.359(6) .
N2 C10 1.350(7) .
N2 C3 1.454(7) .
N3 C15 1.315(7) .
N3 C11 1.330(7) .
N4 C16 1.328(8) .
N4 C20 1.341(7) .
N4 C13 1.459(7) .
C1 C2 1.385(7) .
C2 C3 1.370(9) .
C3 C4 1.389(8) .
C4 C5 1.373(8) .
C6 C7 1.360(7) .
C7 C8 1.385(8) .
C8 C9 1.398(7) .
C8 C8 1.493(11) 2_667
C9 C10 1.364(7) .
C11 C12 1.381(8) .
C12 C13 1.381(8) .
C13 C14 1.365(8) .
C14 C15 1.393(8) .
C16 C17 1.374(8) .
C17 C18 1.371(8) .
C18 C19 1.368(9) .
C18 C18 1.489(11) 2_657
C19 C20 1.385(8) .
C21 C22 1.354(8) .
C21 C26 1.446(7) .
C22 C23 1.413(8) .
C23 C24 1.364(8) .
C24 C25 1.403(8) .
C25 C26 1.423(8) .
C25 C30 1.443(8) .
C26 C27 1.406(8) .
C27 C28 1.372(8) .
C28 C29 1.402(9) .
C29 C30 1.360(8) .
C31 C32 1.499(8) .
C33 C34 1.495(8) 2_665
C34 C33 1.495(8) 2_665
C35 C36 1.499(9) .
C37 C38 1.499(9) .
C39 O6 1.52(2) 2_566
