#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:26:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179377 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/74/4327423.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_4327423
loop_
_publ_author_name
'Tara J. Burchell'
'Dana J. Eisler'
'Richard J. Puddephatt'
_publ_section_title
;
 Self-Assembly Using Dynamic Coordination Chemistry and Hydrogen Bonding:
 Mercury(II) Macrocycles, Polymers and Sheets
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5550
_journal_page_last               5557
_journal_paper_doi               10.1021/ic049500+
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C38 H32 Cl6 Hg2 N8 O4'
_chemical_formula_weight         1278.60
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.207(2)
_cell_angle_beta                 77.648(2)
_cell_angle_gamma                86.289(3)
_cell_formula_units_Z            1
_cell_length_a                   9.0709(4)
_cell_length_b                   10.4009(5)
_cell_length_c                   11.5750(7)
_cell_measurement_temperature    150(2)
_cell_volume                     1053.65(9)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'phiω 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  0.055
_diffrn_reflns_av_sigmaI/netI    0.0741
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9793
_diffrn_reflns_theta_full        27.62
_diffrn_reflns_theta_max         27.62
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    7.708
_exptl_absorpt_correction_T_max  0.5128
_exptl_absorpt_correction_T_min  0.3376
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_description       block
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.073
_refine_diff_density_min         -1.689
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0392
_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)+(0.0295P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                3769
_reflns_number_total             4480
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0495002Bsi20040416_110705_2.cif
_cod_data_source_block           4aDCE
_cod_database_code               4327423
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 0.32491(2) -0.798382(18) -0.53756(2) 0.02714(9) Uani 1 1 d .
Cl1 Cl 0.53289(17) -0.69604(15) -0.50476(18) 0.0414(4) Uani 1 1 d .
Cl2 Cl 0.20654(15) -0.92006(14) -0.64712(16) 0.0350(4) Uani 1 1 d .
N1 N 0.2876(5) -0.9690(4) -0.3588(5) 0.0286(12) Uani 1 1 d .
C1 C 0.1604(6) -1.0369(5) -0.3367(6) 0.0315(16) Uani 1 1 d .
H1A H 0.0808 -1.0034 -0.3754 0.038 Uiso 1 1 calc R
C2 C 0.1411(6) -1.1525(5) -0.2607(6) 0.0294(15) Uani 1 1 d .
H2A H 0.0486 -1.1961 -0.2456 0.035 Uiso 1 1 calc R
C3 C 0.2582(5) -1.2049(5) -0.2060(6) 0.0235(13) Uani 1 1 d .
C4 C 0.3891(6) -1.1352(5) -0.2269(6) 0.0259(14) Uani 1 1 d .
H4B H 0.4704 -1.1672 -0.1897 0.031 Uiso 1 1 calc R
C5 C 0.3992(6) -1.0183(5) -0.3029(6) 0.0293(15) Uani 1 1 d .
H5A H 0.4886 -0.9707 -0.3163 0.035 Uiso 1 1 calc R
C6 C 0.2381(6) -1.3379(5) -0.1326(6) 0.0217(12) Uani 1 1 d .
O1 O 0.1109(4) -1.3728(3) -0.0777(4) 0.0263(10) Uani 1 1 d .
N2 N 0.3649(5) -1.4141(4) -0.1382(5) 0.0240(11) Uani 1 1 d .
H2B H 0.4511 -1.3758 -0.1689 0.029 Uiso 1 1 calc R
C7 C 0.3727(5) -1.5503(5) -0.0993(6) 0.0219(13) Uani 1 1 d .
C8 C 0.3025(5) -1.6055(5) 0.0170(6) 0.0214(12) Uani 1 1 d .
C9 C 0.3144(6) -1.7414(5) 0.0488(6) 0.0289(15) Uani 1 1 d .
H9A H 0.2633 -1.7812 0.1250 0.035 Uiso 1 1 calc R
C10 C 0.4006(6) -1.8167(5) -0.0311(7) 0.0326(17) Uani 1 1 d .
H10A H 0.4111 -1.9081 -0.0086 0.039 Uiso 1 1 calc R
C11 C 0.4712(6) -1.7606(5) -0.1428(6) 0.0309(15) Uani 1 1 d .
H11A H 0.5312 -1.8128 -0.1968 0.037 Uiso 1 1 calc R
C12 C 0.4550(6) -1.6280(5) -0.1766(6) 0.0257(13) Uani 1 1 d .
H12A H 0.5018 -1.5902 -0.2548 0.031 Uiso 1 1 calc R
N3 N 0.2157(5) -1.5283(4) 0.0987(5) 0.0244(11) Uani 1 1 d .
H3A H 0.1507 -1.4710 0.0721 0.029 Uiso 1 1 calc R
C13 C 0.2246(6) -1.5356(5) 0.2145(6) 0.0238(14) Uani 1 1 d .
O2 O 0.3209(4) -1.6025(3) 0.2594(4) 0.0268(10) Uani 1 1 d .
C14 C 0.1079(6) -1.4548(5) 0.2864(6) 0.0269(14) Uani 1 1 d .
C15 C -0.0390(6) -1.4371(5) 0.2645(6) 0.0338(15) Uani 1 1 d .
H15A H -0.0654 -1.4720 0.2007 0.041 Uiso 1 1 calc R
C16 C -0.1433(6) -1.3681(6) 0.3375(7) 0.0358(16) Uani 1 1 d .
H16A H -0.2437 -1.3598 0.3246 0.043 Uiso 1 1 calc R
C17 C 0.0304(6) -1.3260(5) 0.4424(6) 0.0287(15) Uani 1 1 d .
H17A H 0.0563 -1.2830 0.5017 0.034 Uiso 1 1 calc R
C18 C 0.1407(6) -1.3989(5) 0.3786(6) 0.0259(14) Uani 1 1 d .
H18A H 0.2381 -1.4109 0.3974 0.031 Uiso 1 1 calc R
N4 N -0.1125(5) -1.3117(4) 0.4258(5) 0.0293(12) Uani 1 1 d .
Cl50 Cl 0.1413(2) -1.11644(17) 0.1061(2) 0.0563(6) Uani 1 1 d .
C50 C -0.0155(7) -1.0655(5) 0.0373(7) 0.0420(18) Uani 1 1 d .
H50A H -0.0304 -1.1297 -0.0138 0.050 Uiso 1 1 calc R
H50B H -0.1086 -1.0598 0.0993 0.050 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_1
_geom_angle_site_symmetry_3
Cl1 Hg1 Cl2 152.99(7) . .
Cl1 Hg1 N4 103.02(11) . 2_535
Cl2 Hg1 N4 102.04(11) . 2_535
Cl1 Hg1 N1 99.25(11) . .
Cl2 Hg1 N1 92.94(11) . .
N4 Hg1 N1 84.68(16) 2_535 .
C5 N1 C1 117.6(5) . .
C5 N1 Hg1 123.8(4) . .
C1 N1 Hg1 116.5(4) . .
N1 C1 C2 122.9(5) . .
C1 C2 C3 119.3(5) . .
C4 C3 C2 118.3(5) . .
C4 C3 C6 124.0(4) . .
C2 C3 C6 117.6(4) . .
C5 C4 C3 119.0(5) . .
N1 C5 C4 122.8(5) . .
O1 C6 N2 124.6(5) . .
O1 C6 C3 120.3(4) . .
N2 C6 C3 115.0(5) . .
C6 N2 C7 126.3(4) . .
C12 C7 C8 119.9(5) . .
C12 C7 N2 118.2(6) . .
C8 C7 N2 121.8(5) . .
C9 C8 N3 120.0(6) . .
C9 C8 C7 118.6(5) . .
N3 C8 C7 121.4(4) . .
C10 C9 C8 119.9(6) . .
C11 C10 C9 120.5(5) . .
C10 C11 C12 120.0(6) . .
C7 C12 C11 121.0(6) . .
C13 N3 C8 125.1(4) . .
O2 C13 N3 123.6(6) . .
O2 C13 C14 121.5(6) . .
N3 C13 C14 114.9(5) . .
C18 C14 C15 118.3(6) . .
C18 C14 C13 120.8(5) . .
C15 C14 C13 120.9(6) . .
C16 C15 C14 118.3(6) . .
N4 C16 C15 124.1(5) . .
N4 C17 C18 123.8(6) . .
C17 C18 C14 118.8(5) . .
C16 N4 C17 116.6(5) . .
C16 N4 Hg1 114.8(3) . 2_535
C17 N4 Hg1 128.6(4) . 2_535
C50 C50 Cl50 108.9(5) 2_535 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hg1 Cl1 2.3507(13) .
Hg1 Cl2 2.3690(15) .
Hg1 N4 2.407(5) 2_535
Hg1 N1 2.490(5) .
N1 C5 1.348(7) .
N1 C1 1.349(6) .
C1 C2 1.374(7) .
C2 C3 1.391(7) .
C3 C4 1.389(7) .
C3 C6 1.508(7) .
C4 C5 1.383(8) .
C6 O1 1.240(6) .
C6 N2 1.350(6) .
N2 C7 1.421(6) .
C7 C12 1.366(8) .
C7 C8 1.411(8) .
C8 C9 1.409(7) .
C8 N3 1.410(7) .
C9 C10 1.384(9) .
C10 C11 1.373(9) .
C11 C12 1.382(7) .
N3 C13 1.351(8) .
C13 O2 1.234(6) .
C13 C14 1.497(8) .
C14 C18 1.383(8) .
C14 C15 1.404(7) .
C15 C16 1.371(9) .
C16 N4 1.340(8) .
C17 N4 1.346(6) .
C17 C18 1.371(8) .
N4 Hg1 2.407(5) 2_535
Cl50 C50 1.788(6) .
C50 C50 1.506(12) 2_535
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3A O1 0.88 1.96 2.704(6) 140.8 .
N2 H2B O2 0.88 2.12 2.898(6) 146.4 2_625
