#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:26:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179377 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/74/4327424.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_4327424
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            'C44 H44 Br4 Hg2 N8 O6'
_chemical_formula_weight         1501.69
_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                104.566(2)
_cell_angle_beta                 103.513(2)
_cell_angle_gamma                111.298(3)
_cell_formula_units_Z            1
_cell_length_a                   9.3850(4)
_cell_length_b                   12.2421(6)
_cell_length_c                   12.9873(8)
_cell_measurement_temperature    150(2)
_cell_volume                     1255.11(12)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.056
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12383
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    9.345
_exptl_absorpt_correction_T_max  0.6523
_exptl_absorpt_correction_T_min  0.3763
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.987
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.325
_refine_diff_density_min         -1.308
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         5707
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0461
_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)+(0.0505P)²+0.3950P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1134
_reflns_number_gt                3959
_reflns_number_total             5707
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0495002Bsi20040416_110705_3.cif
_cod_data_source_block           4b
_cod_original_cell_volume        1255.11(11)
_cod_database_code               4327424
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 0.96802(3) 0.32015(2) -0.95703(2) 0.04719(12) Uani 1 1 d . . .
Br1 Br 0.77452(9) 0.36728(7) -0.87418(8) 0.0618(2) Uani 1 1 d . . .
Br2 Br 1.05389(12) 0.23810(7) -1.11365(7) 0.0681(3) Uani 1 1 d . . .
N1 N 1.0707(7) 0.2275(5) -0.8289(5) 0.0376(13) Uani 1 1 d . . .
C1 C 1.1653(10) 0.1720(7) -0.8513(7) 0.053(2) Uani 1 1 d . . .
H1A H 1.1996 0.1758 -0.9141 0.064 Uiso 1 1 calc R . .
C2 C 1.2147(9) 0.1096(7) -0.7872(6) 0.0470(18) Uani 1 1 d . . .
H2A H 1.2841 0.0733 -0.8049 0.056 Uiso 1 1 calc R . .
C3 C 1.1641(7) 0.0998(5) -0.6975(5) 0.0287(13) Uani 1 1 d . . .
C4 C 1.0662(8) 0.1574(6) -0.6735(6) 0.0367(15) Uani 1 1 d . . .
H4A H 1.0281 0.1532 -0.6123 0.044 Uiso 1 1 calc R . .
C5 C 1.0257(9) 0.2208(6) -0.7400(6) 0.0421(17) Uani 1 1 d . . .
H5A H 0.9618 0.2622 -0.7214 0.051 Uiso 1 1 calc R . .
C6 C 1.2134(7) 0.0263(5) -0.6327(5) 0.0268(13) Uani 1 1 d . . .
O1 O 1.3442(5) 0.0224(4) -0.6241(4) 0.0368(10) Uani 1 1 d . . .
N2 N 1.1053(5) -0.0349(4) -0.5895(4) 0.0241(10) Uani 1 1 d . . .
H2B H 1.0234 -0.0164 -0.5875 0.029 Uiso 1 1 calc R . .
C7 C 1.1203(7) -0.1278(5) -0.5474(5) 0.0267(13) Uani 1 1 d . . .
C8 C 0.9924(7) -0.2516(5) -0.6031(5) 0.0320(14) Uani 1 1 d . . .
H8A H 0.8984 -0.2692 -0.6641 0.038 Uiso 1 1 calc R . .
C9 C 1.0032(8) -0.3479(6) -0.5693(6) 0.0380(16) Uani 1 1 d . . .
H9A H 0.9167 -0.4313 -0.6071 0.046 Uiso 1 1 calc R . .
C10 C 1.1412(8) -0.3221(6) -0.4798(6) 0.0423(17) Uani 1 1 d . . .
H10A H 1.1504 -0.3883 -0.4577 0.051 Uiso 1 1 calc R . .
C11 C 1.2643(7) -0.2000(6) -0.4235(5) 0.0340(14) Uani 1 1 d . . .
H11A H 1.3576 -0.1829 -0.3621 0.041 Uiso 1 1 calc R . .
C12 C 1.2548(6) -0.1018(5) -0.4547(5) 0.0262(13) Uani 1 1 d . . .
N3 N 1.3832(5) 0.0217(4) -0.3920(4) 0.0275(11) Uani 1 1 d . . .
H3A H 1.4821 0.0359 -0.3920 0.033 Uiso 1 1 calc R . .
C13 C 1.3637(7) 0.1187(5) -0.3321(5) 0.0291(13) Uani 1 1 d . . .
O2 O 1.2309(5) 0.1107(4) -0.3279(4) 0.0392(11) Uani 1 1 d . . .
C14 C 1.5165(7) 0.2421(5) -0.2678(5) 0.0269(13) Uani 1 1 d . . .
C15 C 1.6601(8) 0.2695(6) -0.2868(6) 0.0421(17) Uani 1 1 d . . .
H15A H 1.6686 0.2089 -0.3440 0.051 Uiso 1 1 calc R . .
C16 C 1.7923(8) 0.3850(6) -0.2229(6) 0.0441(18) Uani 1 1 d . . .
H16A H 1.8921 0.4009 -0.2359 0.053 Uiso 1 1 calc R . .
C17 C 1.6503(9) 0.4487(6) -0.1245(6) 0.0499(19) Uani 1 1 d . . .
H17A H 1.6468 0.5115 -0.0662 0.060 Uiso 1 1 calc R . .
C18 C 1.5096(8) 0.3342(6) -0.1840(6) 0.0425(17) Uani 1 1 d . . .
H18A H 1.4121 0.3197 -0.1679 0.051 Uiso 1 1 calc R . .
N4 N 1.7886(6) 0.4749(5) -0.1444(4) 0.0344(12) Uani 1 1 d . . .
O50 O 1.623(3) 0.475(2) -0.540(2) 0.181(10) Uiso 0.50 1 d PD A -1
C51 C 1.582(3) 0.464(3) -0.445(2) 0.097(8) Uiso 0.50 1 d PD A -1
H51A H 1.6839 0.4992 -0.3780 0.116 Uiso 0.50 1 calc PR A -1
H51B H 1.5178 0.3742 -0.4591 0.116 Uiso 0.50 1 calc PR A -1
C52 C 1.488(5) 0.532(4) -0.422(3) 0.166(15) Uiso 0.50 1 d PD A -1
H52A H 1.5470 0.6029 -0.3473 0.199 Uiso 0.50 1 calc PR A -1
H52B H 1.3796 0.4756 -0.4242 0.199 Uiso 0.50 1 calc PR A -1
C53 C 1.468(4) 0.580(3) -0.517(3) 0.137(14) Uiso 0.50 1 d PD A -1
H53A H 1.5223 0.6740 -0.4862 0.165 Uiso 0.50 1 calc PR A -1
H53B H 1.3506 0.5501 -0.5604 0.165 Uiso 0.50 1 calc PR A -1
C54 C 1.547(3) 0.530(2) -0.5910(18) 0.082(6) Uiso 0.50 1 d PD A -1
H54A H 1.4635 0.4689 -0.6662 0.099 Uiso 0.50 1 calc PR A -1
H54B H 1.6276 0.6003 -0.6032 0.099 Uiso 0.50 1 calc PR A -1
O60 O 1.6674(15) 0.0279(12) -0.0224(11) 0.073(3) Uiso 0.50 1 d PD B -1
C61 C 1.513(3) 0.012(4) -0.078(3) 0.114(15) Uiso 0.50 1 d PD B -1
H61A H 1.4473 -0.0737 -0.1374 0.137 Uiso 0.50 1 calc PR B -1
H61B H 1.5201 0.0743 -0.1144 0.137 Uiso 0.50 1 calc PR B -1
C62 C 1.427(2) 0.0299(15) 0.0110(14) 0.055(4) Uiso 0.50 1 d PD B -1
H62A H 1.4511 0.1191 0.0477 0.066 Uiso 0.50 1 calc PR B -1
H62B H 1.3073 -0.0244 -0.0221 0.066 Uiso 0.50 1 calc PR B -1
C63 C 1.517(3) -0.015(2) 0.0907(19) 0.059(7) Uiso 0.50 1 d PD B -1
H63A H 1.5753 0.0505 0.1685 0.071 Uiso 0.50 1 calc PR B -1
H63B H 1.4386 -0.0927 0.0948 0.071 Uiso 0.50 1 calc PR B -1
C64 C 1.632(2) -0.0408(16) 0.0447(16) 0.065(5) Uiso 0.50 1 d PD B -1
H64A H 1.7342 -0.0173 0.1077 0.078 Uiso 0.50 1 calc PR B -1
H64B H 1.5851 -0.1320 -0.0011 0.078 Uiso 0.50 1 calc PR B -1
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_1
_geom_angle_site_symmetry_3
N1 Hg1 N4 92.37(17) . 2_864
N1 Hg1 Br2 97.59(13) . .
N4 Hg1 Br2 97.64(13) 2_864 .
N1 Hg1 Br1 99.84(13) . .
N4 Hg1 Br1 99.38(12) 2_864 .
Br2 Hg1 Br1 155.01(3) . .
C5 N1 C1 117.1(6) . .
C5 N1 Hg1 122.1(4) . .
C1 N1 Hg1 120.6(5) . .
N1 C1 C2 122.7(7) . .
C3 C2 C1 120.1(6) . .
C2 C3 C4 117.5(6) . .
C2 C3 C6 118.8(5) . .
C4 C3 C6 123.6(6) . .
C5 C4 C3 118.8(6) . .
N1 C5 C4 123.8(6) . .
O1 C6 N2 124.4(5) . .
O1 C6 C3 119.3(5) . .
N2 C6 C3 116.2(5) . .
C6 N2 C7 121.8(5) . .
C12 C7 C8 119.5(5) . .
C12 C7 N2 123.1(5) . .
C8 C7 N2 117.5(5) . .
C9 C8 C7 120.2(6) . .
C8 C9 C10 119.9(6) . .
C11 C10 C9 119.7(6) . .
C10 C11 C12 121.4(6) . .
C11 C12 C7 119.2(5) . .
C11 C12 N3 118.7(5) . .
C7 C12 N3 122.1(5) . .
C13 N3 C12 124.1(5) . .
O2 C13 N3 123.7(5) . .
O2 C13 C14 120.2(5) . .
N3 C13 C14 116.1(5) . .
C15 C14 C18 118.0(5) . .
C15 C14 C13 124.5(5) . .
C18 C14 C13 117.5(5) . .
C14 C15 C16 119.7(6) . .
N4 C16 C15 123.7(6) . .
N4 C17 C18 123.7(6) . .
C14 C18 C17 117.8(6) . .
C16 N4 C17 117.0(6) . .
C16 N4 Hg1 119.8(4) . 2_864
C17 N4 Hg1 123.2(4) . 2_864
C54 O50 C51 111.1(18) . .
O50 C51 C52 110.3(18) . .
C51 C52 C53 103.5(17) . .
C52 C53 C54 106.0(16) . .
O50 C54 C53 108.3(18) . .
C64 O60 C61 100(2) . .
O60 C61 C62 109(2) . .
C63 C62 C61 95.7(15) . .
C64 C63 C62 106.8(15) . .
O60 C64 C63 109.0(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hg1 N1 2.445(5) .
Hg1 N4 2.453(5) 2_864
Hg1 Br2 2.4743(9) .
Hg1 Br1 2.4800(9) .
N1 C5 1.330(9) .
N1 C1 1.339(8) .
C1 C2 1.374(10) .
C2 C3 1.374(9) .
C3 C4 1.390(8) .
C3 C6 1.494(8) .
C4 C5 1.375(9) .
C6 O1 1.226(6) .
C6 N2 1.353(7) .
N2 C7 1.416(7) .
C7 C12 1.396(8) .
C7 C8 1.408(8) .
C8 C9 1.384(8) .
C9 C10 1.394(9) .
C10 C11 1.380(9) .
C11 C12 1.387(8) .
C12 N3 1.414(7) .
N3 C13 1.345(7) .
C13 O2 1.229(7) .
C13 C14 1.506(7) .
C14 C15 1.363(9) .
C14 C18 1.389(8) .
C15 C16 1.371(8) .
C16 N4 1.316(8) .
C17 N4 1.323(9) .
C17 C18 1.393(9) .
N4 Hg1 2.453(5) 2_864
O50 C54 1.33(2) .
O50 C51 1.39(2) .
C51 C52 1.45(2) .
C52 C53 1.49(2) .
C53 C54 1.49(2) .
O60 C64 1.371(18) .
O60 C61 1.38(2) .
C61 C62 1.56(2) .
C62 C63 1.52(2) .
C63 C64 1.44(2) .
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
N2 H2B O2 0.88 2.09 2.786(6) 135.2 2_754
N3 H3A O1 0.88 1.99 2.772(6) 147.0 2_854
