#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/69/2236918.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2236918
loop_
_publ_author_name
'Shirvan, Sadif A.'
'Hossaini Sadr, Moayad'
_publ_section_title
;
 catena-Poly[di-μ₃-bromido-hexa-μ₂-bromido-dibromidobis(O-methyl
 pyridine-2-carboximidate-κ²N,N')pentamercury(II)]
;
_journal_coeditor_code           HY2602
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1492
_journal_paper_doi               10.1107/S1600536812046545
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Hg5 Br10 (C7 H8 N2 O)2]'
_chemical_formula_moiety         'C14 H16 Br10 Hg5 N4 O2'
_chemical_formula_sum            'C14 H16 Br10 Hg5 N4 O2'
_chemical_formula_weight         2074.26
_chemical_name_systematic
;
catena-Poly[di-μ₃-bromido-hexa-μ₂-bromido-
dibromidobis(O-methyl
pyridine-2-carboximidate-κ²N,N')pentamercury(II)]
;
_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                92.067(7)
_cell_angle_beta                 102.850(7)
_cell_angle_gamma                101.879(7)
_cell_formula_units_Z            1
_cell_length_a                   7.6768(7)
_cell_length_b                   10.7223(10)
_cell_length_c                   11.0663(10)
_cell_measurement_reflns_used    7320
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      1.89
_cell_volume                     865.86(14)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0839
_diffrn_reflns_av_sigmaI/netI    0.0959
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7320
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    33.645
_exptl_absorpt_correction_T_max  0.2225
_exptl_absorpt_correction_T_min  0.1054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    3.978
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             894
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.894
_refine_diff_density_min         -1.895
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0731P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1483
_reflns_number_gt                2042
_reflns_number_total             3410
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2602.cif
_cod_data_source_block           I
_cod_database_code               2236918
_cod_database_fobs_code          2236918
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
C C1 -0.003(4) 0.838(2) -0.726(2) 0.076(7) Uani d . 1 1
H H1A -0.0886 0.7662 -0.7095 0.091 Uiso calc R 1 1
H H1B 0.0734 0.8091 -0.7743 0.091 Uiso calc R 1 1
H H1C -0.0680 0.8955 -0.7723 0.091 Uiso calc R 1 1
C C2 0.211(2) 0.8446(18) -0.5315(18) 0.046(4) Uani d . 1 1
C C3 0.327(3) 0.9261(17) -0.4289(17) 0.046(4) Uani d . 1 1
C C4 0.329(3) 1.0579(19) -0.4102(19) 0.056(5) Uani d . 1 1
H H4 0.2567 1.0962 -0.4702 0.067 Uiso calc R 1 1
C C5 0.434(3) 1.128(2) -0.3060(19) 0.057(5) Uani d . 1 1
H H5 0.4316 1.2142 -0.2930 0.069 Uiso calc R 1 1
C C6 0.540(3) 1.075(2) -0.223(2) 0.063(6) Uani d . 1 1
H H6 0.6140 1.1230 -0.1517 0.076 Uiso calc R 1 1
C C7 0.539(3) 0.948(2) -0.244(2) 0.065(6) Uani d . 1 1
H H7 0.6186 0.9131 -0.1855 0.078 Uiso calc R 1 1
N N1 0.211(2) 0.7237(14) -0.5445(16) 0.054(4) Uani d . 1 1
H H1D 0.1406 0.6742 -0.6067 0.065 Uiso calc R 1 1
N N2 0.435(3) 0.8714(16) -0.3409(15) 0.059(5) Uani d . 1 1
O O1 0.110(2) 0.9040(13) -0.6109(12) 0.062(4) Uani d . 1 1
Hg Hg1 0.41370(13) 0.64830(8) -0.39109(9) 0.0623(3) Uani d . 1 1
Hg Hg2 0.5000 0.5000 0.0000 0.0588(3) Uani d S 1 2
Hg Hg3 0.95464(12) 0.64042(7) -0.14661(8) 0.0591(3) Uani d . 1 1
Br Br1 0.7283(3) 0.6379(2) -0.4186(2) 0.0619(6) Uani d . 1 1
Br Br2 0.2253(3) 0.5162(2) -0.26046(19) 0.0549(5) Uani d . 1 1
Br Br3 0.6541(3) 0.72282(19) -0.0001(2) 0.0607(5) Uani d . 1 1
Br Br4 1.1178(4) 0.8617(2) -0.1174(3) 0.0788(7) Uani d . 1 1
Br Br5 0.7893(3) 0.41969(18) -0.1371(2) 0.0544(5) Uani d . 1 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'
Hg Hg -2.3894 9.2266 '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'
Br Br -0.2901 2.4595 '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_site_symmetry_1
_geom_angle
O1 C1 H1A . 109.5
O1 C1 H1B . 109.5
H1A C1 H1B . 109.5
O1 C1 H1C . 109.5
H1A C1 H1C . 109.5
H1B C1 H1C . 109.5
N1 C2 O1 . 124.8(18)
N1 C2 C3 . 121.8(16)
O1 C2 C3 . 113.4(17)
N2 C3 C2 . 117.1(16)
N2 C3 C4 . 119.2(17)
C2 C3 C4 . 123.6(17)
C5 C4 C3 . 120.6(18)
C5 C4 H4 . 119.7
C3 C4 H4 . 119.7
C6 C5 C4 . 120(2)
C6 C5 H5 . 120.2
C4 C5 H5 . 120.2
C5 C6 C7 . 119(2)
C5 C6 H6 . 120.5
C7 C6 H6 . 120.5
N2 C7 C6 . 125(2)
N2 C7 H7 . 117.5
C6 C7 H7 . 117.5
C2 N1 Hg1 . 116.5(13)
C2 N1 H1D . 121.7
Hg1 N1 H1D . 121.7
C7 N2 C3 . 116.5(17)
C7 N2 Hg1 . 129.5(14)
C3 N2 Hg1 . 113.9(12)
C2 O1 C1 . 120.6(16)
N1 Hg1 N2 . 70.5(5)
N1 Hg1 Br1 . 120.2(4)
N2 Hg1 Br1 . 104.2(5)
N1 Hg1 Br2 . 107.2(4)
N2 Hg1 Br2 . 109.5(5)
Br1 Hg1 Br2 . 128.56(7)
Br3 Hg2 Br3 2_665 180.0
Br4 Hg3 Br5 . 169.89(9)
Br4 Hg3 Br1 . 98.67(8)
Br5 Hg3 Br1 . 89.75(7)
Hg1 Br1 Hg3 . 103.35(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 O1 . 1.44(3) ?
C1 H1A . 0.9600 ?
C1 H1B . 0.9600 ?
C1 H1C . 0.9600 ?
C2 N1 . 1.30(2) ?
C2 O1 . 1.313(19) ?
C2 C3 . 1.42(3) ?
C3 N2 . 1.36(2) ?
C3 C4 . 1.42(3) ?
C4 C5 . 1.35(3) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.31(3) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.38(3) ?
C6 H6 . 0.9300 ?
C7 N2 . 1.32(3) ?
C7 H7 . 0.9300 ?
Hg1 N1 . 2.322(14) y
N1 H1D . 0.8600 ?
Hg1 N2 . 2.400(16) y
Hg1 Br1 . 2.524(2) y
Hg1 Br2 . 2.534(2) y
Hg2 Br2 . 3.204(2) y
Hg2 Br3 . 2.438(2) y
Hg2 Br5 . 3.189(2) y
Hg3 Br1 . 3.119(2) y
Hg3 Br2 1_655 3.140(2) y
Hg3 Br3 . 3.337(2) y
Hg3 Br4 . 2.418(2) y
Hg3 Br5 . 2.463(2) y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N1 C2 C3 N2 -3(3)
O1 C2 C3 N2 179.0(17)
N1 C2 C3 C4 -179.0(19)
O1 C2 C3 C4 3(3)
N2 C3 C4 C5 -1(3)
C2 C3 C4 C5 176(2)
C3 C4 C5 C6 2(3)
C4 C5 C6 C7 -1(3)
C5 C6 C7 N2 -2(4)
O1 C2 N1 Hg1 177.9(14)
C3 C2 N1 Hg1 0(2)
C6 C7 N2 C3 3(3)
C6 C7 N2 Hg1 -179.3(17)
C2 C3 N2 C7 -178.4(19)
C4 C3 N2 C7 -2(3)
C2 C3 N2 Hg1 4(2)
C4 C3 N2 Hg1 -179.6(15)
N1 C2 O1 C1 -4(3)
C3 C2 O1 C1 173.9(19)
C2 N1 Hg1 N2 1.7(14)
C2 N1 Hg1 Br1 -93.8(14)
C2 N1 Hg1 Br2 106.8(14)
C7 N2 Hg1 N1 180(2)
C3 N2 Hg1 N1 -3.0(13)
C7 N2 Hg1 Br1 -63(2)
C3 N2 Hg1 Br1 114.5(14)
C7 N2 Hg1 Br2 78(2)
C3 N2 Hg1 Br2 -104.9(14)
N1 Hg1 Br1 Hg3 157.3(5)
N2 Hg1 Br1 Hg3 81.8(4)
Br2 Hg1 Br1 Hg3 -48.13(13)
Br4 Hg3 Br1 Hg1 -102.16(10)
Br5 Hg3 Br1 Hg1 72.22(8)
