#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:41:46 +0100 (Fri 25 de Mar de 2016) $
#$Revision: 179931 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/26/7022654.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_7022654
loop_
_publ_author_name
'Wang, Kai-Yao'
'Ye, Dong'
'Zhou, Liu-Jiang'
'Feng, Mei-Ling'
'Huang, Xiao-Ying'
_publ_section_title
;
 Novel mercury selenidoantimonates with structures ranging from
 one-dimensional ribbon to three-dimensional open-framework.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5454
_journal_page_last               5461
_journal_paper_doi               10.1039/c3dt32676d
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'Hg Sb2 Se5, C9 H30 N6 Ni'
_chemical_formula_sum            'C9 H30 Hg N6 Ni Sb2 Se5'
_chemical_formula_weight         1119.99
_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                105.999(4)
_cell_angle_beta                 97.174(4)
_cell_angle_gamma                118.831(5)
_cell_formula_units_Z            2
_cell_length_a                   11.2626(6)
_cell_length_b                   11.5370(6)
_cell_length_c                   12.1698(5)
_cell_measurement_reflns_used    2976
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.0525
_cell_measurement_theta_min      2.2382
_cell_volume                     1267.70(14)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'DIAMOND. Version 3.0. Crystal Impact'
_computing_publication_material  'Windows Word 2003'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 16.2083
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10641
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    16.061
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis CCD; Oxford, 2006'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.934
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.998
_refine_diff_density_min         -1.179
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         5231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0375
_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)+(0.0171P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0673
_reflns_number_gt                4047
_reflns_number_total             5231
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32676d.txt
_cod_data_source_block           compound-1-KW3-9B
_cod_original_cell_volume        1267.70(11)
_cod_database_code               7022654
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 0.69279(3) -0.06806(4) -0.14564(3) 0.03485(10) Uani 1 1 d .
Sb1 Sb 0.67600(5) 0.13570(5) 0.15891(4) 0.02480(12) Uani 1 1 d .
Sb2 Sb 0.95836(5) 0.06274(5) 0.14633(4) 0.02804(13) Uani 1 1 d .
Se1 Se 0.52005(7) 0.10205(8) 0.30057(6) 0.02752(18) Uani 1 1 d .
Se2 Se 0.58131(8) -0.12499(8) 0.03450(6) 0.02888(18) Uani 1 1 d .
Se3 Se 0.89225(8) 0.18399(9) 0.31871(7) 0.0344(2) Uani 1 1 d .
Se4 Se 1.22300(8) 0.22575(8) 0.26111(7) 0.03087(19) Uani 1 1 d .
Se5 Se 0.92858(7) 0.18489(8) 0.00532(7) 0.03201(19) Uani 1 1 d .
Ni1 Ni 0.67928(10) 0.35150(10) 0.72930(8) 0.0307(2) Uani 1 1 d .
N1 N 0.6905(6) 0.1853(6) 0.6130(5) 0.0382(17) Uani 1 1 d .
H1C H 0.6470 0.1069 0.6307 0.046 Uiso 1 1 calc R
H1D H 0.6453 0.1620 0.5365 0.046 Uiso 1 1 calc R
N2 N 0.8965(7) 0.4747(7) 0.7322(5) 0.0476(19) Uani 1 1 d .
H2B H 0.9145 0.5544 0.7202 0.057 Uiso 1 1 calc R
H2C H 0.9558 0.5011 0.8038 0.057 Uiso 1 1 calc R
N3 N 0.6069(7) 0.3984(7) 0.5892(5) 0.0453(19) Uani 1 1 d .
H3D H 0.6605 0.4932 0.6063 0.054 Uiso 1 1 calc R
H3E H 0.6137 0.3517 0.5201 0.054 Uiso 1 1 calc R
N4 N 0.4545(6) 0.2137(7) 0.6963(5) 0.0381(17) Uani 1 1 d .
H4C H 0.4321 0.1247 0.6872 0.046 Uiso 1 1 calc R
H4D H 0.4292 0.2471 0.7590 0.046 Uiso 1 1 calc R
N5 N 0.7275(6) 0.3051(6) 0.8808(5) 0.0280(14) Uani 1 1 d .
H5B H 0.6504 0.2256 0.8787 0.034 Uiso 1 1 calc R
H5C H 0.7981 0.2890 0.8789 0.034 Uiso 1 1 calc R
N6 N 0.6966(6) 0.5236(6) 0.8666(5) 0.0316(15) Uani 1 1 d .
H6D H 0.7819 0.6043 0.8847 0.038 Uiso 1 1 calc R
H6E H 0.6285 0.5383 0.8409 0.038 Uiso 1 1 calc R
C1 C 0.8419(9) 0.2326(9) 0.6263(8) 0.055(3) Uani 1 1 d .
H1A H 0.8829 0.2268 0.6980 0.065 Uiso 1 1 calc R
H1B H 0.8488 0.1722 0.5573 0.065 Uiso 1 1 calc R
C2 C 0.9181(9) 0.3836(10) 0.6352(8) 0.057(3) Uani 1 1 d .
H2A H 0.8752 0.3826 0.5596 0.069 Uiso 1 1 calc R
C3 C 1.0797(10) 0.4443(11) 0.6468(8) 0.075(3) Uani 1 1 d .
H3A H 1.1226 0.5356 0.6396 0.112 Uiso 1 1 calc R
H3B H 1.0874 0.3787 0.5843 0.112 Uiso 1 1 calc R
H3C H 1.1278 0.4556 0.7236 0.112 Uiso 1 1 calc R
C4 C 0.4568(9) 0.3524(9) 0.5766(7) 0.053(3) Uani 1 1 d .
H4A H 0.4130 0.3463 0.4996 0.063 Uiso 1 1 calc R
H4B H 0.4527 0.4224 0.6393 0.063 Uiso 1 1 calc R
C5 C 0.3775(9) 0.2097(9) 0.5854(7) 0.052(2) Uani 1 1 d .
H5A H 0.3772 0.1406 0.5170 0.062 Uiso 1 1 calc R
C6 C 0.2210(9) 0.1580(10) 0.5758(8) 0.064(3) Uani 1 1 d .
H6A H 0.1759 0.1555 0.5020 0.096 Uiso 1 1 calc R
H6B H 0.2172 0.2228 0.6423 0.096 Uiso 1 1 calc R
H6C H 0.1723 0.0637 0.5771 0.096 Uiso 1 1 calc R
C7 C 0.7716(8) 0.4272(8) 0.9918(6) 0.0321(19) Uani 1 1 d .
H7A H 0.8715 0.5001 1.0111 0.039 Uiso 1 1 calc R
H7B H 0.7589 0.3956 1.0580 0.039 Uiso 1 1 calc R
C8 C 0.6812(8) 0.4900(8) 0.9741(6) 0.0311(18) Uani 1 1 d .
H8A H 0.5813 0.4157 0.9579 0.037 Uiso 1 1 calc R
C9 C 0.7243(9) 0.6184(9) 1.0872(7) 0.048(2) Uani 1 1 d .
H9A H 0.7082 0.5879 1.1527 0.072 Uiso 1 1 calc R
H9B H 0.6683 0.6576 1.0730 0.072 Uiso 1 1 calc R
H9C H 0.8233 0.6904 1.1068 0.072 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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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
Se4 Hg1 Se1 107.99(3) 2_755 2_655
Se4 Hg1 Se5 107.19(3) 2_755 .
Se1 Hg1 Se5 126.04(3) 2_655 .
Se4 Hg1 Se2 119.53(3) 2_755 .
Se1 Hg1 Se2 102.80(2) 2_655 .
Se5 Hg1 Se2 93.76(2) . .
Se2 Sb1 Se1 100.10(3) . .
Se2 Sb1 Se3 97.16(3) . .
Se1 Sb1 Se3 93.10(3) . .
Se4 Sb2 Se5 102.49(3) . .
Se4 Sb2 Se3 92.35(3) . .
Se5 Sb2 Se3 97.49(3) . .
Sb1 Se1 Hg1 93.51(3) . 2_655
Sb1 Se2 Hg1 94.66(3) . .
Sb2 Se3 Sb1 89.38(3) . .
Sb2 Se4 Hg1 98.54(3) . 2_755
Sb2 Se5 Hg1 89.60(3) . .
N3 Ni1 N1 94.2(3) . .
N3 Ni1 N6 93.9(2) . .
N1 Ni1 N6 170.5(2) . .
N3 Ni1 N5 171.3(2) . .
N1 Ni1 N5 91.9(2) . .
N6 Ni1 N5 80.7(2) . .
N3 Ni1 N2 92.3(3) . .
N1 Ni1 N2 80.9(2) . .
N6 Ni1 N2 93.8(2) . .
N5 Ni1 N2 94.9(2) . .
N3 Ni1 N4 81.7(2) . .
N1 Ni1 N4 92.8(2) . .
N6 Ni1 N4 93.3(2) . .
N5 Ni1 N4 91.8(2) . .
N2 Ni1 N4 171.0(2) . .
C1 N1 Ni1 110.1(5) . .
C1 N1 H1C 109.6 . .
Ni1 N1 H1C 109.6 . .
C1 N1 H1D 109.6 . .
Ni1 N1 H1D 109.6 . .
H1C N1 H1D 108.2 . .
C2 N2 Ni1 107.7(5) . .
C2 N2 H2B 110.2 . .
Ni1 N2 H2B 110.2 . .
C2 N2 H2C 110.2 . .
Ni1 N2 H2C 110.2 . .
H2B N2 H2C 108.5 . .
C4 N3 Ni1 108.4(5) . .
C4 N3 H3D 110.0 . .
Ni1 N3 H3D 110.0 . .
C4 N3 H3E 110.0 . .
Ni1 N3 H3E 110.0 . .
H3D N3 H3E 108.4 . .
C5 N4 Ni1 108.7(5) . .
C5 N4 H4C 109.9 . .
Ni1 N4 H4C 109.9 . .
C5 N4 H4D 109.9 . .
Ni1 N4 H4D 109.9 . .
H4C N4 H4D 108.3 . .
C7 N5 Ni1 109.4(4) . .
C7 N5 H5B 109.8 . .
Ni1 N5 H5B 109.8 . .
C7 N5 H5C 109.8 . .
Ni1 N5 H5C 109.8 . .
H5B N5 H5C 108.2 . .
C8 N6 Ni1 109.8(4) . .
C8 N6 H6D 109.7 . .
Ni1 N6 H6D 109.7 . .
C8 N6 H6E 109.7 . .
Ni1 N6 H6E 109.7 . .
H6D N6 H6E 108.2 . .
C2 C1 N1 106.8(7) . .
C2 C1 H1A 110.4 . .
N1 C1 H1A 110.4 . .
C2 C1 H1B 110.4 . .
N1 C1 H1B 110.4 . .
H1A C1 H1B 108.6 . .
N2 C2 C1 111.3(7) . .
N2 C2 C3 113.1(7) . .
C1 C2 C3 111.3(8) . .
N2 C2 H2A 106.9 . .
C1 C2 H2A 106.9 . .
C3 C2 H2A 106.9 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N3 C4 C5 109.9(7) . .
N3 C4 H4A 109.7 . .
C5 C4 H4A 109.7 . .
N3 C4 H4B 109.7 . .
C5 C4 H4B 109.7 . .
H4A C4 H4B 108.2 . .
N4 C5 C4 109.8(6) . .
N4 C5 C6 113.0(7) . .
C4 C5 C6 112.0(8) . .
N4 C5 H5A 107.2 . .
C4 C5 H5A 107.2 . .
C6 C5 H5A 107.2 . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N5 C7 C8 109.2(6) . .
N5 C7 H7A 109.8 . .
C8 C7 H7A 109.8 . .
N5 C7 H7B 109.8 . .
C8 C7 H7B 109.8 . .
H7A C7 H7B 108.3 . .
N6 C8 C9 114.1(6) . .
N6 C8 C7 106.4(5) . .
C9 C8 C7 111.1(6) . .
N6 C8 H8A 108.3 . .
C9 C8 H8A 108.3 . .
C7 C8 H8A 108.3 . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hg1 Se4 2.6023(8) 2_755
Hg1 Se1 2.6481(8) 2_655
Hg1 Se5 2.7010(8) .
Hg1 Se2 2.7385(7) .
Sb1 Se2 2.5432(9) .
Sb1 Se1 2.5837(8) .
Sb1 Se3 2.6335(9) .
Sb2 Se4 2.5450(9) .
Sb2 Se5 2.5863(10) .
Sb2 Se3 2.5863(9) .
Se1 Hg1 2.6481(8) 2_655
Se4 Hg1 2.6023(8) 2_755
Ni1 N3 2.110(6) .
Ni1 N1 2.116(6) .
Ni1 N6 2.118(6) .
Ni1 N5 2.135(6) .
Ni1 N2 2.146(6) .
Ni1 N4 2.147(6) .
N1 C1 1.489(9) .
N1 H1C 0.9000 .
N1 H1D 0.9000 .
N2 C2 1.480(9) .
N2 H2B 0.9000 .
N2 H2C 0.9000 .
N3 C4 1.479(10) .
N3 H3D 0.9000 .
N3 H3E 0.9000 .
N4 C5 1.487(9) .
N4 H4C 0.9000 .
N4 H4D 0.9000 .
N5 C7 1.472(8) .
N5 H5B 0.9000 .
N5 H5C 0.9000 .
N6 C8 1.471(8) .
N6 H6D 0.9000 .
N6 H6E 0.9000 .
C1 C2 1.488(11) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 C3 1.573(11) .
C2 H2A 0.9800 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 C5 1.491(11) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C6 1.540(11) .
C5 H5A 0.9800 .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 C8 1.533(10) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C9 1.530(9) .
C8 H8A 0.9800 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
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
N1 H1C Se1 0.90 2.68 3.561(6) 166.5 2_656
N1 H1D Se1 0.90 2.77 3.668(6) 176.8 .
N2 H2B Se3 0.90 2.96 3.772(7) 150.4 2_766
N3 H3D Se4 0.90 2.71 3.543(7) 155.1 2_766
N3 H3E Se1 0.90 2.94 3.780(6) 155.0 .
N4 H4C Se1 0.90 2.95 3.799(7) 157.6 2_656
N5 H5B Se2 0.90 2.78 3.547(5) 144.3 2_656
N5 H5C Se5 0.90 2.85 3.560(6) 136.7 1_556
N6 H6D Se5 0.90 2.79 3.651(6) 159.8 2_766
C4 H4A Se4 0.97 2.88 3.805(8) 160.0 1_455
