#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/18/2201819.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_2201819
loop_
_publ_author_name
'Nockemann, Peter'
'Meyer, Gerd'
_publ_section_title
;
 Bis(tetrabutylammonium) decaiodotetramercurate(II),
 (Bu₄N)₂[Hg₄I₁₀]
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m236
_journal_page_last               m238
_journal_paper_doi               10.1107/S1600536803007335
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '(C16 H36 N)2 [Hg4 I10]'
_chemical_formula_moiety         '2C16 H36 N 1+, Hg4 I10 2-'
_chemical_formula_sum            'C32 H72 Hg4 I10 N2'
_chemical_formula_weight         2556.28
_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                114.33
_cell_angle_beta                 104.18
_cell_angle_gamma                90.18
_cell_formula_units_Z            2
_cell_length_a                   11.681
_cell_length_b                   15.770
_cell_length_c                   18.288
_cell_measurement_reflns_used    37776
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      59.3
_cell_measurement_theta_min      3.6
_cell_volume                     2955.378
_computing_cell_refinement       'X-STEP32 (Stoe & Cie, 2000)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2001)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, Bonn, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
;
Stoe Imaging Plate Diffraction System, IPDS-I
;
_diffrn_measurement_method       φ
_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  0.1069
_diffrn_reflns_av_sigmaI/netI    0.1229
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37776
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.602
_exptl_absorpt_correction_T_max  0.210
_exptl_absorpt_correction_T_min  0.075
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE (Stoe & Cie, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.873
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prismatic needles'
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.232
_refine_diff_density_min         -1.220
_refine_ls_extinction_coef       0.001058(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.746
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         11615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.746
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0383
_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)] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0601
_reflns_number_gt                5987
_reflns_number_total             11615
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt6259.cif
_cod_data_source_block           I
_cod_original_cell_volume        2955.3
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               2201819
_cod_database_fobs_code          2201819
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Hg1 0.38130(5) 0.22200(4) 0.90692(3) 0.04672(14) Uani d . 1 . . Hg
Hg2 0.24241(5) 0.26466(4) 0.48016(3) 0.05259(15) Uani d . 1 . . Hg
Hg3 0.17054(5) 0.26822(4) 0.25961(3) 0.04796(14) Uani d . 1 . . Hg
Hg4 0.32403(5) 0.23488(4) 0.69056(3) 0.05249(15) Uani d . 1 . . Hg
I1 0.21389(6) 0.11121(5) 0.73107(4) 0.03533(18) Uani d . 1 . . I
I2 0.55075(7) 0.11387(6) 0.92013(5) 0.0418(2) Uani d . 1 . . I
I3 0.37342(7) 0.37437(6) 0.44126(5) 0.0456(2) Uani d . 1 . . I
I4 0.27812(8) 0.14200(6) 0.16275(6) 0.0498(2) Uani d . 1 . . I
I5 0.04493(7) 0.40968(7) 0.28468(6) 0.0537(2) Uani d . 1 . . I
I6 0.24863(8) 0.33706(7) 0.99093(6) 0.0580(3) Uani d . 1 . . I
I7 0.40076(7) 0.15357(5) 0.54342(5) 0.03795(19) Uani d . 1 . . I
I8 0.49995(7) 0.34043(6) 0.83231(5) 0.0405(2) Uani d . 1 . . I
I9 0.05955(7) 0.16003(6) 0.34222(5) 0.0404(2) Uani d . 1 . . I
I10 0.16514(7) 0.34376(5) 0.62856(5) 0.03698(19) Uani d . 1 . . I
N1 0.6372(8) 0.3455(6) 0.2355(6) 0.033(2) Uani d . 1 . . N
C1 0.6908(9) 0.3962(7) 0.1937(6) 0.032(3) Uani d . 1 . . C
H1B 0.7112 0.4619 0.2322 0.039 Uiso calc R 1 . . H
H1A 0.7642 0.3709 0.1843 0.039 Uiso calc R 1 . . H
C3 0.7231(9) 0.3759(8) 0.3206(6) 0.033(3) Uani d . 1 . . C
H3B 0.8025 0.3667 0.3136 0.040 Uiso calc R 1 . . H
H3A 0.7221 0.4426 0.3520 0.040 Uiso calc R 1 . . H
C2 0.6193(10) 0.2403(7) 0.1847(7) 0.033(3) Uani d . 1 . . C
H2B 0.5823 0.2122 0.2128 0.040 Uiso calc R 1 . . H
H2A 0.5634 0.2264 0.1312 0.040 Uiso calc R 1 . . H
C6 0.7271(11) 0.1935(8) 0.1690(8) 0.048(3) Uani d . 1 . . C
H6B 0.7912 0.2175 0.2201 0.057 Uiso calc R 1 . . H
H6A 0.7527 0.2066 0.1278 0.057 Uiso calc R 1 . . H
C5 0.6128(10) 0.3898(8) 0.1117(6) 0.035(3) Uani d . 1 . . C
H5B 0.5402 0.4171 0.1202 0.042 Uiso calc R 1 . . H
H5A 0.5914 0.3245 0.0722 0.042 Uiso calc R 1 . . H
C9 0.6784(11) 0.4418(8) 0.0762(7) 0.041(3) Uani d . 1 . . C
H9B 0.6214 0.4513 0.0326 0.049 Uiso calc R 1 . . H
H9A 0.7137 0.5029 0.1200 0.049 Uiso calc R 1 . . H
C13 0.7760(11) 0.3889(9) 0.0405(8) 0.047(3) Uani d . 1 . . C
H13C 0.8149 0.4247 0.0200 0.056 Uiso calc R 1 . . H
H13B 0.7412 0.3292 -0.0044 0.056 Uiso calc R 1 . . H
H13A 0.8330 0.3795 0.0833 0.056 Uiso calc R 1 . . H
C4 0.5129(10) 0.3763(8) 0.2415(7) 0.036(3) Uani d . 1 . . C
H4B 0.4624 0.3586 0.1856 0.043 Uiso calc R 1 . . H
H4A 0.4783 0.3421 0.2660 0.043 Uiso calc R 1 . . H
C8 0.5121(10) 0.4802(8) 0.2922(7) 0.041(3) Uani d . 1 . . C
H8B 0.5518 0.5164 0.2717 0.049 Uiso calc R 1 . . H
H8A 0.5530 0.4982 0.3503 0.049 Uiso calc R 1 . . H
C12 0.3780(11) 0.4986(8) 0.2825(8) 0.043(3) Uani d . 1 . . C
H12B 0.3399 0.4851 0.2248 0.052 Uiso calc R 1 . . H
H12A 0.3373 0.4568 0.2973 0.052 Uiso calc R 1 . . H
C7 0.7001(11) 0.3270(10) 0.3713(8) 0.053(3) Uani d . 1 . . C
H7B 0.7018 0.2601 0.3415 0.064 Uiso calc R 1 . . H
H7A 0.6221 0.3371 0.3808 0.064 Uiso calc R 1 . . H
C11 0.799(2) 0.3666(12) 0.4578(10) 0.109(8) Uani d . 1 . . C
H11B 0.8769 0.3628 0.4477 0.131 Uiso calc R 1 . . H
H11A 0.7916 0.4321 0.4893 0.131 Uiso calc R 1 . . H
C16 0.3674(12) 0.5986(9) 0.3374(9) 0.055(4) Uani d . 1 . . C
H16C 0.2849 0.6078 0.3306 0.066 Uiso calc R 1 . . H
H16B 0.4061 0.6400 0.3220 0.066 Uiso calc R 1 . . H
H16A 0.4044 0.6119 0.3946 0.066 Uiso calc R 1 . . H
C10 0.6987(12) 0.0892(8) 0.1382(9) 0.051(3) Uani d . 1 . . C
H10B 0.6284 0.0679 0.0911 0.061 Uiso calc R 1 . . H
H10A 0.6793 0.0773 0.1820 0.061 Uiso calc R 1 . . H
C14 0.7961(13) 0.0320(10) 0.1119(10) 0.066(4) Uani d . 1 . . C
H14C 0.7709 -0.0330 0.0944 0.079 Uiso calc R 1 . . H
H14B 0.8661 0.0519 0.1581 0.079 Uiso calc R 1 . . H
H14A 0.8135 0.0405 0.0666 0.079 Uiso calc R 1 . . H
N2 0.1871(7) 0.8544(6) 0.2661(5) 0.025(2) Uani d . 1 . . N
C25 0.1782(11) 0.9389(10) 0.4984(7) 0.053(4) Uani d . 1 . . C
H25B 0.2333 0.9385 0.5475 0.064 Uiso calc R 1 . . H
H25A 0.1729 1.0037 0.5076 0.064 Uiso calc R 1 . . H
C21 0.2272(11) 0.8888(9) 0.4227(7) 0.044(3) Uani d . 1 . . C
H21B 0.3102 0.9122 0.4367 0.053 Uiso calc R 1 . . H
H21A 0.2222 0.8221 0.4083 0.053 Uiso calc R 1 . . H
C17 0.1578(10) 0.9046(7) 0.3490(6) 0.032(3) Uani d . 1 . . C
H17B 0.1677 0.9713 0.3642 0.039 Uiso calc R 1 . . H
H17A 0.0742 0.8868 0.3402 0.039 Uiso calc R 1 . . H
C19 0.1084(9) 0.8829(7) 0.2042(6) 0.029(2) Uani d . 1 . . C
H19B 0.1254 0.9501 0.2238 0.035 Uiso calc R 1 . . H
H19A 0.0265 0.8704 0.2032 0.035 Uiso calc R 1 . . H
C23 0.1188(11) 0.8357(8) 0.1153(7) 0.041(3) Uani d . 1 . . C
H23B 0.2011 0.8448 0.1155 0.049 Uiso calc R 1 . . H
H23A 0.0954 0.7689 0.0930 0.049 Uiso calc R 1 . . H
C27 0.0417(10) 0.8747(10) 0.0600(7) 0.047(3) Uani d . 1 . . C
H27B 0.0689 0.9406 0.0805 0.056 Uiso calc R 1 . . H
H27A -0.0394 0.8698 0.0634 0.056 Uiso calc R 1 . . H
C31 0.0431(13) 0.8249(12) -0.0300(8) 0.065(4) Uani d . 1 . . C
H31C -0.0072 0.8525 -0.0621 0.078 Uiso calc R 1 . . H
H31B 0.0146 0.7598 -0.0512 0.078 Uiso calc R 1 . . H
H31A 0.1229 0.8306 -0.0341 0.078 Uiso calc R 1 . . H
C20 0.3188(9) 0.8807(7) 0.2771(6) 0.028(2) Uani d . 1 . . C
H20B 0.3382 0.8428 0.2255 0.034 Uiso calc R 1 . . H
H20A 0.3661 0.8644 0.3200 0.034 Uiso calc R 1 . . H
C24 0.3562(9) 0.9847(8) 0.3008(7) 0.034(3) Uani d . 1 . . C
H24B 0.3246 0.9993 0.2536 0.041 Uiso calc R 1 . . H
H24A 0.3258 1.0250 0.3466 0.041 Uiso calc R 1 . . H
C28 0.4894(9) 0.9998(8) 0.3257(7) 0.035(3) Uani d . 1 . . C
H28B 0.5193 0.9524 0.2832 0.042 Uiso calc R 1 . . H
H28A 0.5199 0.9938 0.3775 0.042 Uiso calc R 1 . . H
C18 0.1714(9) 0.7474(6) 0.2367(7) 0.029(2) Uani d . 1 . . C
H18B 0.1962 0.7178 0.1859 0.035 Uiso calc R 1 . . H
H18A 0.2232 0.7321 0.2787 0.035 Uiso calc R 1 . . H
C22 0.0441(10) 0.7069(8) 0.2204(8) 0.044(3) Uani d . 1 . . C
H22B 0.0166 0.7391 0.2698 0.053 Uiso calc R 1 . . H
H22A -0.0073 0.7172 0.1751 0.053 Uiso calc R 1 . . H
C29 0.0592(15) 0.8946(12) 0.4877(10) 0.079(5) Uani d . 1 . . C
H29C 0.0325 0.9285 0.5365 0.095 Uiso calc R 1 . . H
H29B 0.0643 0.8308 0.4799 0.095 Uiso calc R 1 . . H
H29A 0.0038 0.8959 0.4399 0.095 Uiso calc R 1 . . H
C26 0.0357(11) 0.6017(8) 0.1980(7) 0.040(3) Uani d . 1 . . C
H26B 0.0816 0.5925 0.2456 0.048 Uiso calc R 1 . . H
H26A -0.0466 0.5784 0.1870 0.048 Uiso calc R 1 . . H
C30 0.0794(13) 0.5455(9) 0.1241(9) 0.065(4) Uani d . 1 . . C
H30C 0.0738 0.4808 0.1145 0.078 Uiso calc R 1 . . H
H30B 0.1608 0.5681 0.1343 0.078 Uiso calc R 1 . . H
H30A 0.0318 0.5514 0.0759 0.078 Uiso calc R 1 . . H
C32 0.5330(11) 1.0989(9) 0.3371(8) 0.052(4) Uani d . 1 . . C
H32C 0.6183 1.1080 0.3535 0.063 Uiso calc R 1 . . H
H32B 0.5036 1.1456 0.3795 0.063 Uiso calc R 1 . . H
H32A 0.5039 1.1042 0.2855 0.063 Uiso calc R 1 . . H
C15 0.789(2) 0.316(2) 0.5052(16) 0.167(12) Uani d . 1 . . C
H15C 0.8509 0.3418 0.5566 0.200 Uiso calc R 1 . . H
H15B 0.7965 0.2516 0.4742 0.200 Uiso calc R 1 . . H
H15A 0.7129 0.3218 0.5170 0.200 Uiso calc R 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
I6 Hg1 I2 142.91(4) y
I6 Hg1 I1 104.66(3) y
I2 Hg1 I1 104.76(3) y
I6 Hg1 I8 104.08(3) y
I2 Hg1 I8 99.08(3) y
I1 Hg1 I8 87.89(2) y
I3 Hg2 I9 108.93(3) y
I3 Hg2 I10 120.18(3) y
I9 Hg2 I10 112.23(3) y
I3 Hg2 I7 108.25(3) y
I9 Hg2 I7 114.09(3) y
I10 Hg2 I7 92.33(3) y
I5 Hg3 I4 149.08(4) y
I5 Hg3 I9 101.10(3) y
I4 Hg3 I9 103.60(3) y
I5 Hg3 I3 94.43(3) y
I4 Hg3 I3 105.20(3) y
I9 Hg3 I3 86.82(2) y
I8 Hg4 I1 104.75(3) y
I8 Hg4 I7 114.82(3) y
I1 Hg4 I7 115.92(3) y
I8 Hg4 I10 113.95(3) y
I1 Hg4 I10 114.20(3) y
I7 Hg4 I10 93.49(3) y
Hg4 I1 Hg1 84.53(2) y
Hg2 I3 Hg3 80.86(3) y
Hg4 I7 Hg2 86.95(3) y
Hg4 I8 Hg1 82.50(3) y
Hg2 I9 Hg3 83.38(2) y
Hg2 I10 Hg4 87.22(3) y
C3 N1 C2 113.0(9) y
C3 N1 C1 104.9(8) y
C2 N1 C1 111.6(8) y
C3 N1 C4 111.6(8) y
C2 N1 C4 106.7(8) y
C1 N1 C4 109.1(8) y
C5 C1 N1 116.0(8) n
C7 C3 N1 116.1(9) n
C6 C2 N1 117.1(9) n
C2 C6 C10 109.5(9) n
C1 C5 C9 110.4(9) n
C13 C9 C5 112.9(10) n
C8 C4 N1 114.9(9) n
C4 C8 C12 107.0(9) n
C16 C12 C8 111.2(10) n
C3 C7 C11 109.3(11) n
C15 C11 C7 111.9(18) n
C6 C10 C14 115.3(11) n
C19 N2 C17 108.2(8) y
C19 N2 C20 111.1(7) y
C17 N2 C20 109.4(7) y
C19 N2 C18 111.5(8) y
C17 N2 C18 110.9(8) y
C20 N2 C18 105.7(7) y
C29 C25 C21 112.7(11) n
C17 C21 C25 110.7(10) n
C21 C17 N2 118.5(9) n
N2 C19 C23 116.4(9) n
C27 C23 C19 111.6(10) n
C23 C27 C31 113.2(11) ?
N2 C20 C24 115.9(8) n
C28 C24 C20 107.4(9) n
C24 C28 C32 110.0(10) n
C22 C18 N2 113.7(9) n
C26 C22 C18 111.4(10) n
C30 C26 C22 113.8(10) n
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
Hg1 I6 . 2.6347(11) y
Hg1 I2 . 2.6476(10) y
Hg1 I1 . 3.0800(9) y
Hg1 I8 . 3.2065(10) y
Hg2 I3 . 2.7152(9) y
Hg2 I9 . 2.7489(10) y
Hg2 I10 . 2.8554(9) y
Hg2 I7 . 2.9103(10) y
Hg3 I5 . 2.6167(11) y
Hg3 I4 . 2.6231(11) y
Hg3 I9 . 3.1534(9) y
Hg3 I3 . 3.3150(10) y
Hg4 I8 . 2.7435(10) y
Hg4 I1 . 2.7659(9) y
Hg4 I7 . 2.8346(9) y
Hg4 I10 . 2.8759(11) y
N1 C3 . 1.508(13) y
N1 C2 . 1.514(13) y
N1 C1 . 1.534(12) y
N1 C4 . 1.548(14) y
C1 C5 . 1.515(15) n
C3 C7 . 1.497(15) n
C2 C6 . 1.490(16) n
C6 C10 . 1.507(16) n
C5 C9 . 1.536(14) n
C9 C13 . 1.530(15) n
C4 C8 . 1.516(16) n
C8 C12 . 1.574(16) n
C12 C16 . 1.507(16) n
C7 C11 . 1.58(2) n
C11 C15 . 1.42(3) n
C10 C14 . 1.503(18) n
N2 C19 . 1.497(13) y
N2 C17 . 1.519(12) y
N2 C20 . 1.535(12) y
N2 C18 . 1.541(12) y
C25 C29 . 1.486(17) n
C25 C21 . 1.535(16) n
C21 C17 . 1.510(16) n
C19 C23 . 1.520(14) n
C23 C27 . 1.510(16) n
C27 C31 . 1.509(17) n
C20 C24 . 1.545(14) n
C24 C28 . 1.499(15) n
C28 C32 . 1.556(15) n
C18 C22 . 1.526(14) n
C22 C26 . 1.532(15) n
C26 C30 . 1.492(16) n
