#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/18/2011841.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_2011841
loop_
_publ_author_name
'Bujak, Maciej'
'Osadczuk, Przemysław'
'Zaleski, Jacek'
_publ_section_title
;
 Aminoguanidinium(2+) aminoguanidinium(1+) hexachloroantimonate(III) at
 295 and 92K
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              388
_journal_page_last               391
_journal_paper_doi               10.1107/S0108270101000774
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          '(CH7 N4 )(CH8 N4 )[SbCl6 ]'
_chemical_formula_moiety         'CH7 N4 + , CH8 N4 2+ ,  SbCl6 3- '
_chemical_formula_sum            'C2 H15 Cl6 N8 Sb'
_chemical_formula_weight         485.67
_chemical_name_systematic
;
Aminoguanidinium(1+)(2+) heksachloroantimonate(III)
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.75(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.522(2)
_cell_length_b                   13.856(3)
_cell_length_c                   15.544(3)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     1614.5(6)
_computing_cell_refinement       'Kuma Diffraction Software'
_computing_data_collection       'Kuma Diffraction Software (KUMA, 1996)'
_computing_data_reduction        'Kuma Diffraction Software'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'KM--4 Diffractometer'
_diffrn_measurement_method       'ω--θ scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0000
_diffrn_reflns_av_sigmaI/netI    .0209
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5690
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        1.0
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.695
_exptl_absorpt_correction_T_max  .368
_exptl_absorpt_correction_T_min  .446
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(Sheldrick, 1990)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.998
_exptl_crystal_density_meas      1.990(10)
_exptl_crystal_density_method    'flotation method'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             944
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .30
_refine_diff_density_max         .589
_refine_diff_density_min         -.360
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   -.04(2)
_refine_ls_extinction_coef       .0045(2)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5690
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          .0327
_refine_ls_R_factor_gt           .0244
_refine_ls_shift/su_max          .002
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w = 1/[σ²(Fo²)+(0.0300P)²+1.1741P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_ref         .0645
_reflns_number_gt                5052
_reflns_number_total             5690
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bj1014.cif
_cod_data_source_block           Iat295K
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               2011841
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
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
Sb1 .22309(4) .24869(2) .49848(2) .03317(13) Uani d . 1 . . Sb
Cl1 .1821(3) .08653(10) .43411(11) .0543(4) Uani d . 1 . . Cl
Cl2 .3160(2) .43664(9) .57138(9) .0443(3) Uani d . 1 . . Cl
Cl3 -.0196(2) .32372(12) .39736(10) .0528(4) Uani d . 1 . . Cl
Cl4 .5004(2) .18271(11) .61516(11) .0561(4) Uani d . 1 . . Cl
Cl5 -.0012(2) .21192(12) .61079(11) .0572(4) Uani d . 1 . . Cl
Cl6 .4618(2) .29880(10) .38538(10) .0488(3) Uani d . 1 . . Cl
Sb2 -.22441(3) .73957(2) .50076(2) .03493(12) Uani d . 1 . . Sb
Cl7 -.4371(2) .69473(12) .60557(10) .0516(4) Uani d . 1 . . Cl
Cl8 .0259(2) .79332(12) .37415(11) .0563(4) Uani d . 1 . . Cl
Cl9 -.1997(3) .90379(11) .56122(11) .0600(4) Uani d . 1 . . Cl
Cl10 -.3125(3) .55414(10) .42616(11) .0577(4) Uani d . 1 . . Cl
Cl11 -.4689(2) .79739(11) .39258(10) .0513(4) Uani d . 1 . . Cl
Cl12 .0389(2) .65268(10) .61370(9) .0463(3) Uani d . 1 . . Cl
C1 -.2310(8) .4387(4) .6934(4) .0360(12) Uani d . 1 . . C
N1 -.3051(7) .3636(3) .7257(3) .0458(11) Uani d . 1 . . N
H11 -.3136 .3615 .7830 .130(8) Uiso d R 1 . . H
H12 -.3489 .3139 .6931 .130(8) Uiso d R 1 . . H
N2 -.1768(7) .5132(4) .7412(3) .0581(13) Uani d . 1 . . N
H21 -.1930 .5140 .7979 .130(8) Uiso d R 1 . . H
H22 -.1225 .5631 .7171 .130(8) Uiso d R 1 . . H
N3 -.2013(8) .4434(3) .6089(3) .0460(12) Uani d . 1 . . N
H3 -.1394 .4927 .5883 .086(13) Uiso d R 1 . . H
N4 -.2817(7) .3757(3) .5513(3) .0438(11) Uani d . 1 . . N
H41 -.4016 .3780 .5480 .092(9) Uiso d R 1 . . H
H42 -.2493 .3140 .5618 .092(9) Uiso d R 1 . . H
H43 -.2481 .3910 .4988 .092(9) Uiso d R 1 . . H
C2 .2508(8) .5506(4) .3070(4) .0393(13) Uani d . 1 . . C
N5 .2289(7) .6344(3) .2663(3) .0496(13) Uani d . 1 . . N
H51 .2909 .6433 .2198 .130(8) Uiso d R 1 . . H
H52 .1915 .6861 .2949 .130(8) Uiso d R 1 . . H
N6 .2923(7) .4736(3) .2672(3) .0583(14) Uani d . 1 . . N
H61 .2544 .4767 .2108 .130(8) Uiso d R 1 . . H
H62 .3089 .4144 .2903 .130(8) Uiso d R 1 . . H
N7 .2234(8) .5448(3) .3917(3) .0508(14) Uani d . 1 . . N
H7 .2379 .4882 .4198 .086(13) Uiso d R 1 . . H
N8 .2633(7) .6232(4) .4478(3) .0461(12) Uani d . 1 . . N
H81 .3802 .6373 .4483 .092(9) Uiso d R 1 . . H
H82 .2371 .6072 .5014 .092(9) Uiso d R 1 . . H
H83 .1984 .6749 .4295 .092(9) Uiso d R 1 . . H
C3 .2761(10) .0548(5) .1938(5) .0557(17) Uani d . 1 . . C
N9 .2177(9) .1381(4) .2192(4) .0682(17) Uani d . 1 . . N
H91 .2337 .1414 .2771 .130(8) Uiso d R 1 . . H
H92 .2033 .1968 .1947 .130(8) Uiso d R 1 . . H
N10 .3041(9) -.0206(4) .2491(4) .0809(19) Uani d . 1 . . N
H101 .2849 -.0134 .3051 .130(8) Uiso d R 1 . . H
H102 .3435 -.0774 .2300 .130(8) Uiso d R 1 . . H
N11 .3025(9) .0415(4) .1129(4) .0647(16) Uani d . 1 . . N
H111 .3232 -.0214 .1037 .086(13) Uiso d R 1 . . H
N12 .2686(9) .1151(4) .0566(4) .0657(16) Uani d . 1 . . N
H121 .1794 .1016 .0161 .130(8) Uiso d R 1 . . H
H122 .3592 .1339 .0261 .130(8) Uiso d R 1 . . H
C41 -.2711(18) 1.0688(10) .3362(9) .042(3) Uani d PU .60 . . C
C42 -.241(3) 1.0438(16) .3047(16) .046(5) Uani d PU .40 . . C
N13 -.2870(10) 1.1308(4) .2751(4) .079(2) Uani d . 1 . . N
H131 -.3188 1.1922 .2849 .130(8) Uiso d R 1 . . H
H132 -.2653 1.1121 .2215 .130(8) Uiso d R 1 . . H
N14 -.3009(10) 1.0930(5) .4250(5) .092(2) Uani d . 1 . . N
H141 -.3381 1.1524 .4384 .130(8) Uiso d R 1 . . H
H142 -.2836 1.0478 .4664 .130(8) Uiso d R 1 . . H
N151 -.2162(12) .9813(7) .3195(6) .054(2) Uani d PU .60 . . N
H151 -.2031 .9356 .3607 .086(13) Uiso d PR .60 . . H
N152 -.249(2) 1.0244(10) .3831(9) .055(3) Uani d PU .40 . . N
H152 -.2185 .9664 .4057 .086(13) Uiso d PR .40 . . H
N16 -.1830(9) .9632(4) .2420(4) .0782(18) Uani d . 1 . . N
H161 -.1455 .9042 .2272 .130(8) Uiso d R 1 . . H
H162 -.1971 1.0100 .2019 .130(8) Uiso d R 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -.5866 1.5461 '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
Cl1 Sb1 Cl2 173.19(6) y
Cl1 Sb1 Cl3 93.59(6) y
Cl1 Sb1 Cl4 91.53(5) y
Cl1 Sb1 Cl5 91.59(6) y
Cl1 Sb1 Cl6 92.15(6) y
Cl2 Sb1 Cl3 90.68(5) y
Cl2 Sb1 Cl4 84.13(5) y
Cl2 Sb1 Cl5 93.61(5) y
Cl2 Sb1 Cl6 82.65(5) y
Cl3 Sb1 Cl4 174.79(5) y
Cl3 Sb1 Cl5 91.31(6) y
Cl3 Sb1 Cl6 88.54(5) y
Cl4 Sb1 Cl5 89.49(6) y
Cl4 Sb1 Cl6 90.33(5) y
Cl5 Sb1 Cl6 176.25(5) y
Cl7 Sb2 Cl8 179.34(5) y
Cl7 Sb2 Cl9 90.77(6) y
Cl7 Sb2 Cl10 84.28(5) y
Cl7 Sb2 Cl11 92.51(6) y
Cl7 Sb2 Cl12 86.63(5) y
Cl8 Sb2 Cl9 89.37(6) y
Cl8 Sb2 Cl10 95.50(5) y
Cl8 Sb2 Cl11 86.85(5) y
Cl8 Sb2 Cl12 93.99(5) y
Cl9 Sb2 Cl10 170.96(7) y
Cl9 Sb2 Cl11 89.36(6) y
Cl9 Sb2 Cl12 97.50(6) y
Cl10 Sb2 Cl11 83.32(5) y
Cl10 Sb2 Cl12 89.77(5) y
Cl11 Sb2 Cl12 173.10(5) y
C1 N1 H11 118.4 ?
C1 N1 H12 122.9 ?
C1 N2 H21 120.1 ?
C1 N2 H22 119.9 ?
C1 N3 N4 119.5(5) ?
C1 N3 H3 120.9 ?
N1 C1 N2 122.2(5) ?
N1 C1 N3 121.5(5) ?
N2 C1 N3 116.3(5) ?
N3 N4 H41 113.1 ?
N3 N4 H42 115.2 ?
N3 N4 H43 106.5 ?
N4 N3 H3 119.3 ?
H11 N1 H12 118.7 ?
H21 N2 H22 120.0 ?
H41 N4 H42 107.4 ?
H41 N4 H43 107.1 ?
H42 N4 H43 107.2 ?
C2 N5 H51 116.7 ?
C2 N5 H52 119.5 ?
C2 N6 H61 111.1 ?
C2 N6 H62 126.5 ?
C2 N7 N8 121.0(5) ?
C2 N7 H7 120.1 ?
N5 C2 N7 119.5(5) ?
N6 C2 N5 121.5(5) ?
N6 C2 N7 118.9(5) ?
N7 N8 H81 109.4 ?
N7 N8 H82 109.4 ?
N7 N8 H83 109.7 ?
N8 N7 H7 111.1 ?
H51 N5 H52 119.5 ?
H61 N6 H62 117.0 ?
H81 N8 H82 109.5 ?
H81 N8 H83 109.5 ?
H82 N8 H83 109.5 ?
C3 N9 H91 109.0 ?
C3 N9 H92 134.5 ?
C3 N10 H101 119.9 ?
C3 N10 H102 120.1 ?
C3 N11 N12 118.9(6) ?
C3 N11 H111 109.4 ?
N9 C3 N10 121.7(6) ?
N11 C3 N9 119.9(7) ?
N11 C3 N10 118.3(6) ?
N11 N12 H121 112.7 ?
N11 N12 H122 116.6 ?
N12 N11 H111 130.8 ?
H91 N9 H92 112.2 ?
H101 N10 H102 120.0 ?
H121 N12 H122 104.2 ?
C41 N13 H131 121.2 ?
C41 N13 H132 118.8 ?
C41 N14 H141 120.4 ?
C41 N14 H142 119.6 ?
C41 N151 H151 121.8 ?
C42 N13 H131 149.9 ?
C42 N13 H132 89.9 ?
C42 N152 H152 122.6 ?
C42 N16 H161 156.1 ?
C42 N16 H162 83.9 ?
N13 C41 N151 119.0(12) ?
N13 C41 N14 122.5(10) ?
N13 C42 N16 120.6(18) ?
N14 N152 C42 113.1(16) ?
N14 N152 H142 39.8 ?
N14 N152 H152 124.3 ?
N151 C41 N14 118.4(11) ?
N151 N16 H161 120.6 ?
N151 N16 H162 119.4 ?
N152 C42 N13 120.0(18) ?
N152 C42 N16 119.4(19) ?
N152 N14 H141 161.0 ?
N152 N14 H142 79.0 ?
N16 N151 C41 117.2(10) ?
N16 N151 H151 121.0 ?
H131 N13 H132 120.0 ?
H141 N14 H142 120.0 ?
H142 N152 H152 84.5 ?
H161 N16 H162 120.0 ?
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
Sb1 Cl1 . 2.469(2) y
Sb1 Cl2 . 2.902(2) y
Sb1 Cl3 . 2.532(2) y
Sb1 Cl4 . 2.802(2) y
Sb1 Cl5 . 2.577(2) y
Sb1 Cl6 . 2.705(2) y
Sb2 Cl7 . 2.456(2) y
Sb2 Cl8 . 2.931(2) y
Sb2 Cl9 . 2.463(2) y
Sb2 Cl10 . 2.874(2) y
Sb2 Cl11 . 2.518(2) y
Sb2 Cl12 . 2.807(2) y
C1 N1 . 1.301(7) ?
C1 N2 . 1.316(7) ?
C1 N3 . 1.352(7) ?
N3 N4 . 1.399(7) ?
N1 H11 . .9000 ?
N1 H12 . .9000 ?
N2 H21 . .9000 ?
N2 H22 . .9000 ?
N3 H3 . .9000 ?
N4 H41 . .9000 ?
N4 H42 . .9000 ?
N4 H43 . .9000 ?
C2 N5 . 1.327(7) ?
C2 N6 . 1.284(7) ?
C2 N7 . 1.352(7) ?
N7 N8 . 1.409(7) ?
N5 H51 . .9000 ?
N5 H52 . .8999 ?
N6 H61 . .9000 ?
N6 H62 . .9001 ?
N7 H7 . .9000 ?
N8 H81 . .9000 ?
N8 H82 . .9000 ?
N8 H83 . .9000 ?
C3 N9 . 1.308(8) ?
C3 N10 . 1.359(9) ?
C3 N11 . 1.302(9) ?
N11 N12 . 1.354(8) ?
N9 H91 . .9000 ?
N9 H92 . .9001 ?
N10 H101 . .9000 ?
N10 H102 . .9000 ?
N11 H111 . .9000 ?
N12 H121 . .9000 ?
N12 H122 . .9001 ?
C41 N13 . 1.279(15) ?
C41 N14 . 1.455(15) ?
C41 N151 . 1.314(15) ?
C42 N152 . 1.25(3) ?
C42 N13 . 1.33(2) ?
C42 N16 . 1.57(2) ?
N13 H131 . .9000 ?
N13 H132 . .9000 ?
N14 N152 . 1.232(15) ?
N14 H141 . .9000 ?
N14 H142 . .8999 ?
N151 N16 . 1.275(10) ?
N151 H151 . .9000 ?
N152 H152 . .9001 ?
N16 H161 . .9000 ?
N16 H162 . .9000 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H12 Cl4 1_455 .90 2.41 3.310(5) 172.8
N1 H11 Cl10 2_565 .90 2.51 3.323(5) 150.1
N2 H22 Cl12 . .90 2.43 3.291(5) 159.2
N2 H21 Cl10 2_565 .90 2.44 3.266(5) 152.0
N4 H41 Cl2 1_455 .90 2.33 3.182(5) 157.7
N4 H42 Cl5 . .90 2.41 3.183(5) 143.5
N5 H52 Cl8 . .90 2.35 3.227(5) 164.2
N5 H51 Cl2 2_564 .90 2.58 3.303(5) 137.8
N6 H62 Cl6 . .90 2.41 3.238(5) 153.5
N7 H7 Cl2 . .90 2.49 3.195(5) 136.0
N8 H83 Cl8 . .90 2.22 3.118(6) 174.3
N8 H82 Cl12 . .90 2.47 3.223(5) 141.6
N8 H81 Cl10 1_655 .90 2.63 3.374(6) 140.5
N11 H111 Cl4 2_554 .90 2.60 3.444(6) 156.5
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 C1 N3 N4 12.7(9)
N2 C1 N3 N4 -169.0(5)
N6 C2 N7 N8 148.7(6)
N5 C2 N7 N8 -33.4(9)
N9 C3 N11 N12 .0(11)
N10 C3 N11 N12 177.5(7)
N13 C41 N151 N16 -.5(18)
N14 C41 N151 N16 -176.8(9)
N13 C42 N152 N14 0(3)
N16 C42 N152 N14 -178.3(14)
