#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2007123.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_2007123
loop_
_publ_author_name
'Wendland, F.'
'N\"ather, C.'
'Schur, M.'
'Bensch, W.'
_publ_section_title
;
 H~2~N(CH~2~)~2~NH~3~^+^.[Mn{H~2~N(CH~2~)~2~NH~2~}~3~]^2+^.[Sb
 Se~4~]^3{-^}
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              317
_journal_page_last               319
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '(C2 H9 N2)[Mn(C2 H8 N2)3][SbSe4]'
_chemical_formula_sum            'C8 H33 Mn N8 Sb Se4'
_chemical_formula_weight         733.95
_chemical_name_common
;
Manganese tris(ethylendiamine) ethylenediammonium tetraselenoantimonat
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                104.83(3)
_cell_angle_beta                 92.42(3)
_cell_angle_gamma                110.62(3)
_cell_formula_units_Z            2
_cell_length_a                   8.981(4)
_cell_length_b                   9.720(3)
_cell_length_c                   14.451(4)
_cell_measurement_reflns_used    78
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      12.5
_cell_volume                     1129.1(8)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe, 19??)'
_computing_data_reduction        'REDU4 (Stoe, 19??)'
_computing_molecular_graphics    'XP in SHELXTL/PC (Siemens, 1990)'
_computing_publication_material  'CIFTAB in SHELXL93'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'STOE AED-2 four-circle diffractometer'
_diffrn_measurement_method       \w-\q
_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  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5478
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_time  120
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    8.210
_exptl_absorpt_correction_T_max  0.085
_exptl_absorpt_correction_T_min  0.063
_exptl_absorpt_correction_type   'psi scan (XEMP; Siemens, 1990)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.159
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             698
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.290
_refine_diff_density_min         -1.388
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.991
_refine_ls_goodness_of_fit_obs   1.057
_refine_ls_hydrogen_treatment    'H atoms: see text below'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         5155
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_restrained_S_obs      1.057
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_obs          0.0428
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0769P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.1194
_refine_ls_wR_factor_obs         0.1073
_reflns_number_observed          3713
_reflns_number_total             5155
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    sk1148.cif
_[local]_cod_data_source_block   frank1
_[local]_cod_cif_authors_sg_H-M  'P -1 '
_cod_original_cell_volume        1129.1(7)
_cod_database_code               2007123
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Sb 0.0308(2) 0.0237(2) 0.0258(2) 0.0085(2) 0.00500(15) 0.00772(14)
Se1 0.0647(5) 0.0503(4) 0.0461(4) 0.0303(4) 0.0277(4) 0.0147(3)
Se2 0.0493(4) 0.0243(3) 0.0440(4) 0.0073(3) -0.0029(3) 0.0082(3)
Se3 0.0458(4) 0.0330(3) 0.0314(3) 0.0098(3) 0.0001(3) 0.0140(3)
Se4 0.0363(4) 0.0366(3) 0.0392(4) 0.0069(3) -0.0044(3) 0.0108(3)
Mn 0.0324(5) 0.0301(5) 0.0291(4) 0.0117(4) 0.0064(4) 0.0084(4)
N1 0.139(9) 0.099(7) 0.064(5) 0.088(7) 0.044(5) 0.044(5)
C1 0.075(13) 0.062(11) 0.055(10) 0.031(10) 0.022(9) 0.030(9)
C1' 0.104(16) 0.083(13) 0.026(7) 0.063(13) 0.010(8) 0.023(8)
C2 0.115(9) 0.071(6) 0.042(5) 0.014(6) 0.032(5) 0.008(4)
N2 0.039(3) 0.044(3) 0.046(3) 0.014(3) 0.008(3) -0.001(3)
N3 0.036(3) 0.041(3) 0.058(4) 0.004(3) 0.013(3) 0.008(3)
C3 0.046(5) 0.063(5) 0.055(5) 0.018(4) 0.002(4) -0.004(4)
C4 0.074(6) 0.060(5) 0.054(5) 0.041(5) -0.008(4) 0.010(4)
N4 0.075(5) 0.036(3) 0.043(3) 0.021(3) 0.015(3) 0.015(3)
N5 0.032(3) 0.034(3) 0.073(4) 0.004(3) 0.004(3) -0.002(3)
C5 0.037(4) 0.049(4) 0.061(5) 0.014(3) 0.020(3) 0.018(4)
C6 0.049(4) 0.045(4) 0.036(3) 0.024(3) 0.014(3) 0.006(3)
N6 0.043(3) 0.032(3) 0.039(3) 0.015(3) 0.007(2) 0.007(2)
N7 0.053(5) 0.064(5) 0.067(5) 0.014(4) 0.002(4) -0.006(4)
C7 0.043(5) 0.054(5) 0.076(6) 0.012(4) 0.006(4) 0.008(4)
C8 0.048(5) 0.047(4) 0.061(5) 0.020(4) 0.007(4) -0.003(4)
N8 0.037(3) 0.046(4) 0.039(3) 0.015(3) -0.002(3) 0.003(3)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Sb 0.38247(5) 0.07626(4) 0.22800(3) 0.02712(12) Uani d . 1 . Sb
Se1 0.21693(11) 0.17617(9) 0.33818(6) 0.0505(2) Uani d . 1 . Se
Se2 0.26665(9) -0.20751(7) 0.16392(5) 0.0417(2) Uani d . 1 . Se
Se3 0.38993(9) 0.18711(7) 0.09155(5) 0.0374(2) Uani d . 1 . Se
Se4 0.66344(9) 0.16686(8) 0.30717(5) 0.0396(2) Uani d . 1 . Se
Mn 0.71177(12) 0.69170(10) 0.31491(7) 0.0305(2) Uani d . 1 . Mn
N1 0.7043(13) 0.7985(11) 0.1957(6) 0.084(3) Uani d . 1 . N
H1N 0.8014(13) 0.8678(11) 0.1942(6) 0.100 Uiso d PR 0.50 . H
H2N 0.6319(13) 0.8438(11) 0.2016(6) 0.100 Uiso d PR 0.50 . H
H3N 0.7460(13) 0.9015(11) 0.2202(6) 0.100 Uiso d PR 0.50 . H
H4N 0.6015(13) 0.7701(11) 0.1693(6) 0.100 Uiso d PR 0.50 . H
C1 0.793(3) 0.753(2) 0.1222(13) 0.060(4) Uani d P 0.50 1 C
H1A 0.908(3) 0.806(2) 0.1439(13) 0.072 Uiso calc PR 0.50 1 H
H1B 0.766(3) 0.776(2) 0.0638(13) 0.072 Uiso calc PR 0.50 1 H
C1' 0.650(3) 0.652(2) 0.1017(10) 0.062(5) Uani d P 0.50 2 C
H1A' 0.538(3) 0.588(2) 0.0999(10) 0.074 Uiso calc PR 0.50 2 H
H1B' 0.658(3) 0.686(2) 0.0439(10) 0.074 Uiso calc PR 0.50 2 H
C2 0.7407(16) 0.5719(12) 0.1031(6) 0.083(4) Uani d . 1 . C
H2A 0.6355(16) 0.5216(12) 0.0640(6) 0.100 Uiso calc R 1 1 H
H2B 0.8155(16) 0.5397(12) 0.0652(6) 0.100 Uiso calc R 1 1 H
N2 0.7337(8) 0.5163(7) 0.1875(4) 0.0462(15) Uani d . 1 . N
H5N 0.6481(8) 0.4276(7) 0.1761(4) 0.055 Uiso d R 1 . H
H6N 0.8230(8) 0.4980(7) 0.1998(4) 0.055 Uiso d R 1 . H
N3 0.9839(7) 0.8100(7) 0.3551(5) 0.049(2) Uani d . 1 . N
H7N 1.0146(7) 0.9113(7) 0.3620(5) 0.059 Uiso d R 1 . H
H8N 1.0328(7) 0.7698(7) 0.3086(5) 0.059 Uiso d R 1 . H
C3 1.0284(10) 0.7850(10) 0.4468(6) 0.060(2) Uani d . 1 . C
H3A 1.0036(10) 0.8537(10) 0.4999(6) 0.072 Uiso calc R 1 . H
H3B 1.1433(10) 0.8089(10) 0.4568(6) 0.072 Uiso calc R 1 . H
C4 0.9403(12) 0.6226(10) 0.4467(6) 0.060(2) Uani d . 1 . C
H4A 0.9744(12) 0.5546(10) 0.3985(6) 0.072 Uiso calc R 1 . H
H4B 0.9664(12) 0.6113(10) 0.5095(6) 0.072 Uiso calc R 1 . H
N4 0.7661(9) 0.5795(7) 0.4253(4) 0.051(2) Uani d . 1 . N
H9N 0.7182(9) 0.4767(7) 0.4017(4) 0.061 Uiso d R 1 . H
H10N 0.7269(9) 0.6097(7) 0.4799(4) 0.061 Uiso d R 1 . H
N5 0.4415(7) 0.5697(7) 0.3041(5) 0.052(2) Uani d . 1 . N
H11N 0.4151(7) 0.4679(7) 0.2931(5) 0.063 Uiso d R 1 . H
H12N 0.3896(7) 0.5855(7) 0.2557(5) 0.063 Uiso d R 1 . H
C5 0.3977(9) 0.6363(9) 0.3967(6) 0.049(2) Uani d . 1 . C
H5A 0.4368(9) 0.6020(9) 0.4467(6) 0.058 Uiso calc R 1 . H
H5B 0.2815(9) 0.6009(9) 0.3920(6) 0.058 Uiso calc R 1 . H
C6 0.4675(9) 0.8080(8) 0.4240(5) 0.043(2) Uani d . 1 . C
H6A 0.4207(9) 0.8428(8) 0.3773(5) 0.051 Uiso calc R 1 . H
H6B 0.4419(9) 0.8497(8) 0.4870(5) 0.051 Uiso calc R 1 . H
N6 0.6430(7) 0.8638(6) 0.4268(4) 0.0386(13) Uani d . 1 . N
H13N 0.6778(7) 0.9552(6) 0.4143(4) 0.046 Uiso d R 1 . H
H14N 0.6904(7) 0.8771(6) 0.4863(4) 0.046 Uiso d R 1 . H
N7 1.0319(10) 0.4187(10) 0.2034(6) 0.068(2) Uani d . 1 . N
H15N 1.031(13) 0.338(13) 0.253(8) 0.09(3) Uiso d . 1 . H
H16N 1.09(2) 0.501(19) 0.265(11) 0.17(6) Uiso d . 1 . H
C7 1.0446(11) 0.3447(10) 0.1080(7) 0.062(2) Uani d . 1 . C
H7A 1.1554(11) 0.3544(10) 0.1045(7) 0.074 Uiso calc R 1 . H
H7B 1.0168(11) 0.3958(10) 0.0644(7) 0.074 Uiso calc R 1 . H
C8 0.9371(10) 0.1764(9) 0.0748(6) 0.055(2) Uani d . 1 . C
H8A 0.9567(10) 0.1302(9) 0.0110(6) 0.066 Uiso calc R 1 . H
H8B 0.9641(10) 0.1252(9) 0.1186(6) 0.066 Uiso calc R 1 . H
N8 0.7669(8) 0.1527(8) 0.0712(5) 0.0431(14) Uani d . 1 . N
H17N 0.732(9) 0.159(8) 0.125(5) 0.03(2) Uiso d . 1 . H
H18N 0.725(10) 0.192(9) 0.036(6) 0.05(2) Uiso d . 1 . H
H19N 0.710(9) 0.044(9) 0.035(5) 0.034(18) Uiso d . 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 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'
Mn Mn 0.3368 0.7283 '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'
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
Se3 Sb Se1 106.44(4) y
Se3 Sb Se4 106.93(4) y
Se1 Sb Se4 111.24(5) y
Se3 Sb Se2 108.84(4) y
Se1 Sb Se2 112.34(4) y
Se4 Sb Se2 110.77(5) y
N2 Mn N1 78.2(3) n
N2 Mn N5 94.0(2) n
N1 Mn N5 96.8(3) n
N2 Mn N4 94.6(2) n
N1 Mn N4 168.3(3) n
N5 Mn N4 92.9(3) n
N2 Mn N3 92.0(2) n
N1 Mn N3 93.4(3) n
N5 Mn N3 169.0(3) n
N4 Mn N3 77.5(3) n
N2 Mn N6 168.5(2) n
N1 Mn N6 95.3(3) n
N5 Mn N6 77.2(2) n
N4 Mn N6 93.2(2) n
N3 Mn N6 97.8(2) n
C1 N1 Mn 111.3(8) n
C1' N1 Mn 101.8(7) n
N1 C1 C2 105.2(12) n
C2 C1' N1 110.5(13) n
C1' C2 N2 112.7(11) n
N2 C2 C1 117.0(9) n
C2 N2 Mn 109.3(5) n
C3 N3 Mn 107.6(5) n
N3 C3 C4 111.3(7) n
N4 C4 C3 110.8(7) n
C4 N4 Mn 109.8(5) n
C5 N5 Mn 106.3(4) n
N5 C5 C6 111.0(6) n
N6 C6 C5 110.4(6) n
C6 N6 Mn 110.2(4) n
N7 C7 C8 112.9(8) n
N8 C8 C7 112.2(7) n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Sb Se3 2.4701(10) y
Sb Se1 2.4726(12) y
Sb Se4 2.4753(15) y
Sb Se2 2.4775(13) y
Mn N2 2.235(6) y
Mn N1 2.237(7) y
Mn N5 2.274(6) y
Mn N4 2.275(6) y
Mn N3 2.278(6) y
Mn N6 2.286(5) y
N1 C1 1.43(2) n
N1 C1' 1.61(2) n
C1 C2 1.60(2) n
C1' C2 1.31(2) n
C2 N2 1.450(11) n
N3 C3 1.471(11) n
C3 C4 1.496(13) n
C4 N4 1.467(11) n
N5 C5 1.464(10) n
C5 C6 1.497(10) n
C6 N6 1.470(9) n
N7 C7 1.412(12) n
C7 C8 1.511(12) n
C8 N8 1.460(10) n
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
_geom_torsion_publ_flag
N2 Mn N1 C1 -29.3(11) n
N5 Mn N1 C1 -122.0(11) n
N4 Mn N1 C1 23.(2) n
N3 Mn N1 C1 62.1(11) n
N6 Mn N1 C1 160.3(11) n
N2 Mn N1 C1' 21.5(9) n
N5 Mn N1 C1' -71.2(9) n
N4 Mn N1 C1' 74.2(19) n
N3 Mn N1 C1' 112.9(9) n
N6 Mn N1 C1' -148.9(9) n
C1' N1 C1 C2 -42.4(11) n
Mn N1 C1 C2 45.1(15) n
C1 N1 C1' C2 57.5(16) n
Mn N1 C1' C2 -50.5(16) n
N1 C1' C2 N2 59.6(18) n
N1 C1' C2 C1 -47.5(13) n
N1 C1 C2 C1' 53.6(13) n
N1 C1 C2 N2 -44.7(18) n
C1' C2 N2 Mn -35.7(15) n
C1 C2 N2 Mn 20.6(14) n
N1 Mn N2 C2 3.4(7) n
N5 Mn N2 C2 99.5(7) n
N4 Mn N2 C2 -167.3(6) n
N3 Mn N2 C2 -89.6(7) n
N6 Mn N2 C2 60.0(14) n
N2 Mn N3 C3 -111.9(5) n
N1 Mn N3 C3 169.8(5) n
N5 Mn N3 C3 11.7(15) n
N4 Mn N3 C3 -17.7(5) n
N6 Mn N3 C3 73.9(5) n
Mn N3 C3 C4 43.6(8) n
N3 C3 C4 N4 -55.3(9) n
C3 C4 N4 Mn 36.4(8) n
N2 Mn N4 C4 81.1(5) n
N1 Mn N4 C4 29.8(17) n
N5 Mn N4 C4 175.4(5) n
N3 Mn N4 C4 -10.0(5) n
N6 Mn N4 C4 -107.3(5) n
N2 Mn N5 C5 164.1(5) n
N1 Mn N5 C5 -117.3(5) n
N4 Mn N5 C5 69.3(5) n
N3 Mn N5 C5 40.6(14) n
N6 Mn N5 C5 -23.4(5) n
Mn N5 C5 C6 49.4(8) n
N5 C5 C6 N6 -56.2(9) n
C5 C6 N6 Mn 31.9(7) n
N2 Mn N6 C6 36.0(13) n
N1 Mn N6 C6 91.2(5) n
N5 Mn N6 C6 -4.6(5) n
N4 Mn N6 C6 -96.8(5) n
N3 Mn N6 C6 -174.6(5) n
N7 C7 C8 N8 62.9(11) n