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#$Date: 2016-03-26 02:34:10 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180145 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/42/7104268.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_7104268
loop_
_publ_author_name
'Philippidis, Aggelos'
'Bakas, Thomas'
'Trikalitis, Pantelis N'
_publ_section_title
;
 (H2NC4H8NCH2CH2NH2)2Zn2Sn2Se7: a hybrid ternary semiconductor
 stabilized by amine molecules acting simultaneously as ligands and
 counterions.
;
_journal_issue                   12
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1556
_journal_page_last               1558
_journal_paper_doi               10.1039/b821859e
_journal_volume                  34
_journal_year                    2009
_chemical_formula_sum            'C12 H32 N6 Se7 Sn2 Zn2'
_chemical_formula_weight         1181.28
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.12(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.847(3)
_cell_length_b                   11.216(2)
_cell_length_c                   10.447(2)
_cell_measurement_reflns_used    5084
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      32.4
_cell_measurement_theta_min      3.55
_cell_volume                     1523.5(5)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_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  0.1537
_diffrn_reflns_av_sigmaI/netI    0.2356
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23628
_diffrn_reflns_theta_full        32.40
_diffrn_reflns_theta_max         32.40
_diffrn_reflns_theta_min         3.51
_exptl_absorpt_coefficient_mu    11.551
_exptl_absorpt_correction_T_max  0.3322
_exptl_absorpt_correction_T_min  0.0648
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.040
_refine_diff_density_min         -2.680
_refine_diff_density_rms         0.318
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         10094
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.1701
_refine_ls_R_factor_gt           0.0832
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0447P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1579
_reflns_number_gt                5168
_reflns_number_total             10094
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7104250
_cod_data_source_file            b821859e.txt
_cod_data_source_block           (AEP)2Zn2Sn2Se7
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7104268
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.30574(5) 0.26123(6) 0.94674(8) 0.01839(17) Uani 1 1 d . . .
Sn2 Sn 0.83375(5) 0.45235(6) 1.04671(8) 0.01900(17) Uani 1 1 d . . .
Zn1 Zn 1.05510(9) 0.25821(13) 1.03025(15) 0.0255(3) Uani 1 1 d . . .
Zn2 Zn 0.53988(9) 0.46258(12) 0.93237(14) 0.0238(3) Uani 1 1 d . . .
Se1 Se 0.67785(9) 0.32874(10) 0.93058(14) 0.0290(3) Uani 1 1 d . . .
Se2 Se 0.97204(8) 0.31819(11) 1.19398(13) 0.0264(3) Uani 1 1 d . . .
Se3 Se 0.36883(8) 0.38676(10) 0.79057(12) 0.0238(3) Uani 1 1 d . . .
Se4 Se 0.90606(9) 0.55256(10) 0.88410(14) 0.0285(3) Uani 1 1 d . . .
Se5 Se 0.19915(9) 0.09984(10) 0.78299(14) 0.0257(3) Uani 1 1 d . . .
Se6 Se 0.45255(9) 0.17183(10) 1.14077(13) 0.0247(3) Uani 1 1 d . . .
Se7 Se 0.19612(9) 0.39006(11) 1.03486(17) 0.0425(4) Uani 1 1 d . . .
N1 N 0.5394(6) 0.4716(8) 1.1322(10) 0.021(2) Uani 1 1 d . . .
H1NA H 0.5256 0.3986 1.1574 0.025 Uiso 1 1 calc R . .
H1NB H 0.6026 0.4924 1.1880 0.025 Uiso 1 1 calc R . .
C2 C 0.4485(10) 0.5378(16) 1.2882(15) 0.046(4) Uani 1 1 d . . .
H2A H 0.3979 0.5936 1.2977 0.056 Uiso 1 1 calc R . .
H2B H 0.4240 0.4575 1.2931 0.056 Uiso 1 1 calc R . .
N2 N 0.4527(7) 0.0566(9) 0.6026(11) 0.028(2) Uani 1 1 d . . .
C3 C 0.4378(13) -0.0215(13) 1.4881(18) 0.064(6) Uani 1 1 d . . .
H3A H 0.4489 -0.1036 1.5190 0.077 Uiso 1 1 calc R . .
H3B H 0.4867 -0.0022 1.4435 0.077 Uiso 1 1 calc R . .
C4 C 0.6715(11) 0.4939(13) 0.6115(18) 0.048(3) Uani 1 1 d U . .
H4A H 0.6822 0.4434 0.6905 0.058 Uiso 1 1 calc R . .
H4B H 0.7204 0.4706 0.5682 0.058 Uiso 1 1 calc R . .
N3 N 0.6882(10) 0.6201(12) 0.6544(13) 0.053(4) Uani 1 1 d . . .
H3C H 0.7547 0.6300 0.7062 0.063 Uiso 1 1 calc R . .
H3D H 0.6500 0.6368 0.7066 0.063 Uiso 1 1 calc R . .
C5 C 0.3386(14) 0.2075(14) 0.4621(19) 0.063(6) Uani 1 1 d . . .
H5A H 0.3338 0.2884 0.4274 0.076 Uiso 1 1 calc R . .
H5B H 0.2907 0.1993 0.5110 0.076 Uiso 1 1 calc R . .
C6 C 0.4455(10) 0.1833(12) 0.5559(15) 0.039(3) Uani 1 1 d U . .
H6A H 0.4627 0.2364 0.6338 0.047 Uiso 1 1 calc R . .
H6B H 0.4939 0.1972 0.5088 0.047 Uiso 1 1 calc R . .
N4 N 0.9551(8) 0.2462(10) 0.8283(10) 0.035(3) Uani 1 1 d . . .
H4C H 0.9173 0.3134 0.8081 0.043 Uiso 1 1 calc R . .
H4D H 0.9931 0.2436 0.7737 0.043 Uiso 1 1 calc R . .
C7 C 0.1133(9) 0.6467(17) 0.2035(11) 0.074(6) Uani 1 1 d D . .
H7A H 0.1405 0.6387 0.1298 0.089 Uiso 1 1 calc R . .
H7B H 0.0722 0.5762 0.2012 0.089 Uiso 1 1 calc R . .
C8 C 0.2055(9) 0.643(2) 0.3380(12) 0.073(6) Uani 1 1 d D . .
H8A H 0.2400 0.5666 0.3462 0.087 Uiso 1 1 calc R . .
H8B H 0.2542 0.7049 0.3372 0.087 Uiso 1 1 calc R . .
N5 N 0.1719(8) 0.6604(11) 0.4544(12) 0.044(3) Uani 1 1 d . . .
C9 C 0.7334(12) 0.1926(19) 1.4286(18) 0.064(6) Uani 1 1 d . . .
H9A H 0.7040 0.2652 1.4498 0.077 Uiso 1 1 calc R . .
H9B H 0.6828 0.1295 1.4141 0.077 Uiso 1 1 calc R . .
C10 C 0.7587(11) 0.2104(16) 1.3011(15) 0.051(5) Uani 1 1 d . . .
H10A H 0.6954 0.2237 1.2252 0.061 Uiso 1 1 calc R . .
H10B H 0.8009 0.2812 1.3115 0.061 Uiso 1 1 calc R . .
N6 N 0.1876(9) 0.6102(12) 0.7301(13) 0.049(4) Uani 1 1 d . . .
H6C H 0.1666 0.6316 0.7993 0.059 Uiso 1 1 calc R . .
H6D H 0.2330 0.5503 0.7603 0.059 Uiso 1 1 calc R . .
C11 C 0.9021(12) 0.0633(18) 1.380(2) 0.073(7) Uani 1 1 d . . .
H11A H 0.9613 0.1141 1.3932 0.088 Uiso 1 1 calc R . .
H11B H 0.9185 -0.0163 1.3578 0.088 Uiso 1 1 calc R . .
C12 C 0.1256(13) 0.5600(18) 0.4853(18) 0.069(6) Uani 1 1 d . . .
H12A H 0.1710 0.4927 0.4915 0.082 Uiso 1 1 calc R . .
H12B H 0.0628 0.5448 0.4093 0.082 Uiso 1 1 calc R . .
C1 C 0.4639(8) 0.5571(10) 1.1499(12) 0.020(2) Uani 1 1 d U . .
H1A H 0.3987 0.5472 1.0764 0.024 Uiso 1 1 calc R . .
H1B H 0.4878 0.6378 1.1456 0.024 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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'
Sn Sn -0.6537 1.4246 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Se7 Sn1 Se3 107.78(5) . . ?
Se7 Sn1 Se6 110.95(6) . . ?
Se3 Sn1 Se6 112.13(5) . . ?
Se7 Sn1 Se5 111.72(5) . . ?
Se3 Sn1 Se5 102.07(5) . . ?
Se6 Sn1 Se5 111.83(5) . . ?
Se1 Sn2 Se2 108.36(5) . . ?
Se1 Sn2 Se4 113.46(6) . . ?
Se2 Sn2 Se4 106.59(5) . . ?
Se1 Sn2 Se5 111.22(5) . 2_657 ?
Se2 Sn2 Se5 103.92(5) . 2_657 ?
Se4 Sn2 Se5 112.63(5) . 2_657 ?
N4 Zn1 Se7 107.9(3) . 1_655 ?
N4 Zn1 Se2 114.4(3) . . ?
Se7 Zn1 Se2 112.54(7) 1_655 . ?
N4 Zn1 Se4 107.0(3) . 2_747 ?
Se7 Zn1 Se4 119.17(7) 1_655 2_747 ?
Se2 Zn1 Se4 95.70(7) . 2_747 ?
N1 Zn2 Se1 108.0(2) . . ?
N1 Zn2 Se3 106.4(2) . . ?
Se1 Zn2 Se3 112.08(7) . . ?
N1 Zn2 Se6 106.1(3) . 2_657 ?
Se1 Zn2 Se6 117.67(7) . 2_657 ?
Se3 Zn2 Se6 105.91(6) . 2_657 ?
Zn2 Se1 Sn2 101.72(6) . . ?
Zn1 Se2 Sn2 100.30(6) . . ?
Zn2 Se3 Sn1 106.11(6) . . ?
Zn1 Se4 Sn2 105.12(7) 2_757 . ?
Sn1 Se5 Sn2 100.90(5) . 2_647 ?
Zn2 Se6 Sn1 103.62(5) 2_647 . ?
Zn1 Se7 Sn1 103.11(6) 1_455 . ?
C1 N1 Zn2 113.7(7) . . ?
N2 C2 C1 108.4(11) 2_657 . ?
C3 N2 C2 112.8(11) 1_554 2_647 ?
C3 N2 C6 109.4(11) 1_554 . ?
C2 N2 C6 109.3(11) 2_647 . ?
N2 C3 C4 108.8(13) 1_556 2_647 ?
N3 C4 C3 109.3(12) . 2_657 ?
C4 N3 C5 114.1(12) . 2_656 ?
C6 C5 N3 108.9(13) . 2_646 ?
C5 C6 N2 109.1(11) . . ?
C7 N4 Zn1 116.2(8) 2_646 . ?
N4 C7 C8 120.6(14) 2_656 . ?
N5 C8 C7 110.8(11) . . ?
C12 N5 C8 113.0(15) . . ?
C12 N5 C9 110.5(13) . 2_657 ?
C8 N5 C9 105.8(12) . 2_657 ?
N5 C9 C10 110.4(13) 2_647 . ?
N6 C10 C9 113.1(14) 2_647 . ?
C10 N6 C11 117.6(13) 2_657 2_657 ?
N6 C11 C12 107.9(14) 2_647 2_647 ?
N5 C12 C11 117.4(15) . 2_657 ?
N1 C1 C2 110.9(10) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 Se7 2.4903(16) . ?
Sn1 Se3 2.5274(15) . ?
Sn1 Se6 2.5321(16) . ?
Sn1 Se5 2.5777(15) . ?
Sn2 Se1 2.5004(14) . ?
Sn2 Se2 2.5043(14) . ?
Sn2 Se4 2.5143(17) . ?
Sn2 Se5 2.5821(16) 2_657 ?
Zn1 N4 2.092(10) . ?
Zn1 Se7 2.4367(19) 1_655 ?
Zn1 Se2 2.461(2) . ?
Zn1 Se4 2.4657(19) 2_747 ?
Zn2 N1 2.092(10) . ?
Zn2 Se1 2.4349(18) . ?
Zn2 Se3 2.4725(18) . ?
Zn2 Se6 2.4816(19) 2_657 ?
Se4 Zn1 2.4657(19) 2_757 ?
Se5 Sn2 2.5821(16) 2_647 ?
Se6 Zn2 2.4816(19) 2_647 ?
Se7 Zn1 2.4367(19) 1_455 ?
N1 C1 1.477(14) . ?
C2 N2 1.464(16) 2_657 ?
C2 C1 1.55(2) . ?
N2 C3 1.439(19) 1_554 ?
N2 C2 1.464(16) 2_647 ?
N2 C6 1.495(17) . ?
C3 N2 1.439(19) 1_556 ?
C3 C4 1.52(2) 2_647 ?
C4 N3 1.48(2) . ?
C4 C3 1.52(2) 2_657 ?
N3 C5 1.51(2) 2_656 ?
C5 C6 1.49(2) . ?
C5 N3 1.51(2) 2_646 ?
N4 C7 1.428(18) 2_646 ?
C7 N4 1.428(18) 2_656 ?
C7 C8 1.540(9) . ?
C8 N5 1.46(2) . ?
N5 C12 1.39(2) . ?
N5 C9 1.498(19) 2_657 ?
C9 N5 1.498(19) 2_647 ?
C9 C10 1.50(2) . ?
C10 N6 1.45(2) 2_647 ?
N6 C10 1.45(2) 2_657 ?
N6 C11 1.47(2) 2_657 ?
C11 N6 1.47(2) 2_647 ?
C11 C12 1.58(3) 2_647 ?
C12 C11 1.58(3) 2_657 ?
