#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:24:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179244 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/64/4316488.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_4316488
loop_
_publ_author_name
'Malte Behrens'
'Marie-Eve Ordolff'
'Christian Näther'
'Wolfgang Bensch'
'Klaus-Dieter Becker'
'Catherine Guillot-Deudon'
'Alain Lafond'
'Jason A. Cody'
_publ_section_title
;
 New Three-Dimensional Thiostannates Composed of Linked Cu8S12 Clusters
 and the First Example of a Mixed-Metal Cu7SnS12 Cluster
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8305
_journal_page_last               8309
_journal_paper_doi               10.1021/ic100688z
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'Cu7 Sn4 S12, 3(C2 H9 N2)'
_chemical_formula_sum            'C6 H27 Cu7 N6 S12 Sn4'
_chemical_formula_weight         1487.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.5317(19)
_cell_length_b                   13.5317(19)
_cell_length_c                   28.933(6)
_cell_measurement_reflns_used    17299
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      6.43
_cell_measurement_theta_min      34.99
_cell_volume                     4588.1(13)
_computing_cell_refinement       'Bruker AXS Collect'
_computing_data_collection       'Bruker AXS Collect'
_computing_data_reduction        'Bruker AXS Collect'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker KappaCCD'
_diffrn_measurement_method       'omega scan'
_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  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            15872
_diffrn_reflns_theta_full        34.99
_diffrn_reflns_theta_max         34.99
_diffrn_reflns_theta_min         6.43
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.800
_exptl_absorpt_correction_T_max  0.6562
_exptl_absorpt_correction_T_min  0.5794
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Sheldrick, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4200
_exptl_crystal_size_max          0.066
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.190
_refine_diff_density_min         -1.360
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         2222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+96.2338P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0780
_reflns_number_gt                1901
_reflns_number_total             2222
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100688z_si_002_2.cif
_cod_data_source_block           r-3c
_cod_original_cell_volume        4588.0(13)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4316488
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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 0.3333 0.17899(3) 0.4167 0.01272(7) Uani 1 2 d S . .
Sn2 Sn 0.60623(14) 0.22685(14) 0.35182(5) 0.0158(3) Uani 0.17 1 d P . 1
Cu1 Cu 0.6667 0.3333 0.43093(4) 0.0306(2) Uani 1 3 d S . .
Cu2 Cu 0.54686(7) 0.12397(7) 0.36887(3) 0.02893(16) Uani 0.83 1 d P . 2
S1 S 0.49900(8) 0.16433(8) 0.43778(3) 0.01646(16) Uani 1 1 d . . .
S2 S 0.27064(8) 0.25387(8) 0.47833(3) 0.01652(16) Uani 1 1 d . . .
N1 N 0.4240(4) 0.5248(4) 0.44650(17) 0.0327(9) Uani 1 1 d . . .
H1N1 H 0.4149 0.5065 0.4771 0.049 Uiso 1 1 calc R . .
H2N1 H 0.4640 0.4951 0.4328 0.049 Uiso 1 1 calc R . .
H3N1 H 0.3543 0.4955 0.4328 0.049 Uiso 0.50 1 calc PR . .
C1A C 0.4870(5) 0.6502(4) 0.44128(16) 0.0297(10) Uani 1 1 d . . .
H1A H 0.4440 0.6825 0.4566 0.036 Uiso 1 1 calc R . .
H1B H 0.5622 0.6821 0.4566 0.036 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
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
S2 Sn1 S2 106.63(5) 12 . ?
S2 Sn1 S1 112.50(3) 12 12 ?
S2 Sn1 S1 105.50(3) . 12 ?
S2 Sn1 S1 105.50(3) 12 . ?
S2 Sn1 S1 112.49(3) . . ?
S1 Sn1 S1 114.10(5) 12 . ?
Sn2 Sn2 Sn2 82.35(13) 32 33_545 ?
Sn2 Sn2 Sn2 90.000(1) 32 2_655 ?
Sn2 Sn2 Sn2 48.83(7) 33_545 2_655 ?
Sn2 Sn2 Sn2 48.83(7) 32 3_665 ?
Sn2 Sn2 Sn2 90.002(1) 33_545 3_665 ?
Sn2 Sn2 Sn2 60.0 2_655 3_665 ?
Sn2 Sn2 Cu1 112.81(8) 32 . ?
Sn2 Sn2 Cu1 112.81(8) 33_545 . ?
Sn2 Sn2 Cu1 65.45(3) 2_655 . ?
Sn2 Sn2 Cu1 65.45(3) 3_665 . ?
Sn2 Sn2 S2 141.10(12) 32 11 ?
Sn2 Sn2 S2 73.17(8) 33_545 11 ?
Sn2 Sn2 S2 95.76(10) 2_655 11 ?
Sn2 Sn2 S2 155.69(10) 3_665 11 ?
Cu1 Sn2 S2 104.48(6) . 11 ?
Sn2 Sn2 S2 71.21(9) 32 28 ?
Sn2 Sn2 S2 109.64(11) 33_545 28 ?
Sn2 Sn2 S2 154.34(4) 2_655 28 ?
Sn2 Sn2 S2 113.67(9) 3_665 28 ?
Cu1 Sn2 S2 137.52(7) . 28 ?
S2 Sn2 S2 88.90(5) 11 28 ?
Sn2 Sn2 Sn2 52.78(4) 32 31_655 ?
Sn2 Sn2 Sn2 52.78(4) 33_545 31_655 ?
Sn2 Sn2 Sn2 37.22(4) 2_655 31_655 ?
Sn2 Sn2 Sn2 37.22(4) 3_665 31_655 ?
Cu1 Sn2 Sn2 84.47(7) . 31_655 ?
S2 Sn2 Sn2 123.41(9) 11 31_655 ?
S2 Sn2 Sn2 121.53(9) 28 31_655 ?
Sn2 Sn2 S1 117.48(9) 32 . ?
Sn2 Sn2 S1 156.67(11) 33_545 . ?
Sn2 Sn2 S1 115.16(4) 2_655 . ?
Sn2 Sn2 S1 94.48(6) 3_665 . ?
Cu1 Sn2 S1 49.99(4) . . ?
S2 Sn2 S1 94.65(6) 11 . ?
S2 Sn2 S1 89.47(6) 28 . ?
Sn2 Sn2 S1 128.14(9) 31_655 . ?
S1 Cu1 S1 119.256(12) 2_655 . ?
S1 Cu1 S1 119.256(12) 2_655 3_665 ?
S1 Cu1 S1 119.256(12) . 3_665 ?
S1 Cu1 Sn2 96.69(5) 2_655 . ?
S1 Cu1 Sn2 69.11(5) . . ?
S1 Cu1 Sn2 117.93(6) 3_665 . ?
S1 Cu1 Sn2 69.11(5) 2_655 2_655 ?
S1 Cu1 Sn2 117.93(6) . 2_655 ?
S1 Cu1 Sn2 96.69(5) 3_665 2_655 ?
Sn2 Cu1 Sn2 49.10(6) . 2_655 ?
S1 Cu1 Sn2 117.93(6) 2_655 3_665 ?
S1 Cu1 Sn2 96.69(5) . 3_665 ?
S1 Cu1 Sn2 69.11(5) 3_665 3_665 ?
Sn2 Cu1 Sn2 49.10(6) . 3_665 ?
Sn2 Cu1 Sn2 49.10(6) 2_655 3_665 ?
S1 Cu1 Cu2 97.10(3) 2_655 . ?
S1 Cu1 Cu2 47.20(3) . . ?
S1 Cu1 Cu2 135.17(4) 3_665 . ?
Sn2 Cu1 Cu2 25.23(4) . . ?
Sn2 Cu1 Cu2 71.26(5) 2_655 . ?
Sn2 Cu1 Cu2 71.04(5) 3_665 . ?
S1 Cu1 Cu2 47.20(3) 2_655 2_655 ?
S1 Cu1 Cu2 135.17(4) . 2_655 ?
S1 Cu1 Cu2 97.10(3) 3_665 2_655 ?
Sn2 Cu1 Cu2 71.04(5) . 2_655 ?
Sn2 Cu1 Cu2 25.23(4) 2_655 2_655 ?
Sn2 Cu1 Cu2 71.26(5) 3_665 2_655 ?
Cu2 Cu1 Cu2 88.81(4) . 2_655 ?
S1 Cu1 Cu2 135.17(4) 2_655 3_665 ?
S1 Cu1 Cu2 97.10(3) . 3_665 ?
S1 Cu1 Cu2 47.20(3) 3_665 3_665 ?
Sn2 Cu1 Cu2 71.26(5) . 3_665 ?
Sn2 Cu1 Cu2 71.04(5) 2_655 3_665 ?
Sn2 Cu1 Cu2 25.23(4) 3_665 3_665 ?
Cu2 Cu1 Cu2 88.81(4) . 3_665 ?
Cu2 Cu1 Cu2 88.81(4) 2_655 3_665 ?
S1 Cu2 S2 126.82(5) . 11 ?
S1 Cu2 S2 117.28(5) . 28 ?
S2 Cu2 S2 112.56(3) 11 28 ?
S1 Cu2 Cu1 48.32(3) . . ?
S2 Cu2 Cu1 103.17(4) 11 . ?
S2 Cu2 Cu1 136.18(4) 28 . ?
Cu2 S1 Cu1 84.47(5) . . ?
Cu2 S1 Sn1 100.78(4) . . ?
Cu1 S1 Sn1 113.07(4) . . ?
Cu2 S1 Sn2 27.48(4) . . ?
Cu1 S1 Sn2 60.90(5) . . ?
Sn1 S1 Sn2 96.46(5) . . ?
Cu2 S2 Cu2 90.14(5) 11_455 34 ?
Cu2 S2 Sn1 108.75(4) 11_455 . ?
Cu2 S2 Sn1 105.51(4) 34 . ?
Cu2 S2 Sn2 29.17(4) 11_455 11_455 ?
Cu2 S2 Sn2 63.71(5) 34 11_455 ?
Sn1 S2 Sn2 102.70(5) . 11_455 ?
Cu2 S2 Sn2 63.88(5) 11_455 34 ?
Cu2 S2 Sn2 28.82(4) 34 34 ?
Sn1 S2 Sn2 101.70(5) . 34 ?
Sn2 S2 Sn2 35.62(6) 11_455 34 ?
C1A N1 H1N1 109.5 . . ?
C1A N1 H2N1 109.5 . . ?
H1N1 N1 H2N1 109.5 . . ?
C1A N1 H3N1 109.5 . . ?
H1N1 N1 H3N1 109.5 . . ?
H2N1 N1 H3N1 109.5 . . ?
C1A C1A N1 111.0(5) 11_565 . ?
C1A C1A H1A 109.4 11_565 . ?
N1 C1A H1A 109.4 . . ?
C1A C1A H1B 109.4 11_565 . ?
N1 C1A H1B 109.4 . . ?
H1A C1A H1B 108.0 . . ?
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 S2 2.4061(10) 12 ?
Sn1 S2 2.4061(10) . ?
Sn1 S1 2.4254(10) 12 ?
Sn1 S1 2.4254(10) . ?
Sn2 Sn2 1.646(2) 32 ?
Sn2 Sn2 1.647(2) 33_545 ?
Sn2 Sn2 2.168(3) 2_655 ?
Sn2 Sn2 2.168(3) 3_665 ?
Sn2 Cu1 2.6086(19) . ?
Sn2 S2 2.6760(19) 11 ?
Sn2 S2 2.7057(19) 28 ?
Sn2 Sn2 2.722(3) 31_655 ?
Sn2 S1 2.7891(19) . ?
Cu1 S1 2.2865(10) 2_655 ?
Cu1 S1 2.2865(10) . ?
Cu1 S1 2.2865(10) 3_665 ?
Cu1 Sn2 2.6086(19) 2_655 ?
Cu1 Sn2 2.6086(19) 3_665 ?
Cu1 Cu2 3.0471(11) . ?
Cu1 Cu2 3.0470(11) 2_655 ?
Cu1 Cu2 3.0470(11) 3_665 ?
Cu2 S1 2.2463(13) . ?
Cu2 S2 2.2477(13) 11 ?
Cu2 S2 2.2833(12) 28 ?
S2 Cu2 2.2478(13) 11_455 ?
S2 Cu2 2.2833(12) 34 ?
S2 Sn2 2.6761(19) 11_455 ?
S2 Sn2 2.7057(19) 34 ?
N1 C1A 1.477(7) . ?
N1 H1N1 0.9100 . ?
N1 H2N1 0.9100 . ?
N1 H3N1 0.9100 . ?
C1A C1A 1.476(10) 11_565 ?
C1A H1A 0.9900 . ?
C1A H1B 0.9900 . ?
