#------------------------------------------------------------------------------
#$Date: 2016-03-26 12:36:50 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180229 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/15/7111573.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_7111573
loop_
_publ_author_name
'Zhang, Ren-Chun'
'Yao, Hua-Gang'
'Ji, Shou-Hua'
'Liu, Mei-Chen'
'Ji, Min'
'An, Yong-Lin'
_publ_section_title
;
 (H2en)2Cu8Sn3S12: a trigonal CuS3-based open-framework sulfide with
 interesting ion-exchange properties
;
_journal_issue                   25
_journal_name_full               'Chemical Communications'
_journal_page_first              4550
_journal_page_last               4552
_journal_paper_doi               10.1039/b924581b
_journal_volume                  46
_journal_year                    2010
_chemical_formula_sum            'C24 Cu80 N24 S120 Sn30'
_chemical_formula_weight         13115.58
_chemical_name_systematic
;
?
;
_space_group_IT_number           222
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 4a 2bc 3'
_symmetry_space_group_name_H-M   'P n -3 n :2'
_atom_sites_solution_hydrogens   none
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   25.4484(4)
_cell_length_b                   25.4484(4)
_cell_length_c                   25.4484(4)
_cell_measurement_reflns_used    6670
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.331
_cell_measurement_theta_min      2.264
_cell_volume                     16480.9(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Smart Apex II CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       2
_diffrn_reflns_number            3172
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    8.037
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             12104
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         1.109
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         3172
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0319
_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)+(0.0438P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0834
_reflns_number_gt                2195
_reflns_number_total             3172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B924581Bsup1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      Pn-3n
_cod_database_code               7111573
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x, y'
'z, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y'
'-z+1/2, x, -y+1/2'
'y, z, x'
'-y+1/2, z, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x'
'y, x, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y, -x+1/2, z'
'-y+1/2, x, z'
'x, z, -y+1/2'
'-x+1/2, z, y'
'-x+1/2, -z+1/2, -y+1/2'
'x, -z+1/2, y'
'z, y, -x+1/2'
'z, -y+1/2, x'
'-z+1/2, y, x'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x-1/2, -y, z-1/2'
'-x, y-1/2, z-1/2'
'-z, -x, -y'
'-z, x-1/2, y-1/2'
'z-1/2, x-1/2, -y'
'z-1/2, -x, y-1/2'
'-y, -z, -x'
'y-1/2, -z, x-1/2'
'-y, z-1/2, x-1/2'
'y-1/2, z-1/2, -x'
'-y, -x, z-1/2'
'y-1/2, x-1/2, z-1/2'
'-y, x-1/2, -z'
'y-1/2, -x, -z'
'-x, -z, y-1/2'
'x-1/2, -z, -y'
'x-1/2, z-1/2, y-1/2'
'-x, z-1/2, -y'
'-z, -y, x-1/2'
'-z, y-1/2, -x'
'z-1/2, -y, -x'
'z-1/2, y-1/2, x-1/2'
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
Sn1 Sn 0.115013(13) 0.566896(13) 0.378707(13) 0.02541(11) Uani 1 1 d .
Sn2 Sn 0.0000 0.7500 0.2500 0.02313(16) Uani 1 4 d S
Cu4 Cu 0.10367(2) 0.51888(3) 0.50700(3) 0.03676(18) Uani 1 1 d .
Cu1 Cu 0.08943(3) 0.62480(3) 0.25286(2) 0.03719(18) Uani 1 1 d .
Cu3 Cu 0.06638(3) 0.43362(3) 0.43362(3) 0.0360(3) Uani 1 3 d S
S5 S 0.05344(5) 0.69107(5) 0.30059(5) 0.0305(3) Uani 1 1 d .
S1 S 0.13569(5) 0.49037(5) 0.43044(5) 0.0292(3) Uani 1 1 d .
S3 S 0.02348(5) 0.58394(5) 0.39590(5) 0.0275(3) Uani 1 1 d .
Cu2 Cu -0.00899(2) 0.65211(2) 0.34873(2) 0.034 Uani 1 1 d .
S2 S 0.16596(5) 0.64244(5) 0.40467(5) 0.0295(3) Uani 1 1 d .
S4 S 0.12310(6) 0.55074(6) 0.28688(5) 0.0474(4) Uani 1 1 d .
N1 N 0.09465(19) 0.7500 0.40535(19) 0.0472(18) Uiso 1 2 d SD
N2 N -0.0094(2) 0.7500 0.5094(2) 0.068(2) Uiso 1 2 d SD
C1 C 0.0437(4) 0.7393(6) 0.4306(5) 0.081(5) Uiso 0.50 1 d PD
C2 C 0.0435(4) 0.7558(5) 0.4878(5) 0.072(4) Uiso 0.50 1 d PD
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
S4 Sn1 S1 112.19(5) . .
S4 Sn1 S3 107.03(5) . .
S1 Sn1 S3 104.92(4) . .
S4 Sn1 S2 111.10(5) . .
S1 Sn1 S2 112.17(4) . .
S3 Sn1 S2 109.06(4) . .
S5 Sn2 S5 108.74(3) 4_565 41_565
S5 Sn2 S5 110.94(6) 4_565 .
S5 Sn2 S5 108.74(3) 41_565 .
S5 Sn2 S5 108.74(3) 4_565 44_566
S5 Sn2 S5 110.94(6) 41_565 44_566
S5 Sn2 S5 108.74(3) . 44_566
S1 Cu4 S3 127.29(5) . 7
S1 Cu4 S3 123.61(5) . 34_566
S3 Cu4 S3 107.49(3) 7 34_566
S1 Cu4 Cu3 48.76(4) . .
S3 Cu4 Cu3 101.36(4) 7 .
S3 Cu4 Cu3 137.20(4) 34_566 .
S4 Cu1 S2 121.23(5) . 23
S4 Cu1 S5 124.85(5) . .
S2 Cu1 S5 113.73(5) 23 .
S1 Cu3 S1 118.985(15) . 7
S1 Cu3 S1 118.985(15) . 10
S1 Cu3 S1 118.984(15) 7 10
S1 Cu3 Cu4 47.40(4) . .
S1 Cu3 Cu4 98.81(4) 7 .
S1 Cu3 Cu4 134.71(5) 10 .
S1 Cu3 Cu4 98.81(4) . 10
S1 Cu3 Cu4 134.71(5) 7 10
S1 Cu3 Cu4 47.40(4) 10 10
Cu4 Cu3 Cu4 88.61(3) . 10
S1 Cu3 Cu4 134.71(5) . 7
S1 Cu3 Cu4 47.40(4) 7 7
S1 Cu3 Cu4 98.81(4) 10 7
Cu4 Cu3 Cu4 88.61(3) . 7
Cu4 Cu3 Cu4 88.61(3) 10 7
Cu2 S5 Cu1 104.48(5) . .
Cu2 S5 Sn2 99.69(5) . .
Cu1 S5 Sn2 113.94(5) . .
Cu4 S1 Cu3 83.83(5) . .
Cu4 S1 Sn1 97.73(5) . .
Cu3 S1 Sn1 111.24(5) . .
Cu4 S3 Cu4 95.75(5) 10 31_566
Cu4 S3 Cu2 119.83(6) 10 .
Cu4 S3 Cu2 105.67(5) 31_566 .
Cu4 S3 Sn1 108.02(5) 10 .
Cu4 S3 Sn1 113.13(5) 31_566 .
Cu2 S3 Sn1 113.22(5) . .
S2 Cu2 S5 133.04(5) 31_566 .
S2 Cu2 S3 115.20(5) 31_566 .
S5 Cu2 S3 111.74(5) . .
Cu2 S2 Cu1 96.25(5) 34_566 21
Cu2 S2 Sn1 105.34(5) 34_566 .
Cu1 S2 Sn1 112.69(5) 21 .
Cu1 S4 Sn1 101.56(6) . .
C2 C1 N1 158.3(16) 24_565 .
N1 C1 C2 111.7(8) . .
C1 C2 N2 151.8(17) 24_565 .
N2 C2 C1 109.6(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 S4 2.3818(14) .
Sn1 S1 2.4090(12) .
Sn1 S3 2.4095(13) .
Sn1 S2 2.4110(12) .
Sn2 S5 2.3991(12) 4_565
Sn2 S5 2.3992(12) 41_565
Sn2 S5 2.3992(12) .
Sn2 S5 2.3992(12) 44_566
Cu4 S1 2.2330(14) .
Cu4 S3 2.2353(13) 7
Cu4 S3 2.2653(14) 34_566
Cu4 Cu3 3.0157(10) .
Cu1 S4 2.2441(15) .
Cu1 S2 2.2616(13) 23
Cu1 S5 2.2712(14) .
Cu3 S1 2.2811(12) .
Cu3 S1 2.2811(12) 7
Cu3 S1 2.2811(12) 10
Cu3 Cu4 3.0157(10) 10
Cu3 Cu4 3.0157(10) 7
S5 Cu2 2.2379(14) .
S3 Cu4 2.2353(13) 10
S3 Cu4 2.2653(14) 31_566
S3 Cu2 2.2655(13) .
Cu2 S2 2.2368(14) 31_566
S2 Cu2 2.2368(14) 34_566
S2 Cu1 2.2616(13) 21
N1 C1 1.473(8) .
N1 C1 1.473(8) 24_565
N2 C2 1.462(8) 24_565
N2 C2 1.462(8) .
C1 C2 1.514(9) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 8 1 ' '
2 0.000 0.000 0.500 8 1 ' '
3 0.183 0.237 0.244 2282 696 ' '
4 0.000 0.500 0.000 8 1 ' '
5 0.000 0.500 0.500 8 1 ' '
6 -0.185 0.731 0.737 2282 696 ' '
7 0.500 0.000 0.000 8 1 ' '
8 0.500 0.000 0.500 8 1 ' '
9 0.500 0.500 0.000 8 1 ' '
10 0.500 0.500 0.500 8 1 ' '
