#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/38/4313875.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_4313875
loop_
_publ_author_name
'Yonglin An'
'Min Ji'
'Menghe Baiyin'
'Xin Liu'
'Cuiying Jia'
'Dehe Wang'
_publ_section_title
;
 A Solvothermal Synthesis and the Structure of K4Ag2Sn3S9.2KOH
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4248
_journal_page_last               4249
_journal_paper_doi               10.1021/ic034186p
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'Ag2 H2 K6 O2 S9 Sn3'
_chemical_formula_weight         1128.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 103.874(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8071(2)
_cell_length_b                   27.3508(11)
_cell_length_c                   10.5008(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2176.82(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Rigaku RAXIS_RAPID'
_diffrn_measurement_method       θ-/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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4895
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    7.167
_exptl_absorpt_correction_T_max  0.3003
_exptl_absorpt_correction_T_min  0.1746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Higashi,1995
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.739
_refine_diff_density_min         -1.559
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         4895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0292P)²+18.3310P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                4517
_reflns_number_total             4895
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034186psi20030502_091735.cif
_cod_data_source_block           anyl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2176.82(11)
_cod_original_formula_sum        'H2 Ag2 K6 O2 S9 Sn3'
_cod_database_code               4313875
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-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 0.32916(5) 0.371099(14) -0.00835(4) 0.01591(10) Uani 1 1 d . . .
Sn2 Sn 0.00048(5) 0.363767(13) -0.36340(4) 0.01444(9) Uani 1 1 d . . .
Sn3 Sn 0.25983(5) 0.486953(14) -0.23696(4) 0.01749(10) Uani 1 1 d . . .
Ag1 Ag -0.35968(8) 0.38280(2) -0.67995(6) 0.03346(13) Uani 1 1 d . . .
Ag2 Ag -0.51484(7) 0.374805(19) -0.33062(6) 0.03018(13) Uani 1 1 d . . .
S9 S 0.0508(2) 0.33555(5) -0.13670(15) 0.0198(3) Uani 1 1 d . . .
S8 S -0.0165(2) 0.45151(5) -0.36630(16) 0.0227(3) Uani 1 1 d . . .
S7 S 0.4954(2) 0.46849(6) -0.32901(16) 0.0232(3) Uani 1 1 d . . .
S6 S 0.3404(2) 0.34817(6) 0.20997(15) 0.0234(3) Uani 1 1 d . . .
S5 S 0.2076(2) 0.33169(6) -0.46889(16) 0.0211(3) Uani 1 1 d . . .
S4 S -0.29088(19) 0.33801(5) -0.46230(14) 0.0187(3) Uani 1 1 d . . .
S3 S 0.5625(2) 0.34281(6) -0.09089(16) 0.0222(3) Uani 1 1 d . . .
S2 S 0.2818(2) 0.45817(5) -0.01365(15) 0.0249(3) Uani 1 1 d . . .
S1 S 0.1642(2) 0.56765(5) -0.22234(16) 0.0240(3) Uani 1 1 d . . .
K6 K -0.6770(3) 0.2500 -1.2267(2) 0.0262(4) Uani 1 2 d S . .
K5 K -0.0972(3) 0.2500 -0.6216(2) 0.0304(4) Uani 1 2 d S . .
K4 K -0.1771(3) 0.2500 -1.0138(2) 0.0325(5) Uani 1 2 d S . .
K3 K -0.5756(3) 0.2500 -1.5863(3) 0.0353(5) Uani 1 2 d S . .
K2 K -0.2420(2) 0.55781(6) -0.38416(16) 0.0326(3) Uani 1 1 d . . .
K1 K 0.1823(2) 0.56480(5) 0.08624(15) 0.0295(3) Uani 1 1 d . . .
OW1 O -0.3524(11) 0.2500 -1.2778(8) 0.0335(16) Uani 1 2 d S . .
OW2 O -0.4090(10) 0.2500 -0.8053(8) 0.0364(17) Uani 1 2 d S . .
OW3 O -0.0673(8) 0.3144(2) -0.8151(6) 0.0399(13) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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'
O O 0.0106 0.0060 '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
S3 Sn1 S6 115.04(6) . . ?
S3 Sn1 S2 116.70(6) . . ?
S6 Sn1 S2 104.78(6) . . ?
S3 Sn1 S9 109.34(6) . . ?
S6 Sn1 S9 104.41(5) . . ?
S2 Sn1 S9 105.48(6) . . ?
S5 Sn2 S4 112.38(5) . . ?
S5 Sn2 S8 114.26(6) . . ?
S4 Sn2 S8 104.30(5) . . ?
S5 Sn2 S9 112.04(6) . . ?
S4 Sn2 S9 104.25(5) . . ?
S8 Sn2 S9 108.86(6) . . ?
S7 Sn3 S1 121.77(6) . . ?
S7 Sn3 S2 116.64(6) . . ?
S1 Sn3 S2 100.99(6) . . ?
S7 Sn3 S8 111.18(6) . . ?
S1 Sn3 S8 98.99(6) . . ?
S2 Sn3 S8 104.71(6) . . ?
S1 Ag1 S6 128.16(6) 3_564 1_454 ?
S1 Ag1 S4 128.91(6) 3_564 . ?
S6 Ag1 S4 101.74(5) 1_454 . ?
S7 Ag2 S5 118.69(6) 1_455 1_455 ?
S7 Ag2 S3 109.32(5) 1_455 1_455 ?
S5 Ag2 S3 111.08(6) 1_455 1_455 ?
S7 Ag2 S4 110.89(5) 1_455 . ?
S5 Ag2 S4 95.85(5) 1_455 . ?
S3 Ag2 S4 110.23(5) 1_455 . ?
Sn2 S9 Sn1 108.82(6) . . ?
Sn2 S8 Sn3 110.40(6) . . ?
Sn3 S7 Ag2 101.13(6) . 1_655 ?
Sn1 S6 Ag1 99.15(6) . 1_656 ?
Sn2 S5 Ag2 98.30(6) . 1_655 ?
Sn2 S4 Ag1 103.01(6) . . ?
Sn2 S4 Ag2 109.85(6) . . ?
Ag1 S4 Ag2 105.13(6) . . ?
Sn1 S3 Ag2 103.17(6) . 1_655 ?
Sn1 S2 Sn3 108.43(6) . . ?
Sn3 S1 Ag1 104.68(7) . 3_564 ?
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 S3 2.3296(16) . ?
Sn1 S6 2.3580(15) . ?
Sn1 S2 2.4085(15) . ?
Sn1 S9 2.4660(15) . ?
Sn2 S5 2.3387(15) . ?
Sn2 S4 2.3698(14) . ?
Sn2 S8 2.4034(15) . ?
Sn2 S9 2.4431(15) . ?
Sn3 S7 2.3288(17) . ?
Sn3 S1 2.3469(15) . ?
Sn3 S2 2.4404(16) . ?
Sn3 S8 2.4564(16) . ?
Ag1 S1 2.4433(17) 3_564 ?
Ag1 S6 2.5333(17) 1_454 ?
Ag1 S4 2.5347(16) . ?
Ag2 S7 2.5634(16) 1_455 ?
Ag2 S5 2.5859(16) 1_455 ?
Ag2 S3 2.5958(17) 1_455 ?
Ag2 S4 2.6724(17) . ?
S7 Ag2 2.5634(16) 1_655 ?
S6 Ag1 2.5333(17) 1_656 ?
S5 Ag2 2.5859(16) 1_655 ?
S3 Ag2 2.5958(17) 1_655 ?
S1 Ag1 2.4433(17) 3_564 ?
