#------------------------------------------------------------------------------
#$Date: 2017-07-11 15:10:40 +0300 (Tue, 11 Jul 2017) $
#$Revision: 198633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/08/4320812.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_4320812
loop_
_publ_author_name
'Michael Brorson'
'Alan Hazell'
'Claus J. H. Jacobsen'
'Iver Schmidt'
'Jørgen Villadsen'
_publ_contact_author
;
Michael Brorson
Haldor Topsøe Research Laboratories
Nymøllevej 55
DK-2800 Lyngby
Denmark
;
_publ_section_title
;
 Preparation and Crystal Structures of Formato Complexes of the
 [MIV₃O₄]⁴⁺ and [MIV₃S₄]⁴⁺ (M = Mo,W) Clusters. Convenient
 Precursors to the Corresponding Aqua Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1346
_journal_page_last               1350
_journal_paper_doi               10.1021/ic9906656
_journal_volume                  39
_journal_year                    2000
_chemical_formula_structural     K6[W3S4(HCO2)9]HCO2.2.27H2O.0.73CH3OH
_chemical_formula_sum            'C10.73 H17.46 K6 O23 S4 W3'
_chemical_formula_weight         1428.920
_chemical_name_systematic        ?
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90
_cell_angle_beta                 118.94(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.605(6)
_cell_length_b                   14.458(7)
_cell_length_c                   13.627(5)
_cell_measurement_radiation      'Mo K\a'
_cell_measurement_reflns_used    30
_cell_measurement_temperature    294
_cell_measurement_theta_max      14.4
_cell_measurement_theta_min      10.1
_cell_measurement_wavelength     0.71073
_cell_volume                     3380(2)
_computing_cell_refinement       MAD
_computing_data_collection       'MAD (Allibon, 1995)'
_computing_data_reduction        'KRYSTAL (Hazell, 1995)'
_computing_molecular_graphics
;                                  
      ORTEP-III (Burnett & Johnson, 1996), KRYSTAL                    
;
_computing_publication_material  KRYSTAL
_computing_structure_refinement  'modified ORFLS(1962), KRYSTAL'
_computing_structure_solution
;                                  
      SIR92 (Altomare et al., 1994) KRYSTAL                           
;
_diffrn_ambient_temperature      294
_diffrn_measurement_device       'Huber four-circle diffractometer'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           'Ag K\a'
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4989
_diffrn_reflns_reduction_process 4794
_diffrn_reflns_theta_max         22.5
_diffrn_reflns_theta_min         1.3
_diffrn_standards_decay_%        8
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    6.121
_exptl_absorpt_correction_T_max  0.513
_exptl_absorpt_correction_T_min  0.326
_exptl_absorpt_correction_type   integration,DATAP,KRYSTAL(Hazell,1995)
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.807
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2663.360
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.9(2)
_refine_diff_density_min         -1.9(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.224
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    2
_refine_ls_number_parameters     234
_refine_ls_number_reflns         2656
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.046
_refine_ls_shift/esd_max         0.037
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/{[σcs(F²)+1.03F²]^1/2^-|F|}²'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.055
_reflns_number_observed          2656
_reflns_number_total             4664
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            ic9906656_1.cif
_cod_data_source_block           compound(2)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '
1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^' was changed to 'calc'. New
tag '_refine_ls_weighting_details' was created. The value of the new
tag was set to 'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constrained' was replaced with
the value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

'_atom_site_thermal_displace_type' value 'Uij' was replaced with the
value 'Uani' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'
(29 times).

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        3381(2)
_cod_original_sg_symbol_Hall     '-C 2y '
_cod_database_code               4320812
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
+x,-y,+z
-x,-y,-z
-x,+y,-z
1/2+x,1/2+y,+z
1/2+x,1/2-y,+z
1/2-x,1/2-y,-z
1/2-x,1/2+y,-z
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_occupancy
W1 0.21784(5) 0.00000 0.06604(6) 0.0249(5) Uani 0.50
W2 0.30898(3) 0.09525(4) 0.26047(5) 0.0248(3) Uani 1.00
S1 0.2027(3) 0.0000 0.2268(4) 0.026(3) Uani 0.50
S2 0.4179(3) 0.0000 0.3335(4) 0.030(3) Uani 0.50
S3 0.3026(2) 0.1195(2) 0.0890(3) 0.030(2) Uani 1.00
O1 0.1843(8) 0.0000 -0.1090(12) 0.039(11) Uani 0.50
C2 0.2257(14) 0.0000 -0.1562(19) 0.041(17) Uani 0.50
O3 0.2005(9) 0.0000 -0.2597(12) 0.044(12) Uani 0.50
O4 0.1203(5) 0.0904(7) 0.0024(8) 0.037(7) Uani 1.00
C5 0.0985(10) 0.1578(11) -0.0631(15) 0.049(13) Uani 1.00
O6 0.0363(7) 0.1971(8) -0.1016(10) 0.058(10) Uani 1.00
O7 0.3171(6) 0.1143(8) 0.4216(8) 0.039(7) Uani 1.00
C8 0.3741(9) 0.1122(9) 0.5174(12) 0.034(10) Uani 1.00
O9 0.3716(7) 0.1257(9) 0.6046(9) 0.057(10) Uani 1.00
O10 0.3884(6) 0.2098(7) 0.3222(8) 0.036(7) Uani 1.00
C11 0.4536(8) 0.2222(10) 0.3227(12) 0.032(10) Uani 1.00
O12 0.4987(6) 0.2846(7) 0.3708(9) 0.046(8) Uani 1.00
O13 0.2288(6) 0.2035(7) 0.2371(8) 0.040(8) Uani 1.00
C14 0.2096(9) 0.2753(11) 0.1785(13) 0.039(11) Uani 1.00
O15 0.1594(7) 0.3315(8) 0.1717(9) 0.053(9) Uani 1.00
O16 0.0111(10) 0.0000 0.4036(14) 0.057(15) Uani 0.50
C17 0.0073(16) 0.0000 0.3110(22) 0.051(19) Uani 0.50
O18 0.0656(12) 0.0000 0.2932(19) 0.073(19) Uani 0.50
K1 0.1624(4) 0.5000 0.2779(5) 0.050(4) Uani 0.50
K2 0.1057(2) 0.1961(3) 0.2881(3) 0.054(3) Uani 1.00
K3 0.1013(2) 0.1204(3) 0.5722(3) 0.052(3) Uani 1.00
K4 0.0000 0.3463(7) 0.0000 0.038(6) Uani 0.25
K5 -0.0107(7) 0.0000 -0.0364(8) 0.045(9) Uani 0.25
O19 0.4943(13) 0.0000 0.1313(19) 0.105(23) Uani 0.50
O20 0.7899(13) 0.1889(16) 0.4711(19) 0.079(8) Uiso 0.64(2)
C18 0.7987(33) 0.0000 0.5211(48) 0.106(19) Uiso 0.36
O21 0.8036(21) 0.0771(26) 0.5180(31) 0.063(11) Uiso 0.36
H2 0.2806 0.0000 -0.1093 0.049 Uiso 0.50
H5 0.1346 0.1806 -0.0850 0.058 Uiso 1.00
H8 0.4236 0.0990 0.5238 0.041 Uiso 1.00
H11 0.4673 0.1793 0.2823 0.038 Uiso 1.00
H14 0.2352 0.2878 0.1360 0.046 Uiso 1.00
H17 -0.0432 0.0000 0.2473 0.062 Uiso 0.50
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
4 0 -1
2 0 -6
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_2
_geom_angle_site_symmetry_3
O4 W1 O4 76.0(5) . . 2_555
O1 W1 O4 79.4(4) . . .
S3 W1 O4 92.4(3) . . .
S3 W1 O4 164.1(3) 2_555 . .
S1 W1 O4 83.4(3) . . .
W2 W1 O4 97.0(3) . . .
W2 W1 O4 137.7(3) 2_555 . .
O1 W1 O4 79.4(4) . . 2_555
S3 W1 O4 164.1(3) . . 2_555
S3 W1 O4 92.4(3) 2_555 . 2_555
S1 W1 O4 83.4(3) . . 2_555
W2 W1 O4 137.7(3) . . 2_555
W2 W1 O4 97.0(3) 2_555 . 2_555
S3 W1 O1 87.9(3) . . .
S3 W1 O1 87.9(3) 2_555 . .
S1 W1 O1 158.1(4) . . .
W2 W1 O1 141.2(2) . . .
W2 W1 O1 141.2(2) 2_555 . .
S3 W1 S3 96.8(2) . . 2_555
S1 W1 S3 106.3(1) . . .
W2 W1 S3 53.44(9) . . .
W2 W1 S3 98.90(9) 2_555 . .
S1 W1 S3 106.3(1) . . 2_555
W2 W1 S3 98.90(10) . . 2_555
W2 W1 S3 53.44(9) 2_555 . 2_555
W2 W1 S1 54.31(9) . . .
W2 W1 S1 54.31(9) 2_555 . .
W2 W1 W2 60.25(4) . . 2_555
O7 W2 O13 75.1(4) . . .
O10 W2 O13 80.5(4) . . .
S3 W2 O13 93.6(3) . . .
S2 W2 O13 163.5(3) . . .
S1 W2 O13 83.2(3) . . .
W1 W2 O13 97.8(3) . . .
W2 W2 O13 137.3(3) 2_555 . .
O7 W2 O10 79.6(4) . . .
S3 W2 O7 163.8(3) . . .
S2 W2 O7 92.3(3) . . .
S1 W2 O7 84.0(3) . . .
W1 W2 O7 138.2(3) . . .
W2 W2 O7 97.4(3) 2_555 . .
S3 W2 O10 87.3(3) . . .
S2 W2 O10 87.0(3) . . .
S1 W2 O10 159.2(3) . . .
W1 W2 O10 140.9(3) . . .
W2 W2 O10 140.5(3) 2_555 . .
S2 W2 S3 96.5(2) . . .
S1 W2 S3 106.4(1) . . .
W1 W2 S3 53.6(1) . . .
W2 W2 S3 98.74(9) 2_555 . .
S1 W2 S2 106.3(1) . . .
W1 W2 S2 98.7(1) . . .
W2 W2 S2 53.61(8) 2_555 . .
W1 W2 S1 54.3(1) . . .
W2 W2 S1 54.14(7) 2_555 . .
W1 W2 W2 59.87(2) . . 2_555
W1 S1 W2 71.4(1) . . .
W1 S1 W2 71.4(1) . . 2_555
W2 S1 W2 71.7(1) . . 2_555
W2 S2 W2 72.8(2) . . 2_555
W1 S3 W2 72.9(1) . . .
W1 O1 C2 130.0(15) . . .
W1 O4 C5 134.5(10) . . .
W2 O7 C8 131.2(10) . . .
W2 O10 C11 129.7(9) . . .
W2 O13 C14 132.6(10) . . .
O3 C2 H2 117.4(23) . . .
O1 C2 H2 117.4(22) . . .
O1 C2 O3 125.3(22) . . .
O6 C5 H5 116.5(15) . . .
O4 C5 H5 116.5(15) . . .
O4 C5 O6 126.9(16) . . .
O9 C8 H8 117.4(15) . . .
O7 C8 H8 117.4(14) . . .
O7 C8 O9 125.2(15) . . .
O12 C11 H11 117.7(13) . . .
O10 C11 H11 117.7(14) . . .
O10 C11 O12 124.6(13) . . .
O15 C14 H14 117.5(15) . . .
O13 C14 H14 117.5(15) . . .
O13 C14 O15 124.9(14) . . .
O16 C17 H17 117.3(29) . . .
O18 C17 H17 117.3(29) . . .
O16 C17 O18 125.4(26) . . .
O21 C18 O21 167(8) . . 2_555
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
W1 O4 2.124(10) . .
W1 O4 2.124(10) . 2_555
W1 O1 2.146(15) . .
W1 S3 2.311(4) . .
W1 S3 2.311(4) . 2_555
W1 S1 2.349(5) . .
W1 W2 2.744(1) . .
W1 W2 2.744(1) . 2_555
W2 O13 2.130(10) . .
W2 O7 2.141(9) . .
W2 O10 2.147(10) . .
W2 S3 2.305(4) . .
W2 S2 2.321(4) . .
W2 S1 2.351(4) . .
W2 W2 2.754(2) . 2_555
O1 C2 1.256(25) . .
C2 H2 0.949(23) . .
C2 O3 1.249(25) . .
O4 C5 1.248(17) . .
C5 H5 0.950(16) . .
C5 O6 1.212(18) . .
O7 C8 1.242(17) . .
C8 H8 0.950(15) . .
C8 O9 1.228(16) . .
O10 C11 1.289(15) . .
C11 H11 0.950(14) . .
C11 O12 1.210(16) . .
O13 C14 1.252(17) . .
C14 H14 0.950(15) . .
C14 O15 1.245(17) . .
O16 C17 1.227(29) . .
C17 H17 0.949(25) . .
C17 O18 1.279(31) . .
K5 K5 0.870(19) . 3_555
C18 O21 1.122(37) . .
C18 O21 1.122(37) . 2_555
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
W1 O1 C2 O3 180(6) . . . .
W1 O4 C5 O6 171(1) . . . .
W2 O7 C8 O9 179(1) . . . .
W2 O10 C11 O12 171(1) . . . .
W2 O13 C14 O15 178(1) . . . .
