#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/46/2004636.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2004636
loop_
_publ_author_name
'Blake, A. J.'
'Grimditch, R. S.'
'Parsons, S.'
'Schröder, M.'
_publ_section_title
;
 Tetrakis(dimethyl sulfoxide-O)copper(II) Bis(perchlorate)
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              514
_journal_page_last               516
_journal_paper_doi               10.1107/S0108270195013795
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[Cu (C2 H6 O S)4] , 2Cl O4 '
_chemical_formula_moiety         'C8 H24 Cu O4 S4 2+, 2Cl O4 -'
_chemical_formula_sum            'C8 H24 Cl2 Cu O12 S4'
_chemical_formula_weight         574.95
_chemical_name_systematic
;
 Tetrakis(dimethylsulphoxide-κ-O)copper(II) bis(perchlorate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 112.065(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.280(3)
_cell_length_b                   10.426(2)
_cell_length_c                   16.112(4)
_cell_measurement_reflns_used    52
_cell_measurement_temperature    240.0(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      10
_cell_volume                     2223.1(9)
_computing_cell_refinement       'DIF4 (Stoe & Cie, 1992)'
_computing_data_collection       'DIF4 (Stoe & Cie, 1992)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1995)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1992)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      240.0(2)
_diffrn_measurement_device       'Stoe Stadi-4 four-circle diffractometer'
_diffrn_measurement_method
;
ω-θ scans with ω scan width (1.0 + 0.35 tanθ)°
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  n.a.
_diffrn_reflns_av_sigmaI/netI    0.1406
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3495
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.648
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   '\y scans (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Column
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.70
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.977
_refine_ls_goodness_of_fit_obs   1.119
_refine_ls_hydrogen_treatment
;
Placed in calculated positions and thereafter allowed to ride on their
parent C atoms with U~iso~(H) = 1.5U~eq~(C).
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3255
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_restrained_S_obs      1.119
_refine_ls_R_factor_all          0.1548
_refine_ls_R_factor_obs          0.0649
_refine_ls_shift/esd_max         0.006
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0418P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1349
_refine_ls_wR_factor_obs         0.1060
_reflns_number_observed          1649
_reflns_number_total             3257
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            kh1069.cif
_cod_data_source_block           bun3cu
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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 'calc w =
1/[\s^2^(Fo^2^)+(0.0418P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0418P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2223.1(8)
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               2004636
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'
loop_
_atom_site_label
_atom_site_occupancy
_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_calc_flag
_atom_site_refinement_flags
_atom_site_type_symbol
Cu 1 -.00265(9) .04887(12) .74794(8) .0333(3) Uani d . Cu
S1 1 -0.2229(2) -.0303(3) .7039(2) .0375(7) Uani d . S
C11 1 -0.3174(7) .0891(10) .6802(7) .055(3) Uani d . C
H11A 1 -0.3064(7) .1539(10) .6416(7) .082 Uiso calc R H
H11B 1 -0.3144(7) .1285(10) .7356(7) .082 Uiso calc R H
H11C 1 -0.3834(7) .0503(10) .6502(7) .082 Uiso calc R H
C12 1 -0.2628(8) -0.1316(11) .7733(8) .068(4) Uani d . C
H12A 1 -0.2174(8) -0.2043(11) .7928(8) .102 Uiso calc R H
H12B 1 -0.3308(8) -0.1619(11) .7398(8) .102 Uiso calc R H
H12C 1 -0.2619(8) -.0837(11) .8252(8) .102 Uiso calc R H
O11 1 -0.1272(4) .0287(6) .7702(4) .037(2) Uani d . O
S2 1 .2180(2) .0079(3) .7684(2) .0452(8) Uani d . S
C21 1 .2998(8) .0796(12) .7200(8) .062(3) Uani d . C
H21A 1 .2747(8) .0609(12) .6564(8) .092 Uiso calc R H
H21B 1 .3674(8) .0450(12) .7485(8) .092 Uiso calc R H
H21C 1 .3015(8) .1717(12) .7288(8) .092 Uiso calc R H
C22 1 .2825(8) .0584(13) .8792(6) .068(4) Uani d . C
H22A 1 .2475(8) .0270(13) .9165(6) .101 Uiso calc R H
H22B 1 .2848(8) .1513(13) .8814(6) .101 Uiso calc R H
H22C 1 .3508(8) .0247(13) .9012(6) .101 Uiso calc R H
O21 1 .1230(4) .0871(6) .7325(4) .040(2) Uani d . O
S3 1 -.0466(2) .1915(3) .5707(2) .0438(7) Uani d . S
C31 1 -0.1259(8) .1005(11) .4792(7) .059(3) Uani d . C
H31A 1 -0.1046(8) .0115(11) .4872(7) .089 Uiso calc R H
H31B 1 -0.1217(8) .1331(11) .4244(7) .089 Uiso calc R H
H31C 1 -0.1951(8) .1067(11) .4757(7) .089 Uiso calc R H
C32 1 -0.1019(9) .3432(11) .5384(8) .068(4) Uani d . C
H32A 1 -.0657(9) .4061(11) .5833(8) .102 Uiso calc R H
H32B 1 -0.1720(9) .3403(11) .5327(8) .102 Uiso calc R H
H32C 1 -.0986(9) .3668(11) .4813(8) .102 Uiso calc R H
O31 1 -.0799(4) .1556(7) .6472(4) .042(2) Uani d . O
S4 1 .0275(2) -0.1471(3) .8991(2) .0417(7) Uani d . S
C41 1 .0697(9) -0.3060(10) .8981(7) .057(3) Uani d . C
H41A 1 .0317(9) -0.3452(10) .8406(7) .086 Uiso calc R H
H41B 1 .0596(9) -0.3548(10) .9453(7) .086 Uiso calc R H
H41C 1 .1409(9) -0.3054(10) .9078(7) .086 Uiso calc R H
C42 1 .1083(7) -0.1002(10) 1.0097(6) .048(3) Uani d . C
H42A 1 .0935(7) -.0123(10) 1.0204(6) .072 Uiso calc R H
H42B 1 .1783(7) -0.1067(10) 1.0156(6) .072 Uiso calc R H
H42C 1 .0969(7) -0.1561(10) 1.0531(6) .072 Uiso calc R H
O41 1 .0711(5) -.0733(7) .8395(4) .049(2) Uani d . O
Cl 1 .0864(2) .3082(3) .9173(2) .0400(7) Uani d . Cl
O1 1 .0216(7) .2207(9) .8590(6) .100(3) Uani d . O
O2 1 .1410(7) .3793(9) .8778(7) .102(3) Uani d . O
O3 1 .0283(6) .3908(9) .9471(6) .093(3) Uani d . O
O4 1 .1548(8) .2422(11) .9899(7) .120(4) Uani d . O
Cl' 1 -.0749(2) -0.2663(3) .6153(2) .0412(7) Uani d . Cl
O1' 1 -0.1213(7) -0.2962(8) .6754(6) .086(3) Uani d . O
O2' 1 -.0007(7) -0.3563(9) .6219(8) .122(4) Uani d . O
O3' 1 -.0306(7) -0.1433(9) .6339(6) .093(3) Uani d . O
O4' 1 -0.1470(7) -0.2646(12) .5291(6) .115(4) Uani d . O
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
S S 0.1246 0.1234 '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_publ_flag
O41 Cu O31 173.7(3) y
O41 Cu O21 88.2(3) y
O31 Cu O21 92.1(2) y
O41 Cu O11 93.5(3) y
O31 Cu O11 86.8(3) y
O21 Cu O11 173.7(3) y
O11 S1 C11 106.2(5) y
O11 S1 C12 102.4(5) y
C11 S1 C12 98.9(6) y
S1 O11 Cu 123.8(3) y
O21 S2 C22 106.3(5) y
O21 S2 C21 104.1(4) y
C22 S2 C21 98.0(6) y
S2 O21 Cu 125.5(4) y
O31 S3 C32 102.6(5) y
O31 S3 C31 104.3(5) y
C32 S3 C31 99.2(6) y
S3 O31 Cu 124.5(4) y
O41 S4 C41 104.2(5) y
O41 S4 C42 103.0(4) y
C41 S4 C42 99.9(5) y
S4 O41 Cu 125.1(4) y
O1 Cl O2 112.8(6) ?
O1 Cl O4 108.9(7) ?
O2 Cl O4 108.2(6) ?
O1 Cl O3 107.8(6) ?
O2 Cl O3 109.6(6) ?
O4 Cl O3 109.5(6) ?
O4' Cl' O2' 110.2(7) ?
O4' Cl' O1' 109.3(6) ?
O2' Cl' O1' 110.0(6) ?
O4' Cl' O3' 107.8(7) ?
O2' Cl' O3' 109.2(6) ?
O1' Cl' O3' 110.2(5) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Cu O41 1.934(6) y
Cu O31 1.936(6) y
Cu O21 1.944(6) y
Cu O11 1.954(6) y
S1 O11 1.513(6) y
S1 C11 1.770(10) y
S1 C12 1.781(10) y
S2 O21 1.505(6) y
S2 C22 1.754(10) y
S2 C21 1.793(10) y
S3 O31 1.524(6) y
S3 C32 1.757(11) y
S3 C31 1.761(10) y
S4 O41 1.534(6) y
S4 C41 1.765(11) y
S4 C42 1.789(10) y
Cl O1 1.385(8) ?
Cl O2 1.390(8) ?
Cl O4 1.392(9) ?
Cl O3 1.401(8) ?
Cl' O4' 1.383(8) ?
Cl' O2' 1.390(8) ?
Cl' O1' 1.397(7) ?
Cl' O3' 1.412(8) ?
