#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/24/2202413.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_2202413
loop_
_publ_author_name
'Jian-Fang Ma'
'Jin Yang'
'Jing-Fu Liu'
_publ_section_title
;
 Hexaaquacopper(II) 3-carboxy-4-hydroxybenzenesulfonate dihydrate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m485
_journal_page_last               m486
_journal_paper_doi               10.1107/S1600536803013084
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Cu (H2 O)6] (C7 H5 O6 S)2, 2H2 O'
_chemical_formula_moiety         'H12 Cu O6 2+, 2C7 H5 O6 S 1-, 2H2 O'
_chemical_formula_sum            'C14 H26 Cu O20 S2'
_chemical_formula_weight         642.01
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.16(2)
_cell_angle_beta                 90.259(18)
_cell_angle_gamma                112.236(12)
_cell_formula_units_Z            1
_cell_length_a                   7.0298(9)
_cell_length_b                   7.0749(15)
_cell_length_c                   13.288(4)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      9.92
_cell_measurement_theta_min      5.36
_cell_volume                     611.2(2)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1990)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       ω
_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  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3134
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.157
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             331
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.524
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2413
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0322
_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)+(0.0566P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                2140
_reflns_number_total             2413
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cf6252.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 'Triclinic' changed to 'triclinic'
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 
;
_cod_database_code               2202413
_cod_database_fobs_code          2202413
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -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_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
C1 0.2205(3) 0.4403(3) 0.65438(15) 0.0244(4) Uani d . 1 . . C
C2 0.2004(3) 0.3313(3) 0.56410(15) 0.0243(4) Uani d . 1 . . C
H2 0.1638 0.1904 0.5634 0.029 Uiso calc R 1 . . H
C3 0.2352(3) 0.4327(3) 0.47369(15) 0.0241(4) Uani d . 1 . . C
C4 0.2928(4) 0.6457(4) 0.47607(17) 0.0284(5) Uani d . 1 . . C
C5 0.3103(4) 0.7531(3) 0.56800(18) 0.0322(5) Uani d . 1 . . C
H5 0.3472 0.8941 0.5695 0.039 Uiso calc R 1 . . H
C6 0.2734(4) 0.6517(3) 0.65644(17) 0.0301(5) Uani d . 1 . . C
H6 0.2835 0.7237 0.7176 0.036 Uiso calc R 1 . . H
C7 0.2117(4) 0.3171(4) 0.37601(17) 0.0305(5) Uani d . 1 . . C
O1 0.3123(3) 0.1933(3) 0.76643(13) 0.0416(5) Uani d . 1 . . O
O2 -0.0378(3) 0.1691(2) 0.76838(12) 0.0308(4) Uani d . 1 . . O
O3 0.2249(3) 0.4634(3) 0.84896(12) 0.0444(5) Uani d . 1 . . O
O4 0.1564(3) 0.1200(3) 0.38535(12) 0.0418(5) Uani d . 1 . . O
H4 0.1452 0.0634 0.3294 0.063 Uiso calc R 1 . . H
O5 0.2416(4) 0.3988(3) 0.29508(12) 0.0467(5) Uani d . 1 . . O
O6 0.3330(3) 0.7531(3) 0.39242(14) 0.0448(5) Uani d . 1 . . O
H6A 0.3181 0.6754 0.3431 0.067 Uiso calc R 1 . . H
OW1 0.6723(3) 0.2571(3) 0.88095(12) 0.0317(4) Uani d D 1 . . O
OW2 0.4356(3) 0.1959(3) 1.08673(14) 0.0378(4) Uani d D 1 . . O
OW3 0.2426(3) -0.0653(3) 0.92333(14) 0.0378(4) Uani d D 1 . . O
OW4 0.8673(3) 0.6598(3) 0.95578(13) 0.0338(4) Uani d D 1 . . O
S1 0.17750(9) 0.30792(8) 0.76709(4) 0.02569(16) Uani d . 1 . . S
Cu1 0.5000 0.0000 1.0000 0.02392(14) Uani d S 1 . . Cu
H1A 0.766(4) 0.237(4) 0.8420(19) 0.036 Uiso d D 1 . . H
H1B 0.577(4) 0.252(4) 0.8364(18) 0.036 Uiso d D 1 . . H
H2A 0.540(4) 0.304(3) 1.109(2) 0.036 Uiso d D 1 . . H
H2B 0.339(4) 0.239(4) 1.071(2) 0.036 Uiso d D 1 . . H
H3A 0.121(3) -0.157(4) 0.936(2) 0.036 Uiso d D 1 . . H
H3B 0.222(4) -0.015(4) 0.8674(16) 0.036 Uiso d D 1 . . H
H4A 0.854(4) 0.621(4) 1.0185(15) 0.036 Uiso d D 1 . . H
H4B 0.819(4) 0.545(3) 0.9187(18) 0.036 Uiso d D 1 . . H
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'
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'
Cu Cu 0.3201 1.2651 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 C6 . . 120.6(2) ?
C2 C1 S1 . . 118.77(17) ?
C6 C1 S1 . . 120.64(17) ?
C1 C2 C3 . . 119.9(2) ?
C1 C2 H2 . . 120.0 ?
C3 C2 H2 . . 120.0 ?
C2 C3 C4 . . 119.39(19) ?
C2 C3 C7 . . 120.5(2) ?
C4 C3 C7 . . 120.11(19) ?
O6 C4 C5 . . 117.6(2) ?
O6 C4 C3 . . 122.5(2) ?
C5 C4 C3 . . 119.9(2) ?
C6 C5 C4 . . 120.3(2) ?
C6 C5 H5 . . 119.8 ?
C4 C5 H5 . . 119.8 ?
C5 C6 C1 . . 119.9(2) ?
C5 C6 H6 . . 120.1 ?
C1 C6 H6 . . 120.1 ?
O5 C7 O4 . . 123.6(2) yes
O5 C7 C3 . . 123.0(2) ?
O4 C7 C3 . . 113.37(19) ?
C7 O4 H4 . . 109.5 ?
C4 O6 H6A . . 109.5 ?
Cu1 OW1 H1A . . 117.9(18) ?
Cu1 OW1 H1B . . 105.7(19) ?
H1A OW1 H1B . . 102(3) ?
Cu1 OW2 H2A . . 116(2) ?
Cu1 OW2 H2B . . 122.3(19) ?
H2A OW2 H2B . . 106(3) ?
Cu1 OW3 H3A . . 127.8(19) ?
Cu1 OW3 H3B . . 128.5(19) ?
H3A OW3 H3B . . 104(3) ?
H4A OW4 H4B . . 105(3) ?
O2 S1 O3 . . 111.03(11) yes
O2 S1 O1 . . 110.55(11) yes
O3 S1 O1 . . 113.44(13) yes
O2 S1 C1 . . 108.60(10) ?
O3 S1 C1 . . 106.18(10) ?
O1 S1 C1 . . 106.73(11) ?
OW2 Cu1 OW2 2_657 . 180.0 ?
OW2 Cu1 OW3 2_657 . 89.33(8) ?
OW2 Cu1 OW3 . . 90.67(8) yes
OW2 Cu1 OW3 2_657 2_657 90.67(8) ?
OW2 Cu1 OW3 . 2_657 89.33(8) ?
OW3 Cu1 OW3 . 2_657 180.0 ?
OW2 Cu1 OW1 2_657 . 87.81(7) ?
OW2 Cu1 OW1 . . 92.19(7) yes
OW3 Cu1 OW1 . . 89.13(7) yes
OW3 Cu1 OW1 2_657 . 90.87(7) ?
OW2 Cu1 OW1 2_657 2_657 92.19(7) ?
OW2 Cu1 OW1 . 2_657 87.81(7) ?
OW3 Cu1 OW1 . 2_657 90.87(7) ?
OW3 Cu1 OW1 2_657 2_657 89.13(7) ?
OW1 Cu1 OW1 . 2_657 180.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.379(3) ?
C1 C6 . 1.397(3) ?
C1 S1 . 1.763(2) ?
C2 C3 . 1.397(3) ?
C2 H2 . 0.930 ?
C3 C4 . 1.403(3) ?
C3 C7 . 1.482(3) ?
C4 O6 . 1.340(3) yes
C4 C5 . 1.394(3) ?
C5 C6 . 1.374(3) ?
C5 H5 . 0.930 ?
C6 H6 . 0.930 ?
C7 O5 . 1.221(3) yes
C7 O4 . 1.310(3) yes
O1 S1 . 1.462(2) yes
O2 S1 . 1.4600(17) yes
O3 S1 . 1.4608(18) yes
O4 H4 . 0.820 ?
O6 H6A . 0.820 ?
OW1 Cu1 . 2.4175(18) yes
OW1 H1A . 0.888(18) ?
OW1 H1B . 0.884(18) ?
OW2 Cu1 . 1.9527(18) yes
OW2 H2A . 0.876(18) ?
OW2 H2B . 0.873(17) ?
OW3 Cu1 . 1.9596(18) yes
OW3 H3A . 0.879(18) ?
OW3 H3B . 0.871(17) ?
OW4 H4A . 0.882(17) ?
OW4 H4B . 0.879(18) ?
Cu1 OW2 2_657 1.9527(18) ?
Cu1 OW3 2_657 1.9596(18) ?
Cu1 OW1 2_657 2.4175(18) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
OW1 H1A O2 1_655 0.888(18) 1.890(18) 2.774(2) 173(3)
OW1 H1B O1 . 0.884(18) 1.965(18) 2.824(3) 164(3)
OW2 H2A O3 2_667 0.876(18) 1.902(18) 2.777(3) 177(3)
OW2 H2B OW4 2_667 0.873(17) 1.880(18) 2.752(3) 177(3)
OW3 H3A OW4 1_445 0.879(18) 1.790(18) 2.668(3) 177(3)
OW3 H3B O1 . 0.871(17) 1.953(18) 2.748(3) 151(3)
OW4 H4A O3 2_667 0.882(17) 1.898(18) 2.770(3) 169(3)
OW4 H4B OW1 . 0.879(18) 1.950(19) 2.794(3) 160(3)
O4 H4 O2 2_556 0.82 1.96 2.726(2) 154
O6 H6A O5 . 0.82 1.91 2.627(3) 146
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
C6 C1 C2 C3 0.7(4)
S1 C1 C2 C3 -179.52(17)
C1 C2 C3 C4 0.8(3)
C1 C2 C3 C7 -179.2(2)
C2 C3 C4 O6 178.5(2)
C7 C3 C4 O6 -1.5(4)
C2 C3 C4 C5 -1.4(4)
C7 C3 C4 C5 178.6(2)
O6 C4 C5 C6 -179.3(2)
C3 C4 C5 C6 0.6(4)
C4 C5 C6 C1 0.8(4)
C2 C1 C6 C5 -1.5(4)
S1 C1 C6 C5 178.72(19)
C2 C3 C7 O5 -179.5(2)
C4 C3 C7 O5 0.5(4)
C2 C3 C7 O4 0.3(3)
C4 C3 C7 O4 -179.7(2)
C2 C1 S1 O2 -64.7(2)
C6 C1 S1 O2 115.0(2)
C2 C1 S1 O3 175.79(19)
C6 C1 S1 O3 -4.4(2)
C2 C1 S1 O1 54.5(2)
C6 C1 S1 O1 -125.7(2)
