#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/24/2202415.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_2202415
loop_
_publ_author_name
'Jian-Fang Ma'
'Jin Yang'
'Jing-Fu Liu'
_publ_section_title
;
 Hexaaquanickel(II) 3-carboxy-4-hydroxybenzenesulfonate tetrahydrate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m483
_journal_page_last               m484
_journal_paper_doi               10.1107/S1600536803013072
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Ni (H2 O)6] (C7 H5 O6 S)2, 4H2 O'
_chemical_formula_moiety         'H12 Ni O6 2+, 2C7 H5 O6 S 1-, 4H2 O'
_chemical_formula_sum            'C14 H30 Ni O22 S2'
_chemical_formula_weight         673.21
_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                92.931(16)
_cell_angle_beta                 96.494(16)
_cell_angle_gamma                102.727(12)
_cell_formula_units_Z            1
_cell_length_a                   6.5380(9)
_cell_length_b                   7.2199(10)
_cell_length_c                   14.534(4)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      9.71
_cell_measurement_theta_min      5.90
_cell_volume                     662.9(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  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0413
_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       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3424
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.83
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.985
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             350
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.465
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2599
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0377
_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)+(0.0506P)²+0.1374P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1010
_reflns_number_gt                2145
_reflns_number_total             2599
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cf6254.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               2202415
_cod_database_fobs_code          2202415
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 0.3984(4) 0.1628(3) 0.35573(17) 0.0278(5) Uani d . 1 . . C
C2 0.3124(4) 0.1629(3) 0.43782(17) 0.0279(5) Uani d . 1 . . C
H2 0.1687 0.1125 0.4380 0.033 Uiso calc R 1 . . H
C3 0.4391(4) 0.2378(3) 0.52047(17) 0.0273(5) Uani d . 1 . . C
C4 0.6558(4) 0.3165(4) 0.51950(18) 0.0295(6) Uani d . 1 . . C
C5 0.7410(4) 0.3130(4) 0.43618(19) 0.0355(6) Uani d . 1 . . C
H5 0.8848 0.3617 0.4355 0.043 Uiso calc R 1 . . H
C6 0.6144(4) 0.2382(4) 0.35461(19) 0.0343(6) Uani d . 1 . . C
H6 0.6722 0.2378 0.2990 0.041 Uiso calc R 1 . . H
C7 0.3473(4) 0.2389(4) 0.60864(18) 0.0316(6) Uani d . 1 . . C
O1 0.0942(4) 0.2087(3) 0.23422(16) 0.0517(6) Uani d . 1 . . O
O2 0.3624(3) 0.0621(3) 0.17979(14) 0.0482(6) Uani d . 1 . . O
O3 0.1033(3) -0.1100(3) 0.26806(13) 0.0381(5) Uani d . 1 . . O
O4 0.1434(3) 0.1633(3) 0.59849(14) 0.0474(6) Uani d . 1 . . O
H4 0.0996 0.1669 0.6491 0.071 Uiso calc R 1 . . H
O5 0.4502(3) 0.3030(3) 0.68376(13) 0.0438(5) Uani d . 1 . . O
O6 0.7848(3) 0.3981(3) 0.59650(14) 0.0432(5) Uani d . 1 . . O
H6A 0.7175 0.3916 0.6410 0.065 Uiso calc R 1 . . H
OW1 0.7004(4) 0.3312(3) 0.97347(16) 0.0486(6) Uani d D 1 . . O
OW2 0.7265(3) 0.7363(3) 0.97940(14) 0.0395(5) Uani d D 1 . . O
OW3 0.6189(3) 0.5222(3) 1.13815(13) 0.0406(5) Uani d D 1 . . O
OW4 0.7348(3) 0.0508(3) 0.09873(15) 0.0427(5) Uani d D 1 . . O
OW5 0.0476(4) 0.5520(3) 0.16465(15) 0.0440(5) Uani d D 1 . . O
S1 0.23022(10) 0.07503(9) 0.25133(4) 0.02897(18) Uani d . 1 . . S
Ni1 0.5000 0.5000 1.0000 0.02897(16) Uani d S 1 . . Ni
H1A 0.750(5) 0.253(4) 1.0117(19) 0.043 Uiso d D 1 . . H
H1B 0.803(4) 0.374(4) 0.940(2) 0.043 Uiso d D 1 . . H
H2A 0.721(5) 0.787(4) 0.9240(15) 0.043 Uiso d D 1 . . H
H2B 0.743(5) 0.835(3) 1.0213(18) 0.043 Uiso d D 1 . . H
H3A 0.589(5) 0.595(4) 1.1831(18) 0.043 Uiso d D 1 . . H
H3B 0.756(3) 0.523(4) 1.153(2) 0.043 Uiso d D 1 . . H
H4A 0.834(4) 0.097(4) 0.1467(17) 0.043 Uiso d D 1 . . H
H4B 0.610(4) 0.028(4) 0.122(2) 0.043 Uiso d D 1 . . H
H5A 0.086(5) 0.463(4) 0.196(2) 0.043 Uiso d D 1 . . H
H5B 0.093(5) 0.658(3) 0.2035(19) 0.043 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'
Ni Ni 0.3393 1.1124 '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 . . 120.3(2) ?
C2 C1 S1 . . 119.0(2) ?
C6 C1 S1 . . 120.7(2) ?
C1 C2 C3 . . 120.4(2) ?
C1 C2 H2 . . 119.8 ?
C3 C2 H2 . . 119.8 ?
C2 C3 C4 . . 119.6(2) ?
C2 C3 C7 . . 120.5(2) ?
C4 C3 C7 . . 119.9(2) ?
O6 C4 C5 . . 118.2(2) ?
O6 C4 C3 . . 122.4(2) ?
C5 C4 C3 . . 119.4(2) ?
C6 C5 C4 . . 120.6(2) ?
C6 C5 H5 . . 119.7 ?
C4 C5 H5 . . 119.7 ?
C5 C6 C1 . . 119.7(3) ?
C5 C6 H6 . . 120.1 ?
C1 C6 H6 . . 120.1 ?
O5 C7 O4 . . 123.3(3) yes
O5 C7 C3 . . 123.7(3) ?
O4 C7 C3 . . 113.0(2) ?
C7 O4 H4 . . 109.5 ?
C4 O6 H6A . . 109.5 ?
Ni1 OW1 H1A . . 127(2) ?
Ni1 OW1 H1B . . 118(2) ?
H1A OW1 H1B . . 106(3) ?
Ni1 OW2 H2A . . 120(2) ?
Ni1 OW2 H2B . . 115(2) ?
H2A OW2 H2B . . 105(3) ?
Ni1 OW3 H3A . . 127(2) ?
Ni1 OW3 H3B . . 118(2) ?
H3A OW3 H3B . . 105(3) ?
H4A OW4 H4B . . 106(3) ?
H5A OW5 H5B . . 104(3) ?
O2 S1 O3 . . 112.45(13) yes
O2 S1 O1 . . 113.34(15) yes
O3 S1 O1 . . 109.89(14) yes
O2 S1 C1 . . 107.45(12) ?
O3 S1 C1 . . 106.75(12) ?
O1 S1 C1 . . 106.54(12) ?
OW1 Ni1 OW1 . 2_667 180.0 ?
OW1 Ni1 OW3 . 2_667 91.04(9) ?
OW1 Ni1 OW3 2_667 2_667 88.96(9) ?
OW1 Ni1 OW3 . . 88.96(9) yes
OW1 Ni1 OW3 2_667 . 91.04(9) ?
OW3 Ni1 OW3 2_667 . 180.0 ?
OW1 Ni1 OW2 . 2_667 90.08(10) ?
OW1 Ni1 OW2 2_667 2_667 89.92(10) ?
OW3 Ni1 OW2 2_667 2_667 90.05(9) ?
OW3 Ni1 OW2 . 2_667 89.95(9) ?
OW1 Ni1 OW2 . . 89.92(10) yes
OW1 Ni1 OW2 2_667 . 90.08(10) ?
OW3 Ni1 OW2 2_667 . 89.95(9) ?
OW3 Ni1 OW2 . . 90.05(9) yes
OW2 Ni1 OW2 2_667 . 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 . 1.375(4) ?
C1 C6 . 1.399(4) ?
C1 S1 . 1.769(3) ?
C2 C3 . 1.390(4) ?
C2 H2 . 0.930 ?
C3 C4 . 1.407(4) ?
C3 C7 . 1.476(3) ?
C4 O6 . 1.346(3) yes
C4 C5 . 1.390(4) ?
C5 C6 . 1.378(4) ?
C5 H5 . 0.930 ?
C6 H6 . 0.930 ?
C7 O5 . 1.226(3) yes
C7 O4 . 1.313(3) yes
O1 S1 . 1.462(2) yes
O2 S1 . 1.437(2) yes
O3 S1 . 1.4569(19) yes
O4 H4 . 0.820 ?
O6 H6A . 0.820 ?
OW1 Ni1 . 2.030(2) yes
OW1 H1A . 0.898(18) ?
OW1 H1B . 0.883(18) ?
OW2 Ni1 . 2.057(2) yes
OW2 H2A . 0.902(18) ?
OW2 H2B . 0.893(18) ?
OW3 Ni1 . 2.054(2) yes
OW3 H3A . 0.882(18) ?
OW3 H3B . 0.894(18) ?
OW4 H4A . 0.894(18) ?
OW4 H4B . 0.902(18) ?
OW5 H5A . 0.872(18) ?
OW5 H5B . 0.902(18) ?
Ni1 OW1 2_667 2.030(2) ?
Ni1 OW3 2_667 2.054(2) ?
Ni1 OW2 2_667 2.057(2) ?
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 OW4 1_556 0.898(18) 1.973(19) 2.820(3) 156(3)
OW1 H1B OW5 2_666 0.883(18) 1.934(19) 2.786(3) 162(3)
OW2 H2A O2 2_666 0.902(18) 2.001(19) 2.867(3) 161(3)
OW2 H2B OW4 1_566 0.893(18) 1.888(19) 2.773(3) 170(3)
OW3 H3B OW5 1_656 0.894(18) 1.861(19) 2.745(3) 169(3)
OW3 H3A O5 2_667 0.882(18) 2.099(19) 2.946(3) 161(3)
OW4 H4B O2 . 0.902(18) 1.964(19) 2.837(3) 163(3)
OW4 H4A O1 1_655 0.894(18) 1.989(19) 2.871(3) 169(3)
OW5 H5B O3 1_565 0.902(18) 1.860(19) 2.731(3) 162(3)
OW5 H5A O1 . 0.872(18) 1.955(19) 2.789(3) 160(3)
O4 H4 O3 2_556 0.82 1.88 2.650(3) 155
O6 H6A O5 . 0.82 1.91 2.631(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 0.0(4)
S1 C1 C2 C3 -177.46(19)
C1 C2 C3 C4 1.0(4)
C1 C2 C3 C7 179.7(2)
C2 C3 C4 O6 177.3(2)
C7 C3 C4 O6 -1.5(4)
C2 C3 C4 C5 -1.9(4)
C7 C3 C4 C5 179.4(2)
O6 C4 C5 C6 -177.4(2)
C3 C4 C5 C6 1.8(4)
C4 C5 C6 C1 -0.8(4)
C2 C1 C6 C5 -0.1(4)
S1 C1 C6 C5 177.3(2)
C2 C3 C7 O5 -179.9(3)
C4 C3 C7 O5 -1.2(4)
C2 C3 C7 O4 0.3(4)
C4 C3 C7 O4 179.1(2)
C2 C1 S1 O2 -170.8(2)
C6 C1 S1 O2 11.8(3)
C2 C1 S1 O3 -49.9(2)
C6 C1 S1 O3 132.6(2)
C2 C1 S1 O1 67.4(2)
C6 C1 S1 O1 -110.0(2)
