#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/34/2203441.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_2203441
loop_
_publ_author_name
'Kazak, Canan'
'Yazicilar, Turan K.'
'Yilmaz, Veysel T.'
_publ_section_title
;
 trans-Tetraaquabis(p-nitrobenzoxasulfamato)cobalt(II)
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m452
_journal_page_last               m454
_journal_paper_doi               10.1107/S1600536804006336
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Co (C6 H3 N2 O5 S)2 (H2 O)4]'
_chemical_formula_moiety         'C12 H14 Co N4 O14 S2'
_chemical_formula_sum            'C12 H14 Co N4 O14 S2'
_chemical_formula_weight         561.32
_chemical_name_systematic
;
trans-Tetraaquabis(p-nitrobenzoxasulfamato)cobalt(II)
;
_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                88.760(11)
_cell_angle_beta                 77.191(10)
_cell_angle_gamma                62.442(9)
_cell_formula_units_Z            1
_cell_length_a                   7.2079(9)
_cell_length_b                   7.3251(10)
_cell_length_c                   10.4032(14)
_cell_measurement_reflns_used    11439
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.18
_cell_measurement_theta_min      2.02
_cell_volume                     472.75(12)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Stoe IPDS-II'
_diffrn_measurement_method       'rotation method'
_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  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5264
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.217
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED; Stoe & Cie, 2002)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             285
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.673
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         1647
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0374
_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)+(0.0729P)²+0.0979P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1004
_reflns_number_gt                1571
_reflns_number_total             1647
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb6026.cif
_cod_data_source_block           I
_cod_original_cell_volume        472.75(11)
_cod_database_code               2203441
_cod_database_fobs_code          2203441
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_type_symbol
Co1 0.0000 0.0000 0.0000 0.02352(19) Uani d S 1 Co
S1 0.20322(9) 0.18184(8) 0.18616(5) 0.0274(2) Uani d . 1 S
N1 0.0182(3) 0.1215(3) 0.18206(16) 0.0280(4) Uani d . 1 N
N2 -0.4760(3) 0.3635(3) 0.69980(18) 0.0357(5) Uani d . 1 N
O1W 0.3165(3) -0.2299(3) -0.02973(16) 0.0369(4) Uani d D 1 O
O2W 0.0879(3) 0.2032(3) -0.10933(16) 0.0391(4) Uani d D 1 O
O1 0.1910(3) 0.3544(3) 0.11558(19) 0.0452(4) Uani d . 1 O
O2 0.4131(3) 0.0073(3) 0.15810(18) 0.0411(4) Uani d . 1 O
O3 0.1385(3) 0.2544(3) 0.34345(16) 0.0403(4) Uani d . 1 O
O4 -0.6546(3) 0.3721(3) 0.72894(16) 0.0463(5) Uani d . 1 O
O5 -0.4080(4) 0.4261(3) 0.77740(17) 0.0502(5) Uani d . 1 O
C1 -0.1129(4) 0.1621(3) 0.30800(19) 0.0260(4) Uani d . 1 C
C2 -0.0459(4) 0.2394(3) 0.4011(2) 0.0292(5) Uani d . 1 C
C3 -0.1545(4) 0.3006(3) 0.5306(2) 0.0319(5) Uani d . 1 C
H3 -0.1061 0.3514 0.5898 0.038 Uiso calc R 1 H
C4 -0.3414(4) 0.2821(3) 0.5679(2) 0.0303(5) Uani d . 1 C
C5 -0.4132(4) 0.2036(3) 0.4808(2) 0.0318(5) Uani d . 1 C
H5 -0.5392 0.1930 0.5101 0.038 Uiso calc R 1 H
C6 -0.2979(4) 0.1409(4) 0.3505(2) 0.0304(5) Uani d . 1 C
H6 -0.3437 0.0854 0.2923 0.037 Uiso calc R 1 H
H1A 0.393(6) -0.342(4) -0.085(3) 0.067(10) Uiso d D 1 H
H1B 0.418(6) -0.255(7) 0.012(4) 0.098(15) Uiso d D 1 H
H2A 0.218(3) 0.184(6) -0.126(3) 0.066(11) Uiso d D 1 H
H2B -0.011(5) 0.325(4) -0.114(4) 0.081(13) 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'
N N 0.0061 0.0033 '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'
Co Co 0.3494 0.9721 '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
O1W Co1 O1W . 2 180.00(17) ?
O1W Co1 O2W . . 92.89(8) yes
O1W Co1 O2W 2 . 87.11(8) yes
O1W Co1 O2W . 2 87.11(8) ?
O1W Co1 O2W 2 2 92.89(8) ?
O2W Co1 O2W . 2 180.00(13) ?
O1W Co1 N1 . 2 89.05(7) ?
O1W Co1 N1 2 2 90.95(7) ?
O2W Co1 N1 . 2 88.45(7) ?
O2W Co1 N1 2 2 91.55(7) ?
O1W Co1 N1 . . 90.95(7) yes
O1W Co1 N1 2 . 89.05(7) yes
O2W Co1 N1 . . 91.55(7) yes
O2W Co1 N1 2 . 88.45(7) yes
N1 Co1 N1 2 . 180.00(4) ?
O1 S1 O2 . . 113.98(12) ?
O1 S1 N1 . . 114.63(11) ?
O2 S1 N1 . . 112.83(10) ?
O1 S1 O3 . . 107.65(11) ?
O2 S1 O3 . . 107.14(11) ?
N1 S1 O3 . . 99.09(9) ?
C1 N1 S1 . . 108.29(14) ?
C1 N1 Co1 . . 130.21(15) ?
S1 N1 Co1 . . 121.50(10) ?
O5 N2 O4 . . 122.6(2) ?
O5 N2 C4 . . 118.1(2) ?
O4 N2 C4 . . 119.3(2) ?
Co1 O1W H1A . . 132(3) ?
Co1 O1W H1B . . 133(3) ?
H1A O1W H1B . . 95(4) ?
Co1 O2W H2A . . 121(3) ?
Co1 O2W H2B . . 118(3) ?
H2A O2W H2B . . 118(4) ?
C2 O3 S1 . . 108.07(13) ?
N1 C1 C6 . . 128.66(19) ?
N1 C1 C2 . . 113.05(19) ?
C6 C1 C2 . . 118.27(19) ?
C3 C2 O3 . . 124.28(19) ?
C3 C2 C1 . . 124.2(2) ?
O3 C2 C1 . . 111.46(18) ?
C2 C3 C4 . . 115.60(19) ?
C2 C3 H3 . . 122.2 ?
C4 C3 H3 . . 122.2 ?
C3 C4 C5 . . 122.7(2) ?
C3 C4 N2 . . 118.6(2) ?
C5 C4 N2 . . 118.6(2) ?
C6 C5 C4 . . 120.2(2) ?
C6 C5 H5 . . 119.9 ?
C4 C5 H5 . . 119.9 ?
C5 C6 C1 . . 119.0(2) ?
C5 C6 H6 . . 120.5 ?
C1 C6 H6 . . 120.5 ?
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
Co1 O1W . 2.0713(18) yes
Co1 O1W 2 2.0713(18) ?
Co1 O2W . 2.0951(16) yes
Co1 O2W 2 2.0951(16) ?
Co1 N1 2 2.1653(16) ?
Co1 N1 . 2.1653(16) yes
S1 O1 . 1.4251(18) ?
S1 O2 . 1.428(2) ?
S1 N1 . 1.5958(18) ?
S1 O3 . 1.6270(16) ?
N1 C1 . 1.381(3) ?
N2 O5 . 1.225(3) ?
N2 O4 . 1.227(3) ?
N2 C4 . 1.445(3) ?
O1W H1A . 0.876(18) ?
O1W H1B . 0.88(5) ?
O2W H2A . 0.860(19) ?
O2W H2B . 0.857(19) ?
O3 C2 . 1.385(3) ?
C1 C6 . 1.388(3) ?
C1 C2 . 1.405(3) ?
C2 C3 . 1.364(3) ?
C3 C4 . 1.385(3) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.388(3) ?
C5 C6 . 1.383(3) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
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
O1W H1A O5 1_644 0.88(3) 1.99(3) 2.853(2) 171(4)
O1W H1B O2 . 0.88(5) 2.46(4) 3.031(2) 123(3)
O1W H1B O1 2_655 0.88(5) 2.59(5) 3.141(3) 121(3)
O1W H1B O5 2_556 0.88(5) 2.50(4) 3.020(3) 118(4)
O2W H2A O4 1_654 0.86(3) 2.34(3) 2.908(2) 124(3)
O2W H2A O2 2_655 0.86(3) 2.31(3) 3.109(3) 156(3)
O2W H2B O1 2_565 0.86(3) 2.09(3) 2.927(3) 164(4)
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_site_symmetry_1
_geom_torsion
O1 S1 N1 C1 . -112.54(16)
O2 S1 N1 C1 . 114.77(16)
O3 S1 N1 C1 . 1.74(16)
O1 S1 N1 Co1 . 67.14(15)
O2 S1 N1 Co1 . -65.55(14)
O3 S1 N1 Co1 . -178.58(11)
O1W Co1 N1 C1 . -126.65(19)
O1W Co1 N1 C1 2 53.35(19)
O2W Co1 N1 C1 . 140.43(19)
O2W Co1 N1 C1 2 -39.57(19)
O1W Co1 N1 S1 . 53.74(12)
O1W Co1 N1 S1 2 -126.25(12)
O2W Co1 N1 S1 . -39.17(12)
O2W Co1 N1 S1 2 140.83(12)
O1 S1 O3 C2 . 117.53(17)
O2 S1 O3 C2 . -119.48(16)
N1 S1 O3 C2 . -2.07(17)
S1 N1 C1 C6 . 177.46(19)
Co1 N1 C1 C6 . -2.2(3)
S1 N1 C1 C2 . -0.9(2)
Co1 N1 C1 C2 . 179.45(14)
S1 O3 C2 C3 . -175.52(19)
S1 O3 C2 C1 . 1.7(2)
N1 C1 C2 C3 . 176.7(2)
C6 C1 C2 C3 . -1.9(3)
N1 C1 C2 O3 . -0.6(3)
C6 C1 C2 O3 . -179.12(19)
O3 C2 C3 C4 . 177.0(2)
C1 C2 C3 C4 . 0.1(3)
C2 C3 C4 C5 . 1.0(3)
C2 C3 C4 N2 . -173.76(18)
O5 N2 C4 C3 . -7.4(3)
O4 N2 C4 C3 . 170.9(2)
O5 N2 C4 C5 . 177.6(2)
O4 N2 C4 C5 . -4.1(3)
C3 C4 C5 C6 . -0.4(3)
N2 C4 C5 C6 . 174.40(19)
C4 C5 C6 C1 . -1.4(3)
N1 C1 C6 C5 . -175.9(2)
C2 C1 C6 C5 . 2.4(3)
