#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/80/2238086.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_2238086
loop_
_publ_author_name
'Li, Wei-Qi'
_publ_section_title
;
 Poly[[aqua{μ₄-2-[(carboxymethyl)sulfanyl]nicotinato-κ⁴O:O':O'':O'''}copper(II)]
 trihydrate]
;
_journal_coeditor_code           XU5692
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m268
_journal_paper_doi               10.1107/S1600536813009604
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Cu (C8 H5 N O4 S) (H2 O)], 3H2 O'
_chemical_formula_moiety         'C8 H7 Cu N O5 S, 3(H2 O)'
_chemical_formula_sum            'C8 H13 Cu N O8 S'
_chemical_formula_weight         346.82
_chemical_name_systematic
'Poly[[aqua{μ₄-2-[(carboxymethyl)sulfanyl]nicotinato-κ⁴O:O':O'':O'''}copper(II)] trihydrate]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.28(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.940(7)
_cell_length_b                   16.639(9)
_cell_length_c                   7.876(4)
_cell_measurement_reflns_used    3501
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.06
_cell_volume                     1294.8(13)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEXII area-detector'
_diffrn_measurement_method       'ω scans'
_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  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20324
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.882
_exptl_absorpt_correction_T_max  .892
_exptl_absorpt_correction_T_min  .812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             708
_exptl_crystal_size_max          .248
_exptl_crystal_size_mid          .092
_exptl_crystal_size_min          .061
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0315
_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)+(0.0455P)²+0.2317P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0848
_reflns_number_gt                2331
_reflns_number_total             2973
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            xu5692.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2238086
_cod_database_fobs_code          2238086
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_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_symmetry_multiplicity
Cu Cu1 1.10928(3) 0.455426(15) 0.48878(4) 0.02469(11) Uani d . 1 1
S S1 0.96122(7) 0.21713(3) 0.44052(8) 0.03032(16) Uani d . 1 1
O O1 0.97500(18) 0.37850(10) 0.3866(2) 0.0338(4) Uani d . 1 1
O O1W 1.2932(2) 0.39085(12) 0.4498(3) 0.0473(5) Uani d . 1 1
H H1WA 1.2787 0.3469 0.4037 0.057 Uiso d R 1 1
H H1WB 1.3419 0.4141 0.3845 0.057 Uiso d R 1 1
O O2 0.7893(2) 0.45444(10) 0.3972(3) 0.0369(4) Uani d . 1 1
O O3 1.0779(2) 0.08898(11) 0.2128(2) 0.0374(4) Uani d . 1 1
O O4 0.89346(19) 0.01319(10) 0.2319(2) 0.0328(4) Uani d . 1 1
N N1 0.7301(2) 0.17934(12) 0.2526(3) 0.0341(5) Uani d . 1 1
C C1 0.5606(3) 0.27286(16) 0.1366(4) 0.0398(7) Uani d . 1 1
H H1A 0.4768 0.2817 0.0745 0.048 Uiso calc R 1 1
C C2 0.7636(3) 0.32137(14) 0.2965(3) 0.0267(5) Uani d . 1 1
C C3 0.6384(3) 0.33602(16) 0.2060(4) 0.0348(6) Uani d . 1 1
H H3A 0.6068 0.3885 0.1919 0.042 Uiso calc R 1 1
C C4 0.6114(3) 0.19624(16) 0.1627(4) 0.0393(7) Uani d . 1 1
H H4A 0.5600 0.1536 0.1147 0.047 Uiso calc R 1 1
C C5 0.8059(3) 0.24081(14) 0.3179(3) 0.0260(5) Uani d . 1 1
C C6 0.8489(3) 0.38985(13) 0.3664(3) 0.0268(5) Uani d . 1 1
C C7 0.9514(3) 0.10887(14) 0.4500(3) 0.0319(6) Uani d . 1 1
H H7A 1.0178 0.0897 0.5403 0.038 Uiso calc R 1 1
H H7B 0.8626 0.0938 0.4794 0.038 Uiso calc R 1 1
C C8 0.9757(3) 0.06765(14) 0.2838(3) 0.0286(5) Uani d . 1 1
O O2W 0.6123(3) -0.00071(16) 0.2997(4) 0.0759(8) Uani d . 1 1
H H2WA 0.6385 -0.0244 0.3907 0.091 Uiso d R 1 1
H H2WB 0.6774 0.0299 0.2886 0.091 Uiso d R 1 1
O O3W 0.3765(3) 0.07734(18) 0.3764(4) 0.0831(9) Uani d . 1 1
H H3WA 0.3048 0.0589 0.3329 0.100 Uiso d R 1 1
H H3WB 0.4364 0.0491 0.3424 0.100 Uiso d R 1 1
O O4W 0.2538(3) 0.24845(18) 0.2749(5) 0.1001(11) Uani d . 1 1
H H4WA 0.2766 0.2280 0.1881 0.120 Uiso d R 1 1
H H4WB 0.1699 0.2362 0.2691 0.120 Uiso d R 1 1
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'
Cu Cu 0.3201 1.2651 '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'
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
O1 Cu1 O2 . 3_766 167.93(8)
O1 Cu1 O3 . 4_566 87.44(9)
O2 Cu1 O3 3_766 4_566 90.03(9)
O1 Cu1 O4 . 2_755 90.75(9)
O2 Cu1 O4 3_766 2_755 89.31(9)
O3 Cu1 O4 4_566 2_755 168.14(8)
O1 Cu1 O1W . . 99.49(9)
O2 Cu1 O1W 3_766 . 92.56(9)
O3 Cu1 O1W 4_566 . 99.18(9)
O4 Cu1 O1W 2_755 . 92.69(9)
O1 Cu1 Cu1 . 3_766 82.33(7)
O2 Cu1 Cu1 3_766 3_766 85.74(7)
O3 Cu1 Cu1 4_566 3_766 86.50(7)
O4 Cu1 Cu1 2_755 3_766 81.64(7)
O1W Cu1 Cu1 . 3_766 174.09(6)
C5 S1 C7 . . 101.32(12)
C6 O1 Cu1 . . 125.29(16)
Cu1 O1W H1WA . . 113.2
Cu1 O1W H1WB . . 114.3
H1WA O1W H1WB . . 103.0
C6 O2 Cu1 . 3_766 120.56(18)
C8 O3 Cu1 . 4_565 120.36(16)
C8 O4 Cu1 . 2_745 125.43(17)
C4 N1 C5 . . 118.0(2)
C4 C1 C3 . . 117.6(3)
C4 C1 H1A . . 121.2
C3 C1 H1A . . 121.2
C3 C2 C5 . . 117.9(2)
C3 C2 C6 . . 119.9(2)
C5 C2 C6 . . 122.2(2)
C1 C3 C2 . . 120.1(2)
C1 C3 H3A . . 119.9
C2 C3 H3A . . 119.9
N1 C4 C1 . . 124.1(3)
N1 C4 H4A . . 117.9
C1 C4 H4A . . 117.9
N1 C5 C2 . . 122.1(2)
N1 C5 S1 . . 117.35(19)
C2 C5 S1 . . 120.48(19)
O1 C6 O2 . . 125.7(2)
O1 C6 C2 . . 116.7(2)
O2 C6 C2 . . 117.5(2)
C8 C7 S1 . . 113.56(17)
C8 C7 H7A . . 108.9
S1 C7 H7A . . 108.9
C8 C7 H7B . . 108.9
S1 C7 H7B . . 108.9
H7A C7 H7B . . 107.7
O4 C8 O3 . . 125.7(2)
O4 C8 C7 . . 116.5(2)
O3 C8 C7 . . 117.8(2)
H2WA O2W H2WB . . 101.8
H3WA O3W H3WB . . 106.2
H4WA O4W H4WB . . 102.4
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
Cu1 O1 . 1.958(2) y
Cu1 O2 3_766 1.9682(19) y
Cu1 O3 4_566 1.9687(19) y
Cu1 O4 2_755 1.9836(19) y
Cu1 O1W . 2.171(2) y
Cu1 Cu1 3_766 2.6524(15) ?
S1 C5 . 1.773(3) ?
S1 C7 . 1.806(3) ?
O1 C6 . 1.261(3) ?
O1W H1WA . 0.8228 ?
O1W H1WB . 0.8384 ?
O2 C6 . 1.263(3) ?
O2 Cu1 3_766 1.9682(19) ?
O3 C8 . 1.263(3) ?
O3 Cu1 4_565 1.9687(19) ?
O4 C8 . 1.258(3) ?
O4 Cu1 2_745 1.9836(19) ?
N1 C4 . 1.337(4) ?
N1 C5 . 1.340(3) ?
C1 C4 . 1.379(4) ?
C1 C3 . 1.382(4) ?
C1 H1A . 0.9300 ?
C2 C3 . 1.386(4) ?
C2 C5 . 1.410(3) ?
C2 C6 . 1.489(3) ?
C3 H3A . 0.9300 ?
C4 H4A . 0.9300 ?
C7 C8 . 1.521(3) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
O2W H2WA . 0.8345 ?
O2W H2WB . 0.8359 ?
O3W H3WA . 0.8165 ?
O3W H3WB . 0.8253 ?
O4W H4WA . 0.8176 ?
O4W H4WB . 0.8547 ?
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 H1WA O4W 1_655 0.82 1.93 2.747(4) 174
O1W H1WB O2W 2_755 0.84 2.11 2.899(4) 156
O2W H2WA O3W 3_656 0.83 2.05 2.843(5) 157
O2W H2WB O4 . 0.84 2.26 2.911(4) 135
O2W H2WB N1 . 0.84 2.56 3.253(4) 141
O3W H3WA O3 1_455 0.82 2.40 3.110(4) 146
O3W H3WB O2W . 0.83 2.00 2.803(5) 165
O4W H4WB S1 1_455 0.85 2.62 3.356(4) 146
