#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/80/2218098.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_2218098
loop_
_publ_author_name
'Ma, Wei-Wu'
'Yang, Ming-Hua'
_publ_section_title
;Diaquabis(2,5-di-4-pyridyl-1,3,4-thiadiazole-κN²)bis(thiocyanato-κN)copper(II)
 dihydrate
;
_journal_coeditor_code           DN2330
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m630
_journal_paper_doi               10.1107/S1600536808008854
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Cu (N C S)2 (C12 H8 N4 S)2 (H2 O)2], 2H2 O'
_chemical_formula_moiety         'C26 H20 Cu N10 O2 S4, 2(H2 O)'
_chemical_formula_sum            'C26 H24 Cu N10 O4 S4'
_chemical_formula_weight         732.33
_chemical_name_systematic
;
Diaquabis(2,5-di-4-pyridyl-1,3,4-thiadiazole-\kN⁵)bis(thiocyanato-
\kN)copper(II) dihydrate
;
_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                104.629(2)
_cell_angle_beta                 93.067(2)
_cell_angle_gamma                112.228(2)
_cell_formula_units_Z            1
_cell_length_a                   7.0555(11)
_cell_length_b                   8.3034(13)
_cell_length_c                   14.849(2)
_cell_measurement_reflns_used    2692
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      1.44
_cell_volume                     768.3(2)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996), ORTEP-3 for Windows (Farrugia,
1997) and
PLATON (Spek, 2003)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_diffrn_measurement_method       'φ and 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  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0648
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3905
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.44
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.034
_exptl_absorpt_correction_T_max  0.8277
_exptl_absorpt_correction_T_min  0.7605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             375
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.689
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0774P)²+0.6059P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1692
_reflns_number_gt                1794
_reflns_number_total             2692
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            dn2330.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      ' P -1'
_cod_database_code               2218098
_cod_database_fobs_code          2218098
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Cu Cu1 0.5000 1.0000 0.0000 0.0423(3) Uani d S 1
S S1 -0.0367(2) 0.7797(2) 0.40422(10) 0.0484(4) Uani d . 1
S S2 0.7893(2) 0.5558(2) -0.03644(12) 0.0477(4) Uani d . 1
N N1 0.6831(7) 0.8539(6) -0.0062(3) 0.0417(11) Uani d . 1
N N2 0.4011(6) 0.9385(6) 0.1283(3) 0.0349(10) Uani d . 1
N N3 0.3261(7) 0.7924(7) 0.4413(3) 0.0486(13) Uani d . 1
N N4 0.2304(8) 0.7563(7) 0.5165(3) 0.0489(13) Uani d . 1
N N5 -0.3536(8) 0.6276(7) 0.7101(3) 0.0511(13) Uani d . 1
O O1 0.2491(5) 0.7683(5) -0.0897(3) 0.0434(9) Uani d . 1
H H1B 0.1349 0.7366 -0.0728 0.065 Uiso d R 1
H H1C 0.2596 0.6773 -0.1223 0.065 Uiso d R 1
O O2 -0.6718(6) 0.4775(6) 0.8112(3) 0.0586(12) Uani d . 1
H H2B -0.5687 0.5204 0.7880 0.088 Uiso d R 1
H H2C -0.6415 0.4525 0.8582 0.088 Uiso d R 1
C C1 0.7271(8) 0.7310(8) -0.0188(4) 0.0347(12) Uani d . 1
C C2 0.2117(9) 0.9123(8) 0.1465(4) 0.0436(14) Uani d . 1
H H2 0.1223 0.9275 0.1043 0.052 Uiso calc R 1
C C3 0.1394(9) 0.8639(8) 0.2240(4) 0.0455(14) Uani d . 1
H H3 0.0025 0.8407 0.2316 0.055 Uiso calc R 1
C C4 0.2713(8) 0.8505(7) 0.2895(4) 0.0379(13) Uani d . 1
C C5 0.4715(9) 0.8795(8) 0.2725(4) 0.0475(15) Uani d . 1
H H5 0.5660 0.8706 0.3150 0.057 Uiso calc R 1
C C6 0.5266(9) 0.9218(8) 0.1915(4) 0.0432(14) Uani d . 1
H H6 0.6604 0.9397 0.1802 0.052 Uiso calc R 1
C C7 0.2060(8) 0.8066(7) 0.3769(4) 0.0395(13) Uani d . 1
C C8 0.0424(9) 0.7481(8) 0.5080(4) 0.0418(13) Uani d . 1
C C9 -0.0929(8) 0.7148(7) 0.5800(4) 0.0379(13) Uani d . 1
C C10 -0.2927(9) 0.7063(8) 0.5682(4) 0.0442(14) Uani d . 1
H H10 -0.3440 0.7292 0.5160 0.053 Uiso calc R 1
C C11 -0.4144(9) 0.6632(8) 0.6357(4) 0.0495(15) Uani d . 1
H H11 -0.5479 0.6593 0.6276 0.059 Uiso calc R 1
C C12 -0.1584(10) 0.6393(9) 0.7221(4) 0.0559(17) Uani d . 1
H H12 -0.1112 0.6178 0.7757 0.067 Uiso calc R 1
C C13 -0.0248(9) 0.6813(8) 0.6596(4) 0.0497(15) Uani d . 1
H H13 0.1090 0.6871 0.6705 0.060 Uiso calc R 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'
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'
Cu Cu 0.3201 1.2651 '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
N1 Cu1 N1 . 2_675 180.0000(10)
N1 Cu1 O1 . 2_675 89.03(16)
N1 Cu1 O1 2_675 2_675 90.97(16)
N1 Cu1 O1 . . 90.97(16)
N1 Cu1 O1 2_675 . 89.03(17)
O1 Cu1 O1 2_675 . 180.0
N1 Cu1 N2 . . 91.15(17)
N1 Cu1 N2 2_675 . 88.85(17)
O1 Cu1 N2 2_675 . 86.47(15)
O1 Cu1 N2 . . 93.53(15)
N1 Cu1 N2 . 2_675 88.85(17)
N1 Cu1 N2 2_675 2_675 91.15(17)
O1 Cu1 N2 2_675 2_675 93.53(15)
O1 Cu1 N2 . 2_675 86.47(14)
N2 Cu1 N2 . 2_675 180.0(2)
C7 S1 C8 . . 87.1(3)
C1 N1 Cu1 . . 159.4(4)
C6 N2 C2 . . 116.5(5)
C6 N2 Cu1 . . 121.5(4)
C2 N2 Cu1 . . 122.0(3)
C7 N3 N4 . . 112.5(5)
C8 N4 N3 . . 112.8(4)
C11 N5 C12 . . 117.1(5)
Cu1 O1 H1B . . 118.7
Cu1 O1 H1C . . 124.5
H1B O1 H1C . . 108.3
H2B O2 H2C . . 110.6
N1 C1 S2 . . 179.8(5)
N2 C2 C3 . . 123.9(5)
N2 C2 H2 . . 118.0
C3 C2 H2 . . 118.0
C4 C3 C2 . . 119.0(5)
C4 C3 H3 . . 120.5
C2 C3 H3 . . 120.5
C3 C4 C5 . . 118.0(5)
C3 C4 C7 . . 121.8(5)
C5 C4 C7 . . 120.2(5)
C6 C5 C4 . . 118.4(5)
C6 C5 H5 . . 120.8
C4 C5 H5 . . 120.8
N2 C6 C5 . . 124.1(5)
N2 C6 H6 . . 118.0
C5 C6 H6 . . 118.0
N3 C7 C4 . . 124.0(5)
N3 C7 S1 . . 113.8(4)
C4 C7 S1 . . 122.1(4)
N4 C8 C9 . . 123.7(5)
N4 C8 S1 . . 113.7(4)
C9 C8 S1 . . 122.6(4)
C13 C9 C10 . . 118.0(5)
C13 C9 C8 . . 119.9(5)
C10 C9 C8 . . 122.0(5)
C11 C10 C9 . . 118.6(5)
C11 C10 H10 . . 120.7
C9 C10 H10 . . 120.7
N5 C11 C10 . . 124.0(6)
N5 C11 H11 . . 118.0
C10 C11 H11 . . 118.0
N5 C12 C13 . . 123.5(6)
N5 C12 H12 . . 118.2
C13 C12 H12 . . 118.2
C12 C13 C9 . . 118.7(6)
C12 C13 H13 . . 120.6
C9 C13 H13 . . 120.6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cu1 N1 . 2.071(4)
Cu1 N1 2_675 2.071(4)
Cu1 O1 2_675 2.118(4)
Cu1 O1 . 2.118(4)
Cu1 N2 . 2.178(4)
Cu1 N2 2_675 2.178(4)
S1 C7 . 1.725(6)
S1 C8 . 1.726(5)
S2 C1 . 1.638(6)
N1 C1 . 1.150(7)
N2 C6 . 1.324(7)
N2 C2 . 1.325(7)
N3 C7 . 1.301(7)
N3 N4 . 1.375(6)
N4 C8 . 1.300(7)
N5 C11 . 1.305(7)
N5 C12 . 1.342(8)
O1 H1B . 0.8214
O1 H1C . 0.8200
O2 H2B . 0.8172
O2 H2C . 0.8159
C2 C3 . 1.372(8)
C2 H2 . 0.9300
C3 C4 . 1.365(8)
C3 H3 . 0.9300
C4 C5 . 1.388(8)
C4 C7 . 1.485(7)
C5 C6 . 1.372(7)
C5 H5 . 0.9300
C6 H6 . 0.9300
C8 C9 . 1.479(7)
C9 C13 . 1.382(7)
C9 C10 . 1.384(7)
C10 C11 . 1.382(8)
C10 H10 . 0.9300
C11 H11 . 0.9300
C12 C13 . 1.372(8)
C12 H12 . 0.9300
C13 H13 . 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
O2 H2B N5 . 0.82 2.03 2.835(6) 168.5
O2 H2C S2 2_566 0.82 2.90 3.541(4) 136.6
O1 H1B S2 1_455 0.82 2.50 3.303(4) 164.3
O1 H1C O2 1_654 0.82 1.95 2.761(6) 171.1
