#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/44/2214457.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_2214457
loop_
_publ_author_name
'Guang-Hua Chen'
'Yuan-Yuan Lin'
'Yan-Ping Yu'
'Bing-Xin Liu'
_publ_section_title
;Di-μ₂-aqua-bis[aqua(2,2'-diamino-4,4'-bi-1,3-thiazole-κ²N,N')(4-nitrobenzoato-κO)cadmium(II)]
 bis(4-nitrobenzoate)
;
_journal_coeditor_code           XU2275
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1915
_journal_page_last               m1916
_journal_paper_doi               10.1107/S1600536807028462
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'[Cd2 (C7 H4 N O4)2 (C6 H10 N4 O2 S2)2] (C7 H4 N O4)2'
_chemical_formula_moiety         'C26 H28 Cd2 N10 O12 S4 2+ , 2C7 H4 N O4 -'
_chemical_formula_sum            'C40 H36 Cd2 N12 O20 S4'
_chemical_formula_weight         1357.85
_chemical_name_systematic
;
Di-μ₂-aqua-bis[aqua(2,2'-diamino-4,4'-bi-1,3-thiazole-κ²N,N')(4-
nitrobenzoato-\kO)cadmium(II)] bis(4-nitrobenzoate)
;
_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           SHELXL97
_cell_angle_alpha                97.7410(10)
_cell_angle_beta                 102.6000(10)
_cell_angle_gamma                100.8170(10)
_cell_formula_units_Z            1
_cell_length_a                   7.6045(10)
_cell_length_b                   10.7869(14)
_cell_length_c                   16.118(2)
_cell_measurement_reflns_used    4280
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      1.96
_cell_volume                     1245.9(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction
'CrystalStructure (Rigaku/MSC and Rigaku, 2002)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al.,  1993)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_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  0.019
_diffrn_reflns_av_sigmaI/netI    0.039
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6467
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.9
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.112
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.40
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.039
_refine_ls_R_factor_gt           0.032
_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)+(0.027P)²+0.7682P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.067
_refine_ls_wR_factor_ref         0.072
_reflns_number_gt                3751
_reflns_number_total             4310
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            xu2275.cif
_cod_data_source_block           I
_cod_database_code               2214457
_cod_database_fobs_code          2214457
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
Cd Cd 0.57818(3) 0.34675(2) 0.481336(15) 0.03068(9) Uani d . 1
O O1 0.6890(3) 0.56396(19) 0.52648(14) 0.0318(5) Uani d . 1
H H1A 0.7300 0.5938 0.4877 0.050 Uiso d R 1
H H1B 0.7772 0.5890 0.5750 0.050 Uiso d R 1
O O2 0.8663(3) 0.3128(2) 0.50161(16) 0.0460(6) Uani d . 1
H H2A 0.9032 0.2898 0.4578 0.050 Uiso d R 1
H H2B 0.9550 0.3491 0.5432 0.050 Uiso d R 1
O O21 0.5914(3) 0.3862(2) 0.34503(14) 0.0425(6) Uani d . 1
O O22 0.7996(3) 0.5726(2) 0.38119(14) 0.0419(6) Uani d . 1
O O23 0.8204(5) 0.5367(3) -0.0475(2) 0.0797(10) Uani d . 1
O O24 0.6407(6) 0.3528(4) -0.0772(2) 0.0953(12) Uani d . 1
O O31 1.1054(3) 0.3710(2) 0.32199(15) 0.0488(7) Uani d . 1
O O32 0.9237(4) 0.2072(2) 0.35451(16) 0.0506(7) Uani d . 1
O O33 0.6588(5) -0.0802(4) -0.0749(2) 0.0964(13) Uani d . 1
O O34 0.8323(6) 0.0790(4) -0.1054(2) 0.0932(12) Uani d . 1
N N11 0.3961(4) 0.1488(2) 0.42375(17) 0.0316(6) Uani d . 1
N N12 0.3833(5) 0.1243(3) 0.27703(19) 0.0543(9) Uani d . 1
H H12A 0.3311 0.0815 0.2257 0.050 Uiso d R 1
H H12B 0.4630 0.1992 0.2858 0.050 Uiso d R 1
N N13 0.5098(3) 0.2598(2) 0.59931(16) 0.0301(6) Uani d . 1
N N14 0.6762(4) 0.4014(3) 0.72924(18) 0.0460(8) Uani d . 1
H H14A 0.6824 0.4245 0.7832 0.050 Uiso d R 1
H H14B 0.7225 0.4557 0.7000 0.050 Uiso d R 1
N N21 0.7267(5) 0.4480(4) -0.0264(2) 0.0540(9) Uani d . 1
N N31 0.7664(6) 0.0236(4) -0.0541(2) 0.0660(11) Uani d . 1
S S11 0.16984(14) -0.05631(9) 0.33490(6) 0.0464(2) Uani d . 1
S S12 0.44067(14) 0.18707(9) 0.73631(6) 0.0455(2) Uani d . 1
C C11 0.3181(4) 0.0854(3) 0.4812(2) 0.0321(8) Uani d . 1
C C12 0.1944(5) -0.0249(3) 0.4448(2) 0.0436(9) Uani d . 1
H H12 0.1305 -0.0774 0.4749 0.052 Uiso calc R 1
C C13 0.3308(5) 0.0853(3) 0.3445(2) 0.0358(8) Uani d . 1
C C14 0.3819(4) 0.1423(3) 0.5736(2) 0.0320(8) Uani d . 1
C C15 0.3295(5) 0.0901(3) 0.6382(2) 0.0424(9) Uani d . 1
H H15 0.2450 0.0125 0.6308 0.051 Uiso calc R 1
C C16 0.5543(5) 0.2946(3) 0.6835(2) 0.0314(7) Uani d . 1
C C21 0.7022(4) 0.4717(3) 0.2335(2) 0.0315(7) Uani d . 1
C C22 0.8271(5) 0.5632(3) 0.2099(2) 0.0427(9) Uani d . 1
H H22 0.9064 0.6296 0.2520 0.051 Uiso calc R 1
C C23 0.8349(5) 0.5569(4) 0.1256(2) 0.0483(10) Uani d . 1
H H23 0.9192 0.6181 0.1100 0.058 Uiso calc R 1
C C24 0.7163(5) 0.4590(4) 0.0644(2) 0.0409(9) Uani d . 1
C C25 0.5894(5) 0.3676(4) 0.0844(2) 0.0462(10) Uani d . 1
H H25 0.5103 0.3019 0.0418 0.055 Uiso calc R 1
C C26 0.5824(5) 0.3758(4) 0.1701(2) 0.0436(9) Uani d . 1
H H26 0.4955 0.3157 0.1851 0.052 Uiso calc R 1
C C27 0.6992(5) 0.4782(3) 0.3278(2) 0.0339(8) Uani d . 1
C C31 0.9354(5) 0.2001(3) 0.2088(2) 0.0357(8) Uani d . 1
C C32 1.0135(5) 0.2538(4) 0.1488(2) 0.0475(10) Uani d . 1
H H32 1.1044 0.3294 0.1666 0.057 Uiso calc R 1
C C33 0.9584(6) 0.1967(4) 0.0623(3) 0.0544(11) Uani d . 1
H H33 1.0099 0.2339 0.0218 0.065 Uiso calc R 1
C C34 0.8269(6) 0.0847(4) 0.0378(2) 0.0492(10) Uani d . 1
C C35 0.7478(6) 0.0278(4) 0.0956(3) 0.0634(12) Uani d . 1
H H35 0.6596 -0.0492 0.0777 0.076 Uiso calc R 1
C C36 0.8020(6) 0.0875(4) 0.1808(3) 0.0554(11) Uani d . 1
H H36 0.7471 0.0511 0.2207 0.067 Uiso calc R 1
C C37 0.9909(5) 0.2639(3) 0.3028(2) 0.0368(8) Uani d . 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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
O2 Cd N11 . . 103.40(9) ?
O2 Cd O1 . . 91.73(8) ?
N11 Cd O1 . . 164.40(8) ?
O2 Cd O21 . . 88.97(9) ?
N11 Cd O21 . . 90.87(9) ?
O1 Cd O21 . . 85.56(8) ?
O2 Cd N13 . . 96.10(9) ?
N11 Cd N13 . . 74.66(9) ?
O1 Cd N13 . . 107.87(8) ?
O21 Cd N13 . . 165.41(9) ?
O2 Cd O1 . 2_666 166.01(8) ?
N11 Cd O1 . 2_666 90.59(8) ?
O1 Cd O1 . 2_666 74.30(8) ?
O21 Cd O1 . 2_666 90.54(8) ?
N13 Cd O1 . 2_666 87.80(8) ?
Cd O1 Cd . 2_666 105.70(8) y
Cd O1 H1A . . 108.5 ?
Cd O1 H1A 2_666 . 100.5 ?
Cd O1 H1B . . 116.5 ?
Cd O1 H1B 2_666 . 116.7 ?
H1A O1 H1B . . 107.5 ?
Cd O2 H2A . . 118.1 ?
Cd O2 H2B . . 125.5 ?
H2A O2 H2B . . 110.8 ?
C27 O21 Cd . . 126.5(2) ?
C13 N11 C11 . . 111.2(3) ?
C13 N11 Cd . . 133.0(2) ?
C11 N11 Cd . . 115.3(2) ?
C13 N12 H12A . . 119.8 ?
C13 N12 H12B . . 118.4 ?
H12A N12 H12B . . 121.4 ?
C16 N13 C14 . . 110.8(3) ?
C16 N13 Cd . . 136.9(2) ?
C14 N13 Cd . . 112.3(2) ?
C16 N14 H14A . . 119.9 ?
C16 N14 H14B . . 117.0 ?
H14A N14 H14B . . 120.8 ?
O24 N21 O23 . . 122.2(4) ?
O24 N21 C24 . . 119.1(4) ?
O23 N21 C24 . . 118.6(4) ?
O33 N31 O34 . . 123.3(4) ?
O33 N31 C34 . . 118.8(4) ?
O34 N31 C34 . . 117.8(4) ?
C12 S11 C13 . . 89.26(17) ?
C15 S12 C16 . . 89.57(16) ?
C12 C11 N11 . . 114.9(3) ?
C12 C11 C14 . . 127.1(3) ?
N11 C11 C14 . . 118.0(3) ?
C11 C12 S11 . . 110.8(3) ?
C11 C12 H12 . . 124.6 ?
S11 C12 H12 . . 124.6 ?
N11 C13 N12 . . 123.5(3) ?
N11 C13 S11 . . 113.9(3) ?
N12 C13 S11 . . 122.6(3) ?
C15 C14 N13 . . 115.3(3) ?
C15 C14 C11 . . 125.7(3) ?
N13 C14 C11 . . 118.9(3) ?
C14 C15 S12 . . 110.4(3) ?
C14 C15 H15 . . 124.8 ?
S12 C15 H15 . . 124.8 ?
N13 C16 N14 . . 125.9(3) ?
N13 C16 S12 . . 113.9(2) ?
N14 C16 S12 . . 120.1(2) ?
C26 C21 C22 . . 118.9(3) ?
C26 C21 C27 . . 121.0(3) ?
C22 C21 C27 . . 120.0(3) ?
C23 C22 C21 . . 120.8(3) ?
C23 C22 H22 . . 119.6 ?
C21 C22 H22 . . 119.6 ?
C22 C23 C24 . . 118.8(3) ?
C22 C23 H23 . . 120.6 ?
C24 C23 H23 . . 120.6 ?
C25 C24 C23 . . 122.5(3) ?
C25 C24 N21 . . 117.9(3) ?
C23 C24 N21 . . 119.7(3) ?
C24 C25 C26 . . 118.0(3) ?
C24 C25 H25 . . 121.0 ?
C26 C25 H25 . . 121.0 ?
C21 C26 C25 . . 120.9(3) ?
C21 C26 H26 . . 119.5 ?
C25 C26 H26 . . 119.5 ?
O22 C27 O21 . . 125.5(3) ?
O22 C27 C21 . . 118.2(3) ?
O21 C27 C21 . . 116.4(3) ?
C32 C31 C36 . . 118.4(3) ?
C32 C31 C37 . . 121.1(3) ?
C36 C31 C37 . . 120.4(3) ?
C31 C32 C33 . . 120.9(3) ?
C31 C32 H32 . . 119.6 ?
C33 C32 H32 . . 119.6 ?
C34 C33 C32 . . 118.6(4) ?
C34 C33 H33 . . 120.7 ?
C32 C33 H33 . . 120.7 ?
C33 C34 C35 . . 122.2(4) ?
C33 C34 N31 . . 119.0(4) ?
C35 C34 N31 . . 118.8(4) ?
C34 C35 C36 . . 118.2(4) ?
C34 C35 H35 . . 120.9 ?
C36 C35 H35 . . 120.9 ?
C35 C36 C31 . . 121.7(4) ?
C35 C36 H36 . . 119.1 ?
C31 C36 H36 . . 119.1 ?
O32 C37 O31 . . 125.6(3) ?
O32 C37 C31 . . 118.0(3) ?
O31 C37 C31 . . 116.3(3) ?
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
Cd O1 . 2.294(2) y
Cd O1 2_666 2.393(2) y
Cd O2 . 2.250(2) y
Cd O21 . 2.313(2) y
Cd N11 . 2.266(3) y
Cd N13 . 2.344(2) y
O1 H1A . 0.8319 ?
O1 H1B . 0.8843 ?
O2 H2A . 0.8386 ?
O2 H2B . 0.8316 ?
O21 C27 . 1.267(4) ?
O22 C27 . 1.244(4) ?
O23 N21 . 1.216(4) ?
O24 N21 . 1.200(4) ?
O31 C37 . 1.263(4) ?
O32 C37 . 1.239(4) ?
O33 N31 . 1.213(5) ?
O34 N31 . 1.223(5) ?
N11 C13 . 1.306(4) ?
N11 C11 . 1.391(4) ?
N12 C13 . 1.331(4) ?
N12 H12A . 0.8599 ?
N12 H12B . 0.8876 ?
N13 C16 . 1.309(4) ?
N13 C14 . 1.395(4) ?
N14 C16 . 1.342(4) ?
N14 H14A . 0.8607 ?
N14 H14B . 0.8708 ?
N21 C24 . 1.473(4) ?
N31 C34 . 1.472(5) ?
S11 C12 . 1.720(4) ?
S11 C13 . 1.734(3) ?
S12 C15 . 1.717(4) ?
S12 C16 . 1.740(3) ?
C11 C12 . 1.340(5) ?
C11 C14 . 1.468(5) ?
C12 H12 . 0.9300 ?
C14 C15 . 1.347(5) ?
C15 H15 . 0.9300 ?
C21 C26 . 1.379(5) ?
C21 C22 . 1.388(5) ?
C21 C27 . 1.516(4) ?
C22 C23 . 1.367(5) ?
C22 H22 . 0.9300 ?
C23 C24 . 1.370(5) ?
C23 H23 . 0.9300 ?
C24 C25 . 1.368(5) ?
C25 C26 . 1.386(5) ?
C25 H25 . 0.9300 ?
C26 H26 . 0.9300 ?
C31 C32 . 1.377(5) ?
C31 C36 . 1.377(5) ?
C31 C37 . 1.510(5) ?
C32 C33 . 1.383(5) ?
C32 H32 . 0.9300 ?
C33 C34 . 1.365(5) ?
C33 H33 . 0.9300 ?
C34 C35 . 1.366(6) ?
C35 C36 . 1.374(5) ?
C35 H35 . 0.9300 ?
C36 H36 . 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
_geom_hbond_publ_flag
O1 H1A O22 . 0.83 1.90 2.662(3) 151 y
O1 H1B O31 2_766 0.88 1.66 2.522(3) 164 y
O2 H2A O32 . 0.84 1.83 2.650(4) 164 y
O2 H2B O22 2_766 0.83 1.95 2.766(3) 165 y
N12 H12A O33 2_655 0.86 2.45 3.164(4) 141 y
N12 H12A O34 2_655 0.86 2.35 3.192(5) 165 y
N12 H12B O21 . 0.89 2.07 2.901(4) 156 y
N14 H14A O24 1_556 0.86 2.54 3.292(4) 147 y
N14 H14B O31 2_766 0.87 2.19 3.014(4) 158 y
