#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/36/2203699.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_2203699
loop_
_publ_author_name
'Xu, Yanqing'
'Yuan, Daqiang'
'Xu, Ying'
'Bi, Wenhua'
'Zhou, Youfu'
'Hong, Maochun'
_publ_section_title
;
 Diaquabis(4,4'-bipyridine
 N,N'-dioxide-κO)bis(dicyanamido)cadmium(II)
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m713
_journal_page_last               m714
_journal_paper_doi               10.1107/S1600536804010281
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Cd (C2 N3)2 (C10 H8 N2 O2)2 (H2 O)2]'
_chemical_formula_moiety         'C24 H20 Cd N10 O6'
_chemical_formula_sum            'C24 H20 Cd N10 O6'
_chemical_formula_weight         656.90
_chemical_name_systematic
;
Diaquabis(4,4'-bipyridine N,N'-dioxide-\kO)bis(dicyanamido)cadmium(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                70.8680(10)
_cell_angle_beta                 79.068(2)
_cell_angle_gamma                73.184(2)
_cell_formula_units_Z            1
_cell_length_a                   8.2040(9)
_cell_length_b                   8.8500(10)
_cell_length_c                   9.6670(10)
_cell_measurement_reflns_used    2950
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.24
_cell_volume                     631.25(12)
_computing_cell_refinement       'SAINT (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'XPREP in SHELXTL (Siemens, 1994)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Siemens SMART CCD'
_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  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3235
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_T_max  .860
_exptl_absorpt_correction_T_min  .766
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             330
_exptl_crystal_size_max          .21
_exptl_crystal_size_mid          .18
_exptl_crystal_size_min          .16
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.426
_refine_ls_extinction_coef       0.0090(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_gt           0.0335
_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)+(0.0209P)²+1.282P] where P=  (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                2100
_reflns_number_total             2180
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ac6100.cif
_cod_data_source_block           I
_cod_database_code               2203699
_cod_database_fobs_code          2203699
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
Cd1 0.5000 0.5000 0.5000 0.03563(16) Uani d S 1 Cd
O1 0.5724(3) 0.6650(3) 0.2675(3) 0.0423(6) Uani d . 1 O
O2 -0.3421(4) 1.5921(3) -0.1297(3) 0.0476(7) Uani d . 1 O
O3 0.4841(4) 0.3122(4) 0.3851(3) 0.0481(7) Uani d . 1 O
N1 0.4568(3) 0.7990(3) 0.2055(3) 0.0318(6) Uani d . 1 N
N2 -0.2105(4) 1.4713(3) -0.0819(3) 0.0328(6) Uani d . 1 N
N3 0.2217(4) 0.6281(4) 0.4838(4) 0.0523(9) Uani d . 1 N
N4 -0.0815(5) 0.7530(5) 0.5109(5) 0.0749(14) Uani d . 1 N
N5 -0.2548(5) 1.0142(5) 0.3718(4) 0.0617(10) Uani d . 1 N
C1 -0.1977(5) 1.4105(4) 0.0645(4) 0.0358(8) Uani d . 1 C
H1 -0.2815 1.4549 0.1297 0.043 Uiso calc R 1 H
C2 -0.0888(5) 1.4091(4) -0.1766(4) 0.0347(8) Uani d . 1 C
H2 -0.0978 1.4531 -0.2771 0.042 Uiso calc R 1 H
C3 -0.0619(4) 1.2839(4) 0.1173(4) 0.0340(8) Uani d . 1 C
H3 -0.0546 1.2437 0.2182 0.041 Uiso calc R 1 H
C4 0.0494(4) 1.2808(4) -0.1273(4) 0.0347(8) Uani d . 1 C
H4 0.1320 1.2388 -0.1944 0.042 Uiso calc R 1 H
C5 0.0649(4) 1.2144(4) 0.0233(4) 0.0304(7) Uani d . 1 C
C6 0.2069(4) 1.0724(4) 0.0824(4) 0.0299(7) Uani d . 1 C
C7 0.2670(5) 1.0542(4) 0.2134(4) 0.0350(8) Uani d . 1 C
H7 0.2215 1.1349 0.2617 0.042 Uiso calc R 1 H
C8 0.2830(4) 0.9505(4) 0.0121(4) 0.0328(7) Uani d . 1 C
H8 0.2501 0.9609 -0.0782 0.039 Uiso calc R 1 H
C9 0.3923(5) 0.9192(4) 0.2725(4) 0.0374(8) Uani d . 1 C
H9 0.4332 0.9102 0.3590 0.045 Uiso calc R 1 H
C10 0.4064(4) 0.8150(4) 0.0758(4) 0.0332(7) Uani d . 1 C
H10 0.4554 0.7336 0.0287 0.040 Uiso calc R 1 H
C11 0.0819(5) 0.6970(5) 0.4906(4) 0.0381(8) Uani d . 1 C
C12 -0.1649(5) 0.8961(5) 0.4321(4) 0.0456(9) Uani d . 1 C
H3A 0.566(7) 0.234(7) 0.375(6) 0.077(18) Uiso d . 1 H
H3B 0.435(8) 0.348(7) 0.302(7) 0.089(19) Uiso 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'
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
N3 Cd1 N3 2_666 . 180.0
N3 Cd1 O1 2_666 . 89.18(11)
N3 Cd1 O1 . . 90.82(11)
N3 Cd1 O1 2_666 2_666 90.82(11)
N3 Cd1 O1 . 2_666 89.18(11)
O1 Cd1 O1 . 2_666 180.00(12)
N3 Cd1 O3 2_666 2_666 92.20(12)
N3 Cd1 O3 . 2_666 87.80(12)
O1 Cd1 O3 . 2_666 92.92(10)
O1 Cd1 O3 2_666 2_666 87.08(10)
N3 Cd1 O3 2_666 . 87.80(12)
N3 Cd1 O3 . . 92.20(12)
O1 Cd1 O3 . . 87.08(10)
O1 Cd1 O3 2_666 . 92.92(10)
O3 Cd1 O3 2_666 . 180.0000(10)
N1 O1 Cd1 . . 119.01(19)
Cd1 O3 H3A . . 123(4)
Cd1 O3 H3B . . 120(4)
H3A O3 H3B . . 105(5)
O1 N1 C10 . . 119.8(3)
O1 N1 C9 . . 119.7(3)
C10 N1 C9 . . 120.5(3)
O2 N2 C2 . . 120.8(3)
O2 N2 C1 . . 119.1(3)
C2 N2 C1 . . 120.1(3)
C11 N3 Cd1 . . 171.8(3)
C11 N4 C12 . . 123.5(4)
N2 C1 C3 . . 120.3(3)
N2 C1 H1 . . 119.9
C3 C1 H1 . . 119.9
N2 C2 C4 . . 121.2(3)
N2 C2 H2 . . 119.4
C4 C2 H2 . . 119.4
C1 C3 C5 . . 121.4(3)
C1 C3 H3 . . 119.3
C5 C3 H3 . . 119.3
C2 C4 C5 . . 119.9(3)
C2 C4 H4 . . 120.0
C5 C4 H4 . . 120.0
C3 C5 C4 . . 117.1(3)
C3 C5 C6 . . 120.7(3)
C4 C5 C6 . . 122.1(3)
C7 C6 C8 . . 117.3(3)
C7 C6 C5 . . 120.6(3)
C8 C6 C5 . . 122.1(3)
C9 C7 C6 . . 121.0(3)
C9 C7 H7 . . 119.5
C6 C7 H7 . . 119.5
C10 C8 C6 . . 120.2(3)
C10 C8 H8 . . 119.9
C6 C8 H8 . . 119.9
N1 C9 C7 . . 120.2(3)
N1 C9 H9 . . 119.9
C7 C9 H9 . . 119.9
N1 C10 C8 . . 120.7(3)
N1 C10 H10 . . 119.7
C8 C10 H10 . . 119.7
N3 C11 N4 . . 170.9(5)
N5 C12 N4 . . 171.7(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cd1 N3 2_666 2.246(3)
Cd1 N3 . 2.246(3)
Cd1 O1 . 2.320(3)
Cd1 O1 2_666 2.320(3)
Cd1 O3 2_666 2.324(3)
Cd1 O3 . 2.324(3)
O1 N1 . 1.328(3)
O2 N2 . 1.311(4)
O3 H3A . 0.83(6)
O3 H3B . 0.89(6)
N1 C10 . 1.346(4)
N1 C9 . 1.352(4)
N2 C2 . 1.342(4)
N2 C1 . 1.352(4)
N3 C11 . 1.134(5)
N4 C11 . 1.288(5)
N4 C12 . 1.310(5)
N5 C12 . 1.138(5)
C1 C3 . 1.370(5)
C1 H1 . 0.9300
C2 C4 . 1.381(5)
C2 H2 . 0.9300
C3 C5 . 1.387(5)
C3 H3 . 0.9300
C4 C5 . 1.395(5)
C4 H4 . 0.9300
C5 C6 . 1.483(5)
C6 C7 . 1.389(5)
C6 C8 . 1.395(5)
C7 C9 . 1.369(5)
C7 H7 . 0.9300
C8 C10 . 1.376(5)
C8 H8 . 0.9300
C9 H9 . 0.9300
C10 H10 . 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
O3 H3A N5 1_645 0.83(6) 2.08(6) 2.900(6) 171(5)
O3 H3B O2 2_575 0.89(6) 1.82(7) 2.706(4) 176(7)
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
N3 Cd1 O1 N1 2_666 -166.3(2)
N3 Cd1 O1 N1 . 13.7(2)
O3 Cd1 O1 N1 2_666 -74.1(2)
O3 Cd1 O1 N1 . 105.9(2)
Cd1 O1 N1 C10 . -120.6(3)
Cd1 O1 N1 C9 . 60.2(4)
O2 N2 C1 C3 . 179.7(3)
C2 N2 C1 C3 . -0.8(5)
O2 N2 C2 C4 . -179.4(3)
C1 N2 C2 C4 . 1.2(5)
N2 C1 C3 C5 . -0.3(6)
N2 C2 C4 C5 . -0.4(5)
C1 C3 C5 C4 . 0.9(5)
C1 C3 C5 C6 . -177.2(3)
C2 C4 C5 C3 . -0.6(5)
C2 C4 C5 C6 . 177.5(3)
C3 C5 C6 C7 . -31.3(5)
C4 C5 C6 C7 . 150.7(3)
C3 C5 C6 C8 . 147.3(3)
C4 C5 C6 C8 . -30.7(5)
C8 C6 C7 C9 . -1.9(5)
C5 C6 C7 C9 . 176.8(3)
C7 C6 C8 C10 . 3.1(5)
C5 C6 C8 C10 . -175.5(3)
O1 N1 C9 C7 . -176.8(3)
C10 N1 C9 C7 . 4.1(5)
C6 C7 C9 N1 . -1.6(6)
O1 N1 C10 C8 . 178.0(3)
C9 N1 C10 C8 . -2.8(5)
C6 C8 C10 N1 . -0.8(5)
