#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/28/2212848.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_2212848
loop_
_publ_author_name
'Zhao-Xun Lian'
'Hao-Hong Li'
_publ_section_title
;Bis(N,N',N''-diethylenetriamine-κ³N)cadmium(II)
 naphthalene-1,5-disulfonate
;
_journal_coeditor_code           DN2133
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m939
_journal_page_last               m941
_journal_paper_doi               10.1107/S1600536807009191
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Cd (C4 H13 N3)2] (C10 H6 O6 S2)'
_chemical_formula_moiety         'C8 H26 Cd N6 2+, C10 H6 O6 S2 2-'
_chemical_formula_sum            'C18 H32 Cd N6 O6 S2'
_chemical_formula_weight         605.02
_chemical_name_systematic
;Bis(N,N',N''-diethylenetriamine-κ³N)cadmium(II)
 naphthalene-1,5-disulfonate
;
_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
_cell_angle_alpha                110.732(3)
_cell_angle_beta                 90.730(2)
_cell_angle_gamma                116.218(2)
_cell_formula_units_Z            1
_cell_length_a                   8.06750(10)
_cell_length_b                   8.89070(10)
_cell_length_c                   9.9507(2)
_cell_measurement_reflns_used    4029
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     586.54(3)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and SHELXTL (Bruker, 1997)'
_computing_publication_material
;
SHELXL97,  enCIFer (Allen et al.,  2004) and publCIF (Westrip,
2007)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4209
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         4.22
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.157
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_correction_T_min  0.674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             310
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.720
_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     151
_refine_ls_number_reflns         3217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0284
_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)+(0.0548P)²+0.0328P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0787
_reflns_number_gt                2994
_reflns_number_total             3217
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            dn2133.cif
_cod_data_source_block           I
_cod_database_code               2212848
_cod_database_fobs_code          2212848
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 Cd1 0.5000 0.5000 0.5000 0.03225(8) Uani d S 1
S S1 0.79889(6) 0.06124(6) 0.30487(4) 0.02934(10) Uani d . 1
O O1 0.6051(2) -0.0563(3) 0.22474(18) 0.0479(4) Uani d . 1
O O2 0.8362(2) 0.0263(2) 0.43086(16) 0.0442(3) Uani d . 1
O O3 0.8623(3) 0.2542(2) 0.34146(18) 0.0479(4) Uani d . 1
N N1 0.5468(3) 0.2702(3) 0.5332(2) 0.0463(4) Uani d . 1
H H1A 0.4431 0.1918 0.5529 0.056 Uiso calc R 1
H H1B 0.5756 0.2072 0.4528 0.056 Uiso calc R 1
N N2 0.6091(2) 0.6136(2) 0.75636(19) 0.0391(4) Uani d . 1
H H2 0.7138 0.7247 0.7850 0.047 Uiso calc R 1
N N3 0.2194(2) 0.4244(3) 0.60111(19) 0.0406(4) Uani d . 1
H H3A 0.1631 0.4876 0.5890 0.049 Uiso calc R 1
H H3B 0.1381 0.3042 0.5538 0.049 Uiso calc R 1
C C1 0.7060(4) 0.3729(4) 0.6593(3) 0.0579(7) Uani d . 1
H H1C 0.8181 0.4506 0.6335 0.070 Uiso calc R 1
H H1D 0.7314 0.2879 0.6841 0.070 Uiso calc R 1
C C2 0.6610(4) 0.4894(4) 0.7908(3) 0.0543(6) Uani d . 1
H H2A 0.5575 0.4103 0.8229 0.065 Uiso calc R 1
H H2B 0.7700 0.5613 0.8708 0.065 Uiso calc R 1
C C3 0.4594(3) 0.6397(3) 0.8277(2) 0.0471(5) Uani d . 1
H H3C 0.4542 0.7431 0.8194 0.057 Uiso calc R 1
H H3D 0.4885 0.6668 0.9311 0.057 Uiso calc R 1
C C4 0.2681(3) 0.4690(3) 0.7573(2) 0.0445(5) Uani d . 1
H H4A 0.2715 0.3668 0.7694 0.053 Uiso calc R 1
H H4B 0.1721 0.4894 0.8062 0.053 Uiso calc R 1
C C5 0.9428(2) 0.0049(2) 0.18365(17) 0.0236(3) Uani d . 1
C C6 0.9397(2) 0.0218(2) 0.04607(17) 0.0230(3) Uani d . 1
C C7 1.0603(2) -0.0505(2) 0.22731(18) 0.0284(3) Uani d . 1
H H7 1.0621 -0.0592 0.3177 0.034 Uiso calc R 1
C C8 1.1782(3) -0.0943(3) 0.1354(2) 0.0319(3) Uani d . 1
H H8 1.2567 -0.1327 0.1654 0.038 Uiso calc R 1
C C9 1.1782(2) -0.0809(2) 0.00269(19) 0.0280(3) Uani d . 1
H H9 1.2565 -0.1107 -0.0566 0.034 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'
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
N1 Cd1 N2 2_666 . 104.96(7)
N1 Cd1 N2 . . 75.04(7)
N1 Cd1 N3 2_666 2_666 92.70(7)
N1 Cd1 N3 . 2_666 87.30(6)
N2 Cd1 N3 . 2_666 104.99(6)
N1 Cd1 N3 . . 92.70(6)
N2 Cd1 N3 . . 75.01(6)
O1 S1 O2 . . 112.82(10)
O1 S1 O3 . . 113.14(11)
O2 S1 O3 . . 112.61(10)
O1 S1 C5 . . 106.62(9)
O2 S1 C5 . . 105.82(8)
O3 S1 C5 . . 105.04(8)
C1 N1 Cd1 . . 103.83(14)
C1 N1 H1A . . 111.0
Cd1 N1 H1A . . 111.0
C1 N1 H1B . . 111.0
Cd1 N1 H1B . . 111.0
H1A N1 H1B . . 109.0
C3 N2 C2 . . 114.43(19)
C3 N2 Cd1 . . 106.59(13)
C2 N2 Cd1 . . 110.47(14)
C3 N2 H2 . . 108.4
C2 N2 H2 . . 108.4
Cd1 N2 H2 . . 108.4
C4 N3 Cd1 . . 109.79(13)
C4 N3 H3A . . 109.7
Cd1 N3 H3A . . 109.7
C4 N3 H3B . . 109.7
Cd1 N3 H3B . . 109.7
H3A N3 H3B . . 108.2
N1 C1 C2 . . 110.43(18)
N1 C1 H1C . . 109.6
C2 C1 H1C . . 109.6
N1 C1 H1D . . 109.6
C2 C1 H1D . . 109.6
H1C C1 H1D . . 108.1
N2 C2 C1 . . 111.93(18)
N2 C2 H2A . . 109.2
C1 C2 H2A . . 109.2
N2 C2 H2B . . 109.2
C1 C2 H2B . . 109.2
H2A C2 H2B . . 107.9
N2 C3 C4 . . 111.01(18)
N2 C3 H3C . . 109.4
C4 C3 H3C . . 109.4
N2 C3 H3D . . 109.4
C4 C3 H3D . . 109.4
H3C C3 H3D . . 108.0
N3 C4 C3 . . 110.89(17)
N3 C4 H4A . . 109.5
C3 C4 H4A . . 109.5
N3 C4 H4B . . 109.5
C3 C4 H4B . . 109.5
H4A C4 H4B . . 108.0
C7 C5 C6 . . 120.85(14)
C7 C5 S1 . . 118.32(12)
C6 C5 S1 . . 120.81(11)
C9 C6 C6 2_755 2_755 118.63(18)
C9 C6 C5 2_755 . 122.68(14)
C6 C6 C5 2_755 . 118.69(17)
C5 C7 C8 . . 120.15(15)
C5 C7 H7 . . 119.9
C8 C7 H7 . . 119.9
C9 C8 C7 . . 120.65(15)
C9 C8 H8 . . 119.7
C7 C8 H8 . . 119.7
C8 C9 C6 . 2_755 121.03(15)
C8 C9 H9 . . 119.5
C6 C9 H9 2_755 . 119.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cd1 N1 . 2.3623(18)
Cd1 N2 . 2.3739(17)
Cd1 N3 . 2.4043(17)
S1 O1 . 1.4513(15)
S1 O2 . 1.4519(15)
S1 O3 . 1.4544(16)
S1 C5 . 1.7822(16)
N1 C1 . 1.474(4)
N1 H1A . 0.9000
N1 H1B . 0.9000
N2 C3 . 1.473(3)
N2 C2 . 1.478(3)
N2 H2 . 0.9100
N3 C4 . 1.462(3)
N3 H3A . 0.9000
N3 H3B . 0.9000
C1 C2 . 1.517(4)
C1 H1C . 0.9700
C1 H1D . 0.9700
C2 H2A . 0.9700
C2 H2B . 0.9700
C3 C4 . 1.525(3)
C3 H3C . 0.9700
C3 H3D . 0.9700
C4 H4A . 0.9700
C4 H4B . 0.9700
C5 C7 . 1.372(2)
C5 C6 . 1.430(2)
C6 C9 2_755 1.423(2)
C6 C6 2_755 1.428(3)
C7 C8 . 1.411(2)
C7 H7 . 0.9300
C8 C9 . 1.368(2)
C8 H8 . 0.9300
C9 H9 . 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
N1 H1A O2 2_656 0.90 2.29 3.181(3) 172.2
N1 H1B O3 . 0.90 2.51 3.223(2) 136.8
N3 H3A O3 2_666 0.90 2.25 3.073(2) 151.1
N3 H3B O2 1_455 0.90 2.45 3.303(2) 158.3
