#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/50/2235012.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_2235012
loop_
_publ_author_name
'Wang, Bi-Qin'
'Yan, Hai-Biao'
'Fang, Ci-Jun'
'Zhang, Zhi'
_publ_section_title
;
 A new dabco-templated metal sulfate: 1,4-diazoniabicyclo[2.2.2]octane
 hexaaquacadmium bis(sulfate)
;
_journal_coeditor_code           HB6712
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m759
_journal_page_last               m760
_journal_paper_doi               10.1107/S1600536812020089
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C6 H14 N2) [Cd (H2 O)6] (S O4)2'
_chemical_formula_moiety         'C6 H14 N2 2+, Cd H12 O6 2+, 2(O4 S -)'
_chemical_formula_sum            'C6 H26 Cd N2 O14 S2'
_chemical_formula_weight         526.81
_chemical_name_systematic
;
1,4-diazoniabicyclo[2.2.2]octane hexaaquacadmium bis(sulfate)
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.10(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.201(2)
_cell_length_b                   12.461(3)
_cell_length_c                   12.377(3)
_cell_measurement_reflns_used    14955
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      3.18
_cell_volume                     1816.8(7)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 2000)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 2000)'
_computing_data_reduction        'RAPID-AUTO (Rigaku, 2000)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg & Putz, 2005)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating anode target'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17238
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    1.502
_exptl_absorpt_correction_T_max  0.818
_exptl_absorpt_correction_T_min  0.621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(RAPID-AUTO; Rigaku, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.555
_refine_ls_extinction_coef       0.0073(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4123
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0262
_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)+(0.0296P)²+1.2094P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0655
_reflns_number_gt                3872
_reflns_number_total             4123
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb6712.cif
_cod_data_source_block           I
_cod_original_cell_volume        1816.8(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2235012
_cod_database_fobs_code          2235012
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
Cd Cd1 0.762711(12) 0.506501(11) 0.729425(12) 0.02484(7) Uani d . 1 1
O O1 0.69454(15) 0.40460(16) 0.57520(15) 0.0434(4) Uani d D 1 1
H H1A 0.6259(15) 0.386(2) 0.564(3) 0.058(10) Uiso d D 1 1
H H1B 0.729(2) 0.3523(19) 0.556(2) 0.045(8) Uiso d D 1 1
O O2 0.81582(14) 0.59718(14) 0.89279(15) 0.0373(4) Uani d D 1 1
H H2A 0.775(2) 0.651(2) 0.899(3) 0.057(10) Uiso d D 1 1
H H2B 0.8838(14) 0.613(2) 0.917(2) 0.044(8) Uiso d D 1 1
O O3 0.83071(16) 0.62381(18) 0.61663(18) 0.0520(5) Uani d D 1 1
H H3A 0.786(2) 0.654(3) 0.561(2) 0.059(10) Uiso d D 1 1
H H3B 0.8981(15) 0.630(3) 0.616(3) 0.065(10) Uiso d D 1 1
O O4 0.93016(14) 0.42094(14) 0.77884(13) 0.0335(3) Uani d D 1 1
H H4A 0.943(3) 0.394(2) 0.8444(15) 0.054(9) Uiso d D 1 1
H H4B 0.937(3) 0.373(2) 0.734(2) 0.066(11) Uiso d D 1 1
O O5 0.59756(15) 0.59730(15) 0.68221(14) 0.0400(4) Uani d D 1 1
H H5A 0.579(3) 0.646(2) 0.719(2) 0.061(10) Uiso d D 1 1
H H5B 0.583(3) 0.610(3) 0.6150(15) 0.076(12) Uiso d D 1 1
O O6 0.67448(15) 0.38020(13) 0.82049(14) 0.0367(4) Uani d D 1 1
H H6A 0.717(2) 0.341(2) 0.868(2) 0.048(8) Uiso d D 1 1
H H6B 0.6206(18) 0.344(2) 0.782(2) 0.042(8) Uiso d D 1 1
S S1 0.56662(4) 0.75687(4) 0.92161(4) 0.02197(11) Uani d . 1 1
O O7 0.53791(18) 0.66368(15) 0.98053(16) 0.0516(5) Uani d . 1 1
O O8 0.69086(14) 0.76330(15) 0.94054(16) 0.0453(4) Uani d . 1 1
O O9 0.52740(14) 0.85701(13) 0.96289(13) 0.0371(4) Uani d . 1 1
O O10 0.51233(14) 0.74705(12) 0.80082(12) 0.0339(3) Uani d . 1 1
S S2 0.93025(4) 0.25840(4) 0.51135(4) 0.02264(11) Uani d . 1 1
O O11 0.96652(16) 0.34160(17) 0.44445(17) 0.0538(5) Uani d . 1 1
O O12 0.80398(13) 0.25778(14) 0.47823(15) 0.0391(4) Uani d . 1 1
O O13 0.97215(15) 0.28065(14) 0.63040(13) 0.0377(4) Uani d . 1 1
O O14 0.97126(16) 0.15212(15) 0.48799(14) 0.0434(4) Uani d . 1 1
N N1 0.78520(16) 1.05733(14) 0.80199(15) 0.0288(4) Uani d . 1 1
H H1E 0.8228 1.0984 0.8608 0.035 Uiso calc R 1 1
N N2 0.68305(16) 0.94584(14) 0.64165(15) 0.0305(4) Uani d . 1 1
H H2E 0.6453 0.9047 0.5830 0.037 Uiso calc R 1 1
C C1 0.7918(3) 1.1099(3) 0.6964(2) 0.0670(10) Uani d . 1 1
H H1C 0.8706 1.1173 0.6951 0.080 Uiso calc R 1 1
H H1D 0.7586 1.1811 0.6918 0.080 Uiso calc R 1 1
C C2 0.8375(2) 0.9493(2) 0.8128(2) 0.0515(7) Uani d . 1 1
H H2C 0.8310 0.9157 0.8816 0.062 Uiso calc R 1 1
H H2D 0.9174 0.9552 0.8155 0.062 Uiso calc R 1 1
C C3 0.6649(2) 1.0471(2) 0.8051(2) 0.0445(6) Uani d . 1 1
H H3C 0.6304 1.1176 0.8009 0.053 Uiso calc R 1 1
H H3D 0.6608 1.0138 0.8748 0.053 Uiso calc R 1 1
C C4 0.7286(2) 1.0432(2) 0.59765(19) 0.0405(5) Uani d . 1 1
H H4C 0.6669 1.0846 0.5509 0.049 Uiso calc R 1 1
H H4D 0.7795 1.0222 0.5528 0.049 Uiso calc R 1 1
C C5 0.7775(2) 0.8816(2) 0.7136(2) 0.0449(6) Uani d . 1 1
H H5C 0.8305 0.8606 0.6710 0.054 Uiso calc R 1 1
H H5D 0.7476 0.8170 0.7391 0.054 Uiso calc R 1 1
C C6 0.60209(19) 0.97960(19) 0.7075(2) 0.0336(5) Uani d . 1 1
H H6C 0.5703 0.9168 0.7344 0.040 Uiso calc R 1 1
H H6D 0.5403 1.0207 0.6604 0.040 Uiso calc 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'
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
_geom_angle_publ_flag
O4 Cd1 O5 178.14(7) n
O4 Cd1 O2 88.00(7) n
O5 Cd1 O2 90.55(7) n
O4 Cd1 O1 94.12(7) n
O5 Cd1 O1 87.45(7) n
O2 Cd1 O1 172.97(7) n
O4 Cd1 O3 91.17(7) n
O5 Cd1 O3 87.90(7) n
O2 Cd1 O3 99.17(8) n
O1 Cd1 O3 87.50(8) n
O4 Cd1 O6 92.83(6) n
O5 Cd1 O6 88.30(7) n
O2 Cd1 O6 88.06(7) n
O1 Cd1 O6 85.14(7) n
O3 Cd1 O6 171.86(7) n
Cd1 O1 H1A 115(2) ?
Cd1 O1 H1B 125(2) ?
H1A O1 H1B 107(2) ?
Cd1 O2 H2A 116(2) ?
Cd1 O2 H2B 118(2) ?
H2A O2 H2B 110(2) ?
Cd1 O3 H3A 121(2) ?
Cd1 O3 H3B 125(2) ?
H3A O3 H3B 112(2) ?
Cd1 O4 H4A 112(2) ?
Cd1 O4 H4B 114(2) ?
H4A O4 H4B 109(2) ?
Cd1 O5 H5A 126(2) ?
Cd1 O5 H5B 108(3) ?
H5A O5 H5B 114(3) ?
Cd1 O6 H6A 117(2) ?
Cd1 O6 H6B 118.2(19) ?
H6A O6 H6B 110(2) ?
O7 S1 O10 109.72(11) ?
O7 S1 O8 109.51(12) ?
O10 S1 O8 109.72(11) ?
O7 S1 O9 110.97(12) ?
O10 S1 O9 108.73(9) ?
O8 S1 O9 108.17(10) ?
O13 S2 O11 111.06(12) ?
O13 S2 O14 108.84(10) ?
O11 S2 O14 110.96(12) ?
O13 S2 O12 110.22(10) ?
O11 S2 O12 106.95(11) ?
O14 S2 O12 108.79(10) ?
C2 N1 C1 111.1(2) ?
C2 N1 C3 109.0(2) ?
C1 N1 C3 110.0(2) ?
C2 N1 H1E 108.9 ?
C1 N1 H1E 108.9 ?
C3 N1 H1E 108.9 ?
C5 N2 C4 110.5(2) ?
C5 N2 C6 110.05(19) ?
C4 N2 C6 109.35(18) ?
C5 N2 H2E 109.0 ?
C4 N2 H2E 109.0 ?
C6 N2 H2E 109.0 ?
N1 C1 C4 109.6(2) ?
N1 C1 H1C 109.7 ?
C4 C1 H1C 109.7 ?
N1 C1 H1D 109.7 ?
C4 C1 H1D 109.7 ?
H1C C1 H1D 108.2 ?
N1 C2 C5 109.16(19) ?
N1 C2 H2C 109.8 ?
C5 C2 H2C 109.8 ?
N1 C2 H2D 109.8 ?
C5 C2 H2D 109.8 ?
H2C C2 H2D 108.3 ?
N1 C3 C6 109.07(18) ?
N1 C3 H3C 109.9 ?
C6 C3 H3C 109.9 ?
N1 C3 H3D 109.9 ?
C6 C3 H3D 109.9 ?
H3C C3 H3D 108.3 ?
N2 C4 C1 108.13(18) ?
N2 C4 H4C 110.1 ?
C1 C4 H4C 110.1 ?
N2 C4 H4D 110.1 ?
C1 C4 H4D 110.1 ?
H4C C4 H4D 108.4 ?
N2 C5 C2 108.66(19) ?
N2 C5 H5C 110.0 ?
C2 C5 H5C 110.0 ?
N2 C5 H5D 110.0 ?
C2 C5 H5D 110.0 ?
H5C C5 H5D 108.3 ?
N2 C6 C3 108.90(18) ?
N2 C6 H6C 109.9 ?
C3 C6 H6C 109.9 ?
N2 C6 H6D 109.9 ?
C3 C6 H6D 109.9 ?
H6C C6 H6D 108.3 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Cd1 O4 2.2437(16) y
Cd1 O5 2.2514(17) y
Cd1 O2 2.2589(17) y
Cd1 O1 2.2629(17) y
Cd1 O3 2.3189(18) y
Cd1 O6 2.3534(17) y
O1 H1A 0.844(17) ?
O1 H1B 0.847(16) ?
O2 H2A 0.848(17) ?
O2 H2B 0.827(17) ?
O3 H3A 0.844(17) ?
O3 H3B 0.829(17) ?
O4 H4A 0.851(17) ?
O4 H4B 0.838(17) ?
O5 H5A 0.825(17) ?
O5 H5B 0.820(17) ?
O6 H6A 0.833(17) ?
O6 H6B 0.839(16) ?
S1 O7 1.4615(18) ?
S1 O10 1.4740(16) ?
S1 O8 1.4746(17) ?
S1 O9 1.4747(16) ?
S2 O13 1.4550(16) ?
S2 O11 1.4654(18) ?
S2 O14 1.4707(17) ?
S2 O12 1.4875(16) ?
N1 C2 1.481(3) ?
N1 C1 1.483(3) ?
N1 C3 1.484(3) ?
N1 H1E 0.9100 ?
N2 C5 1.493(3) ?
N2 C4 1.496(3) ?
N2 C6 1.496(3) ?
N2 H2E 0.9100 ?
C1 C4 1.512(4) ?
C1 H1C 0.9700 ?
C1 H1D 0.9700 ?
C2 C5 1.512(4) ?
C2 H2C 0.9700 ?
C2 H2D 0.9700 ?
C3 C6 1.507(3) ?
C3 H3C 0.9700 ?
C3 H3D 0.9700 ?
C4 H4C 0.9700 ?
C4 H4D 0.9700 ?
C5 H5C 0.9700 ?
C5 H5D 0.9700 ?
C6 H6C 0.9700 ?
C6 H6D 0.9700 ?
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
O1 H1A O9 2_646 0.844(17) 1.849(17) 2.691(2) 176(3)
O1 H1B O12 . 0.847(16) 1.895(18) 2.721(2) 165(3)
O2 H2A O8 . 0.848(17) 1.888(18) 2.725(2) 169(3)
O2 H2B O14 2_756 0.827(17) 1.916(19) 2.720(3) 164(3)
O3 H3A O8 4_575 0.844(17) 1.934(18) 2.775(3) 174(3)
O3 H3B O11 3_766 0.829(17) 2.01(2) 2.802(3) 159(3)
O4 H4A O14 4_566 0.851(17) 1.816(17) 2.666(2) 176(3)
O4 H4B O13 . 0.838(17) 1.850(18) 2.680(2) 171(3)
O5 H5A O10 . 0.825(17) 1.923(18) 2.741(2) 171(3)
O5 H5B O9 4_575 0.820(17) 1.872(19) 2.686(2) 172(4)
O6 H6A O12 4_566 0.833(17) 1.937(17) 2.767(2) 175(3)
O6 H6B O10 2_646 0.839(16) 2.065(17) 2.902(2) 175(3)
N1 H1E O11 4_576 0.91 1.94 2.749(3) 147
N1 H1E O12 4_576 0.91 2.36 3.140(3) 144
N2 H2E O7 4_575 0.91 1.78 2.671(3) 164
