#------------------------------------------------------------------------------
#$Date: 2017-03-27 08:13:23 +0300 (Mon, 27 Mar 2017) $
#$Revision: 194538 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/23/93/2239331.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_2239331
loop_
_publ_author_name
'Ben Rhaiem, Tarek'
'Boughzala, Habib'
_publ_section_title
;
 1,4-Diazoniabicyclo[2.2.2]octane tetrachloridocadmate(II) monohydrate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m178
_journal_paper_doi               10.1107/S1600536814007533
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '(C6 H14 N2) [Cd Cl4] , H2 O'
_chemical_formula_moiety         'C6 H14 N2, Cd Cl4, H2 O'
_chemical_formula_sum            'C6 H16 Cd Cl4 N2 O'
_chemical_formula_weight         386.40
_chemical_name_common
;
1,4-Diazoniabicyclo[2.2.2]octane tetrachloridocadmate(II) monohydrate
;
_chemical_name_systematic
;
1,4-Diazoniabicyclo[2.2.2]octane tetrachloridocadmate(II) monohydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.528(5)
_cell_length_b                   11.653(2)
_cell_length_c                   13.114(6)
_cell_measurement_reflns_used    2837
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2.4
_cell_volume                     1303.2(10)
_computing_cell_refinement       'CAD-4 EXPRESS (Duisenberg, 1992)'
_computing_data_collection       'CAD-4 EXPRESS (Duisenberg, 1992)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_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  0.0747
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5639
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.468
_exptl_absorpt_correction_T_max  0.5357
_exptl_absorpt_correction_T_min  0.2834
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
(North et al. (1968)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.581
_refine_diff_density_min         -1.439
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2837
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0480
_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)+(0.0587P)²+1.6133P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1338
_reflns_number_gt                2632
_reflns_number_total             2837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ds2238sup1.cf
_cod_data_source_block           I
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-03-27
;
_cod_database_code               2239331
_cod_database_fobs_code          2239331
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -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
_atom_site_attached_hydrogens
Cd Cd 0.74636(5) 0.52500(4) 0.50315(3) 0.04606(17) Uani d . 1 1 0
Cl Cl1 0.52000(18) 0.40196(13) 0.46103(13) 0.0465(3) Uani d . 1 1 0
Cl Cl2 0.7583(2) 0.53068(14) 0.69230(11) 0.0544(4) Uani d . 1 1 0
Cl Cl3 0.9940(2) 0.43346(15) 0.46078(15) 0.0557(4) Uani d . 1 1 0
Cl Cl4 0.6884(2) 0.71103(15) 0.41831(12) 0.0542(4) Uani d . 1 1 0
C C1 0.4091(7) 0.6836(5) 0.2060(5) 0.0457(13) Uani d . 1 1 0
H H1A 0.498(5) 0.6620(12) 0.153(3) 0.055 Uiso calc R 1 1 0
H H1B 0.4419(18) 0.761(4) 0.2435(19) 0.055 Uiso calc R 1 1 0
C C2 0.2540(8) 0.6998(6) 0.1512(5) 0.0514(13) Uani d . 1 1 0
H H2A 0.2282(17) 0.776(5) 0.1496(5) 0.062 Uiso calc R 1 1 0
H H2B 0.2617(9) 0.6741(16) 0.086(4) 0.062 Uiso calc R 1 1 0
C C3 0.2824(8) 0.6248(7) 0.3636(6) 0.0583(18) Uani d D 1 1 0
H H3A 0.3266(11) 0.6796(11) 0.4005(8) 0.070 Uiso calc RD 1 1 0
H H3B 0.2613(9) 0.5660(12) 0.4042(9) 0.070 Uiso calc RD 1 1 0
C C4 0.1319(9) 0.6690(6) 0.3149(6) 0.065(2) Uani d D 1 1 0
H H4A 0.0481(16) 0.6394(8) 0.3470(8) 0.078 Uiso calc RD 1 1 0
H H4B 0.1274(9) 0.7458(14) 0.3198(7) 0.078 Uiso calc RD 1 1 0
C C5 0.3284(9) 0.4857(5) 0.2294(6) 0.0519(16) Uani d D 1 1 0
H H5A 0.3330(9) 0.4244(11) 0.2713(9) 0.062 Uiso calc RD 1 1 0
H H5B 0.3874(13) 0.4708(6) 0.1738(11) 0.062 Uiso calc RD 1 1 0
C C6 0.1623(9) 0.5077(6) 0.1985(7) 0.0586(18) Uani d D 1 1 0
H H6A 0.0970(14) 0.4692(9) 0.2392(9) 0.070 Uiso calc RD 1 1 0
H H6B 0.1468(9) 0.4843(7) 0.1344(12) 0.070 Uiso calc RD 1 1 0
N N1 0.3888(6) 0.5887(5) 0.2823(4) 0.0431(11) Uani d D 1 1 0
H H1 0.477(2) 0.5730(6) 0.3082(7) 0.052 Uiso calc RD 1 1 0
N N2 0.1318(6) 0.6341(5) 0.2067(5) 0.0554(15) Uani d D 1 1 0
H H2 0.043(2) 0.6488(6) 0.1811(8) 0.067 Uiso calc RD 1 1 0
O O 0.1563(8) 0.2409(6) 0.3238(6) 0.0861(19) Uani d . 1 1 2
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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
Cl3 Cd Cl1 111.93(7)
Cl3 Cd Cl2 101.80(6)
Cl1 Cd Cl2 105.73(6)
Cl3 Cd Cl4 116.95(6)
Cl1 Cd Cl4 104.53(6)
Cl2 Cd Cl4 115.58(6)
N1 C1 C2 107.9(5)
N1 C1 H1A 110.1
C2 C1 H1A 110.1
N1 C1 H1B 110.1
C2 C1 H1B 110.1
H1A C1 H1B 108.4
N2 C2 C1 108.4(5)
N2 C2 H2A 110.0
C1 C2 H2A 110.0
N2 C2 H2B 110.0
C1 C2 H2B 110.0
H2A C2 H2B 108.4
N1 C3 C4 108.4(6)
N1 C3 H3A 110.0
C4 C3 H3A 110.0
N1 C3 H3B 110.0
C4 C3 H3B 110.0
H3A C3 H3B 108.4
N2 C4 C3 108.0(5)
N2 C4 H4A 110.1
C3 C4 H4A 110.1
N2 C4 H4B 110.1
C3 C4 H4B 110.1
H4A C4 H4B 108.4
N1 C5 C6 108.5(5)
N1 C5 H5A 110.0
C6 C5 H5A 110.0
N1 C5 H5B 110.0
C6 C5 H5B 110.0
H5A C5 H5B 108.4
C5 C6 N2 108.3(5)
C5 C6 H6A 110.0
N2 C6 H6A 110.0
C5 C6 H6B 110.0
N2 C6 H6B 110.0
H6A C6 H6B 108.4
C3 N1 C5 111.1(6)
C3 N1 C1 110.2(5)
C5 N1 C1 109.0(5)
C3 N1 H1 108.8
C5 N1 H1 108.8
C1 N1 H1 108.8
C4 N2 C2 109.2(6)
C4 N2 C6 109.9(6)
C2 N2 C6 110.5(6)
C4 N2 H2 109.1
C2 N2 H2 109.1
C6 N2 H2 109.1
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cd Cl3 2.430(2)
Cd Cl1 2.4673(18)
Cd Cl2 2.4835(19)
Cd Cl4 2.4864(17)
C1 N1 1.502(8)
C1 C2 1.517(9)
C1 H1A 1.0614
C1 H1B 1.0614
C2 N2 1.485(8)
C2 H2A 0.9127
C2 H2B 0.9127
C3 N1 1.461(9)
C3 C4 1.524(10)
C3 H3A 0.8860
C3 H3B 0.8860
C4 N2 1.476(11)
C4 H4A 0.8977
C4 H4B 0.8977
C5 N1 1.479(9)
C5 C6 1.496(10)
C5 H5A 0.9026
C5 H5B 0.9026
C6 N2 1.499(9)
C6 H6A 0.8931
C6 H6B 0.8931
N1 H1 0.8477
N2 H2 0.8420
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
N2 H2 O 4_555 0.84 2.01 2.7830(10) 151
