#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/79/2017961.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_2017961
loop_
_publ_author_name
'Cai, Ying'
_publ_section_title
;
 Mononuclear and dinuclear bromide--nitrite cadmium(II) complexes with
 related 1,4-diazabicyclo[2.2.2]octane ligands
;
_journal_coeditor_code           SQ3272
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m13
_journal_page_last               m16
_journal_paper_doi               10.1107/S010827011005167X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Cd Br (C8 H14 N3) (N O2)2 (H2 O)], H2 O'
_chemical_formula_moiety         'C8 H16 Br Cd N5 O5, H2 O'
_chemical_formula_sum            'C8 H18 Br Cd N5 O6'
_chemical_formula_weight         472.58
_chemical_name_systematic
;aquabromido(1-cyanomethyl-4-aza-1-azoniabicyclo[2.2.2]octane-
κN⁴)bis(nitrito-κ²O,O')cadmium(II) monohydrate
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.505(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.343(2)
_cell_length_b                   16.254(5)
_cell_length_c                   12.850(4)
_cell_measurement_reflns_used    4571
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5126
_cell_measurement_theta_min      2.9774
_cell_volume                     1512.6(8)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.2714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16104
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    4.119
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.474
_refine_diff_density_min         -0.858
_refine_ls_extinction_coef       0.0055(11)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3458
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0352
_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)+(0.0736P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1232
_reflns_number_gt                3110
_reflns_number_total             3458
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sq3272.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2017961
_cod_database_fobs_code          2017961
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_disorder_assembly
_atom_site_disorder_group
C C1 0.2992(7) 0.6297(3) 0.7637(4) 0.0275(10) Uani d . 1 . .
H H1A 0.3909 0.6630 0.8079 0.033 Uiso d R 1 . .
H H1B 0.2320 0.6651 0.7098 0.033 Uiso d R 1 . .
C C2 0.3962(7) 0.5613(3) 0.7113(4) 0.0284(10) Uani d . 1 . .
H H2A 0.3997 0.5753 0.6383 0.034 Uiso d R 1 . .
H H2B 0.5220 0.5547 0.7476 0.034 Uiso d R 1 . .
C C3 0.2665(7) 0.5296(3) 0.8967(4) 0.0307(11) Uani d . 1 . .
H H3A 0.1902 0.5114 0.9471 0.037 Uiso d R 1 . .
H H3B 0.3802 0.5518 0.9358 0.037 Uiso d R 1 . .
C C4 0.3108(8) 0.4564(3) 0.8309(4) 0.0324(11) Uani d . 1 . .
H H4A 0.4363 0.4380 0.8552 0.039 Uiso d R 1 . .
H H4B 0.2277 0.4111 0.8384 0.039 Uiso d R 1 . .
C C5 0.0147(6) 0.5555(3) 0.7566(4) 0.0298(11) Uani d . 1 . .
H H5A -0.0631 0.5977 0.7189 0.036 Uiso d R 1 . .
H H5B -0.0601 0.5232 0.7970 0.036 Uiso d R 1 . .
C C6 0.0902(6) 0.4996(3) 0.6775(4) 0.0280(10) Uani d . 1 . .
H H6A 0.0212 0.4484 0.6692 0.034 Uiso d R 1 . .
H H6B 0.0769 0.5264 0.6092 0.034 Uiso d R 1 . .
C C7 0.3627(8) 0.4154(3) 0.6535(4) 0.0316(11) Uani d . 1 . .
H H7A 0.4950 0.4107 0.6759 0.038 Uiso d R 1 . .
H H7B 0.3073 0.3633 0.6678 0.038 Uiso d R 1 . .
C C8 0.3254(7) 0.4310(3) 0.5413(4) 0.0295(10) Uani d . 1 . .
N N1 0.1689(5) 0.5945(2) 0.8292(3) 0.0202(7) Uani d . 1 . .
N N2 0.2893(5) 0.4822(2) 0.7169(3) 0.0219(8) Uani d . 1 . .
N N3 0.2950(7) 0.4459(3) 0.4532(4) 0.0422(11) Uani d . 1 . .
N N4 -0.3010(5) 0.6625(2) 0.9524(3) 0.0259(8) Uani d DU 1 . .
N N5 0.2563(5) 0.8420(2) 0.9520(3) 0.0269(8) Uani d DU 1 . .
O O1 -0.2233(6) 0.6158(3) 0.9155(4) 0.0497(10) Uani d DU 1 . .
O O2 -0.2363(6) 0.7303(3) 0.9817(4) 0.0515(11) Uani d DU 1 . .
O O3 0.3111(6) 0.7861(3) 0.9084(4) 0.0496(10) Uani d DU 1 . .
O O4 0.1159(6) 0.8418(3) 0.9881(4) 0.0526(10) Uani d DU 1 . .
O O5 -0.0829(5) 0.7616(2) 0.7690(3) 0.0405(9) Uani d D 1 . .
H H5WA -0.0188 0.7869 0.7298 0.061 Uiso d RD 1 . .
H H5WB -0.1732 0.7296 0.7485 0.061 Uiso d RD 1 . .
O O6 0.5766(6) 0.7698(3) 1.1547(3) 0.0488(10) Uani d . 1 . .
H H6WA 0.5076 0.7313 1.1706 0.073 Uiso d R 1 . .
H H6WB 0.5543 0.7781 1.0885 0.073 Uiso d R 1 . .
Br Br1 0.19401(7) 0.63980(3) 1.12733(4) 0.03482(17) Uani d . 1 . .
Cd Cd1 0.05508(4) 0.700406(19) 0.93323(2) 0.02336(14) 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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
N1 C1 C2 . . 110.9(4) ?
N1 C1 H1A . . 109.4 ?
C2 C1 H1A . . 109.4 ?
N1 C1 H1B . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 108.1 ?
N2 C2 C1 . . 108.2(4) ?
N2 C2 H2A . . 110.0 ?
C1 C2 H2A . . 110.1 ?
N2 C2 H2B . . 110.1 ?
C1 C2 H2B . . 110.1 ?
H2A C2 H2B . . 108.4 ?
N1 C3 C4 . . 111.1(4) ?
N1 C3 H3A . . 109.4 ?
C4 C3 H3A . . 109.4 ?
N1 C3 H3B . . 109.4 ?
C4 C3 H3B . . 109.4 ?
H3A C3 H3B . . 108.0 ?
N2 C4 C3 . . 108.9(4) ?
N2 C4 H4A . . 109.9 ?
C3 C4 H4A . . 109.9 ?
N2 C4 H4B . . 110.0 ?
C3 C4 H4B . . 109.9 ?
H4A C4 H4B . . 108.3 ?
N1 C5 C6 . . 110.3(4) ?
N1 C5 H5A . . 109.7 ?
C6 C5 H5A . . 109.7 ?
N1 C5 H5B . . 109.5 ?
C6 C5 H5B . . 109.5 ?
H5A C5 H5B . . 108.1 ?
N2 C6 C5 . . 109.1(3) ?
N2 C6 H6A . . 109.8 ?
C5 C6 H6A . . 109.9 ?
N2 C6 H6B . . 109.8 ?
C5 C6 H6B . . 109.8 ?
H6A C6 H6B . . 108.3 ?
C8 C7 N2 . . 112.7(4) ?
C8 C7 H7A . . 109.0 ?
N2 C7 H7A . . 109.0 ?
C8 C7 H7B . . 109.1 ?
N2 C7 H7B . . 109.1 ?
H7A C7 H7B . . 107.8 ?
N3 C8 C7 . . 177.9(5) ?
C3 N1 C5 . . 108.1(4) ?
C3 N1 C1 . . 108.2(4) ?
C5 N1 C1 . . 107.7(3) ?
C3 N1 Cd1 . . 111.3(3) ?
C5 N1 Cd1 . . 110.8(3) ?
C1 N1 Cd1 . . 110.6(3) ?
C6 N2 C4 . . 108.8(4) ?
C6 N2 C7 . . 111.7(4) ?
C4 N2 C7 . . 109.5(3) ?
C6 N2 C2 . . 108.0(4) ?
C4 N2 C2 . . 108.2(4) ?
C7 N2 C2 . . 110.5(4) ?
O1 N4 O2 . . 123.1(5) ?
O3 N5 O4 . . 124.6(4) ?
N4 O1 Cd1 . . 93.3(3) ?
N4 O2 Cd1 . . 93.1(3) ?
N5 O3 Cd1 . . 92.8(3) ?
N5 O4 Cd1 . . 91.1(3) ?
Cd1 O5 H5WA . . 121.8 ?
Cd1 O5 H5WB . . 102.3 ?
H5WA O5 H5WB . . 126.3 ?
H6WA O6 H6WB . . 109.5 ?
O2 Cd1 O5 . . 83.00(15) ?
O2 Cd1 O3 . . 132.41(14) ?
O5 Cd1 O3 . . 82.45(15) ?
O2 Cd1 N1 . . 134.50(13) ?
O5 Cd1 N1 . . 86.75(13) yes
O3 Cd1 N1 . . 89.43(13) yes
O2 Cd1 O4 . . 81.96(15) ?
O5 Cd1 O4 . . 83.89(16) ?
O3 Cd1 O4 . . 51.57(14) yes
N1 Cd1 O4 . . 140.72(14) ?
O2 Cd1 O1 . . 50.46(15) yes
O5 Cd1 O1 . . 85.77(14) ?
O3 Cd1 O1 . . 167.12(16) yes
N1 Cd1 O1 . . 84.71(14) yes
O4 Cd1 O1 . . 132.21(15) ?
O2 Cd1 Br1 . . 92.94(12) ?
O5 Cd1 Br1 . . 175.22(10) yes
O3 Cd1 Br1 . . 98.55(11) ?
N1 Cd1 Br1 . . 97.92(9) yes
O4 Cd1 Br1 . . 93.06(12) ?
O1 Cd1 Br1 . . 93.61(11) ?
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
C1 N1 . 1.489(5) ?
C1 C2 . 1.535(6) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9699 ?
C2 N2 . 1.514(6) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C3 N1 . 1.474(6) ?
C3 C4 . 1.526(6) ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9701 ?
C4 N2 . 1.506(6) ?
C4 H4A . 0.9701 ?
C4 H4B . 0.9701 ?
C5 N1 . 1.485(5) ?
C5 C6 . 1.533(6) ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9699 ?
C6 N2 . 1.493(6) ?
C6 H6A . 0.9702 ?
C6 H6B . 0.9699 ?
C7 C8 . 1.444(7) ?
C7 N2 . 1.510(6) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C8 N3 . 1.144(7) ?
N1 Cd1 . 2.413(4) yes
N4 O1 . 1.102(5) ?
N4 O2 . 1.234(5) ?
N5 O3 . 1.172(5) ?
N5 O4 . 1.199(5) ?
O1 Cd1 . 2.443(4) yes
O2 Cd1 . 2.376(4) yes
O3 Cd1 . 2.403(4) yes
O4 Cd1 . 2.424(4) yes
O5 Cd1 . 2.401(4) yes
O5 H5WA . 0.8500 ?
O5 H5WB . 0.8500 ?
O6 H6WA . 0.8501 ?
O6 H6WB . 0.8500 ?
Br1 Cd1 . 2.7187(9) yes
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
O5 H5WA Br1 4_575 0.85 2.50 3.352(4) 174.9
O5 H5WB O6 4_475 0.85 2.02 2.731(6) 140.1
O6 H6WA Br1 . 0.85 2.72 3.486(5) 150.5
O6 H6WB O2 1_655 0.85 2.36 2.872(6) 119.6
