#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/29/2212901.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_2212901
loop_
_publ_author_name
'Tong-Liang Hu'
'Jin-Lei Tian'
_publ_section_title
trans-Bis[(2E)-3-(N,N-dimethylamino)-1-(2-pyridyl)prop-2-en-1-one-κ²N,O]bis(perchlorato-κO)cadmium(II)
_journal_coeditor_code           HB2326
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1092
_journal_page_last               m1093
_journal_paper_doi               10.1107/S1600536807011890
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Cd (Cl O4)2 (C10 H12 N2 O)2]'
_chemical_formula_moiety         'C20 H24 Cd Cl2 N4 O10'
_chemical_formula_sum            'C20 H24 Cd Cl2 N4 O10'
_chemical_formula_weight         663.73
_chemical_name_systematic
;
trans-Bis[(2E)-3-(N,N-dimethylamino)-1-(2-pyridyl)prop-2-en-1-one-
k²N,O]bis(perchlorato-\kO)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                78.656(3)
_cell_angle_beta                 79.377(3)
_cell_angle_gamma                71.775(2)
_cell_formula_units_Z            1
_cell_length_a                   7.3648(19)
_cell_length_b                   9.3606(19)
_cell_length_c                   9.839(2)
_cell_measurement_reflns_used    2384
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.02
_cell_measurement_theta_min      2.38
_cell_volume                     626.2(2)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker SMART 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  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3030
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1998)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             334
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.742
_refine_ls_extinction_coef       0.063(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0324
_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)+(0.0555P)²+0.2561P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                2070
_reflns_number_total             2154
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb2326.cif
_cod_data_source_block           I
_cod_original_cell_volume        626.2(3)
_cod_database_code               2212901
_cod_database_fobs_code          2212901
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
C C1 1.1947(4) 0.2471(4) 0.0505(3) 0.0457(6) Uani d . 1
H H1 1.3000 0.1970 -0.0078 0.055 Uiso calc R 1
C C2 1.2020(5) 0.3732(4) 0.0973(3) 0.0491(7) Uani d . 1
H H2 1.3104 0.4082 0.0716 0.059 Uiso calc R 1
C C3 1.0462(5) 0.4470(4) 0.1828(3) 0.0496(7) Uani d . 1
H H3 1.0473 0.5334 0.2155 0.060 Uiso calc R 1
C C4 0.8873(4) 0.3920(3) 0.2201(3) 0.0453(6) Uani d . 1
H H4 0.7803 0.4410 0.2778 0.054 Uiso calc R 1
C C5 0.8900(4) 0.2634(3) 0.1705(3) 0.0342(5) Uani d . 1
C C6 0.7282(4) 0.1886(3) 0.2092(3) 0.0353(5) Uani d . 1
C C7 0.5798(4) 0.2379(3) 0.3148(3) 0.0397(6) Uani d . 1
H H7 0.5754 0.3190 0.3581 0.048 Uiso calc R 1
C C8 0.4389(4) 0.1629(3) 0.3537(3) 0.0393(6) Uani d . 1
H H8 0.4504 0.0846 0.3045 0.047 Uiso calc R 1
C C9 0.1528(5) 0.1021(4) 0.4793(4) 0.0551(8) Uani d . 1
H H9A 0.1914 0.0266 0.4180 0.083 Uiso calc R 1
H H9B 0.0275 0.1689 0.4633 0.083 Uiso calc R 1
H H9C 0.1483 0.0530 0.5747 0.083 Uiso calc R 1
C C10 0.2522(5) 0.3091(5) 0.5371(4) 0.0704(10) Uani d . 1
H H10A 0.2143 0.2713 0.6327 0.106 Uiso calc R 1
H H10B 0.1500 0.3945 0.5042 0.106 Uiso calc R 1
H H10C 0.3662 0.3404 0.5308 0.106 Uiso calc R 1
Cd Cd1 1.0000 0.0000 0.0000 0.04458(17) Uani d S 1
Cl Cl1 1.31039(11) -0.25699(8) 0.23206(8) 0.0485(2) Uani d . 1
N N1 1.0410(3) 0.1929(3) 0.0856(2) 0.0379(5) Uani d . 1
N N2 0.2916(3) 0.1899(3) 0.4517(3) 0.0449(6) Uani d . 1
O O1 0.7378(3) 0.0806(2) 0.1478(2) 0.0513(5) Uani d . 1
O O2 1.1165(4) -0.1933(4) 0.2003(3) 0.0745(8) Uani d . 1
O O3 1.3995(5) -0.1404(4) 0.2096(4) 0.0995(11) Uani d . 1
O O4 1.2990(5) -0.3296(5) 0.3723(4) 0.1066(12) Uani d . 1
O O5 1.4107(5) -0.3643(4) 0.1414(5) 0.1078(13) 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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
N1 C1 C2 . . 122.4(3) ?
N1 C1 H1 . . 118.8 ?
C2 C1 H1 . . 118.8 ?
C1 C2 C3 . . 118.6(3) ?
C1 C2 H2 . . 120.7 ?
C3 C2 H2 . . 120.7 ?
C2 C3 C4 . . 119.5(3) ?
C2 C3 H3 . . 120.3 ?
C4 C3 H3 . . 120.3 ?
C5 C4 C3 . . 119.0(3) ?
C5 C4 H4 . . 120.5 ?
C3 C4 H4 . . 120.5 ?
N1 C5 C4 . . 121.3(2) ?
N1 C5 C6 . . 114.9(2) ?
C4 C5 C6 . . 123.8(2) ?
O1 C6 C7 . . 122.6(2) ?
O1 C6 C5 . . 118.2(2) ?
C7 C6 C5 . . 119.1(2) ?
C8 C7 C6 . . 118.2(3) ?
C8 C7 H7 . . 120.9 ?
C6 C7 H7 . . 120.9 ?
N2 C8 C7 . . 127.3(3) ?
N2 C8 H8 . . 116.3 ?
C7 C8 H8 . . 116.3 ?
N2 C9 H9A . . 109.5 ?
N2 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
N2 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
N2 C10 H10A . . 109.5 ?
N2 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
N2 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
O1 Cd1 O1 . 2_755 180.0 ?
O1 Cd1 N1 . . 73.63(8) y
O1 Cd1 N1 2_755 . 106.37(8) ?
O1 Cd1 N1 . 2_755 106.37(8) ?
O1 Cd1 N1 2_755 2_755 73.63(8) ?
N1 Cd1 N1 . 2_755 180.0 ?
O1 Cd1 O2 . . 85.36(9) ?
O1 Cd1 O2 2_755 . 94.64(9) ?
N1 Cd1 O2 . . 94.00(10) ?
N1 Cd1 O2 2_755 . 86.00(10) ?
O1 Cd1 O2 . 2_755 94.64(9) ?
O1 Cd1 O2 2_755 2_755 85.36(9) ?
N1 Cd1 O2 . 2_755 86.00(10) ?
N1 Cd1 O2 2_755 2_755 94.00(10) ?
O2 Cd1 O2 . 2_755 180.0 ?
O3 Cl1 O4 . . 112.9(2) ?
O3 Cl1 O5 . . 109.3(2) ?
O4 Cl1 O5 . . 110.3(3) ?
O3 Cl1 O2 . . 109.0(2) ?
O4 Cl1 O2 . . 106.76(19) ?
O5 Cl1 O2 . . 108.4(2) ?
C5 N1 C1 . . 119.1(2) ?
C5 N1 Cd1 . . 114.95(16) ?
C1 N1 Cd1 . . 125.7(2) ?
C8 N2 C10 . . 123.2(3) ?
C8 N2 C9 . . 121.0(3) ?
C10 N2 C9 . . 115.8(3) ?
C6 O1 Cd1 . . 117.84(16) ?
Cl1 O2 Cd1 . . 127.83(16) ?
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 . 1.343(4) ?
C1 C2 . 1.368(5) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.370(5) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.383(4) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.379(4) ?
C4 H4 . 0.9300 ?
C5 N1 . 1.336(3) ?
C5 C6 . 1.518(3) ?
C6 O1 . 1.254(3) ?
C6 C7 . 1.393(4) ?
C7 C8 . 1.385(4) ?
C7 H7 . 0.9300 ?
C8 N2 . 1.308(4) ?
C8 H8 . 0.9300 ?
C9 N2 . 1.459(4) ?
C9 H9A . 0.9600 ?
C9 H9B . 0.9600 ?
C9 H9C . 0.9600 ?
C10 N2 . 1.453(5) ?
C10 H10A . 0.9600 ?
C10 H10B . 0.9600 ?
C10 H10C . 0.9600 ?
Cd1 O1 . 2.213(2) y
Cd1 O1 2_755 2.213(2) ?
Cd1 N1 . 2.257(2) y
Cd1 N1 2_755 2.257(2) ?
Cd1 O2 . 2.479(3) y
Cd1 O2 2_755 2.479(3) ?
Cl1 O3 . 1.404(3) ?
Cl1 O4 . 1.413(3) ?
Cl1 O5 . 1.413(3) ?
Cl1 O2 . 1.432(3) ?
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
N1 C1 C2 C3 . -0.2(5)
C1 C2 C3 C4 . 0.4(5)
C2 C3 C4 C5 . 0.2(5)
C3 C4 C5 N1 . -1.2(4)
C3 C4 C5 C6 . 177.3(3)
N1 C5 C6 O1 . -8.0(4)
C4 C5 C6 O1 . 173.4(3)
N1 C5 C6 C7 . 169.4(2)
C4 C5 C6 C7 . -9.2(4)
O1 C6 C7 C8 . 0.6(4)
C5 C6 C7 C8 . -176.6(2)
C6 C7 C8 N2 . 178.4(3)
C4 C5 N1 C1 . 1.4(4)
C6 C5 N1 C1 . -177.2(2)
C4 C5 N1 Cd1 . -173.8(2)
C6 C5 N1 Cd1 . 7.6(3)
C2 C1 N1 C5 . -0.7(4)
C2 C1 N1 Cd1 . 174.0(2)
O1 Cd1 N1 C5 . -4.32(17)
O1 Cd1 N1 C5 2_755 175.68(17)
O2 Cd1 N1 C5 . -88.29(19)
O2 Cd1 N1 C5 2_755 91.71(19)
O1 Cd1 N1 C1 . -179.2(2)
O1 Cd1 N1 C1 2_755 0.8(2)
O2 Cd1 N1 C1 . 96.8(2)
O2 Cd1 N1 C1 2_755 -83.2(2)
C7 C8 N2 C10 . 0.6(5)
C7 C8 N2 C9 . 179.1(3)
C7 C6 O1 Cd1 . -173.1(2)
C5 C6 O1 Cd1 . 4.2(3)
N1 Cd1 O1 C6 . -0.1(2)
N1 Cd1 O1 C6 2_755 179.9(2)
O2 Cd1 O1 C6 . 95.4(2)
O2 Cd1 O1 C6 2_755 -84.6(2)
O3 Cl1 O2 Cd1 . 42.5(3)
O4 Cl1 O2 Cd1 . 164.8(3)
O5 Cl1 O2 Cd1 . -76.4(3)
O1 Cd1 O2 Cl1 . -145.9(2)
O1 Cd1 O2 Cl1 2_755 34.1(2)
N1 Cd1 O2 Cl1 . -72.7(2)
N1 Cd1 O2 Cl1 2_755 107.3(2)
