#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/94/2229483.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_2229483
loop_
_publ_author_name
'Suleiman Gwaram, Nura'
'Khaledi, Hamid'
'Mohd Ali, Hapipah'
_publ_section_title
;
 Dichlorido{N,N-dimethyl-N'-[1-(pyridin-2-yl)ethylidene]ethane-1,2-diamine-κ³N,N',N''}cadmium
;
_journal_coeditor_code           PV2387
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m348
_journal_paper_doi               10.1107/S1600536811005538
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Cd Cl2 (C11 H17 N3)]'
_chemical_formula_moiety         'C11 H17 Cd Cl2 N3'
_chemical_formula_sum            'C11 H17 Cd Cl2 N3'
_chemical_formula_weight         374.58
_chemical_name_systematic
;
Dichlorido{N,N-dimethyl-N'-
[1-(pyridin-2-yl)ethylidene]ethane-1,2-diamine-
κ³N,N',N''}cadmium
;
_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                102.5340(10)
_cell_angle_beta                 103.3650(10)
_cell_angle_gamma                97.8500(10)
_cell_formula_units_Z            2
_cell_length_a                   8.0276(2)
_cell_length_b                   9.6048(2)
_cell_length_c                   10.0851(2)
_cell_measurement_reflns_used    5105
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.65
_cell_measurement_theta_min      2.22
_cell_volume                     724.09(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and 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  0.0138
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5023
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    1.859
_exptl_absorpt_correction_T_max  0.9293
_exptl_absorpt_correction_T_min  0.6744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.391
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0165
_refine_ls_R_factor_gt           0.0155
_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)+(0.0151P)²+0.4207P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0377
_refine_ls_wR_factor_ref         0.0384
_reflns_number_gt                2547
_reflns_number_total             2652
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            pv2387.cif
_cod_data_source_block           I
_cod_database_code               2229483
_cod_database_fobs_code          2229483
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd Cd1 -0.076971(16) 0.190459(13) 0.205336(13) 0.01438(5) Uani d . 1 . .
Cl Cl1 -0.19397(6) 0.14396(5) -0.04976(5) 0.02368(11) Uani d . 1 . .
Cl Cl2 -0.21885(7) 0.34705(5) 0.35214(5) 0.02337(11) Uani d . 1 . .
N N1 -0.1880(2) -0.04027(16) 0.23109(16) 0.0155(3) Uani d . 1 . .
N N2 0.1417(2) 0.10346(17) 0.33828(16) 0.0171(3) Uani d . 1 . .
N N3 0.1925(2) 0.34724(17) 0.22918(16) 0.0187(3) Uani d . 1 . .
C C1 -0.3543(3) -0.1088(2) 0.1769(2) 0.0193(4) Uani d . 1 . .
H H1 -0.4351 -0.0611 0.1283 0.023 Uiso calc R 1 . .
C C2 -0.4143(3) -0.2472(2) 0.1886(2) 0.0214(4) Uani d . 1 . .
H H2 -0.5330 -0.2941 0.1471 0.026 Uiso calc R 1 . .
C C3 -0.2973(3) -0.3147(2) 0.2619(2) 0.0233(4) Uani d . 1 . .
H H3 -0.3346 -0.4091 0.2719 0.028 Uiso calc R 1 . .
C C4 -0.1247(3) -0.2432(2) 0.3208(2) 0.0202(4) Uani d . 1 . .
H H4 -0.0429 -0.2874 0.3732 0.024 Uiso calc R 1 . .
C C5 -0.0729(2) -0.1063(2) 0.30211(19) 0.0166(4) Uani d . 1 . .
C C6 0.1124(2) -0.0244(2) 0.35613(19) 0.0173(4) Uani d . 1 . .
C C7 0.2517(3) -0.0968(2) 0.4217(2) 0.0244(4) Uani d . 1 . .
H H7A 0.2968 -0.1510 0.3482 0.037 Uiso calc R 1 . .
H H7B 0.2025 -0.1639 0.4697 0.037 Uiso calc R 1 . .
H H7C 0.3470 -0.0229 0.4902 0.037 Uiso calc R 1 . .
C C8 0.3182(2) 0.1896(2) 0.3762(2) 0.0212(4) Uani d . 1 . .
H H8A 0.3840 0.1458 0.3117 0.025 Uiso calc R 1 . .
H H8B 0.3803 0.1910 0.4737 0.025 Uiso calc R 1 . .
C C9 0.3074(3) 0.3439(2) 0.3656(2) 0.0211(4) Uani d . 1 . .
H H9A 0.2626 0.3932 0.4431 0.025 Uiso calc R 1 . .
H H9B 0.4260 0.3985 0.3773 0.025 Uiso calc R 1 . .
C C10 0.2668(3) 0.2957(2) 0.1115(2) 0.0246(4) Uani d . 1 . .
H H10A 0.3822 0.3559 0.1282 0.037 Uiso calc R 1 . .
H H10B 0.1898 0.3027 0.0233 0.037 Uiso calc R 1 . .
H H10C 0.2779 0.1942 0.1045 0.037 Uiso calc R 1 . .
C C11 0.1656(3) 0.4971(2) 0.2359(2) 0.0286(5) Uani d . 1 . .
H H11A 0.2779 0.5613 0.2511 0.043 Uiso calc R 1 . .
H H11B 0.1150 0.5301 0.3140 0.043 Uiso calc R 1 . .
H H11C 0.0860 0.4995 0.1470 0.043 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'
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'
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
N2 Cd1 N1 . . 69.42(5) ?
N2 Cd1 N3 . . 73.39(5) ?
N1 Cd1 N3 . . 141.34(5) ?
N2 Cd1 Cl1 . . 131.13(4) ?
N1 Cd1 Cl1 . . 98.62(4) ?
N3 Cd1 Cl1 . . 97.82(4) ?
N2 Cd1 Cl2 . . 112.49(4) ?
N1 Cd1 Cl2 . . 100.86(4) ?
N3 Cd1 Cl2 . . 102.71(4) ?
Cl1 Cd1 Cl2 . . 116.315(17) ?
C1 N1 C5 . . 119.09(16) ?
C1 N1 Cd1 . . 124.01(12) ?
C5 N1 Cd1 . . 116.87(12) ?
C6 N2 C8 . . 121.86(16) ?
C6 N2 Cd1 . . 120.70(13) ?
C8 N2 Cd1 . . 116.44(11) ?
C10 N3 C11 . . 110.06(16) ?
C10 N3 C9 . . 111.56(15) ?
C11 N3 C9 . . 108.99(15) ?
C10 N3 Cd1 . . 110.95(11) ?
C11 N3 Cd1 . . 110.21(12) ?
C9 N3 Cd1 . . 104.94(11) ?
N1 C1 C2 . . 122.72(18) ?
N1 C1 H1 . . 118.6 ?
C2 C1 H1 . . 118.6 ?
C3 C2 C1 . . 118.40(18) ?
C3 C2 H2 . . 120.8 ?
C1 C2 H2 . . 120.8 ?
C2 C3 C4 . . 119.34(18) ?
C2 C3 H3 . . 120.3 ?
C4 C3 H3 . . 120.3 ?
C3 C4 C5 . . 119.17(18) ?
C3 C4 H4 . . 120.4 ?
C5 C4 H4 . . 120.4 ?
N1 C5 C4 . . 121.26(17) ?
N1 C5 C6 . . 115.96(16) ?
C4 C5 C6 . . 122.77(17) ?
N2 C6 C7 . . 123.96(18) ?
N2 C6 C5 . . 116.71(16) ?
C7 C6 C5 . . 119.29(16) ?
C6 C7 H7A . . 109.5 ?
C6 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
C6 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
N2 C8 C9 . . 109.01(16) ?
N2 C8 H8A . . 109.9 ?
C9 C8 H8A . . 109.9 ?
N2 C8 H8B . . 109.9 ?
C9 C8 H8B . . 109.9 ?
H8A C8 H8B . . 108.3 ?
N3 C9 C8 . . 112.34(15) ?
N3 C9 H9A . . 109.1 ?
C8 C9 H9A . . 109.1 ?
N3 C9 H9B . . 109.1 ?
C8 C9 H9B . . 109.1 ?
H9A C9 H9B . . 107.9 ?
N3 C10 H10A . . 109.5 ?
N3 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
N3 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
N3 C11 H11A . . 109.5 ?
N3 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
N3 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
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
Cd1 N2 . 2.3188(15) ?
Cd1 N1 . 2.3644(15) ?
Cd1 N3 . 2.3909(16) ?
Cd1 Cl1 . 2.4434(5) ?
Cd1 Cl2 . 2.4561(5) ?
N1 C1 . 1.335(2) ?
N1 C5 . 1.350(2) ?
N2 C6 . 1.277(2) ?
N2 C8 . 1.459(2) ?
N3 C10 . 1.471(2) ?
N3 C11 . 1.474(2) ?
N3 C9 . 1.478(2) ?
C1 C2 . 1.389(3) ?
C1 H1 . 0.9500 ?
C2 C3 . 1.379(3) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.388(3) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.390(3) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.499(3) ?
C6 C7 . 1.497(3) ?
C7 H7A . 0.9800 ?
C7 H7B . 0.9800 ?
C7 H7C . 0.9800 ?
C8 C9 . 1.522(3) ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C10 H10A . 0.9800 ?
C10 H10B . 0.9800 ?
C10 H10C . 0.9800 ?
C11 H11A . 0.9800 ?
C11 H11B . 0.9800 ?
C11 H11C . 0.9800 ?
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
C7 H7B Cl2 2_556 0.98 2.77 3.679(2) 155
