#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/13/2221319.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_2221319
loop_
_publ_author_name
'Dong, Hua-Ze'
'Chu, Zhao-Lian'
'Hu, Nai-Liang'
_publ_section_title
Diaquadibromidobis[3-dimethylamino-1-(4-pyridyl-κN)prop-2-en-1-one]cadmium(II)
_journal_coeditor_code           CV2525
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m358
_journal_paper_doi               10.1107/S1600536809007028
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Cd Br2 (C10 H12 N2 O)2 (H2 O)2]'
_chemical_formula_moiety         'C20 H28 Br2 Cd N4 O4'
_chemical_formula_sum            'C20 H28 Br2 Cd N4 O4'
_chemical_formula_weight         660.68
_chemical_name_systematic
;
Diaquadibromidobis[3-dimethylamino-1-(4-pyridyl-κN)prop-2-en-1-
one]cadmium(II)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 114.456(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.362(3)
_cell_length_b                   8.4360(9)
_cell_length_c                   14.6371(16)
_cell_measurement_reflns_used    3328
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.79
_cell_measurement_theta_min      2.63
_cell_volume                     2401.1(5)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_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  0.0732
_diffrn_reflns_av_sigmaI/netI    0.0583
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6227
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    4.271
_exptl_absorpt_correction_T_max  0.424
_exptl_absorpt_correction_T_min  0.407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.926
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0353
_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)+(0.0479P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                2085
_reflns_number_total             2356
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cv2525.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2221319
_cod_database_fobs_code          2221319
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Cd Cd1 0.5000 0.5000 0.5000 0.02740(13) Uani d S 1 . .
Br Br1 0.626658(19) 0.61470(5) 0.54529(3) 0.04254(15) Uani d . 1 . .
C C1 0.44435(18) 0.8564(4) 0.4098(2) 0.0332(8) Uani d . 1 . .
H H1 0.4561 0.8760 0.4775 0.040 Uiso calc R 1 . .
C C2 0.43309(18) 0.6830(4) 0.2848(2) 0.0350(8) Uani d . 1 . .
H H2 0.4368 0.5807 0.2639 0.042 Uiso calc R 1 . .
C C3 0.42099(19) 0.9802(4) 0.3443(2) 0.0317(8) Uani d . 1 . .
H H3 0.4171 1.0810 0.3673 0.038 Uiso calc R 1 . .
C C4 0.40298(16) 0.9534(4) 0.2423(2) 0.0270(7) Uani d . 1 . .
C C5 0.40919(18) 0.7997(4) 0.2139(2) 0.0341(8) Uani d . 1 . .
H H5 0.3971 0.7758 0.1467 0.041 Uiso calc R 1 . .
C C6 0.33391(18) 1.0483(5) 0.0698(2) 0.0337(8) Uani d . 1 . .
H H6 0.3149 0.9472 0.0558 0.040 Uiso calc R 1 . .
C C7 0.38011(16) 1.0865(4) 0.1687(2) 0.0276(7) Uani d . 1 . .
C C8 0.2340(2) 0.9862(5) -0.1300(3) 0.0524(11) Uani d . 1 . .
H H8A 0.2646 0.9016 -0.1281 0.079 Uiso calc R 1 . .
H H8B 0.1990 0.9969 -0.1970 0.079 Uiso calc R 1 . .
H H8C 0.2131 0.9631 -0.0848 0.079 Uiso calc R 1 . .
C C9 0.2647(2) 1.2464(5) -0.1787(3) 0.0423(9) Uani d . 1 . .
H H9A 0.2856 1.3452 -0.1492 0.063 Uiso calc R 1 . .
H H9B 0.2167 1.2629 -0.2196 0.063 Uiso calc R 1 . .
H H9C 0.2866 1.2058 -0.2195 0.063 Uiso calc R 1 . .
C C10 0.31637(17) 1.1583(4) -0.0065(2) 0.0299(7) Uani d . 1 . .
H H10 0.3371 1.2575 0.0093 0.036 Uiso calc R 1 . .
N N1 0.45139(14) 0.7084(3) 0.38242(19) 0.0311(6) Uani d . 1 . .
N N2 0.27261(15) 1.1335(4) -0.1000(2) 0.0338(7) Uani d . 1 . .
O O1 0.40227(12) 1.2232(3) 0.19871(16) 0.0343(5) Uani d . 1 . .
O O2 0.50607(12) 0.3380(3) 0.37287(16) 0.0368(6) Uani d . 1 . .
H H2A 0.4661 0.3344 0.3253 0.044 Uiso d R 1 . .
H H2B 0.5323 0.3885 0.3525 0.044 Uiso d 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'
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'
Br Br -0.2901 2.4595 '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
O2 Cd1 O2 5_666 . 180.0 ?
O2 Cd1 N1 5_666 5_666 90.43(9) ?
O2 Cd1 N1 . 5_666 89.57(9) ?
O2 Cd1 N1 5_666 . 89.57(9) ?
O2 Cd1 N1 . . 90.43(9) ?
N1 Cd1 N1 5_666 . 180.00(11) ?
O2 Cd1 Br1 5_666 5_666 91.41(6) ?
O2 Cd1 Br1 . 5_666 88.59(6) ?
N1 Cd1 Br1 5_666 5_666 90.33(7) ?
N1 Cd1 Br1 . 5_666 89.67(7) ?
O2 Cd1 Br1 5_666 . 88.59(6) ?
O2 Cd1 Br1 . . 91.41(6) ?
N1 Cd1 Br1 5_666 . 89.67(7) ?
N1 Cd1 Br1 . . 90.33(7) ?
Br1 Cd1 Br1 5_666 . 180.000(15) ?
N1 C1 C3 . . 123.8(3) ?
N1 C1 H1 . . 118.1 ?
C3 C1 H1 . . 118.1 ?
N1 C2 C5 . . 123.3(3) ?
N1 C2 H2 . . 118.3 ?
C5 C2 H2 . . 118.3 ?
C1 C3 C4 . . 119.1(3) ?
C1 C3 H3 . . 120.5 ?
C4 C3 H3 . . 120.5 ?
C5 C4 C3 . . 117.0(3) ?
C5 C4 C7 . . 122.1(3) ?
C3 C4 C7 . . 120.9(3) ?
C2 C5 C4 . . 119.9(3) ?
C2 C5 H5 . . 120.0 ?
C4 C5 H5 . . 120.0 ?
C10 C6 C7 . . 121.2(3) ?
C10 C6 H6 . . 119.4 ?
C7 C6 H6 . . 119.4 ?
O1 C7 C6 . . 124.8(3) ?
O1 C7 C4 . . 118.4(3) ?
C6 C7 C4 . . 116.8(3) ?
N2 C8 H8A . . 109.5 ?
N2 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
N2 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
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 C6 . . 125.0(3) ?
N2 C10 H10 . . 117.5 ?
C6 C10 H10 . . 117.5 ?
C2 N1 C1 . . 116.8(3) ?
C2 N1 Cd1 . . 120.2(2) ?
C1 N1 Cd1 . . 122.8(2) ?
C10 N2 C9 . . 121.4(3) ?
C10 N2 C8 . . 121.3(3) ?
C9 N2 C8 . . 117.2(3) ?
Cd1 O2 H2A . . 107.7 ?
Cd1 O2 H2B . . 104.3 ?
H2A O2 H2B . . 108.3 ?
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 O2 5_666 2.355(2) ?
Cd1 O2 . 2.355(2) ?
Cd1 N1 5_666 2.377(3) ?
Cd1 N1 . 2.377(3) ?
Cd1 Br1 5_666 2.6855(5) ?
Cd1 Br1 . 2.6855(5) ?
C1 N1 . 1.339(4) ?
C1 C3 . 1.365(5) ?
C1 H1 . 0.9300 ?
C2 N1 . 1.333(4) ?
C2 C5 . 1.366(5) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.398(4) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.385(5) ?
C4 C7 . 1.491(4) ?
C5 H5 . 0.9300 ?
C6 C10 . 1.379(5) ?
C6 C7 . 1.411(4) ?
C6 H6 . 0.9300 ?
C7 O1 . 1.255(4) ?
C8 N2 . 1.455(5) ?
C8 H8A . 0.9600 ?
C8 H8B . 0.9600 ?
C8 H8C . 0.9600 ?
C9 N2 . 1.449(4) ?
C9 H9A . 0.9600 ?
C9 H9B . 0.9600 ?
C9 H9C . 0.9600 ?
C10 N2 . 1.316(4) ?
C10 H10 . 0.9300 ?
O2 H2A . 0.8500 ?
O2 H2B . 0.8501 ?
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
O2 H2A O1 1_545 0.85 2.02 2.770(3) 147.0
O2 H2B O1 2_645 0.85 2.31 2.751(4) 113.0
