#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/15/2211533.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_2211533
loop_
_publ_author_name
'Chuan-Bi Li'
'Wei Fang'
'En-Jie Dong'
'Bo Liu'
'Yan-Wei Li'
_publ_section_title
Dichlorobis(pyrazino[2,3-f][1,10]phenanthroline-κ²N,N')cadmium(II)
_journal_coeditor_code           NG2133
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3247
_journal_page_last               m3248
_journal_paper_doi               10.1107/S1600536806045582
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Cd Cl2 (C28 H16 N8)]'
_chemical_formula_moiety         'C28 H16 Cd Cl2 N8'
_chemical_formula_sum            'C28 H16 Cd Cl2 N8'
_chemical_formula_weight         647.80
_chemical_name_systematic
;
Dichlorobis(pyrazino[2,3-f][1,10]phenanthroline-κ²N,N']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                 95.267(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4987(11)
_cell_length_b                   12.5070(17)
_cell_length_c                   22.768(3)
_cell_measurement_reflns_used    3544
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      25.97
_cell_measurement_theta_min      2.91
_cell_volume                     2409.9(6)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2002)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      292(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            6690
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.166
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.382
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.161
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0250
_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)+(0.031P)²+2.0151P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0622
_reflns_number_gt                2170
_reflns_number_total             2382
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng2133.cif
_cod_data_source_block           I
_cod_original_cell_volume        2409.8(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2211533
_cod_database_fobs_code          2211533
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
Cd Cd1 0.5000 0.637044(19) 0.7500 0.03245(10) Uani d S 1
Cl Cl1 0.68009(7) 0.76647(5) 0.80996(3) 0.04233(16) Uani d . 1
N N1 0.6923(2) 0.59046(16) 0.68470(8) 0.0323(4) Uani d . 1
C C4 0.7446(3) 0.50358(18) 0.59417(10) 0.0311(5) Uani d . 1
N N4 0.7795(2) 0.42081(17) 0.50061(9) 0.0394(5) Uani d . 1
C C14 0.6480(3) 0.52306(17) 0.63961(9) 0.0289(5) Uani d . 1
C C5 0.6871(3) 0.43451(18) 0.54536(10) 0.0324(5) Uani d . 1
C C9 0.4400(3) 0.40415(19) 0.59257(10) 0.0323(5) Uani d . 1
C C13 0.4937(3) 0.47118(17) 0.63901(10) 0.0301(5) Uani d . 1
N N3 0.4811(3) 0.32346(17) 0.49905(9) 0.0409(5) Uani d . 1
C C10 0.2898(3) 0.35765(19) 0.59360(12) 0.0397(6) Uani d . 1
H H10A 0.2497 0.3131 0.5631 0.048 Uiso calc R 1
C C8 0.5385(3) 0.38581(18) 0.54454(10) 0.0325(5) Uani d . 1
C C1 0.8336(3) 0.6366(2) 0.68640(11) 0.0374(5) Uani d . 1
H H1A 0.8640 0.6827 0.7174 0.045 Uiso calc R 1
C C11 0.2038(3) 0.3789(2) 0.63991(13) 0.0438(6) Uani d . 1
H H11A 0.1046 0.3484 0.6416 0.053 Uiso calc R 1
C C6 0.7203(3) 0.3602(2) 0.45660(11) 0.0436(6) Uani d . 1
H H6A 0.7797 0.3494 0.4248 0.052 Uiso calc R 1
C C2 0.9378(3) 0.6189(2) 0.64390(12) 0.0416(6) Uani d . 1
H H2A 1.0370 0.6509 0.6472 0.050 Uiso calc R 1
C C7 0.5732(3) 0.3119(2) 0.45575(11) 0.0445(6) Uani d . 1
H H7A 0.5380 0.2698 0.4235 0.053 Uiso calc R 1
C C3 0.8925(3) 0.5534(2) 0.59696(11) 0.0388(6) Uani d . 1
H H3B 0.9593 0.5423 0.5674 0.047 Uiso calc R 1
N N2 0.4060(2) 0.49370(16) 0.68416(8) 0.0350(4) Uani d . 1
C C12 0.2662(3) 0.4467(2) 0.68457(11) 0.0411(6) Uani d . 1
H H12A 0.2071 0.4597 0.7162 0.049 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'
N N 0.0061 0.0033 '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 Cd1 N1 . 2_656 151.67(10) ?
N1 Cd1 N2 . . 68.85(6) y
N1 Cd1 N2 2_656 . 89.94(6) ?
N1 Cd1 N2 . 2_656 89.94(6) ?
N1 Cd1 N2 2_656 2_656 68.85(6) ?
N2 Cd1 N2 . 2_656 84.65(10) ?
N1 Cd1 Cl1 . . 94.44(5) y
N1 Cd1 Cl1 2_656 . 103.58(5) ?
N2 Cd1 Cl1 . . 162.22(5) y
N2 Cd1 Cl1 2_656 . 89.47(5) ?
N1 Cd1 Cl1 . 2_656 103.58(5) ?
N1 Cd1 Cl1 2_656 2_656 94.44(5) ?
N2 Cd1 Cl1 . 2_656 89.47(5) ?
N2 Cd1 Cl1 2_656 2_656 162.22(5) ?
Cl1 Cd1 Cl1 . 2_656 100.76(3) ?
C1 N1 C14 . . 118.6(2) ?
C1 N1 Cd1 . . 123.08(16) ?
C14 N1 Cd1 . . 117.82(14) ?
C3 C4 C14 . . 118.3(2) ?
C3 C4 C5 . . 122.4(2) ?
C14 C4 C5 . . 119.3(2) ?
C6 N4 C5 . . 116.0(2) ?
N1 C14 C4 . . 121.8(2) ?
N1 C14 C13 . . 118.02(19) ?
C4 C14 C13 . . 120.1(2) ?
N4 C5 C8 . . 121.3(2) ?
N4 C5 C4 . . 118.2(2) ?
C8 C5 C4 . . 120.5(2) ?
C13 C9 C10 . . 118.1(2) ?
C13 C9 C8 . . 119.6(2) ?
C10 C9 C8 . . 122.2(2) ?
N2 C13 C9 . . 122.5(2) ?
N2 C13 C14 . . 117.2(2) ?
C9 C13 C14 . . 120.3(2) ?
C7 N3 C8 . . 116.0(2) ?
C11 C10 C9 . . 119.0(2) ?
C11 C10 H10A . . 120.5 ?
C9 C10 H10A . . 120.5 ?
N3 C8 C5 . . 121.5(2) ?
N3 C8 C9 . . 118.4(2) ?
C5 C8 C9 . . 120.1(2) ?
N1 C1 C2 . . 122.9(2) ?
N1 C1 H1A . . 118.6 ?
C2 C1 H1A . . 118.6 ?
C10 C11 C12 . . 119.2(2) ?
C10 C11 H11A . . 120.4 ?
C12 C11 H11A . . 120.4 ?
N4 C6 C7 . . 122.8(2) ?
N4 C6 H6A . . 118.6 ?
C7 C6 H6A . . 118.6 ?
C3 C2 C1 . . 119.1(2) ?
C3 C2 H2A . . 120.4 ?
C1 C2 H2A . . 120.4 ?
N3 C7 C6 . . 122.4(2) ?
N3 C7 H7A . . 118.8 ?
C6 C7 H7A . . 118.8 ?
C2 C3 C4 . . 119.2(2) ?
C2 C3 H3B . . 120.4 ?
C4 C3 H3B . . 120.4 ?
C12 N2 C13 . . 118.0(2) ?
C12 N2 Cd1 . . 124.61(16) ?
C13 N2 Cd1 . . 116.74(15) ?
N2 C12 C11 . . 123.1(2) ?
N2 C12 H12A . . 118.4 ?
C11 C12 H12A . . 118.4 ?
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 N1 . 2.3805(18) y
Cd1 N1 2_656 2.3805(19) ?
Cd1 N2 . 2.425(2) y
Cd1 N2 2_656 2.425(2) ?
Cd1 Cl1 . 2.5382(7) y
Cd1 Cl1 2_656 2.5382(7) ?
N1 C1 . 1.330(3) ?
N1 C14 . 1.355(3) ?
C4 C3 . 1.400(3) ?
C4 C14 . 1.400(3) ?
C4 C5 . 1.456(3) ?
N4 C6 . 1.318(3) ?
N4 C5 . 1.353(3) ?
C14 C13 . 1.462(3) ?
C5 C8 . 1.401(3) ?
C9 C13 . 1.393(3) ?
C9 C10 . 1.405(3) ?
C9 C8 . 1.455(3) ?
C13 N2 . 1.354(3) ?
N3 C7 . 1.321(3) ?
N3 C8 . 1.351(3) ?
C10 C11 . 1.363(4) ?
C10 H10A . 0.9300 ?
C1 C2 . 1.388(3) ?
C1 H1A . 0.9300 ?
C11 C12 . 1.391(4) ?
C11 H11A . 0.9300 ?
C6 C7 . 1.388(4) ?
C6 H6A . 0.9300 ?
C2 C3 . 1.373(4) ?
C2 H2A . 0.9300 ?
C7 H7A . 0.9300 ?
C3 H3B . 0.9300 ?
N2 C12 . 1.326(3) ?
C12 H12A . 0.9300 ?
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 Cd1 N1 C1 2_656 -134.28(19)
N2 Cd1 N1 C1 . -178.2(2)
N2 Cd1 N1 C1 2_656 -93.94(19)
Cl1 Cd1 N1 C1 . -4.48(19)
Cl1 Cd1 N1 C1 2_656 97.72(19)
N1 Cd1 N1 C14 2_656 53.67(15)
N2 Cd1 N1 C14 . 9.72(15)
N2 Cd1 N1 C14 2_656 94.01(16)
Cl1 Cd1 N1 C14 . -176.53(15)
Cl1 Cd1 N1 C14 2_656 -74.33(16)
C1 N1 C14 C4 . -2.0(3)
Cd1 N1 C14 C4 . 170.39(16)
C1 N1 C14 C13 . 178.7(2)
Cd1 N1 C14 C13 . -8.9(3)
C3 C4 C14 N1 . 1.8(3)
C5 C4 C14 N1 . -176.9(2)
C3 C4 C14 C13 . -178.9(2)
C5 C4 C14 C13 . 2.3(3)
C6 N4 C5 C8 . 0.6(3)
C6 N4 C5 C4 . -178.0(2)
C3 C4 C5 N4 . -1.7(3)
C14 C4 C5 N4 . 177.0(2)
C3 C4 C5 C8 . 179.7(2)
C14 C4 C5 C8 . -1.6(3)
C10 C9 C13 N2 . -0.8(3)
C8 C9 C13 N2 . 178.2(2)
C10 C9 C13 C14 . -179.0(2)
C8 C9 C13 C14 . 0.1(3)
N1 C14 C13 N2 . -0.5(3)
C4 C14 C13 N2 . -179.8(2)
N1 C14 C13 C9 . 177.7(2)
C4 C14 C13 C9 . -1.6(3)
C13 C9 C10 C11 . -0.7(4)
C8 C9 C10 C11 . -179.7(2)
C7 N3 C8 C5 . -0.2(4)
C7 N3 C8 C9 . 178.1(2)
N4 C5 C8 N3 . -0.2(4)
C4 C5 C8 N3 . 178.4(2)
N4 C5 C8 C9 . -178.4(2)
C4 C5 C8 C9 . 0.1(3)
C13 C9 C8 N3 . -177.7(2)
C10 C9 C8 N3 . 1.3(3)
C13 C9 C8 C5 . 0.6(3)
C10 C9 C8 C5 . 179.6(2)
C14 N1 C1 C2 . 0.2(4)
Cd1 N1 C1 C2 . -171.84(19)
C9 C10 C11 C12 . 0.6(4)
C5 N4 C6 C7 . -0.6(4)
N1 C1 C2 C3 . 1.9(4)
C8 N3 C7 C6 . 0.2(4)
N4 C6 C7 N3 . 0.3(4)
C1 C2 C3 C4 . -2.0(4)
C14 C4 C3 C2 . 0.2(4)
C5 C4 C3 C2 . 179.0(2)
C9 C13 N2 C12 . 2.3(3)
C14 C13 N2 C12 . -179.5(2)
C9 C13 N2 Cd1 . -168.78(17)
C14 C13 N2 Cd1 . 9.4(3)
N1 Cd1 N2 C12 . 179.6(2)
N1 Cd1 N2 C12 2_656 18.8(2)
N2 Cd1 N2 C12 2_656 87.6(2)
Cl1 Cd1 N2 C12 . 158.77(16)
Cl1 Cd1 N2 C12 2_656 -75.6(2)
N1 Cd1 N2 C13 . -9.95(15)
N1 Cd1 N2 C13 2_656 -170.72(16)
N2 Cd1 N2 C13 2_656 -101.96(17)
Cl1 Cd1 N2 C13 . -30.8(3)
Cl1 Cd1 N2 C13 2_656 94.84(16)
C13 N2 C12 C11 . -2.4(4)
Cd1 N2 C12 C11 . 167.9(2)
C10 C11 C12 N2 . 1.0(4)
