#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/05/2230544.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_2230544
loop_
_publ_author_name
'Vallejo, Daniel'
'Beobide, Garikoitz'
'Castillo, Oscar'
'Luque, Antonio'
_publ_section_title
;
 Bis(1,10-phenanthroline-κ²N,N')bis(thiocyanato-κN)cadmium
;
_journal_coeditor_code           ZJ2006
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m704
_journal_page_last               m705
_journal_paper_doi               10.1107/S160053681101289X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Cd (N C S)2 (C12 H8 N2)2]'
_chemical_formula_moiety         'C26 H16 Cd N6 S2'
_chemical_formula_sum            'C26 H16 Cd N6 S2'
_chemical_formula_weight         588.97
_chemical_name_systematic
;
Bis(1,10-phenanthroline-κ²N,N')bis(thiocyanato-
κN)cadmium
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5295(2)
_cell_length_b                   9.91538(18)
_cell_length_c                   17.5297(2)
_cell_measurement_reflns_used    19593
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.07
_cell_measurement_theta_min      3.01
_cell_volume                     2351.61(6)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur'
_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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19593
_diffrn_reflns_theta_full        30.07
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.562
_refine_diff_density_min         -0.825
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         3444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0398
_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)+(0.0606P)²+3.0087P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                2606
_reflns_number_total             3444
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            zj2006.cif
_cod_data_source_block           I
_cod_original_cell_volume        2351.62(6)
_cod_database_code               2230544
_cod_database_fobs_code          2230544
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, 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_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd Cd 0.0000 0.31999(3) 0.7500 0.01949(10) Uani d S 1 2 . .
S S1 -0.16408(7) 0.01037(9) 0.56558(5) 0.0346(2) Uani d . 1 1 . .
N N1 -0.00666(17) 0.4887(3) 0.84583(15) 0.0237(5) Uani d . 1 1 . .
N N2 -0.16737(19) 0.3741(3) 0.77514(14) 0.0213(5) Uani d . 1 1 . .
N N3 -0.0504(2) 0.1673(3) 0.66235(16) 0.0308(6) Uani d . 1 1 . .
C C13 -0.0980(2) 0.1038(3) 0.62292(16) 0.0224(5) Uani d . 1 1 . .
C C12 -0.0987(2) 0.5344(3) 0.86435(16) 0.0226(6) Uani d . 1 1 . .
C C9 -0.3426(2) 0.3557(4) 0.75684(17) 0.0283(6) Uani d . 1 1 . .
H H9 -0.3950 0.3137 0.7321 0.034 Uiso calc R 1 1 . .
C C11 -0.1831(2) 0.4731(3) 0.82731(15) 0.0215(5) Uani d . 1 1 . .
C C7 -0.2791(2) 0.5182(3) 0.84580(16) 0.0254(6) Uani d . 1 1 . .
C C8 -0.3593(2) 0.4548(4) 0.80914(18) 0.0303(7) Uani d . 1 1 . .
H H8 -0.4236 0.4806 0.8206 0.036 Uiso calc R 1 1 . .
C C1 0.0703(3) 0.5433(3) 0.88069(19) 0.0313(7) Uani d . 1 1 . .
H H1 0.1330 0.5104 0.8695 0.038 Uiso calc R 1 1 . .
C C4 -0.1141(2) 0.6393(3) 0.91695(18) 0.0283(6) Uani d . 1 1 . .
C C10 -0.2452(3) 0.3186(3) 0.74108(16) 0.0256(6) Uani d . 1 1 . .
H H10 -0.2342 0.2517 0.7049 0.031 Uiso calc R 1 1 . .
C C3 -0.0296(3) 0.6967(4) 0.9512(2) 0.0370(8) Uani d . 1 1 . .
H H3 -0.0362 0.7674 0.9857 0.044 Uiso calc R 1 1 . .
C C2 0.0618(3) 0.6478(4) 0.9335(2) 0.0381(8) Uani d . 1 1 . .
H H2 0.1179 0.6839 0.9564 0.046 Uiso calc R 1 1 . .
C C6 -0.2909(2) 0.6262(4) 0.89896(18) 0.0313(7) Uani d . 1 1 . .
H H6 -0.3541 0.6573 0.9103 0.038 Uiso calc R 1 1 . .
C C5 -0.2122(3) 0.6839(3) 0.93295(19) 0.0315(7) Uani d . 1 1 . .
H H5 -0.2220 0.7540 0.9674 0.038 Uiso calc R 1 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'
Co Co 0.3494 0.9721 '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
N3 Cd N3 . 4_556 95.97(15) y
N3 Cd N2 . 4_556 108.26(9) y
N3 Cd N2 4_556 4_556 89.42(10) ?
N3 Cd N2 . . 89.42(10) y
N3 Cd N2 4_556 . 108.26(9) ?
N2 Cd N2 4_556 . 153.81(12) y
N3 Cd N1 . 4_556 90.14(10) y
N3 Cd N1 4_556 4_556 160.29(9) ?
N2 Cd N1 4_556 4_556 70.87(8) ?
N2 Cd N1 . 4_556 90.48(8) y
N3 Cd N1 . . 160.29(9) y
N3 Cd N1 4_556 . 90.14(10) ?
N2 Cd N1 4_556 . 90.48(8) ?
N2 Cd N1 . . 70.87(8) y
N1 Cd N1 4_556 . 90.34(13) y
C1 N1 C12 . . 118.2(3) ?
C1 N1 Cd . . 125.9(2) ?
C12 N1 Cd . . 115.94(18) ?
C10 N2 C11 . . 118.5(3) ?
C10 N2 Cd . . 125.4(2) ?
C11 N2 Cd . . 116.04(19) ?
C13 N3 Cd . . 162.9(3) ?
N3 C13 S1 . . 178.6(3) ?
N1 C12 C4 . . 122.5(3) ?
N1 C12 C11 . . 118.3(2) ?
C4 C12 C11 . . 119.2(3) ?
C8 C9 C10 . . 118.7(3) ?
C8 C9 H9 . . 120.7 ?
C10 C9 H9 . . 120.7 ?
N2 C11 C7 . . 121.9(3) ?
N2 C11 C12 . . 118.8(3) ?
C7 C11 C12 . . 119.3(3) ?
C8 C7 C11 . . 117.5(3) ?
C8 C7 C6 . . 123.1(3) ?
C11 C7 C6 . . 119.4(3) ?
C9 C8 C7 . . 120.1(3) ?
C9 C8 H8 . . 120.0 ?
C7 C8 H8 . . 120.0 ?
N1 C1 C2 . . 123.1(3) ?
N1 C1 H1 . . 118.4 ?
C2 C1 H1 . . 118.4 ?
C12 C4 C3 . . 117.3(3) ?
C12 C4 C5 . . 119.7(3) ?
C3 C4 C5 . . 123.0(3) ?
N2 C10 C9 . . 123.3(3) ?
N2 C10 H10 . . 118.3 ?
C9 C10 H10 . . 118.3 ?
C2 C3 C4 . . 119.6(3) ?
C2 C3 H3 . . 120.2 ?
C4 C3 H3 . . 120.2 ?
C3 C2 C1 . . 119.3(3) ?
C3 C2 H2 . . 120.4 ?
C1 C2 H2 . . 120.4 ?
C5 C6 C7 . . 121.2(3) ?
C5 C6 H6 . . 119.4 ?
C7 C6 H6 . . 119.4 ?
C6 C5 C4 . . 121.1(3) ?
C6 C5 H5 . . 119.5 ?
C4 C5 H5 . . 119.5 ?
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
Cd N3 . 2.262(3) y
Cd N3 4_556 2.262(3) ?
Cd N2 4_556 2.369(3) ?
Cd N2 . 2.369(3) y
Cd N1 4_556 2.372(3) ?
Cd N1 . 2.372(3) y
S1 C13 . 1.634(3) ?
N1 C1 . 1.323(4) ?
N1 C12 . 1.365(4) ?
N2 C10 . 1.329(4) ?
N2 C11 . 1.358(4) ?
N3 C13 . 1.135(4) ?
C12 C4 . 1.405(4) ?
C12 C11 . 1.448(4) ?
C9 C8 . 1.362(5) ?
C9 C10 . 1.396(5) ?
C9 H9 . 0.9300 ?
C11 C7 . 1.411(4) ?
C7 C8 . 1.409(5) ?
C7 C6 . 1.429(5) ?
C8 H8 . 0.9300 ?
C1 C2 . 1.394(5) ?
C1 H1 . 0.9300 ?
C4 C3 . 1.410(5) ?
C4 C5 . 1.428(5) ?
C10 H10 . 0.9300 ?
C3 C2 . 1.364(5) ?
C3 H3 . 0.9300 ?
C2 H2 . 0.9300 ?
C6 C5 . 1.347(5) ?
C6 H6 . 0.9300 ?
C5 H5 . 0.9300 ?
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
C8 H8 N3 6_567 0.93 2.54 3.373(4) 149
