#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/79/2227900.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_2227900
loop_
_publ_author_name
'A. Shaker, Shayma'
'Khaledi, Hamid'
'Mohd Ali, Hapipah'
_publ_section_title
;
 Di-μ-thiocyanato-κ²N:S;κ²S:N-bis[bis(2-methyl-1H-benzimidazole-κN³)(thiocyanato-κN)cadmium(II)]
;
_journal_coeditor_code           PK2278
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1464
_journal_paper_doi               10.1107/S1600536810042443
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Cd2 (N C S)4 (C8 H8 N2)4]'
_chemical_formula_moiety         'C36 H32 Cd2 N12 S4'
_chemical_formula_sum            'C36 H32 Cd2 N12 S4'
_chemical_formula_weight         985.78
_chemical_name_systematic
;
Di-μ-thiocyanato-κ²N:S;κ²S:N-
bis[bis(2-methyl-1H-benzimidazole-κN³)(thiocyanato-
κN)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                 97.8640(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1519(11)
_cell_length_b                   10.2098(6)
_cell_length_c                   21.7385(13)
_cell_measurement_reflns_used    4666
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      2.29
_cell_volume                     3990.8(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9361
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    1.319
_exptl_absorpt_correction_T_max  0.8473
_exptl_absorpt_correction_T_min  0.6341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.313
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3593
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0169P)²+6.0676P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0470
_reflns_number_gt                3213
_reflns_number_total             3593
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pk2278.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2227900
_cod_database_fobs_code          2227900
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 0.611050(9) 0.354819(16) 0.590885(7) 0.01561(6) Uani d . 1 . .
S S1 0.88100(3) 0.33657(6) 0.67126(3) 0.02608(15) Uani d U 1 . .
S S2 0.63546(3) 0.42113(7) 0.47897(3) 0.02741(16) Uani d . 1 . .
N N1 0.62322(10) 0.41831(19) 0.69141(9) 0.0181(4) Uani d . 1 . .
N N2 0.63781(11) 0.5391(2) 0.77688(9) 0.0211(5) Uani d D 1 . .
H H2N 0.6364(14) 0.609(2) 0.7982(11) 0.025 Uiso d D 1 . .
N N3 0.57608(10) 0.14637(19) 0.58946(8) 0.0166(4) Uani d . 1 . .
N N4 0.50684(11) -0.0294(2) 0.59628(9) 0.0193(4) Uani d D 1 . .
H H4N 0.4715(12) -0.075(2) 0.6062(11) 0.023 Uiso d D 1 . .
N N5 0.73824(11) 0.3290(2) 0.60377(10) 0.0258(5) Uani d . 1 . .
N N6 0.49556(11) 0.4528(2) 0.57293(9) 0.0227(5) Uani d . 1 . .
C C1 0.57531(15) 0.6482(2) 0.68162(12) 0.0279(6) Uani d . 1 . .
H H1A 0.5852 0.6462 0.6384 0.042 Uiso calc R 1 . .
H H1B 0.5953 0.7293 0.7014 0.042 Uiso calc R 1 . .
H H1C 0.5215 0.6444 0.6826 0.042 Uiso calc R 1 . .
C C2 0.61150(12) 0.5342(2) 0.71553(11) 0.0195(5) Uani d . 1 . .
C C3 0.67023(13) 0.4198(2) 0.79411(11) 0.0199(5) Uani d . 1 . .
C C4 0.70777(13) 0.3741(3) 0.85017(11) 0.0256(6) Uani d . 1 . .
H H4 0.7157 0.4277 0.8862 0.031 Uiso calc R 1 . .
C C5 0.73278(13) 0.2465(3) 0.85032(11) 0.0267(6) Uani d . 1 . .
H H5 0.7590 0.2115 0.8875 0.032 Uiso calc R 1 . .
C C6 0.72085(13) 0.1674(3) 0.79777(11) 0.0244(6) Uani d . 1 . .
H H6 0.7376 0.0791 0.8004 0.029 Uiso calc R 1 . .
C C7 0.68519(13) 0.2141(2) 0.74170(11) 0.0207(5) Uani d . 1 . .
H H7 0.6782 0.1606 0.7056 0.025 Uiso calc R 1 . .
C C8 0.66004(12) 0.3433(2) 0.74051(10) 0.0180(5) Uani d . 1 . .
C C9 0.47424(14) 0.1670(2) 0.65538(11) 0.0235(6) Uani d . 1 . .
H H9A 0.5070 0.1980 0.6921 0.035 Uiso calc R 1 . .
H H9B 0.4369 0.1074 0.6683 0.035 Uiso calc R 1 . .
H H9C 0.4493 0.2419 0.6333 0.035 Uiso calc R 1 . .
C C10 0.51909(12) 0.0964(2) 0.61350(10) 0.0180(5) Uani d . 1 . .
C C11 0.55900(12) -0.0656(2) 0.55862(10) 0.0179(5) Uani d . 1 . .
C C12 0.57193(13) -0.1818(2) 0.52880(11) 0.0215(5) Uani d . 1 . .
H H12 0.5417 -0.2570 0.5316 0.026 Uiso calc R 1 . .
C C13 0.63096(14) -0.1828(2) 0.49486(11) 0.0224(5) Uani d . 1 . .
H H13 0.6421 -0.2610 0.4743 0.027 Uiso calc R 1 . .
C C14 0.67477(13) -0.0712(2) 0.49010(11) 0.0221(5) Uani d . 1 . .
H H14 0.7146 -0.0752 0.4660 0.027 Uiso calc R 1 . .
C C15 0.66144(13) 0.0441(2) 0.51961(10) 0.0191(5) Uani d . 1 . .
H H15 0.6914 0.1194 0.5164 0.023 Uiso calc R 1 . .
C C16 0.60252(12) 0.0460(2) 0.55436(10) 0.0162(5) Uani d . 1 . .
C C17 0.79736(13) 0.3327(2) 0.63127(11) 0.0190(5) Uani d U 1 . .
C C18 0.55777(13) 0.4945(2) 0.44892(10) 0.0181(5) 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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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 Cd1 N1 . . 106.16(7) ?
N3 Cd1 N5 . . 99.90(7) ?
N1 Cd1 N5 . . 87.22(7) ?
N3 Cd1 N6 . . 99.32(7) ?
N1 Cd1 N6 . . 90.32(7) ?
N5 Cd1 N6 . . 160.55(7) ?
N3 Cd1 S2 . . 108.61(5) ?
N1 Cd1 S2 . . 144.74(5) ?
N5 Cd1 S2 . . 81.28(5) ?
N6 Cd1 S2 . . 89.77(5) ?
C18 S2 Cd1 . . 103.94(8) ?
C2 N1 C8 . . 105.77(19) ?
C2 N1 Cd1 . . 129.77(16) ?
C8 N1 Cd1 . . 123.42(15) ?
C2 N2 C3 . . 108.3(2) ?
C2 N2 H2N . . 122.1(18) ?
C3 N2 H2N . . 129.4(18) ?
C10 N3 C16 . . 106.11(19) ?
C10 N3 Cd1 . . 126.99(16) ?
C16 N3 Cd1 . . 126.17(15) ?
C10 N4 C11 . . 108.57(19) ?
C10 N4 H4N . . 123.9(18) ?
C11 N4 H4N . . 127.4(18) ?
C17 N5 Cd1 . . 154.70(19) ?
C18 N6 Cd1 5_666 . 164.86(18) ?
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
N1 C2 N2 . . 111.7(2) ?
N1 C2 C1 . . 126.1(2) ?
N2 C2 C1 . . 122.2(2) ?
N2 C3 C4 . . 132.2(2) ?
N2 C3 C8 . . 105.3(2) ?
C4 C3 C8 . . 122.4(2) ?
C5 C4 C3 . . 116.1(2) ?
C5 C4 H4 . . 121.9 ?
C3 C4 H4 . . 121.9 ?
C4 C5 C6 . . 122.2(2) ?
C4 C5 H5 . . 118.9 ?
C6 C5 H5 . . 118.9 ?
C7 C6 C5 . . 121.6(2) ?
C7 C6 H6 . . 119.2 ?
C5 C6 H6 . . 119.2 ?
C6 C7 C8 . . 117.1(2) ?
C6 C7 H7 . . 121.5 ?
C8 C7 H7 . . 121.5 ?
C3 C8 C7 . . 120.6(2) ?
C3 C8 N1 . . 108.9(2) ?
C7 C8 N1 . . 130.5(2) ?
C10 C9 H9A . . 109.5 ?
C10 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
C10 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
N3 C10 N4 . . 111.5(2) ?
N3 C10 C9 . . 125.3(2) ?
N4 C10 C9 . . 123.2(2) ?
N4 C11 C12 . . 132.7(2) ?
N4 C11 C16 . . 105.1(2) ?
C12 C11 C16 . . 122.2(2) ?
C13 C12 C11 . . 116.7(2) ?
C13 C12 H12 . . 121.7 ?
C11 C12 H12 . . 121.7 ?
C12 C13 C14 . . 121.5(2) ?
C12 C13 H13 . . 119.2 ?
C14 C13 H13 . . 119.2 ?
C15 C14 C13 . . 121.5(2) ?
C15 C14 H14 . . 119.2 ?
C13 C14 H14 . . 119.2 ?
C14 C15 C16 . . 117.5(2) ?
C14 C15 H15 . . 121.2 ?
C16 C15 H15 . . 121.2 ?
C15 C16 C11 . . 120.5(2) ?
C15 C16 N3 . . 130.7(2) ?
C11 C16 N3 . . 108.8(2) ?
N5 C17 S1 . . 179.1(2) ?
N6 C18 S2 5_666 . 178.5(2) ?
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 N3 . 2.2199(19) ?
Cd1 N1 . 2.2611(19) ?
Cd1 N5 . 2.302(2) ?
Cd1 N6 . 2.307(2) ?
Cd1 S2 . 2.6207(7) ?
S1 C17 . 1.644(2) ?
S2 C18 . 1.651(2) ?
N1 C2 . 1.323(3) ?
N1 C8 . 1.406(3) ?
N2 C2 . 1.355(3) ?
N2 C3 . 1.382(3) ?
N2 H2N . 0.856(17) ?
N3 C10 . 1.323(3) ?
N3 C16 . 1.401(3) ?
N4 C10 . 1.347(3) ?
N4 C11 . 1.384(3) ?
N4 H4N . 0.844(16) ?
N5 C17 . 1.155(3) ?
N6 C18 5_666 1.152(3) ?
C1 C2 . 1.482(3) ?
C1 H1A . 0.9800 ?
C1 H1B . 0.9800 ?
C1 H1C . 0.9800 ?
C3 C4 . 1.393(3) ?
C3 C8 . 1.394(3) ?
C4 C5 . 1.379(4) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.392(4) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.385(3) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.394(3) ?
C7 H7 . 0.9500 ?
C9 C10 . 1.488(3) ?
C9 H9A . 0.9800 ?
C9 H9B . 0.9800 ?
C9 H9C . 0.9800 ?
C11 C12 . 1.388(3) ?
C11 C16 . 1.396(3) ?
C12 C13 . 1.382(3) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.401(3) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.378(3) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.391(3) ?
C15 H15 . 0.9500 ?
C18 N6 5_666 1.152(3) ?
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
N2 H2N S1 4_656 0.856(17) 2.445(18) 3.273(2) 163(2)
N4 H4N S1 3_445 0.844(16) 2.481(18) 3.281(2) 159(2)
