#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/91/2229179.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_2229179
loop_
_publ_author_name
'Suleiman Gwaram, Nura'
'Ikmal Hisham, Nurul Azimah'
'Khaledi, Hamid'
'Mohd Ali, Hapipah'
_publ_section_title
;
 Di-μ-thiocyanato-κ²N:S;κ²S:N-bis({2-morpholino-N-[1-(2-pyridyl)ethylidene]ethanamine-κ³N,N',N''}(thiocyanato-κN)cadmium)
;
_journal_coeditor_code           OM2400
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m251
_journal_paper_doi               10.1107/S1600536811002480
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Cd2 (N C S)4 (C13 H19 N3 O)2]'
_chemical_formula_moiety         'C30 H38 Cd2 N10 O2 S4'
_chemical_formula_sum            'C30 H38 Cd2 N10 O2 S4'
_chemical_formula_weight         923.74
_chemical_name_systematic
;
Di-μ-thiocyanato-κ²N:S;κ²S:N-
bis({2-morpholino-N-[1-(2-pyridyl)ethylidene]ethanamine-
κ³N,N',N''}(thiocyanato-κN)cadmium)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 107.853(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.2934(2)
_cell_length_b                   26.4035(5)
_cell_length_c                   10.0111(3)
_cell_measurement_reflns_used    7745
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.27
_cell_volume                     1835.02(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15344
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    1.430
_exptl_absorpt_correction_T_max  0.9065
_exptl_absorpt_correction_T_min  0.6126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.453
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4008
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0227
_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)+(0.0141P)²+1.4854P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0469
_reflns_number_gt                3638
_reflns_number_total             4008
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om2400.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2229179
_cod_database_fobs_code          2229179
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.88459(2) 0.089861(5) 0.314896(15) 0.01292(5) Uani d . 1 . .
S S1 0.67607(7) 0.05268(2) 0.46956(6) 0.01758(11) Uani d U 1 . .
S S2 0.45365(9) 0.20002(2) -0.00994(6) 0.02685(13) Uani d U 1 . .
O O1 1.0113(3) 0.19368(6) 0.65208(18) 0.0309(4) Uani d . 1 . .
N N1 0.7974(2) 0.02944(6) 0.12874(18) 0.0153(4) Uani d . 1 . .
N N2 0.9534(2) 0.11963(7) 0.11679(18) 0.0166(4) Uani d . 1 . .
N N3 1.0711(3) 0.16656(7) 0.38989(19) 0.0166(4) Uani d . 1 . .
N N4 0.6008(3) 0.13692(7) 0.2228(2) 0.0214(4) Uani d . 1 . .
N N5 1.1395(3) 0.03924(7) 0.42969(19) 0.0194(4) Uani d . 1 . .
C C1 0.7455(3) -0.01826(8) 0.1403(2) 0.0181(4) Uani d . 1 . .
H H1 0.7435 -0.0300 0.2296 0.022 Uiso calc R 1 . .
C C2 0.6942(3) -0.05172(9) 0.0281(2) 0.0217(5) Uani d . 1 . .
H H2 0.6593 -0.0857 0.0402 0.026 Uiso calc R 1 . .
C C3 0.6952(3) -0.03430(9) -0.1020(2) 0.0226(5) Uani d . 1 . .
H H3 0.6596 -0.0561 -0.1812 0.027 Uiso calc R 1 . .
C C4 0.7486(3) 0.01527(9) -0.1153(2) 0.0203(5) Uani d . 1 . .
H H4 0.7495 0.0279 -0.2040 0.024 Uiso calc R 1 . .
C C5 0.8011(3) 0.04641(8) 0.0022(2) 0.0163(4) Uani d . 1 . .
C C6 0.8705(3) 0.09967(8) -0.0016(2) 0.0183(4) Uani d . 1 . .
C C7 0.8396(4) 0.12483(10) -0.1409(2) 0.0303(6) Uani d . 1 . .
H H7A 0.9115 0.1567 -0.1277 0.045 Uiso calc R 1 . .
H H7B 0.7020 0.1317 -0.1840 0.045 Uiso calc R 1 . .
H H7C 0.8849 0.1025 -0.2023 0.045 Uiso calc R 1 . .
C C8 1.0294(3) 0.17102(8) 0.1330(2) 0.0212(5) Uani d . 1 . .
H H8A 0.9225 0.1957 0.1163 0.025 Uiso calc R 1 . .
H H8B 1.0991 0.1775 0.0640 0.025 Uiso calc R 1 . .
C C9 1.1654(3) 0.17704(8) 0.2811(2) 0.0203(5) Uani d . 1 . .
H H9A 1.2757 0.1537 0.2943 0.024 Uiso calc R 1 . .
H H9B 1.2165 0.2120 0.2932 0.024 Uiso calc R 1 . .
C C10 1.2234(3) 0.16048(9) 0.5272(2) 0.0228(5) Uani d . 1 . .
H H10A 1.3057 0.1911 0.5475 0.027 Uiso calc R 1 . .
H H10B 1.3056 0.1311 0.5230 0.027 Uiso calc R 1 . .
C C11 1.1333(4) 0.15259(9) 0.6422(2) 0.0285(5) Uani d . 1 . .
H H11A 1.0571 0.1209 0.6241 0.034 Uiso calc R 1 . .
H H11B 1.2364 0.1488 0.7328 0.034 Uiso calc R 1 . .
C C12 0.8634(4) 0.19928(9) 0.5217(3) 0.0266(5) Uani d . 1 . .
H H12A 0.7776 0.2276 0.5287 0.032 Uiso calc R 1 . .
H H12B 0.7852 0.1680 0.5009 0.032 Uiso calc R 1 . .
C C13 0.9472(3) 0.20975(8) 0.4035(2) 0.0207(5) Uani d . 1 . .
H H13A 0.8418 0.2144 0.3145 0.025 Uiso calc R 1 . .
H H13B 1.0243 0.2413 0.4233 0.025 Uiso calc R 1 . .
C C14 0.5395(3) 0.16332(8) 0.1265(2) 0.0164(4) Uani d U 1 . .
C C15 0.7869(3) -0.00104(8) 0.5288(2) 0.0142(4) Uani d U 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'
S S 0.1246 0.1234 '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
N5 Cd1 N2 . . 105.70(6) ?
N5 Cd1 N4 . . 171.05(6) ?
N2 Cd1 N4 . . 83.16(6) ?
N5 Cd1 N1 . . 89.01(6) ?
N2 Cd1 N1 . . 68.63(6) ?
N4 Cd1 N1 . . 93.18(6) ?
N5 Cd1 N3 . . 92.28(6) ?
N2 Cd1 N3 . . 74.62(6) ?
N4 Cd1 N3 . . 91.32(6) ?
N1 Cd1 N3 . . 142.12(6) ?
N5 Cd1 S1 . . 90.78(5) ?
N2 Cd1 S1 . . 158.33(4) ?
N4 Cd1 S1 . . 80.32(5) ?
N1 Cd1 S1 . . 98.30(4) ?
N3 Cd1 S1 . . 119.52(4) ?
C15 S1 Cd1 . . 102.77(7) ?
C12 O1 C11 . . 109.23(17) ?
C1 N1 C5 . . 118.92(18) ?
C1 N1 Cd1 . . 125.41(14) ?
C5 N1 Cd1 . . 115.67(13) ?
C6 N2 C8 . . 123.20(19) ?
C6 N2 Cd1 . . 119.39(14) ?
C8 N2 Cd1 . . 113.20(13) ?
C9 N3 C10 . . 108.44(17) ?
C9 N3 C13 . . 110.88(17) ?
C10 N3 C13 . . 107.49(17) ?
C9 N3 Cd1 . . 105.72(12) ?
C10 N3 Cd1 . . 112.63(13) ?
C13 N3 Cd1 . . 111.67(13) ?
C14 N4 Cd1 . . 135.42(16) ?
C15 N5 Cd1 3_756 . 154.57(17) ?
N1 C1 C2 . . 123.1(2) ?
N1 C1 H1 . . 118.5 ?
C2 C1 H1 . . 118.5 ?
C3 C2 C1 . . 118.2(2) ?
C3 C2 H2 . . 120.9 ?
C1 C2 H2 . . 120.9 ?
C2 C3 C4 . . 119.2(2) ?
C2 C3 H3 . . 120.4 ?
C4 C3 H3 . . 120.4 ?
C3 C4 C5 . . 119.4(2) ?
C3 C4 H4 . . 120.3 ?
C5 C4 H4 . . 120.3 ?
N1 C5 C4 . . 121.2(2) ?
N1 C5 C6 . . 116.03(18) ?
C4 C5 C6 . . 122.76(19) ?
N2 C6 C7 . . 125.3(2) ?
N2 C6 C5 . . 115.71(19) ?
C7 C6 C5 . . 118.9(2) ?
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 . . 108.61(18) ?
N2 C8 H8A . . 110.0 ?
C9 C8 H8A . . 110.0 ?
N2 C8 H8B . . 110.0 ?
C9 C8 H8B . . 110.0 ?
H8A C8 H8B . . 108.3 ?
N3 C9 C8 . . 112.74(18) ?
N3 C9 H9A . . 109.0 ?
C8 C9 H9A . . 109.0 ?
N3 C9 H9B . . 109.0 ?
C8 C9 H9B . . 109.0 ?
H9A C9 H9B . . 107.8 ?
N3 C10 C11 . . 110.18(19) ?
N3 C10 H10A . . 109.6 ?
C11 C10 H10A . . 109.6 ?
N3 C10 H10B . . 109.6 ?
C11 C10 H10B . . 109.6 ?
H10A C10 H10B . . 108.1 ?
O1 C11 C10 . . 112.1(2) ?
O1 C11 H11A . . 109.2 ?
C10 C11 H11A . . 109.2 ?
O1 C11 H11B . . 109.2 ?
C10 C11 H11B . . 109.2 ?
H11A C11 H11B . . 107.9 ?
O1 C12 C13 . . 111.19(19) ?
O1 C12 H12A . . 109.4 ?
C13 C12 H12A . . 109.4 ?
O1 C12 H12B . . 109.4 ?
C13 C12 H12B . . 109.4 ?
H12A C12 H12B . . 108.0 ?
N3 C13 C12 . . 109.51(18) ?
N3 C13 H13A . . 109.8 ?
C12 C13 H13A . . 109.8 ?
N3 C13 H13B . . 109.8 ?
C12 C13 H13B . . 109.8 ?
H13A C13 H13B . . 108.2 ?
N4 C14 S2 . . 179.4(2) ?
N5 C15 S1 3_756 . 178.34(19) ?
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 N5 . 2.2922(18) ?
Cd1 N2 . 2.3267(17) ?
Cd1 N4 . 2.3469(18) ?
Cd1 N1 . 2.3866(17) ?
Cd1 N3 . 2.4269(17) ?
Cd1 S1 . 2.6679(5) ?
S1 C15 . 1.650(2) ?
S2 C14 . 1.635(2) ?
O1 C12 . 1.423(3) ?
O1 C11 . 1.426(3) ?
N1 C1 . 1.330(3) ?
N1 C5 . 1.352(3) ?
N2 C6 . 1.268(3) ?
N2 C8 . 1.456(3) ?
N3 C9 . 1.482(3) ?
N3 C10 . 1.487(3) ?
N3 C13 . 1.487(3) ?
N4 C14 . 1.162(3) ?
N5 C15 3_756 1.158(3) ?
C1 C2 . 1.388(3) ?
C1 H1 . 0.9500 ?
C2 C3 . 1.383(3) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.384(3) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.389(3) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.499(3) ?
C6 C7 . 1.498(3) ?
C7 H7A . 0.9800 ?
C7 H7B . 0.9800 ?
C7 H7C . 0.9800 ?
C8 C9 . 1.518(3) ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C10 C11 . 1.505(3) ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
C12 C13 . 1.514(3) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C15 N5 3_756 1.158(3) ?
