#------------------------------------------------------------------------------
#$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/2008252.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_2008252
loop_
_publ_author_name
'Moore, S. L.'
'Squattrito, P. J.'
_publ_section_title
;
Bis(1,3-propanediamine-N,N')bis(thiocyanato-N)nickel(II)
;
_journal_issue 3
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 332
_journal_page_last 334
_journal_volume 55
_journal_year 1999
_chemical_formula_iupac '[Ni (N C S)2 (C3 H10 N2)2]'
_chemical_formula_moiety 'C8 H20 N6 Ni S2'
_chemical_formula_structural
;
[Ni (NCS)2 (C3 N2 H10)2]
;
_chemical_formula_sum 'C8 H20 N6 Ni S2'
_chemical_formula_weight 323.11
_chemical_melting_point 483
_space_group_IT_number 45
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'I 2 -2c'
_symmetry_space_group_name_H-M 'I b a 2'
_audit_creation_method 'from TEXRAY.INF file'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.579(2)
_cell_length_b 17.550(2)
_cell_length_c 11.111(5)
_cell_measurement_reflns_used 19
_cell_measurement_temperature 296
_cell_measurement_theta_max 19.8
_cell_measurement_theta_min 16.4
_cell_volume 1477.9(8)
_computing_cell_refinement 'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1988)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1991)'
_computing_molecular_graphics 'ORTEPII (Johnson, 1976)'
_computing_publication_material TEXSAN
_computing_structure_refinement TEXSAN
_computing_structure_solution 'MITHRIL (Gilmore, 1983)'
_diffrn_ambient_temperature 296
_diffrn_measurement_device_type 'Rigaku AFC-6S'
_diffrn_measurement_method \w-2\q
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'X-ray tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.7107
_diffrn_reflns_av_R_equivalents 0.00
_diffrn_reflns_av_sigmaI/netI 0.035
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 1526
_diffrn_reflns_theta_max 25
_diffrn_standards_decay_% 0.00
_diffrn_standards_interval_count 150
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 1.58
_exptl_absorpt_correction_T_max 0.881
_exptl_absorpt_correction_T_min 0.775
_exptl_absorpt_correction_type '\y scan'
_exptl_absorpt_process_details '(North et al., 1968)'
_exptl_crystal_colour blue-violet
_exptl_crystal_density_diffrn 1.452
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 680
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.08
_refine_diff_density_max 0.67
_refine_diff_density_min -0.29
_refine_ls_abs_structure_details
'Flack (1983); refined using a complete set of Friedel pairs'
_refine_ls_abs_structure_Flack -0.019(16)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 2.12
_refine_ls_hydrogen_treatment refxyz
_refine_ls_matrix_type full
_refine_ls_number_constraints 0
_refine_ls_number_parameters 107
_refine_ls_number_reflns 1370
_refine_ls_number_restraints 0
_refine_ls_R_factor_gt 0.040
_refine_ls_shift/su_max 0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details 'w = 4F~o~^2^/\s^2^(F~o~^2^)'
_refine_ls_weighting_scheme sigma
_refine_ls_wR_factor_ref 0.050
_reflns_number_gt 1370
_reflns_number_total 1526
_reflns_threshold_expression I>0
_[local]_cod_data_source_file fr1148.cif
_[local]_cod_data_source_block FR1148
_[local]_cod_chemical_formula_sum_orig 'C8 H20 N6 Ni S2 '
_cod_original_cell_volume 1477.0(10)
_cod_database_code 2008252
loop_
_symmetry_equiv_pos_as_xyz
' +x, +y, +z'
' -x, -y, +z'
' -x, +y,1/2+z'
' +x, -y,1/2+z'
' 1/2+x, 1/2+y, 1/2+z'
' 1/2-x, 1/2-y, 1/2+z'
' 1/2-x, 1/2+y, +z'
' 1/2+x, 1/2-y, +z'
loop_
_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_occupancy
Ni 0 0 0 0.02410(10) Uij 1.0
S 0.45789(10) 0.12160(6) 0.22870(10) 0.0654(3) Uij 1.0
N1 0.1546(3) 0.0546(2) 0.1334(3) 0.0329(9) Uij 1.0
N2 0.1270(3) 0.0671(2) -0.1359(3) 0.0323(9) Uij 1.0
N3 -0.1948(3) 0.0867(2) 0.0028(4) 0.0343(7) Uij 1.0
C1 0.2825(4) 0.0811(2) 0.1718(3) 0.0319(9) Uij 1.0
C2 0.1456(4) 0.1502(2) -0.1146(3) 0.0340(10) Uij 1.0
C3 -0.0303(5) 0.1900(2) -0.0986(3) 0.0390(10) Uij 1.0
C4 -0.1341(4) 0.1661(2) 0.0126(5) 0.0394(10) Uij 1.0
H(1) 0.220(4) 0.049(2) -0.146(3) 0.0351 Uij 1.0
H(2) 0.057(3) 0.059(2) -0.205(3) 0.0351 Uij 1.0
H(3) 0.215(4) 0.160(2) -0.045(3) 0.0419 Uij 1.0
H(4) 0.201(4) 0.176(2) -0.187(3) 0.0419 Uij 1.0
H(5) -0.002(5) 0.248(2) -0.092(3) 0.0434 Uij 1.0
H(6) -0.105(4) 0.184(2) -0.172(3) 0.0434 Uij 1.0
H(7) -0.050(5) 0.176(2) 0.072(3) 0.0446 Uij 1.0
H(8) -0.235(4) 0.2000(10) 0.022(3) 0.0446 Uij 1.0
H(9) -0.255(5) 0.074(2) 0.044(3) 0.0388 Uij 1.0
H(10) -0.259(5) 0.081(2) -0.063(3) 0.0388 Uij 1.0
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ni 0.0215(2) 0.0288(2) 0.0220(2) -0.0031(3) 0.0000 0.0000
S 0.0310(4) 0.0955(7) 0.0696(9) -0.0151(4) 0.0002(6) -0.0364(7)
N1 0.032(2) 0.036(2) 0.030(2) -0.0050(10) -0.0050(10) -0.0020(10)
N2 0.029(2) 0.036(2) 0.033(2) -0.0030(10) 0.0030(10) -0.0010(10)
N3 0.0280(10) 0.0410(10) 0.0340(10) -0.0010(10) 0.004(2) 0.005(2)
C1 0.033(2) 0.037(2) 0.026(2) 0.0020(10) 0.006(2) -0.003(2)
C2 0.036(2) 0.031(2) 0.035(2) -0.008(2) 0.004(2) 0.005(2)
C3 0.042(2) 0.034(2) 0.041(2) -0.002(2) -0.003(2) 0.007(2)
C4 0.037(2) 0.032(2) 0.050(2) 0.0080(10) 0.006(2) -0.002(2)
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni 0.285 1.113 'International Tables'
S 0.110 0.124 'International Tables'
N 0.004 0.003 'International Tables'
C 0.002 0.002 'International Tables'
H 0.000 0.000 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
1 5 0
-1 5 0
1 2 -3
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Ni N1 2_555 91.2(2) yes
N1 Ni N2 ? 89.80(10) yes
N1 Ni N2 2_555 171.90(10) yes
N1 Ni N3 ? 92.80(10) yes
N1 Ni N3 2_555 86.00(10) yes
N2 Ni N2 2_555 90.4(2) yes
N2 Ni N3 ? 85.90(10) yes
N2 Ni N3 2_555 95.30(10) yes
N3 Ni N3 2_555 178.3(3) yes
Ni N1 C1 ? 154.6(3) yes
Ni N2 C2 ? 118.0(2) yes
Ni N3 C4 ? 117.6(2) yes
S C1 N1 ? 177.5(3) yes
N2 C2 C3 ? 112.9(3) yes
C2 C3 C4 ? 115.0(3) yes
N3 C4 C3 ? 111.3(4) yes
Ni N2 H(1) ? 106(2) no
Ni N2 H(2) ? 103.0(10) no
C2 N2 H(1) ? 109(2) no
C2 N2 H(2) ? 109.0(10) no
H(1) N2 H(2) ? 109(3) no
Ni N3 H(9) ? 104(3) no
Ni N3 H(10) ? 107(2) no
C4 N3 H(9) ? 117(3) no
C4 N3 H(10) ? 109(2) no
H(9) N3 H(10) ? 98(3) no
N2 C2 H(3) ? 111.0(10) no
N2 C2 H(4) ? 110.0(10) no
C3 C2 H(3) ? 107.0(10) no
C3 C2 H(4) ? 104.0(10) no
H(3) C2 H(4) ? 109(2) no
C2 C3 H(5) ? 106(2) no
C2 C3 H(6) ? 110.0(10) no
C4 C3 H(5) ? 108.0(10) no
C4 C3 H(6) ? 109.0(10) no
H(5) C3 H(6) ? 105(2) no
N3 C4 H(7) ? 115(2) no
N3 C4 H(8) ? 110.0(10) no
C3 C4 H(7) ? 99(2) no
C3 C4 H(8) ? 108(2) no
H(7) C4 H(8) ? 110(2) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ni N1 2.118(3) yes
Ni N2 2.143(3) yes
Ni N3 2.121(2) yes
S C1 1.635(3) yes
N1 C1 1.157(4) yes
N2 C2 1.484(4) yes
N3 C4 1.471(4) yes
C2 C3 1.515(5) yes
C3 C4 1.523(6) yes
N2 H(1) 0.78(3) no
N2 H(2) 0.94(3) no
N3 H(9) 0.68(4) no
N3 H(10) 0.88(4) no
C2 H(3) 0.95(3) no
C2 H(4) 1.01(3) no
C3 H(5) 1.03(3) no
C3 H(6) 1.00(3) no
C4 H(7) 0.93(3) no
C4 H(8) 0.97(3) no