#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/50/2215051.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_2215051
loop_
_publ_author_name
'Zhong-Lu You'
'Seik Weng Ng'
_publ_section_title
(1,3-Propanediamine-κ²N,N')bis(thiocyanato-κN)copper(II)
_journal_coeditor_code           CI2424
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2347
_journal_page_last               m2347
_journal_paper_doi               10.1107/S1600536807039645
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Cu (N C S)2 (C3 H10 N2)]'
_chemical_formula_moiety         'C5 H10 Cu N4 S2'
_chemical_formula_sum            'C5 H10 Cu N4 S2'
_chemical_formula_weight         253.83
_chemical_name_systematic
;
(1,3-Propanediamine-κ²N,N')bis(thiocyanato-κN)\
copper(II)
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.9505(17)
_cell_length_b                   20.478(6)
_cell_length_c                   8.475(2)
_cell_measurement_reflns_used    4527
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.7
_cell_volume                     1032.7(5)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4393
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.99
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.473
_exptl_absorpt_correction_T_max  0.5548
_exptl_absorpt_correction_T_min  0.5049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.361
_refine_ls_abs_structure_details 'Flack (1983), 593 Friedel pairs'
_refine_ls_abs_structure_Flack   0.50(2)
_refine_ls_extinction_coef       0.0100(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1287
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0231
_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)+(0.0479P)²+0.1407P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0657
_reflns_number_gt                1264
_reflns_number_total             1287
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ci2424.cif
_cod_data_source_block           I
_cod_database_code               2215051
_cod_database_fobs_code          2215051
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
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
Cu Cu1 0.5000 0.701275(15) 0.5000 0.04011(15) Uani d S 1 . .
S S1 0.5000 0.80305(4) 0.0035(2) 0.0479(2) Uani d S 1 A .
S S2 0.5000 0.92135(5) 0.6725(2) 0.0766(4) Uani d S 1 A .
N N3 0.5000 0.72640(19) 0.2739(4) 0.0501(7) Uani d S 1 A .
N N4 0.5000 0.79405(14) 0.5584(5) 0.0516(8) Uani d S 1 A .
C C4 0.5000 0.75676(17) 0.1619(4) 0.0404(7) Uani d S 1 . .
C C5 0.5000 0.84648(18) 0.6040(5) 0.0481(8) Uani d S 1 . .
N N1 0.5000 0.67852(16) 0.7296(4) 0.0495(7) Uani d SPDU 1 A -1
H H11 0.6242 0.6940 0.7656 0.059 Uiso calc PR 0.25 A -1
H H12 0.3953 0.7021 0.7703 0.059 Uiso calc PR 0.25 A -1
H H13 0.5656 0.7100 0.7786 0.059 Uiso calc PR 0.25 A -2
H H14 0.3623 0.6783 0.7603 0.059 Uiso calc PR 0.25 A -2
N N2 0.5000 0.60769(14) 0.4330(4) 0.0529(9) Uani d SPDU 1 A -1
H H21 0.3721 0.6005 0.3890 0.064 Uiso calc PR 0.25 A -1
H H22 0.5999 0.6040 0.3603 0.064 Uiso calc PR 0.25 A -1
H H23 0.3616 0.5964 0.4224 0.064 Uiso calc PR 0.25 A -2
H H24 0.5587 0.6065 0.3403 0.064 Uiso calc PR 0.25 A -2
C C1 0.477(2) 0.6158(3) 0.8026(9) 0.052(2) Uani d PDU 0.25 A -1
H H1A 0.3715 0.6191 0.8896 0.063 Uiso calc PR 0.25 A -1
H H1B 0.6209 0.6025 0.8453 0.063 Uiso calc PR 0.25 A -1
C C2 0.396(2) 0.5649(4) 0.6890(11) 0.072(3) Uani d PDU 0.25 A -1
H H2A 0.2458 0.5770 0.6544 0.086 Uiso calc PR 0.25 A -1
H H2B 0.3826 0.5239 0.7453 0.086 Uiso calc PR 0.25 A -1
C C3 0.539(3) 0.5537(6) 0.5448(12) 0.064(3) Uani d PDU 0.25 A -1
H H3A 0.6960 0.5521 0.5743 0.077 Uiso calc PR 0.25 A -1
H H3B 0.5000 0.5125 0.4959 0.077 Uiso calc SPR 0.50 A -1
C C1' 0.6032(17) 0.6171(4) 0.7849(11) 0.052(2) Uani d PDU 0.25 A -2
H H1'1 0.5751 0.6111 0.8967 0.063 Uiso calc PR 0.25 A -2
H H1'2 0.7644 0.6181 0.7680 0.063 Uiso calc PR 0.25 A -2
C C2' 0.497(4) 0.5609(4) 0.6903(10) 0.072(3) Uani d PDU 0.25 A -2
H H2'1 0.3377 0.5690 0.6767 0.086 Uiso calc PR 0.25 A -2
H H2'2 0.5147 0.5202 0.7476 0.086 Uiso calc PR 0.25 A -2
C C3' 0.611(3) 0.5552(6) 0.5270(12) 0.064(3) Uani d PDU 0.25 A -2
H H3'1 0.7717 0.5626 0.5348 0.077 Uiso calc PR 0.25 A -2
H H3'2 0.5848 0.5126 0.4807 0.077 Uiso calc PR 0.25 A -2
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
_geom_angle_publ_flag
N4 Cu1 N3 89.57(16) y
N4 Cu1 N2 178.10(16) y
N3 Cu1 N2 88.53(15) y
N4 Cu1 N1 88.87(16) y
N3 Cu1 N1 178.44(16) y
N2 Cu1 N1 93.03(14) y
C4 N3 Cu1 161.8(4) ?
C5 N4 Cu1 174.8(4) ?
N3 C4 S1 178.0(4) ?
N4 C5 S2 179.1(4) ?
C1 N1 Cu1 129.0(4) ?
C1 N1 H11 105.0 ?
Cu1 N1 H11 105.0 ?
C1 N1 H12 105.0 ?
Cu1 N1 H12 105.0 ?
H11 N1 H12 105.9 ?
C3 N2 Cu1 122.4(5) ?
C3 N2 H21 106.7 ?
Cu1 N2 H21 106.7 ?
C3 N2 H22 106.7 ?
Cu1 N2 H22 106.7 ?
H21 N2 H22 106.6 ?
N1 C1 C2 112.1(6) ?
N1 C1 H1A 109.2 ?
C2 C1 H1A 109.2 ?
N1 C1 H1B 109.2 ?
C2 C1 H1B 109.2 ?
H1A C1 H1B 107.9 ?
C1 C2 C3 116.4(8) ?
C1 C2 H2A 108.2 ?
C3 C2 H2A 108.2 ?
C1 C2 H2B 108.2 ?
C3 C2 H2B 108.2 ?
H2A C2 H2B 107.3 ?
N2 C3 C2 108.6(7) ?
N2 C3 H3A 110.0 ?
C2 C3 H3A 110.0 ?
N2 C3 H3B 110.0 ?
C2 C3 H3B 110.0 ?
H3A C3 H3B 108.3 ?
C2' C1' H1'1 110.2 ?
C2' C1' H1'2 110.2 ?
H1'1 C1' H1'2 108.5 ?
C1' C2' C3' 110.1(10) ?
C1' C2' H2'1 109.6 ?
C3' C2' H2'1 109.6 ?
C1' C2' H2'2 109.6 ?
C3' C2' H2'2 109.6 ?
H2'1 C2' H2'2 108.2 ?
C2' C3' H3'1 111.1 ?
C2' C3' H3'2 111.1 ?
H3'1 C3' H3'2 109.1 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 N4 1.963(3) y
Cu1 N3 1.984(3) y
Cu1 N2 1.999(3) y
Cu1 N1 2.001(3) y
S1 C4 1.644(4) ?
S2 C5 1.639(4) ?
N3 C4 1.134(5) ?
N4 C5 1.141(5) ?
N1 C1 1.432(7) ?
N1 H11 0.86 ?
N1 H12 0.86 ?
N2 C3 1.473(9) ?
N2 H21 0.86 ?
N2 H22 0.86 ?
C1 C2 1.499(9) ?
C1 H1A 0.97 ?
C1 H1B 0.97 ?
C2 C3 1.507(9) ?
C2 H2A 0.97 ?
C2 H2B 0.97 ?
C3 H3A 0.97 ?
C3 H3B 0.97 ?
C1' C2' 1.537(10) ?
C1' H1'1 0.97 ?
C1' H1'2 0.97 ?
C2' C3' 1.545(10) ?
C2' H2'1 0.97 ?
C2' H2'2 0.97 ?
C3' H3'1 0.97 ?
C3' H3'2 0.97 ?
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
N4 Cu1 N3 C4 0
N2 Cu1 N3 C4 180
N4 Cu1 N1 C1 172.9(7)
N2 Cu1 N1 C1 -7.1(7)
N3 Cu1 N2 C3 169.4(7)
N1 Cu1 N2 C3 -10.6(7)
Cu1 N1 C1 C2 -13.6(13)
N1 C1 C2 C3 58.3(14)
Cu1 N2 C3 C2 46.8(12)
C1 C2 C3 N2 -76.4(13)
