#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2008362.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_2008362
loop_
_publ_author_name
'Vr\'abel, V.'
'Garaj, J.'
'Siv\'y, J.'
'Oktavec, D.'
_publ_section_title
;
 Aquadiisothiocyanato(<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethylethylenediamine-<i>N</i>,<i>N</i>')copper(II)
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              551
_journal_page_last               553
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[Cu (N1 C1 S1)2 (C6 H16 N2) (H2 O1)]'
_chemical_formula_moiety         'C8 H18 Cu N4 O S2'
_chemical_formula_sum            'C8 H18 Cu N4 O S2'
_chemical_formula_weight         313.92
_chemical_name_systematic
;
Aqua(N,N,N',N'-tetramethylethylenediamine)diisothiocyanato-copper(II)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.
_cell_angle_beta                 98.40(2)
_cell_angle_gamma                90.
_cell_formula_units_Z            2
_cell_length_a                   7.095(2)
_cell_length_b                   11.761(4)
_cell_length_c                   8.419(3)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.8
_cell_measurement_theta_min      11.4
_cell_volume                     695.0(4)
_computing_cell_refinement       'Syntex P2~1~ software'
_computing_data_collection       'Syntex P2~1~ software'
_computing_data_reduction        'XP21 (Pavel\<c\'ik, 1987)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Syntex P2~1~'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2132
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.858
_exptl_absorpt_correction_T_max  0.830
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_type   '\y scan (North et al., 1968)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_meas      1.510(10)
_exptl_crystal_density_method    'flotation in bromoform/hexane'
_exptl_crystal_description       block
_exptl_crystal_F_000             326
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.269
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.100(13)
_refine_ls_extinction_coef       0.0047(17)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   0.830
_refine_ls_goodness_of_fit_obs   0.901
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.830
_refine_ls_restrained_S_obs      0.901
_refine_ls_R_factor_all          0.033
_refine_ls_R_factor_obs          0.024
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0392P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.060
_refine_ls_wR_factor_obs         0.059
_reflns_number_observed          1786
_reflns_number_total             2132
_reflns_observed_criterion       I>2\s(I)
_[local]_cod_data_source_file    gs1023.cif
_[local]_cod_data_source_block   gs1023
_[local]_cod_cif_authors_sg_H-M  'P 21'
_cod_original_cell_volume        695.1(4)
_cod_database_code               2008362
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
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
Cu1 0.02935(14) 0.03057(14) 0.03340(14) -0.0051(2) 0.00397(10) -0.0012(2)
S1 0.0577(5) 0.0542(5) 0.0393(4) -0.0101(4) -0.0030(4) -0.0032(4)
S2 0.0731(6) 0.0551(6) 0.0514(5) -0.0337(5) 0.0059(4) 0.0033(4)
O1 0.067(2) 0.057(2) 0.0476(15) 0.0210(14) 0.0155(14) 0.0079(14)
N1 0.0392(12) 0.048(2) 0.0340(12) -0.0033(11) 0.0025(10) -0.0037(10)
N2 0.0337(12) 0.0418(13) 0.0505(15) -0.0033(11) 0.0169(11) -0.0060(12)
N3 0.0511(14) 0.054(2) 0.0409(13) -0.0053(13) -0.0003(12) -0.0053(12)
N4 0.047(2) 0.054(2) 0.055(2) -0.0200(14) 0.0076(12) 0.0006(14)
C1 0.050(2) 0.078(3) 0.059(2) -0.023(2) 0.001(2) -0.022(2)
C2 0.030(2) 0.078(3) 0.074(3) -0.015(2) 0.010(2) -0.019(2)
C3 0.070(3) 0.072(3) 0.053(2) 0.017(3) -0.003(2) 0.011(2)
C4 0.062(2) 0.071(3) 0.044(2) 0.006(2) 0.014(2) -0.010(2)
C5 0.049(2) 0.079(3) 0.067(2) 0.010(2) 0.021(2) -0.022(2)
C6 0.065(3) 0.057(3) 0.089(3) -0.009(2) 0.034(3) 0.019(2)
C7 0.0418(15) 0.0362(14) 0.0338(13) 0.0051(13) 0.0056(11) 0.0023(12)
C8 0.0362(15) 0.043(2) 0.0369(13) -0.0055(13) 0.0056(12) -0.0038(12)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_type_symbol
Cu1 0.13862(4) 0.2500 0.34416(3) 0.03117(9) Uani d 1 Cu
S1 0.46100(14) 0.38961(9) 0.82799(10) 0.0514(2) Uani d 1 S
S2 0.5473(2) 0.54013(10) 0.23124(12) 0.0602(3) Uani d 1 S
O1 0.3044(5) 0.0775(3) 0.3793(4) 0.0566(7) Uani d 1 O
H1 0.362(7) 0.041(5) 0.320(6) 0.060(14) Uiso d 1 H
H2 0.313(8) 0.066(5) 0.455(7) 0.069(19) Uiso d 1 H
N1 0.0195(4) 0.2162(2) 0.1155(3) 0.0407(6) Uani d 1 N
N2 -0.1145(4) 0.2002(2) 0.4102(3) 0.0409(6) Uani d 1 N
N3 0.2433(4) 0.2900(3) 0.5659(3) 0.0494(7) Uani d 1 N
N4 0.3239(4) 0.3524(3) 0.2665(4) 0.0518(7) Uani d 1 N
C1 -0.1415(6) 0.1403(5) 0.1298(6) 0.0632(12) Uani d 1 C
H1A -0.064(7) 0.057(5) 0.163(5) 0.067(13) Uiso d 1 H
H1B -0.238(7) 0.141(5) 0.030(7) 0.093(18) Uiso d 1 H
C2 -0.2472(5) 0.1863(5) 0.2580(6) 0.0604(11) Uani d 1 C
H2A -0.306(7) 0.280(5) 0.236(6) 0.072(15) Uiso d 1 H
H2B -0.335(6) 0.130(4) 0.286(6) 0.066(13) Uiso d 1 H
C3 -0.0408(8) 0.3226(5) 0.0310(6) 0.0665(12) Uani d 1 C
H3A 0.056(7) 0.382(4) 0.032(5) 0.059(13) Uiso d 1 H
H3B -0.132(8) 0.372(6) 0.101(7) 0.083(16) Uiso d 1 H
H3C -0.128(7) 0.294(5) -0.059(6) 0.082(15) Uiso d 1 H
C4 0.1513(7) 0.1568(4) 0.0217(5) 0.0586(10) Uani d 1 C
H4A 0.277(7) 0.216(5) 0.021(6) 0.086(16) Uiso d 1 H
H4B 0.081(6) 0.130(4) -0.070(6) 0.058(12) Uiso d 1 H
H4C 0.194(8) 0.099(5) 0.072(7) 0.084(18) Uiso d 1 H
C5 -0.1944(6) 0.2870(4) 0.5083(6) 0.0636(11) Uani d 1 C
H5A -0.186(6) 0.360(5) 0.438(6) 0.068(14) Uiso d 1 H
H5B -0.115(7) 0.308(5) 0.600(6) 0.078(15) Uiso d 1 H
H5C -0.329(6) 0.269(5) 0.522(5) 0.076(13) Uiso d 1 H
C6 -0.0922(8) 0.0922(4) 0.4971(7) 0.0683(12) Uani d 1 C
H6A -0.008(7) 0.100(4) 0.586(6) 0.055(12) Uiso d 1 H
H6B -0.040(7) 0.032(6) 0.418(6) 0.084(16) Uiso d 1 H
H6C -0.227(6) 0.072(4) 0.516(5) 0.069(13) Uiso d 1 H
C7 0.3348(4) 0.3312(3) 0.6733(3) 0.0373(6) Uani d 1 C
C8 0.4168(4) 0.4311(3) 0.2513(4) 0.0387(6) Uani d 1 C
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'
O O 0.0106 0.0060 '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 89.48(13) yes
N4 Cu1 N1 90.60(12) yes
N3 Cu1 N1 176.65(13) yes
N4 Cu1 N2 157.64(13) ?
N3 Cu1 N2 92.05(12) ?
N1 Cu1 N2 86.61(11) yes
N4 Cu1 O1 102.99(14) yes
N3 Cu1 O1 88.53(13) yes
N1 Cu1 O1 94.72(12) yes
N2 Cu1 O1 99.35(12) yes
Cu1 O1 H1 132.(3) ?
Cu1 O1 H2 106.(5) ?
H1 O1 H2 121.(6) ?
C3 N1 C1 112.5(4) ?
C3 N1 C4 107.7(3) ?
C1 N1 C4 108.4(3) ?
C3 N1 Cu1 110.1(3) ?
C1 N1 Cu1 105.2(2) ?
C4 N1 Cu1 112.9(2) ?
C6 N2 C5 110.0(4) ?
C6 N2 C2 110.2(4) ?
C5 N2 C2 108.2(3) ?
C6 N2 Cu1 110.5(3) ?
C5 N2 Cu1 112.2(2) ?
C2 N2 Cu1 105.6(2) ?
C7 N3 Cu1 161.4(3) ?
C8 N4 Cu1 161.7(3) ?
N1 C1 C2 108.5(3) ?
N1 C1 H1A 101.(2) ?
C2 C1 H1A 114.(2) ?
N1 C1 H1B 112.(3) ?
C2 C1 H1B 104.(3) ?
H1A C1 H1B 117.(4) ?
N2 C2 C1 109.8(3) ?
N2 C2 H2A 101.(2) ?
C1 C2 H2A 115.(2) ?
N2 C2 H2B 103.(3) ?
C1 C2 H2B 110.(3) ?
H2A C2 H2B 117.(3) ?
N1 C3 H3A 117.(3) ?
N1 C3 H3B 110.(3) ?
H3A C3 H3B 95.(4) ?
N1 C3 H3C 101.(3) ?
H3A C3 H3C 128.(4) ?
H3B C3 H3C 104.(4) ?
N1 C4 H4A 106.(3) ?
N1 C4 H4B 108.(3) ?
H4A C4 H4B 123.(4) ?
N1 C4 H4C 109.(4) ?
H4A C4 H4C 106.(5) ?
H4B C4 H4C 105.(5) ?
N2 C5 H5A 101.(3) ?
N2 C5 H5B 114.(3) ?
H5A C5 H5B 100.(4) ?
N2 C5 H5C 112.(3) ?
H5A C5 H5C 112.(4) ?
H5B C5 H5C 116.(4) ?
N2 C6 H6A 110.(3) ?
N2 C6 H6B 106.(3) ?
H6A C6 H6B 110.(4) ?
N2 C6 H6C 104.(3) ?
H6A C6 H6C 115.(4) ?
H6B C6 H6C 112.(4) ?
N3 C7 S1 178.8(3) yes
N4 C8 S2 179.6(3) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 N4 1.964(3) yes
Cu1 N3 1.963(3) yes
Cu1 N1 2.026(3) yes
Cu1 N2 2.042(3) yes
Cu1 O1 2.342(3) yes
S1 C7 1.622(3) yes
S2 C8 1.605(3) yes
O1 H1 0.81(6) ?
O1 H2 0.64(6) ?
N1 C3 1.471(5) ?
N1 C1 1.468(5) yes
N1 C4 1.484(5) ?
N2 C6 1.462(5) ?
N2 C5 1.478(5) ?
N2 C2 1.484(5) yes
N3 C7 1.141(4) yes
N4 C8 1.154(4) yes
C1 C2 1.502(6) yes
C1 H1A 1.14(5) ?
C1 H1B 1.00(6) ?
C2 H2A 1.19(6) ?
C2 H2B 0.96(5) ?
C3 H3A 0.98(5) ?
C3 H3B 1.11(7) ?
C3 H3C 0.96(5) ?
C4 H4A 1.13(5) ?
C4 H4B 0.91(5) ?
C4 H4C 0.84(6) ?
C5 H5A 1.04(5) ?
C5 H5B 0.92(5) ?
C5 H5C 1.00(4) ?
C6 H6A 0.89(5) ?
C6 H6B 1.07(6) ?
C6 H6C 1.02(5) ?
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 N1 C3 -56.0(3)
N3 Cu1 N1 C3 35.(2)
N2 Cu1 N1 C3 101.8(3)
O1 Cu1 N1 C3 -159.1(3)
N4 Cu1 N1 C1 -177.5(3)
N3 Cu1 N1 C1 -86.(2)
N2 Cu1 N1 C1 -19.7(3)
O1 Cu1 N1 C1 79.4(3)
N4 Cu1 N1 C4 64.4(3)
N3 Cu1 N1 C4 156.(2)
N2 Cu1 N1 C4 -137.8(3)
O1 Cu1 N1 C4 -38.6(3)
N4 Cu1 N2 C6 -166.3(4)
N3 Cu1 N2 C6 -72.7(3)
N1 Cu1 N2 C6 110.4(3)
O1 Cu1 N2 C6 16.1(3)
N4 Cu1 N2 C5 -43.1(5)
N3 Cu1 N2 C5 50.5(3)
N1 Cu1 N2 C5 -126.4(3)
O1 Cu1 N2 C5 139.4(3)
N4 Cu1 N2 C2 74.6(4)
N3 Cu1 N2 C2 168.2(3)
N1 Cu1 N2 C2 -8.7(3)
O1 Cu1 N2 C2 -103.0(3)
N4 Cu1 N3 C7 0.6(9)
N1 Cu1 N3 C7 -91.(2)
N2 Cu1 N3 C7 -157.1(9)
O1 Cu1 N3 C7 103.6(9)
N3 Cu1 N4 C8 -45.2(9)
N1 Cu1 N4 C8 131.4(9)
N2 Cu1 N4 C8 48.9(10)
O1 Cu1 N4 C8 -133.6(9)
C3 N1 C1 C2 -75.5(5)
C4 N1 C1 C2 165.5(4)
Cu1 N1 C1 C2 44.4(4)
C6 N2 C2 C1 -83.6(5)
C5 N2 C2 C1 156.1(4)
Cu1 N2 C2 C1 35.8(4)
N1 C1 C2 N2 -55.4(5)
Cu1 N3 C7 S1 147.(14)
Cu1 N4 C8 S2 9.E1(5)