#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006548.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_2006548
loop_
_publ_author_name
'Kurihara, H.'
'Nishikiori, S.-I.'
'Iwamoto, T.'
_publ_section_title
;
 Monodentate Ligation of Tetracyanonickelate(II):
 (2-Aminoethanol)[<i>N</i>-(2-aminoethyl)-1,2-ethanediamine][tetracyanonickelato(II)]copper(II)--Water
 (1/2)
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1409
_journal_page_last               1411
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac
'[Cu Ni (CN)4 (C4 H13 N3) (C2 H7 N O)], 2H2 O'
_chemical_formula_moiety         '[Cu(C6 H20 N4 O){Ni(CN)4}], 2H2 O'
_chemical_formula_structural
'(Ni (C N)4) (Cd (C4 H13 N3) (C2 H7 N O) (H2 O)2 '
_chemical_formula_sum            'C10 H24 Cu N8 Ni O3'
_chemical_formula_weight         426.62
_chemical_name_common            '[Cu{Ni(CN)~4~}(dien)(mea)].2H~2~O'
_chemical_name_systematic
;
Tetracyanonickelato(II){N-(2-aminoethyl)-1,2-ethanediamine}(2-aminoeth
anol)copper(II)-water(1/2)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.90(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.097(5)
_cell_length_b                   9.869(5)
_cell_length_c                   17.325(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.5
_cell_measurement_theta_min      12.9
_cell_volume                     1833.6(13)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
1988)
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'AFC5 Rigaku Denki diffractometer'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'AFC5 Rigaku Denki sealed tube X-ray source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4793
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.211
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_meas      1.540(10)
_exptl_crystal_density_method    floatation
_exptl_crystal_description       column
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.719
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.102
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_obs      1.102
_refine_ls_R_factor_obs          0.0433
_refine_ls_shift/esd_max         0.100
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0629P)^2^+0.9030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_obs         0.1087
_reflns_number_observed          3209
_reflns_number_total             4688
_reflns_observed_criterion       >3sigma(F)
_[local]_cod_data_source_file    ab1476.cif
_[local]_cod_data_source_block   NiCudien
_cod_original_cell_volume        1834.0(10)
_cod_database_code               2006548
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Cu 0.0301(2) 0.0355(3) 0.0308(2) 0.0008(2) 0.0128(2) -0.0004(2)
Ni 0.0413(3) 0.0311(3) 0.0293(3) -0.0012(2) 0.0128(2) 0.0023(2)
C1 0.046(2) 0.032(2) 0.040(2) 0.002(2) 0.019(2) -0.001(2)
N1 0.071(3) 0.045(2) 0.048(2) 0.007(2) 0.028(2) 0.009(2)
C2 0.039(2) 0.047(2) 0.035(2) -0.005(2) 0.011(2) -0.002(2)
N2 0.054(2) 0.065(3) 0.057(2) 0.000(2) 0.019(2) -0.017(2)
C3 0.039(2) 0.049(2) 0.036(2) -0.002(2) 0.013(2) 0.005(2)
N3 0.060(3) 0.060(3) 0.048(2) 0.003(2) 0.015(2) 0.019(2)
C4 0.056(3) 0.032(2) 0.033(2) 0.001(2) 0.013(2) 0.008(2)
N4 0.077(3) 0.039(2) 0.045(2) 0.009(2) 0.025(2) 0.002(2)
N11 0.050(3) 0.065(3) 0.053(2) 0.010(2) 0.031(2) 0.006(2)
C12 0.083(4) 0.067(4) 0.042(3) 0.014(3) 0.036(3) -0.001(3)
C13 0.073(4) 0.055(3) 0.031(2) 0.003(3) 0.012(2) -0.004(2)
N14 0.051(2) 0.029(2) 0.036(2) 0.004(2) 0.010(2) 0.001(2)
C15 0.032(2) 0.046(3) 0.049(2) -0.001(2) 0.002(2) -0.006(2)
C16 0.033(2) 0.040(3) 0.059(3) -0.006(2) 0.016(2) -0.002(2)
N17 0.034(2) 0.036(2) 0.037(2) 0.001(2) 0.0160(10) 0.002(2)
N21 0.033(2) 0.031(2) 0.042(2) -0.002(2) 0.016(2) -0.0002(15)
C22 0.030(2) 0.046(3) 0.054(3) 0.003(2) 0.006(2) -0.003(2)
C23 0.049(3) 0.038(2) 0.049(2) 0.008(2) 0.009(2) 0.008(2)
O24 0.039(2) 0.031(2) 0.055(2) 0.0020(10) 0.0130(10) -0.0010(10)
OW1 0.062(2) 0.048(2) 0.058(2) 0.016(2) 0.028(2) 0.009(2)
OW2 0.067(2) 0.075(3) 0.076(2) 0.009(2) 0.029(2) -0.025(2)
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
Cu 0.34230(4) 0.18920(5) 0.17848(3) 0.03120(10) Uani d 1 Cu
Ni 0.27283(5) 0.62359(5) -0.00049(3) 0.0332(2) Uani d 1 Ni
C1 0.2872(4) 0.4996(4) 0.0827(2) 0.0380(8) Uani d 1 C
N1 0.2950(4) 0.4264(4) 0.1349(2) 0.0520(10) Uani d 1 N
C2 0.3441(4) 0.4998(5) -0.0571(2) 0.0399(9) Uani d 1 C
N2 0.3842(4) 0.4219(5) -0.0933(2) 0.0580(10) Uani d 1 N
C3 0.2580(4) 0.7525(5) -0.0811(2) 0.0407(9) Uani d 1 C
N3 0.2501(4) 0.8345(5) -0.1289(2) 0.0560(10) Uani d 1 N
C4 0.1945(4) 0.7417(4) 0.0549(2) 0.0403(9) Uani d 1 C
N4 0.1439(4) 0.8104(4) 0.0900(2) 0.0520(10) Uani d 1 N
N11 0.4447(4) 0.1841(6) 0.0953(3) 0.0530(10) Uani d 1 N
H11A 0.461(6) 0.271(7) 0.090(4) 0.09(2) Uiso calc 1 H
H11B 0.518(6) 0.165(6) 0.114(3) 0.06(2) Uiso calc 1 H
C12 0.3722(6) 0.1048(7) 0.0255(3) 0.0605(15) Uani d 1 C
H12A 0.397(5) 0.135(6) -0.011(4) 0.07(2) Uiso calc 1 H
H12B 0.392(6) 0.013(7) 0.040(4) 0.08(2) Uiso calc 1 H
C13 0.2381(5) 0.1344(6) 0.0139(3) 0.0530(10) Uani d 1 C
H13A 0.211(4) 0.225(5) -0.002(3) 0.040(10) Uiso calc 1 H
H13B 0.188(5) 0.086(6) -0.024(3) 0.06(2) Uiso calc 1 H
N14 0.2088(4) 0.1094(4) 0.0907(2) 0.0390(8) Uani d 1 N
H14 0.214(4) 0.040(5) 0.095(3) 0.030(10) Uiso calc 1 H
C15 0.0873(4) 0.1562(5) 0.0998(3) 0.0440(10) Uani d 1 C
H15A 0.022(5) 0.115(5) 0.064(3) 0.06(2) Uiso calc 1 H
H15B 0.084(4) 0.256(5) 0.082(3) 0.050(10) Uiso calc 1 H
C16 0.0899(4) 0.1341(5) 0.1865(3) 0.0430(10) Uani d 1 C
H16A 0.023(5) 0.163(6) 0.199(3) 0.07(2) Uiso calc 1 H
H16B 0.089(5) 0.044(6) 0.195(3) 0.06(2) Uiso calc 1 H
N17 0.2047(3) 0.1954(4) 0.2370(2) 0.0343(7) Uani d 1 N
H17A 0.229(5) 0.152(6) 0.297(4) 0.08(2) Uiso calc 1 H
H17B 0.194(4) 0.278(5) 0.248(3) 0.030(10) Uiso calc 1 H
N21 0.4799(3) 0.2464(4) 0.2722(2) 0.0345(7) Uani d 1 N
H21A 0.518(4) 0.314(5) 0.259(3) 0.050(10) Uiso calc 1 H
H21B 0.449(4) 0.268(5) 0.309(3) 0.040(10) Uiso calc 1 H
C22 0.5690(4) 0.1383(5) 0.3047(3) 0.0440(10) Uani d 1 C
H22A 0.629(5) 0.165(5) 0.352(3) 0.060(10) Uiso calc 1 H
H22B 0.621(4) 0.123(5) 0.268(3) 0.050(10) Uiso calc 1 H
C23 0.5017(4) 0.0091(5) 0.3147(3) 0.0460(10) Uani d 1 C
H23A 0.559(5) -0.064(6) 0.340(3) 0.07(2) Uiso calc 1 H
H23B 0.449(5) 0.015(6) 0.360(3) 0.09(2) Uiso calc 1 H
O24 0.4234(3) -0.0359(3) 0.2399(2) 0.0415(7) Uani d 1 O
OW1 0.1775(3) 0.0498(3) -0.2402(2) 0.0539(8) Uani d 1 O
OW2 0.4172(4) 0.1692(4) -0.1733(2) 0.0710(10) Uani d 1 O
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
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'
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
N14 Cu N21 173.0(2) ?
N14 Cu N17 83.5(2) ?
N21 Cu N17 95.8(2) ?
N14 Cu N11 83.8(2) ?
N21 Cu N11 97.6(2) ?
N17 Cu N11 166.0(2) ?
N14 Cu N1 94.8(2) ?
N21 Cu N1 92.2(2) ?
N17 Cu N1 89.80(10) ?
N11 Cu N1 85.5(2) ?
N14 Cu O24 95.05(13) ?
N21 Cu O24 77.97(12) ?
N17 Cu O24 92.77(12) ?
N11 Cu O24 94.2(2) ?
N1 Cu O24 170.05(12) ?
C4 Ni C3 89.7(2) ?
C4 Ni C1 88.4(2) ?
C3 Ni C1 177.9(2) ?
C4 Ni C2 177.1(2) ?
C3 Ni C2 91.2(2) ?
C1 Ni C2 90.7(2) ?
N1 C1 Ni 178.1(4) yes
C1 N1 Cu 143.7(3) yes
N2 C2 Ni 177.8(4) ?
N3 C3 Ni 178.0(4) ?
N4 C4 Ni 177.3(4) ?
C12 N11 Cu 107.5(3) ?
C13 C12 N11 108.8(4) ?
N14 C13 C12 107.0(4) ?
C13 N14 C15 117.8(4) ?
C13 N14 Cu 109.3(3) ?
C15 N14 Cu 108.4(3) ?
N14 C15 C16 106.1(4) ?
N17 C16 C15 108.9(3) ?
C16 N17 Cu 109.6(3) ?
C22 N21 Cu 113.9(3) ?
N21 C22 C23 110.8(4) ?
O24 C23 C22 111.2(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Cu N14 1.992(4) yes
Cu N21 2.003(4) yes
Cu N17 2.039(3) yes
Cu N11 2.053(4) yes
Cu N1 2.474(4) yes
Cu O24 2.527(3) yes
Ni C4 1.861(4) yes
Ni C3 1.865(4) yes
Ni C1 1.865(4) yes
Ni C2 1.866(4) yes
C1 N1 1.144(5) yes
C2 N2 1.151(6) yes
C3 N3 1.145(6) yes
C4 N4 1.150(5) yes
N11 C12 1.490(8) ?
C12 C13 1.479(8) ?
C13 N14 1.471(6) ?
N14 C15 1.471(6) ?
C15 C16 1.510(7) ?
C16 N17 1.477(6) ?
N21 C22 1.465(6) ?
C22 C23 1.510(7) ?
C23 O24 1.433(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
N14 Cu N1 C1 -58.1(7)
N21 Cu N1 C1 122.7(6)
N17 Cu N1 C1 -141.5(6)
N11 Cu N1 C1 25.3(6)
C3 Ni C4 N4 145(9)
C1 Ni C4 N4 -36(5)
N14 Cu N11 C12 -9.6(4)
N21 Cu N11 C12 163.4(4)
N17 Cu N11 C12 -34.0(10)
N1 Cu N11 C12 -105.0(4)
Cu N11 C12 C13 36.5(6)
N11 C12 C13 N14 -53.3(6)
C12 C13 N14 C15 168.4(4)
C12 C13 N14 Cu 44.1(5)
N21 Cu N14 C13 -121.0(10)
N17 Cu N14 C13 155.2(3)
N11 Cu N14 C13 -19.0(3)
N1 Cu N14 C13 65.9(3)
N21 Cu N14 C15 110.0(10)
N17 Cu N14 C15 25.6(3)
N11 Cu N14 C15 -148.6(3)
N1 Cu N14 C15 -63.7(3)
C13 N14 C15 C16 -172.8(4)
Cu N14 C15 C16 -48.0(4)
N14 C15 C16 N17 51.0(5)
C15 C16 N17 Cu -29.9(5)
N14 Cu N17 C16 2.8(3)
N21 Cu N17 C16 -170.2(3)
N11 Cu N17 C16 27.6(9)
N1 Cu N17 C16 97.6(3)
N14 Cu N21 C22 26.0(10)
N17 Cu N21 C22 109.8(3)
N11 Cu N21 C22 -74.5(3)
N1 Cu N21 C22 -160.2(3)
Cu N21 C22 C23 -46.9(5)
N21 C22 C23 O24 59.6(5)