#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:46:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179127 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/89/4308942.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4308942
loop_
_publ_author_name
'Enrique Colacio'
'Ikram Ben Maimoun'
'Francesc Lloret'
'José Suárez-Varela'
_publ_section_title
;
[Ni(cyclam)(μ1,3-dca)2Cu(μ1,5-dca)2]: A Genuine 3D Bimetallic
Coordination Polymer Containing Both μ1,3- and μ1,5-Bidentate Dicyanamide
Bridges and a Ferromagnetic Interaction between Copper(II) and Nickel(II)
Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3771
_journal_page_last               3773
_journal_paper_doi               10.1021/ic050369v
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C18 H24 Cu N16 Ni'
_chemical_formula_weight         586.78
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 102.151(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2128(16)
_cell_length_b                   13.145(2)
_cell_length_c                   18.350(3)
_cell_measurement_reflns_used    3314
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.51
_cell_measurement_theta_min      2.56
_cell_volume                     2408.2(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'WINGX v. 1.64'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7500
_diffrn_reflns_theta_full        28.17
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    1.708
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   'empirical (Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0262
_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)+(0.0331P)²+2.1637P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                2399
_reflns_number_total             2728
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050369vsi20050310_085419.cif
_cod_data_source_block           1
_cod_database_code               4308942
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_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
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu 0.5000 0.992950(18) 0.7500 0.01088(9) Uani 1 2 d S . .
Ni Ni 1.0000 1.0000 1.0000 0.01299(9) Uani 1 2 d S . .
N4 N 0.56013(14) 0.99080(10) 0.88220(8) 0.0169(3) Uani 1 1 d . . .
N7 N 0.30758(17) 0.72317(12) 0.80906(9) 0.0325(4) Uani 1 1 d . . .
N8 N 0.63890(14) 1.09851(11) 0.75211(8) 0.0194(3) Uani 1 1 d . . .
N3 N 0.80140(15) 0.99548(10) 0.93663(8) 0.0172(3) Uani 1 1 d . . .
N5 N 0.37497(15) 0.93308(14) 0.93919(9) 0.0285(4) Uani 1 1 d . . .
N2 N 0.97770(15) 0.85590(11) 1.04256(9) 0.0208(3) Uani 1 1 d . . .
N6 N 0.36754(14) 0.88372(10) 0.75677(8) 0.0192(3) Uani 1 1 d . . .
N1 N 0.92586(15) 1.05285(11) 1.08979(8) 0.0197(3) Uani 1 1 d . . .
C3 C 0.89150(19) 0.87038(15) 1.09729(11) 0.0263(4) Uani 1 1 d . . .
C8 C 0.46576(16) 0.96023(13) 0.91650(9) 0.0175(3) Uani 1 1 d . . .
C4 C 0.92946(19) 0.77704(14) 0.98589(12) 0.0278(4) Uani 1 1 d . . .
C9 C 0.33479(16) 0.80745(13) 0.77818(9) 0.0182(3) Uani 1 1 d . . .
C6 C 0.68656(17) 0.99202(11) 0.91528(9) 0.0141(3) Uani 1 1 d . . .
C10 C 0.71582(17) 1.16027(12) 0.77571(9) 0.0175(3) Uani 1 1 d . . .
C2 C 0.93358(19) 0.96630(16) 1.14177(10) 0.0256(4) Uani 1 1 d . . .
C1 C 0.98717(19) 1.14670(15) 1.12554(11) 0.0272(4) Uani 1 1 d . . .
C5 C 1.0193(2) 0.76616(15) 0.93004(12) 0.0312(4) Uani 1 1 d . . .
H41 H 0.839(2) 0.7961(14) 0.9593(11) 0.019(5) Uiso 1 1 d . . .
H2 H 0.877(2) 0.9757(15) 1.1776(12) 0.025(5) Uiso 1 1 d . . .
H31 H 0.7986(19) 0.8775(14) 1.0688(10) 0.016(4) Uiso 1 1 d . . .
H1 H 0.841(2) 1.0659(14) 1.0722(11) 0.018(5) Uiso 1 1 d . . .
H21 H 1.026(2) 0.9618(15) 1.1700(11) 0.020(5) Uiso 1 1 d . . .
H3 H 0.893(2) 0.8109(17) 1.1302(13) 0.038(6) Uiso 1 1 d . . .
H5 H 1.113(2) 0.7576(16) 0.9581(12) 0.031(6) Uiso 1 1 d . . .
H4 H 0.921(2) 0.7115(16) 1.0116(12) 0.034(6) Uiso 1 1 d . . .
H51 H 0.995(2) 0.7010(16) 0.9017(12) 0.031(6) Uiso 1 1 d . . .
H20 H 1.076(2) 1.1317(15) 1.1455(11) 0.025(5) Uiso 1 1 d . . .
H22 H 1.056(2) 0.8362(16) 1.0683(12) 0.028(6) Uiso 1 1 d . . .
H10 H 0.943(2) 1.1676(17) 1.1666(12) 0.035(6) Uiso 1 1 d . . .
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'
Ni Ni 0.3393 1.1124 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Cu N8 90.96(9) . 2_656 ?
N8 Cu N6 175.13(6) . . ?
N8 Cu N6 90.76(7) 2_656 . ?
N8 Cu N6 90.76(6) . 2_656 ?
N8 Cu N6 175.13(6) 2_656 2_656 ?
N6 Cu N6 87.91(9) . 2_656 ?
N8 Cu N4 87.60(5) . . ?
N8 Cu N4 93.36(5) 2_656 . ?
N6 Cu N4 87.75(5) . . ?
N6 Cu N4 91.27(5) 2_656 . ?
N8 Cu N4 93.36(5) . 2_656 ?
N8 Cu N4 87.60(5) 2_656 2_656 ?
N6 Cu N4 91.27(5) . 2_656 ?
N6 Cu N4 87.75(5) 2_656 2_656 ?
N4 Cu N4 178.64(7) . 2_656 ?
N1 Ni N1 180.000(1) 5_777 . ?
N1 Ni N2 94.61(6) 5_777 . ?
N1 Ni N2 85.39(6) . . ?
N1 Ni N2 85.39(6) 5_777 5_777 ?
N1 Ni N2 94.61(6) . 5_777 ?
N2 Ni N2 180.00(3) . 5_777 ?
N1 Ni N3 91.26(6) 5_777 . ?
N1 Ni N3 88.74(6) . . ?
N2 Ni N3 90.73(5) . . ?
N2 Ni N3 89.27(5) 5_777 . ?
N1 Ni N3 88.74(6) 5_777 5_777 ?
N1 Ni N3 91.26(6) . 5_777 ?
N2 Ni N3 89.27(5) . 5_777 ?
N2 Ni N3 90.73(5) 5_777 5_777 ?
N3 Ni N3 180.0 . 5_777 ?
C6 N4 C8 122.13(15) . . ?
C6 N4 Cu 119.51(11) . . ?
C8 N4 Cu 115.66(11) . . ?
C9 N7 C10 122.33(16) . 3_445 ?
C10 N8 Cu 158.93(14) . . ?
C6 N3 Ni 166.84(14) . . ?
C4 N2 C3 114.19(15) . . ?
C4 N2 Ni 114.92(12) . . ?
C3 N2 Ni 105.39(11) . . ?
C9 N6 Cu 153.81(14) . . ?
C1 N1 C2 113.44(15) . . ?
C1 N1 Ni 116.26(11) . . ?
C2 N1 Ni 106.05(11) . . ?
N2 C3 C2 109.32(15) . . ?
N5 C8 N4 172.91(18) . . ?
N2 C4 C5 112.43(15) . . ?
N6 C9 N7 173.69(18) . . ?
N3 C6 N4 172.18(18) . . ?
N8 C10 N7 173.29(18) . 3 ?
N1 C2 C3 108.84(15) . . ?
N1 C1 C5 112.11(15) . 5_777 ?
C4 C5 C1 115.64(16) . 5_777 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu N8 1.9789(14) . ?
Cu N8 1.9789(14) 2_656 ?
Cu N6 1.9945(14) . ?
Cu N6 1.9945(14) 2_656 ?
Cu N4 2.3739(15) . ?
Cu N4 2.3739(15) 2_656 ?
Ni N1 2.0727(14) 5_777 ?
Ni N1 2.0727(14) . ?
Ni N2 2.0796(15) . ?
Ni N2 2.0796(15) 5_777 ?
Ni N3 2.1158(15) . ?
Ni N3 2.1158(15) 5_777 ?
N4 C6 1.306(2) . ?
N4 C8 1.320(2) . ?
N7 C9 1.301(2) . ?
N7 C10 1.302(2) 3_445 ?
N8 C10 1.149(2) . ?
N3 C6 1.157(2) . ?
N5 C8 1.150(2) . ?
N2 C4 1.477(2) . ?
N2 C3 1.480(2) . ?
N6 C9 1.152(2) . ?
N1 C1 1.474(2) . ?
N1 C2 1.476(2) . ?
C3 C2 1.514(3) . ?
C4 C5 1.520(3) . ?
C10 N7 1.302(2) 3 ?
C1 C5 1.526(3) 5_777 ?
C5 C1 1.526(3) 5_777 ?
