#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:17:52 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179103 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/65/4306522.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_4306522
loop_
_publ_author_name
'Olivier Jeannin'
'Rodolphe Clérac'
'Thomas Cauchy'
'Marc Fourmigué'
_publ_section_title
;
Ferromagnetic Interactions in Heterobimetallic Chains Formed through the
Secondary Coordination of Dithiolene Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10656
_journal_page_last               10661
_journal_paper_doi               10.1021/ic801343b
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C10 H24 N4 Ni, C8 Cu F6 N2 S4'
_chemical_formula_sum            'C18 H24 Cu F6 N6 Ni S4'
_chemical_formula_weight         688.92
_chemical_name_common            '[Ni(cyclam)][Cu(tfadt)2]'
_chemical_name_systematic
;
 ?
;
_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'
_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                 97.292(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5773(12)
_cell_length_b                   10.8899(11)
_cell_length_c                   11.4306(9)
_cell_measurement_reflns_used    66
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.48
_cell_measurement_theta_min      2.47
_cell_volume                     1306.0(2)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8854
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    1.918
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.6438
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             690
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0416
_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)+(0.0596P)²+0.9722P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1288
_reflns_number_gt                1908
_reflns_number_total             2975
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801343b_si_002.cif
_cod_data_source_block           ojec151
_cod_database_code               4306522
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_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
Ni Ni 0.0000 0.0000 0.5000 0.0305(2) Uani 1 2 d S . .
Cu Cu 0.5000 -0.5000 0.5000 0.0324(2) Uani 1 2 d S . .
S1 S 0.40316(10) -0.32048(10) 0.53497(10) 0.0448(3) Uani 1 1 d . . .
S2 S 0.31336(10) -0.57787(9) 0.41462(11) 0.0502(3) Uani 1 1 d . . .
C1 C 0.2519(3) -0.3442(3) 0.4592(3) 0.0335(8) Uani 1 1 d . . .
C2 C 0.2130(4) -0.4528(4) 0.4086(3) 0.0367(9) Uani 1 1 d . . .
C3 C 0.1732(3) -0.2372(4) 0.4553(3) 0.0363(9) Uani 1 1 d . . .
C4 C 0.0841(4) -0.4729(4) 0.3429(4) 0.0496(11) Uani 1 1 d . . .
C1A C 0.1272(5) 0.1323(4) 0.3349(4) 0.0557(12) Uani 1 1 d . . .
H1A1 H 0.1711 0.0626 0.3058 0.067 Uiso 1 1 calc R . .
H1A2 H 0.1672 0.2069 0.3112 0.067 Uiso 1 1 calc R . .
C2A C 0.2660(4) 0.1041(4) 0.5245(5) 0.0611(14) Uani 1 1 d . . .
H2A1 H 0.3224 0.1685 0.5036 0.073 Uiso 1 1 calc R . .
H2A2 H 0.2969 0.0266 0.4975 0.073 Uiso 1 1 calc R . .
C3A C 0.2686(5) 0.1004(4) 0.6570(5) 0.0701(16) Uani 1 1 d . . .
H3A1 H 0.2238 0.1720 0.6810 0.084 Uiso 1 1 calc R . .
H3A2 H 0.3566 0.1069 0.6927 0.084 Uiso 1 1 calc R . .
C4A C 0.2106(5) -0.0131(4) 0.7063(4) 0.0623(14) Uani 1 1 d . . .
H4A1 H 0.2476 -0.0857 0.6751 0.075 Uiso 1 1 calc R . .
H4A2 H 0.2319 -0.0140 0.7914 0.075 Uiso 1 1 calc R . .
C5A C 0.0107(5) -0.1304(4) 0.7155(4) 0.0573(13) Uani 1 1 d . . .
H5A1 H 0.0183 -0.1327 0.8009 0.069 Uiso 1 1 calc R . .
H5A2 H 0.0536 -0.2021 0.6889 0.069 Uiso 1 1 calc R . .
N1 N 0.1171(3) -0.1489(3) 0.4577(3) 0.0437(8) Uani 1 1 d . . .
N1A N 0.1360(3) 0.1269(3) 0.4650(3) 0.0419(8) Uani 1 1 d . . .
H1A H 0.1109 0.2013 0.4900 0.050 Uiso 1 1 calc R . .
N2A N 0.0709(3) -0.0179(3) 0.6769(3) 0.0443(9) Uani 1 1 d . . .
H2A H 0.0387 0.0459 0.7153 0.053 Uiso 1 1 calc R . .
F1 F 0.0864(3) -0.4989(4) 0.2314(3) 0.1133(15) Uani 1 1 d . . .
F2 F 0.0028(3) -0.3838(3) 0.3501(4) 0.1091(14) Uani 1 1 d . . .
F3 F 0.0256(3) -0.5709(3) 0.3815(3) 0.0828(9) Uani 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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 '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
N1A Ni N1A 180.00(18) . 3_556 ?
N1A Ni N2A 94.42(14) . . ?
N1A Ni N2A 85.58(14) 3_556 . ?
N1A Ni N2A 85.58(14) . 3_556 ?
N1A Ni N2A 94.42(14) 3_556 3_556 ?
N2A Ni N2A 180.0 . 3_556 ?
N1A Ni N1 91.49(13) . . ?
N1A Ni N1 88.51(13) 3_556 . ?
N2A Ni N1 90.06(13) . . ?
N2A Ni N1 89.94(13) 3_556 . ?
N1A Ni N1 88.51(13) . 3_556 ?
N1A Ni N1 91.49(13) 3_556 3_556 ?
N2A Ni N1 89.94(13) . 3_556 ?
N2A Ni N1 90.06(13) 3_556 3_556 ?
N1 Ni N1 180.00(18) . 3_556 ?
S2 Cu S2 180.00(6) 3_646 . ?
S2 Cu S1 90.59(4) 3_646 3_646 ?
S2 Cu S1 89.41(4) . 3_646 ?
S2 Cu S1 89.41(4) 3_646 . ?
S2 Cu S1 90.59(4) . . ?
S1 Cu S1 180.00(6) 3_646 . ?
C1 S1 Cu 101.07(13) . . ?
C2 S2 Cu 102.80(14) . . ?
C2 C1 C3 123.6(3) . . ?
C2 C1 S1 123.5(3) . . ?
C3 C1 S1 112.9(3) . . ?
C1 C2 C4 123.5(4) . . ?
C1 C2 S2 121.3(3) . . ?
C4 C2 S2 115.2(3) . . ?
N1 C3 C1 175.3(4) . . ?
F2 C4 F1 108.4(4) . . ?
F2 C4 F3 103.7(4) . . ?
F1 C4 F3 102.4(4) . . ?
F2 C4 C2 115.4(4) . . ?
F1 C4 C2 113.2(4) . . ?
F3 C4 C2 112.6(4) . . ?
N1A C1A C5A 108.6(3) . 3_556 ?
N1A C2A C3A 111.4(4) . . ?
C2A C3A C4A 115.8(4) . . ?
N2A C4A C3A 112.6(3) . . ?
N2A C5A C1A 109.4(4) . 3_556 ?
C3 N1 Ni 166.6(3) . . ?
C2A N1A C1A 114.0(3) . . ?
C2A N1A Ni 115.4(3) . . ?
C1A N1A Ni 105.4(3) . . ?
C5A N2A C4A 114.8(3) . . ?
C5A N2A Ni 104.7(2) . . ?
C4A N2A Ni 116.5(3) . . ?
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
Ni N1A 2.070(3) . ?
Ni N1A 2.070(3) 3_556 ?
Ni N2A 2.074(3) . ?
Ni N2A 2.074(3) 3_556 ?
Ni N1 2.133(3) . ?
Ni N1 2.133(3) 3_556 ?
Cu S2 2.2538(11) 3_646 ?
Cu S2 2.2538(11) . ?
Cu S1 2.2660(10) 3_646 ?
Cu S1 2.2660(10) . ?
S1 C1 1.739(4) . ?
S2 C2 1.723(4) . ?
C1 C2 1.358(5) . ?
C1 C3 1.429(5) . ?
C2 C4 1.486(6) . ?
C3 N1 1.132(5) . ?
C4 F2 1.306(5) . ?
C4 F1 1.309(5) . ?
C4 F3 1.336(5) . ?
C1A N1A 1.479(5) . ?
C1A C5A 1.500(7) 3_556 ?
C2A N1A 1.475(5) . ?
C2A C3A 1.512(7) . ?
C3A C4A 1.519(7) . ?
C4A N2A 1.475(6) . ?
C5A N2A 1.474(6) . ?
C5A C1A 1.500(7) 3_556 ?
