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#$Date: 2016-03-25 12:38:46 +0100 (vie 25 de mar de 2016) $
#$Revision: 179855 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/51/7015160.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_7015160
loop_
_publ_author_name
'Rigamonti, Luca'
'Forni, Alessandra'
'Pievo, Roberta'
'Reedijk, Jan'
'Pasini, Alessandro'
_publ_section_title
;
 Synthesis, crystal structures and magnetic properties of dinuclear
 copper(II) compounds with NNO tridentate Schiff base ligands and
 bridging aliphatic diamine and aromatic diimine linkers.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3381
_journal_page_last               3393
_journal_paper_doi               10.1039/c0dt01304h
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C22 H32 Cu2 N6 O2, 2(Cl O4)'
_chemical_formula_sum            'C22 H32 Cl2 Cu2 N6 O10'
_chemical_formula_weight         738.52
_chemical_name_common
;
((mu-piperazine)bis-((E)-2-((2-
aminoethylimino)methyl)phenolato-copper(ii)))diperchlorate
;
_chemical_name_systematic
;
((μ-piperazine)bis-[(E)-2-((2-aminoethylimino)methyl)phenolato-
copper(II)])diperchlorate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.566(1)
_cell_angle_beta                 98.300(1)
_cell_angle_gamma                93.424(1)
_cell_formula_units_Z            1
_cell_length_a                   7.2758(3)
_cell_length_b                   8.7094(4)
_cell_length_c                   10.8201(5)
_cell_measurement_reflns_used    8907
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.095
_cell_measurement_theta_min      2.349
_cell_volume                     675.51(5)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP III ( Burnett&Johnson, 1996)'
_computing_publication_material  'SHELXL-97,PARST (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Burla et al., 2004)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker SMART APEX'
_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  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12659
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         32.41
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    1.840
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS, Bruker, 1997
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             378
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         4548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0312P)²+0.2962P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0629
_reflns_number_gt                4158
_reflns_number_total             4548
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01304h.txt
_cod_data_source_block           (II)
_cod_database_code               7015160
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.354107(19) 0.166432(15) 0.224772(12) 0.01513(5) Uani 1 d . . .
Cl1 Cl 0.83885(4) 0.64938(3) 0.37827(3) 0.02112(6) Uani 1 d . . .
O1P O 0.75719(18) 0.51321(14) 0.42471(12) 0.0400(3) Uani 1 d . . .
O2P O 0.98722(18) 0.60926(17) 0.31183(13) 0.0449(3) Uani 1 d . . .
O3P O 0.69735(16) 0.71679(15) 0.29537(11) 0.0366(3) Uani 1 d . . .
O4P O 0.90793(17) 0.75757(14) 0.48194(11) 0.0399(3) Uani 1 d . . .
O1 O 0.34942(13) -0.02954(10) 0.13861(8) 0.01848(16) Uani 1 d . . .
N1 N 0.36483(16) 0.38271(12) 0.30735(10) 0.0216(2) Uani 1 d . . .
H1A H 0.2731 0.3904 0.3572 0.026 Uiso 1 calc R . .
H1B H 0.4784 0.4062 0.3564 0.026 Uiso 1 calc R . .
N2 N 0.22168(13) 0.25688(11) 0.08118(9) 0.01607(17) Uani 1 d . . .
N3 N 0.47318(14) 0.05817(11) 0.37418(9) 0.01522(17) Uani 1 d . . .
H3A H 0.5604 -0.0022 0.3439 0.018 Uiso 1 calc R . .
C1 C 0.33705(17) 0.49017(14) 0.20620(12) 0.0198(2) Uani 1 d . . .
H1C H 0.4535 0.5075 0.1702 0.024 Uiso 1 calc R . .
H1D H 0.3019 0.5908 0.2399 0.024 Uiso 1 calc R . .
C2 C 0.18299(17) 0.41794(14) 0.10628(12) 0.0198(2) Uani 1 d . . .
H2A H 0.0608 0.4235 0.1358 0.024 Uiso 1 calc R . .
H2B H 0.1798 0.4735 0.0290 0.024 Uiso 1 calc R . .
C3 C 0.16498(16) 0.18872(14) -0.02807(11) 0.0172(2) Uani 1 d . . .
H3B H 0.0990 0.2466 -0.0893 0.021 Uiso 1 calc R . .
C4 C 0.19451(16) 0.03137(14) -0.06383(11) 0.0169(2) Uani 1 d . . .
C5 C 0.12643(17) -0.02449(16) -0.18859(11) 0.0207(2) Uani 1 d . . .
H5 H 0.0611 0.0415 -0.2435 0.025 Uiso 1 calc R . .
C6 C 0.15270(17) -0.17257(16) -0.23244(11) 0.0235(2) Uani 1 d . . .
H6 H 0.1040 -0.2093 -0.3160 0.028 Uiso 1 calc R . .
C7 C 0.25257(17) -0.26760(15) -0.15147(12) 0.0225(2) Uani 1 d . . .
H7 H 0.2750 -0.3686 -0.1814 0.027 Uiso 1 calc R . .
C8 C 0.31922(17) -0.21692(14) -0.02850(12) 0.0194(2) Uani 1 d . . .
H8 H 0.3865 -0.2839 0.0244 0.023 Uiso 1 calc R . .
C9 C 0.28901(15) -0.06711(13) 0.01995(11) 0.01584(19) Uani 1 d . . .
C10 C 0.57691(16) 0.15222(13) 0.48473(10) 0.01609(19) Uani 1 d . . .
H10A H 0.4904 0.2190 0.5215 0.019 Uiso 1 calc R . .
H10B H 0.6752 0.2198 0.4572 0.019 Uiso 1 calc R . .
C11 C 0.33418(16) -0.05257(13) 0.41555(11) 0.0165(2) Uani 1 d . . .
H11A H 0.2727 -0.1199 0.3424 0.020 Uiso 1 calc R . .
H11B H 0.2374 0.0055 0.4494 0.020 Uiso 1 calc R . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
O1 Cu1 N2 93.38(4) . . ?
O1 Cu1 N1 176.25(4) . . ?
N2 Cu1 N1 84.09(4) . . ?
O1 Cu1 N3 84.02(4) . . ?
N2 Cu1 N3 174.98(4) . . ?
N1 Cu1 N3 98.71(4) . . ?
O2P Cl1 O4P 110.00(8) . . ?
O2P Cl1 O3P 109.59(8) . . ?
O4P Cl1 O3P 109.43(7) . . ?
O2P Cl1 O1P 110.00(8) . . ?
O4P Cl1 O1P 108.92(8) . . ?
O3P Cl1 O1P 108.87(7) . . ?
C9 O1 Cu1 127.43(8) . . ?
C1 N1 Cu1 107.47(8) . . ?
C1 N1 H1A 110.2 . . ?
Cu1 N1 H1A 110.2 . . ?
C1 N1 H1B 110.2 . . ?
Cu1 N1 H1B 110.2 . . ?
H1A N1 H1B 108.5 . . ?
C3 N2 C2 119.58(10) . . ?
C3 N2 Cu1 126.65(8) . . ?
C2 N2 Cu1 113.75(8) . . ?
C10 N3 C11 109.76(9) . . ?
C10 N3 Cu1 119.22(7) . . ?
C11 N3 Cu1 110.33(7) . . ?
C10 N3 H3A 105.5 . . ?
C11 N3 H3A 105.5 . . ?
Cu1 N3 H3A 105.5 . . ?
N1 C1 C2 107.79(10) . . ?
N1 C1 H1C 110.1 . . ?
C2 C1 H1C 110.1 . . ?
N1 C1 H1D 110.1 . . ?
C2 C1 H1D 110.1 . . ?
H1C C1 H1D 108.5 . . ?
N2 C2 C1 107.62(9) . . ?
N2 C2 H2A 110.2 . . ?
C1 C2 H2A 110.2 . . ?
N2 C2 H2B 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
N2 C3 C4 124.68(11) . . ?
N2 C3 H3B 117.7 . . ?
C4 C3 H3B 117.7 . . ?
C5 C4 C9 119.80(11) . . ?
C5 C4 C3 117.39(11) . . ?
C9 C4 C3 122.81(10) . . ?
C6 C5 C4 121.55(12) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C5 C6 C7 118.70(11) . . ?
C5 C6 H6 120.6 . . ?
C7 C6 H6 120.6 . . ?
C8 C7 C6 121.12(12) . . ?
C8 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C7 C8 C9 121.27(12) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 H8 119.4 . . ?
O1 C9 C8 117.81(10) . . ?
O1 C9 C4 124.71(10) . . ?
C8 C9 C4 117.48(10) . . ?
N3 C10 C11 112.19(9) . 2_656 ?
N3 C10 H10A 109.2 . . ?
C11 C10 H10A 109.2 2_656 . ?
N3 C10 H10B 109.2 . . ?
C11 C10 H10B 109.2 2_656 . ?
H10A C10 H10B 107.9 . . ?
N3 C11 C10 112.14(9) . 2_656 ?
N3 C11 H11A 109.2 . . ?
C10 C11 H11A 109.2 2_656 . ?
N3 C11 H11B 109.2 . . ?
C10 C11 H11B 109.2 2_656 . ?
H11A C11 H11B 107.9 . . ?
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
Cu1 O1 1.8892(9) . ?
Cu1 N2 1.9426(10) . ?
Cu1 N1 2.0262(11) . ?
Cu1 N3 2.0337(10) . ?
Cl1 O2P 1.4291(12) . ?
Cl1 O4P 1.4311(10) . ?
Cl1 O3P 1.4424(12) . ?
Cl1 O1P 1.4450(12) . ?
O1 C9 1.3100(13) . ?
N1 C1 1.4835(16) . ?
N1 H1A 0.9200 . ?
N1 H1B 0.9200 . ?
N2 C3 1.2894(15) . ?
N2 C2 1.4637(15) . ?
N3 C10 1.4883(14) . ?
N3 C11 1.4905(15) . ?
N3 H3A 0.9300 . ?
C1 C2 1.5174(17) . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.4378(17) . ?
C3 H3B 0.9500 . ?
C4 C5 1.4145(16) . ?
C4 C9 1.4204(16) . ?
C5 C6 1.3800(19) . ?
C5 H5 0.9500 . ?
C6 C7 1.400(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.3841(17) . ?
C7 H7 0.9500 . ?
C8 C9 1.4170(16) . ?
C8 H8 0.9500 . ?
C10 C11 1.5224(16) 2_656 ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C10 1.5225(16) 2_656 ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Cu1 O1 C9 5.65(10) . . . . ?
N3 Cu1 O1 C9 -178.66(10) . . . . ?
N2 Cu1 N1 C1 -20.96(8) . . . . ?
N3 Cu1 N1 C1 163.24(8) . . . . ?
O1 Cu1 N2 C3 -1.15(10) . . . . ?
N1 Cu1 N2 C3 176.08(11) . . . . ?
O1 Cu1 N2 C2 177.45(8) . . . . ?
N1 Cu1 N2 C2 -5.33(8) . . . . ?
O1 Cu1 N3 C10 162.02(9) . . . . ?
N1 Cu1 N3 C10 -15.38(9) . . . . ?
O1 Cu1 N3 C11 -69.63(7) . . . . ?
N1 Cu1 N3 C11 112.96(8) . . . . ?
Cu1 N1 C1 C2 42.07(11) . . . . ?
C3 N2 C2 C1 -151.45(11) . . . . ?
Cu1 N2 C2 C1 29.84(12) . . . . ?
N1 C1 C2 N2 -46.80(13) . . . . ?
C2 N2 C3 C4 179.98(11) . . . . ?
Cu1 N2 C3 C4 -1.50(17) . . . . ?
N2 C3 C4 C5 -178.66(11) . . . . ?
N2 C3 C4 C9 0.84(19) . . . . ?
C9 C4 C5 C6 -1.32(18) . . . . ?
C3 C4 C5 C6 178.19(11) . . . . ?
C4 C5 C6 C7 -1.33(18) . . . . ?
C5 C6 C7 C8 2.02(19) . . . . ?
C6 C7 C8 C9 -0.04(19) . . . . ?
Cu1 O1 C9 C8 172.54(8) . . . . ?
Cu1 O1 C9 C4 -7.72(17) . . . . ?
C7 C8 C9 O1 177.19(11) . . . . ?
C7 C8 C9 C4 -2.57(17) . . . . ?
C5 C4 C9 O1 -176.53(11) . . . . ?
C3 C4 C9 O1 3.99(18) . . . . ?
C5 C4 C9 C8 3.21(16) . . . . ?
C3 C4 C9 C8 -176.28(11) . . . . ?
C11 N3 C10 C11 54.61(13) . . . 2_656 ?
Cu1 N3 C10 C11 -176.78(7) . . . 2_656 ?
C10 N3 C11 C10 -54.59(13) . . . 2_656 ?
Cu1 N3 C11 C10 172.08(7) . . . 2_656 ?
