#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:38:46 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179855 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/51/7015162.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_7015162
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         'C24 H36 Cu2 N6 O2, 2(Cl O4)'
_chemical_formula_sum            'C24 H36 Cl2 Cu2 N6 O10'
_chemical_formula_weight         766.57
_chemical_name_common
;
((mu-piperazine)bis-((E)-2-((2-
aminopropylimino)methyl)phenolato-copper(ii)))diperchlorate
;
_chemical_name_systematic
;
((μ-piperazine)bis-[(E)-2-((2-aminopropylimino)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                95.3740(10)
_cell_angle_beta                 106.0920(10)
_cell_angle_gamma                99.7760(10)
_cell_formula_units_Z            1
_cell_length_a                   7.8017(5)
_cell_length_b                   9.3998(6)
_cell_length_c                   10.7936(6)
_cell_measurement_reflns_used    8867
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      31.960
_cell_measurement_theta_min      2.223
_cell_volume                     741.16(8)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.942
_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  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15842
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         32.34
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    1.681
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS, Bruker, 1997
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             394
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0284
_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)+(0.0423P)²+0.2337P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                4463
_reflns_number_total             4995
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01304h.txt
_cod_data_source_block           (IV)
_cod_database_code               7015162
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 0.15990(2) 0.352450(17) 0.289340(15) 0.03074(6) Uani 1 d . . .
O1 O 0.14277(16) 0.53501(12) 0.36692(10) 0.0384(2) Uani 1 d . . .
N1 N 0.1397(2) 0.16422(15) 0.17899(14) 0.0428(3) Uani 1 d . . .
H1A H 0.0202 0.1234 0.1480 0.051 Uiso 1 calc R . .
H1B H 0.1758 0.1873 0.1098 0.051 Uiso 1 calc R . .
N2 N 0.29917(17) 0.30277(15) 0.45695(12) 0.0354(2) Uani 1 d . . .
N3 N 0.03663(16) 0.44108(13) 0.12414(11) 0.0311(2) Uani 1 d . . .
H3 H -0.0394 0.4917 0.1510 0.037 Uiso 1 calc R . .
C1 C 0.2347(3) 0.04740(19) 0.2288(2) 0.0507(4) Uani 1 d . . .
H1C H 0.3565 0.0661 0.2200 0.061 Uiso 1 calc R . .
H1D H 0.1696 -0.0458 0.1766 0.061 Uiso 1 calc R . .
C2 C 0.2471(3) 0.03903(19) 0.3692(2) 0.0510(4) Uani 1 d . . .
H2A H 0.1260 0.0309 0.3788 0.061 Uiso 1 calc R . .
H2B H 0.2893 -0.0490 0.3922 0.061 Uiso 1 calc R . .
C3 C 0.3714(2) 0.1672(2) 0.46296(18) 0.0479(4) Uani 1 d . . .
H3A H 0.3932 0.1434 0.5508 0.057 Uiso 1 calc R . .
H3B H 0.4876 0.1844 0.4448 0.057 Uiso 1 calc R . .
C4 C 0.3394(2) 0.38661(18) 0.56692(14) 0.0373(3) Uani 1 d . . .
H4 H 0.4078 0.3533 0.6394 0.045 Uiso 1 calc R . .
C5 C 0.29144(19) 0.52513(17) 0.59087(13) 0.0348(3) Uani 1 d . . .
C6 C 0.3469(2) 0.5976(2) 0.72100(15) 0.0442(3) Uani 1 d . . .
H6 H 0.4128 0.5544 0.7874 0.053 Uiso 1 calc R . .
C7 C 0.3054(2) 0.7301(2) 0.75104(16) 0.0498(4) Uani 1 d . . .
H7 H 0.3458 0.7778 0.8365 0.060 Uiso 1 calc R . .
C8 C 0.2018(2) 0.79241(19) 0.65162(17) 0.0445(3) Uani 1 d . . .
H8 H 0.1715 0.8814 0.6717 0.053 Uiso 1 calc R . .
C9 C 0.1436(2) 0.72422(17) 0.52398(15) 0.0375(3) Uani 1 d . . .
H9 H 0.0721 0.7666 0.4596 0.045 Uiso 1 calc R . .
C10 C 0.19139(18) 0.59091(15) 0.49012(13) 0.0319(2) Uani 1 d . . .
C11 C 0.17166(19) 0.55601(16) 0.09721(13) 0.0341(3) Uani 1 d . . .
H11A H 0.2548 0.5104 0.0627 0.041 Uiso 1 calc R . .
H11B H 0.2424 0.6186 0.1782 0.041 Uiso 1 calc R . .
C12 C -0.0811(2) 0.35155(15) -0.00046(13) 0.0351(3) Uani 1 d . . .
H12A H -0.1745 0.2812 0.0171 0.042 Uiso 1 calc R . .
H12B H -0.0081 0.2979 -0.0389 0.042 Uiso 1 calc R . .
Cl2 Cl -0.30832(5) -0.17607(5) 0.12989(4) 0.04525(9) Uani 1 d . . .
O1P O -0.2348(3) -0.0501(2) 0.0817(2) 0.0869(6) Uani 1 d . . .
O2P O -0.4611(3) -0.1560(3) 0.1686(3) 0.0982(7) Uani 1 d . . .
O3P O -0.1728(3) -0.2012(3) 0.2364(2) 0.1269(11) Uani 1 d . . .
O4P O -0.3599(4) -0.2940(2) 0.0278(2) 0.1070(8) Uani 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'
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 93.06(5) . . ?
O1 Cu1 N1 169.17(5) . . ?
N2 Cu1 N1 97.28(6) . . ?
O1 Cu1 N3 79.14(4) . . ?
N2 Cu1 N3 170.37(5) . . ?
N1 Cu1 N3 90.87(5) . . ?
C10 O1 Cu1 129.75(9) . . ?
C1 N1 Cu1 122.95(11) . . ?
C1 N1 H1A 106.6 . . ?
Cu1 N1 H1A 106.6 . . ?
C1 N1 H1B 106.6 . . ?
Cu1 N1 H1B 106.6 . . ?
H1A N1 H1B 106.6 . . ?
C4 N2 C3 115.21(13) . . ?
C4 N2 Cu1 123.39(11) . . ?
C3 N2 Cu1 121.36(11) . . ?
C12 N3 C11 109.50(10) . . ?
C12 N3 Cu1 123.66(9) . . ?
C11 N3 Cu1 110.28(8) . . ?
C12 N3 H3 103.7 . . ?
C11 N3 H3 103.7 . . ?
Cu1 N3 H3 103.7 . . ?
N1 C1 C2 111.98(14) . . ?
N1 C1 H1C 109.2 . . ?
C2 C1 H1C 109.2 . . ?
N1 C1 H1D 109.2 . . ?
C2 C1 H1D 109.2 . . ?
H1C C1 H1D 107.9 . . ?
C3 C2 C1 114.35(15) . . ?
C3 C2 H2A 108.7 . . ?
C1 C2 H2A 108.7 . . ?
C3 C2 H2B 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
N2 C3 C2 113.67(14) . . ?
N2 C3 H3A 108.8 . . ?
C2 C3 H3A 108.8 . . ?
N2 C3 H3B 108.8 . . ?
C2 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
N2 C4 C5 127.75(13) . . ?
N2 C4 H4 116.1 . . ?
C5 C4 H4 116.1 . . ?
C10 C5 C6 119.22(15) . . ?
C10 C5 C4 122.52(13) . . ?
C6 C5 C4 118.26(14) . . ?
C7 C6 C5 121.40(16) . . ?
C7 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C6 C7 C8 119.08(15) . . ?
C6 C7 H7 120.5 . . ?
C8 C7 H7 120.5 . . ?
C9 C8 C7 121.12(16) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C10 120.70(15) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
O1 C10 C9 118.50(13) . . ?
O1 C10 C5 123.12(13) . . ?
C9 C10 C5 118.37(13) . . ?
N3 C11 C12 112.11(11) . 2_565 ?
N3 C11 H11A 109.2 . . ?
C12 C11 H11A 109.2 2_565 . ?
N3 C11 H11B 109.2 . . ?
C12 C11 H11B 109.2 2_565 . ?
H11A C11 H11B 107.9 . . ?
N3 C12 C11 112.25(11) . 2_565 ?
N3 C12 H12A 109.2 . . ?
C11 C12 H12A 109.2 2_565 . ?
N3 C12 H12B 109.2 . . ?
C11 C12 H12B 109.2 2_565 . ?
H12A C12 H12B 107.9 . . ?
O3P Cl2 O2P 109.66(17) . . ?
O3P Cl2 O4P 110.87(18) . . ?
O2P Cl2 O4P 109.42(15) . . ?
O3P Cl2 O1P 108.32(14) . . ?
O2P Cl2 O1P 111.35(14) . . ?
O4P Cl2 O1P 107.19(15) . . ?
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 1.8800(11) . ?
Cu1 N2 1.9780(12) . ?
Cu1 N1 1.9952(13) . ?
Cu1 N3 2.0972(11) . ?
O1 C10 1.3077(16) . ?
N1 C1 1.487(2) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C4 1.290(2) . ?
N2 C3 1.478(2) . ?
N3 C12 1.4838(17) . ?
N3 C11 1.4844(18) . ?
N3 H3 0.9100 . ?
C1 C2 1.501(3) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 C3 1.499(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.435(2) . ?
C4 H4 0.9300 . ?
C5 C10 1.412(2) . ?
C5 C6 1.417(2) . ?
C6 C7 1.371(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.395(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.380(2) . ?
C8 H8 0.9300 . ?
C9 C10 1.411(2) . ?
C9 H9 0.9300 . ?
C11 C12 1.5211(19) 2_565 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C11 1.5211(19) 2_565 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
Cl2 O3P 1.399(2) . ?
Cl2 O2P 1.4026(18) . ?
Cl2 O4P 1.4070(19) . ?
Cl2 O1P 1.4330(18) . ?
