#------------------------------------------------------------------------------
#$Date: 2025-08-21 12:25:49 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301846 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/70/7007012.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_7007012
loop_
_publ_author_name
'El Fallah, M. Salah'
'Badyine, Fatima'
'Vicente, Ramon'
'Escuer, Albert'
'Solans, Xavier'
'Font-Bardia, Mercè'
_publ_section_title
;
 Complementarity and countercomplementarity in polynuclear copper(II)
 complexes with R2NCH2CH(OH)CH2NR2 (R = H, CH3): crystal structures and
 magnetic study.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2934
_journal_page_last               2942
_journal_paper_doi               10.1039/b516392g
_journal_year                    2006
_chemical_formula_moiety         'C11 H20 Cu2 N4 O3 S2'
_chemical_formula_sum            'C11 H20 Cu2 N4 O3 S2'
_chemical_formula_weight         447.52
_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                104.62(8)
_cell_angle_beta                 99.86(6)
_cell_angle_gamma                106.10(8)
_cell_formula_units_Z            2
_cell_length_a                   8.455(4)
_cell_length_b                   9.114(9)
_cell_length_c                   12.744(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      6
_cell_volume                     881.7(13)
_computing_cell_refinement       CAD-4/PC
_computing_data_collection       'CAD-4/PC (Kretschmar, 1996)'
_computing_data_reduction        'CFEO (Solans, 1978)'
_computing_molecular_graphics    'ORTEP3.2 (Brueggemann & Schmid, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'four cicle diffractometer'
_diffrn_measurement_method       'ω-2θ scan'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    1.3370
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5112
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.663
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.799
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         5112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.799
_refine_ls_R_factor_all          0.4170
_refine_ls_R_factor_gt           0.0579
_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)+(0.0061P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                991
_reflns_number_total             5112
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b516392g.txt
_cod_data_source_block           complex3
_cod_depositor_comments
;

2018-03-05
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     'C22 H40 Cu4 N8 O6 S4'
_cod_original_formula_sum        'C22 H40 Cu4 N8 O6 S4'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     895.02
_cod_database_code               7007012
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.86883(19) 0.78349(18) 0.79484(13) 0.0439(5) Uani 1 1 d . . .
Cu2 Cu 1.04086(18) 0.52244(17) 0.64460(12) 0.0371(5) Uani 1 1 d . . .
S1 S 1.3482(4) 0.2721(4) 0.4382(3) 0.0602(11) Uani 1 1 d . . .
S2 S 0.7883(5) 1.2474(4) 1.0024(3) 0.0742(12) Uani 1 1 d . . .
O1 O 1.1965(8) 0.7378(9) 0.6850(6) 0.050(3) Uani 1 1 d . . .
O2 O 1.0717(9) 0.9081(8) 0.7731(6) 0.041(2) Uani 1 1 d . . .
O3 O 0.8989(8) 0.5835(8) 0.7320(5) 0.0327(19) Uani 1 1 d . . .
N1 N 0.9389(13) 0.2977(11) 0.6559(9) 0.048(3) Uani 1 1 d . . .
N2 N 0.6775(12) 0.6571(12) 0.8467(8) 0.048(3) Uani 1 1 d . . .
N3 N 1.1690(10) 0.4500(10) 0.5366(7) 0.034(3) Uani 1 1 d . . .
N4 N 0.8302(14) 0.9794(13) 0.8620(9) 0.066(4) Uani 1 1 d . . .
C1 C 1.0679(17) 0.2863(17) 0.7453(13) 0.137(6) Uani 1 1 d . . .
H1A H 1.1039 0.3817 0.8092 0.205 Uiso 1 1 calc R . .
H1B H 1.1644 0.2761 0.7177 0.205 Uiso 1 1 calc R . .
H1C H 1.0191 0.1938 0.7670 0.205 Uiso 1 1 calc R . .
C2 C 0.896(2) 0.1668(16) 0.5599(12) 0.141(8) Uani 1 1 d . . .
H2A H 0.9968 0.1602 0.5373 0.211 Uiso 1 1 calc R . .
H2B H 0.8189 0.1796 0.5007 0.211 Uiso 1 1 calc R . .
H2C H 0.8412 0.0699 0.5752 0.211 Uiso 1 1 calc R . .
C3 C 0.7852(15) 0.2979(15) 0.6949(10) 0.075(4) Uani 1 1 d . . .
H3A H 0.7647 0.2226 0.7371 0.091 Uiso 1 1 calc R . .
H3B H 0.6881 0.2611 0.6303 0.091 Uiso 1 1 calc R . .
C4 C 0.7993(17) 0.4578(15) 0.7660(11) 0.062(4) Uani 1 1 d . . .
H4 H 0.8673 0.4701 0.8401 0.075 Uiso 1 1 calc R . .
C5 C 0.6469(15) 0.4939(16) 0.7870(11) 0.071(4) Uani 1 1 d . . .
H5A H 0.5649 0.4648 0.7154 0.085 Uiso 1 1 calc R . .
H5B H 0.5959 0.4272 0.8290 0.085 Uiso 1 1 calc R . .
C6 C 0.7288(14) 0.6884(12) 0.9683(10) 0.084(5) Uani 1 1 d . . .
H6A H 0.7275 0.7931 1.0066 0.125 Uiso 1 1 calc R . .
H6B H 0.8417 0.6843 0.9892 0.125 Uiso 1 1 calc R . .
H6C H 0.6508 0.6083 0.9886 0.125 Uiso 1 1 calc R . .
C7 C 0.5109(15) 0.6791(14) 0.8174(9) 0.082(5) Uani 1 1 d . . .
H7A H 0.5164 0.7824 0.8636 0.123 Uiso 1 1 calc R . .
H7B H 0.4247 0.5960 0.8296 0.123 Uiso 1 1 calc R . .
H7C H 0.4832 0.6732 0.7398 0.123 Uiso 1 1 calc R . .
C8 C 1.2455(14) 0.3764(13) 0.4956(8) 0.033(3) Uani 1 1 d . . .
C9 C 0.8092(17) 1.0853(16) 0.9206(11) 0.064(4) Uani 1 1 d . . .
C10 C 1.1887(17) 0.8793(15) 0.7407(10) 0.040(4) Uani 1 1 d . . .
C11 C 1.3530(14) 1.0151(13) 0.7563(9) 0.078(4) Uani 1 1 d . . .
H11A H 1.3892 0.9978 0.6882 0.117 Uiso 1 1 calc R . .
H11B H 1.4400 1.0167 0.8163 0.117 Uiso 1 1 calc R . .
H11C H 1.3332 1.1161 0.7743 0.117 Uiso 1 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'
S S 0.1246 0.1234 '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
O2 Cu1 O3 94.4(3) . . ?
O2 Cu1 N4 88.5(4) . . ?
O3 Cu1 N4 176.9(4) . . ?
O2 Cu1 N2 169.5(4) . . ?
O3 Cu1 N2 86.4(3) . . ?
N4 Cu1 N2 90.6(4) . . ?
O3 Cu2 O1 93.7(3) . . ?
O3 Cu2 N3 173.5(3) . . ?
O1 Cu2 N3 89.2(3) . . ?
O3 Cu2 N1 86.1(3) . . ?
O1 Cu2 N1 157.8(4) . . ?
N3 Cu2 N1 93.4(4) . . ?
C10 O1 Cu2 131.8(8) . . ?
C10 O2 Cu1 134.7(8) . . ?
C4 O3 Cu2 114.6(7) . . ?
C4 O3 Cu1 111.9(7) . . ?
Cu2 O3 Cu1 133.3(4) . . ?
C2 N1 C3 108.8(11) . . ?
C2 N1 C1 110.1(11) . . ?
C3 N1 C1 109.2(10) . . ?
C2 N1 Cu2 118.0(8) . . ?
C3 N1 Cu2 105.8(7) . . ?
C1 N1 Cu2 104.6(8) . . ?
C5 N2 C6 111.3(10) . . ?
C5 N2 C7 104.3(10) . . ?
C6 N2 C7 108.8(9) . . ?
C5 N2 Cu1 104.6(7) . . ?
C6 N2 Cu1 110.6(7) . . ?
C7 N2 Cu1 117.0(8) . . ?
C8 N3 Cu2 157.6(9) . . ?
C9 N4 Cu1 166.0(12) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 C4 112.6(11) . . ?
N1 C3 H3A 109.1 . . ?
C4 C3 H3A 109.1 . . ?
N1 C3 H3B 109.1 . . ?
C4 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
O3 C4 C5 108.5(10) . . ?
O3 C4 C3 111.6(11) . . ?
C5 C4 C3 120.7(12) . . ?
O3 C4 H4 104.8 . . ?
C5 C4 H4 104.8 . . ?
C3 C4 H4 104.8 . . ?
N2 C5 C4 114.5(11) . . ?
N2 C5 H5A 108.6 . . ?
C4 C5 H5A 108.6 . . ?
N2 C5 H5B 108.6 . . ?
C4 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 S1 179.0(11) . . ?
N4 C9 S2 176.0(14) . . ?
O2 C10 O1 128.6(12) . . ?
O2 C10 C11 120.7(12) . . ?
O1 C10 C11 110.7(12) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
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 O2 1.884(7) . ?
Cu1 O3 1.902(6) . ?
Cu1 N4 1.917(10) . ?
Cu1 N2 2.024(10) . ?
Cu2 O3 1.872(6) . ?
Cu2 O1 1.917(8) . ?
Cu2 N3 1.988(9) . ?
Cu2 N1 2.042(9) . ?
S1 C8 1.587(11) . ?
S2 C9 1.653(14) . ?
O1 C10 1.332(13) . ?
O2 C10 1.203(13) . ?
O3 C4 1.431(12) . ?
N1 C2 1.387(13) . ?
N1 C3 1.468(12) . ?
N1 C1 1.482(14) . ?
N2 C5 1.417(12) . ?
N2 C6 1.466(12) . ?
N2 C7 1.476(12) . ?
N3 C8 1.149(10) . ?
N4 C9 1.139(12) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.469(13) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.466(13) . ?
C4 H4 0.9800 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C10 C11 1.526(14) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139152484
