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#$Date: 2025-08-21 00:21:57 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301837 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/99/4319941.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_4319941
loop_
_publ_author_name
'Lei Zhang'
'Liang-Fu Tang'
'Zhi-Hong Wang'
'Miao Du'
'Miguel Julve'
'Francesc Lloret'
'Ji-Tao Wang'
_publ_contact_author_address
; laboratoir Chimie et Biologie
  des Centres Redox Biologiques
  DBMS-CB/CEA-Grenoble/CNRS/Universite Joseph Fourier
  17 rue Martyrs, 38054 Grenoble
  Cedex 9, France 
;
_publ_contact_author_email       lzhang@cea.fr
_publ_contact_author_fax         '(33) 04 76 88 91 24'
_publ_contact_author_name        'Dr. Lei Zhang'
_publ_section_title
;
 Ferromagnetic Coupling in a One-Dimensional Molecular Railroad Copper(II)
 Azido Compound Containing a Defective Double Cubane Motif
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3619
_journal_page_last               3622
_journal_paper_doi               10.1021/ic001406f
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C7 H8 Cu2 N16'
_chemical_formula_weight         443.37
_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                110.756(2)
_cell_angle_beta                 97.6260(10)
_cell_angle_gamma                103.771(2)
_cell_formula_units_Z            2
_cell_length_a                   7.4073(6)
_cell_length_b                   9.8470(8)
_cell_length_c                   11.9043(10)
_cell_measurement_temperature    293(2)
_cell_volume                     765.75(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0141
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3589
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    2.810
_exptl_absorpt_correction_T_max  0.5401
_exptl_absorpt_correction_T_min  0.4396
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.0123(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0301
_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)+(0.0565P)²+0.2689P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0882
_reflns_number_gt                2797
_reflns_number_total             3082
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001406f.cif
_cod_data_source_block           IC001406f
_cod_database_code               4319941
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 -0.11473(4) 0.10147(3) 0.31405(2) 0.02916(12) Uani 1 1 d . . .
Cu2 Cu -0.23798(4) -0.00003(3) 0.51957(3) 0.03132(12) Uani 1 1 d . . .
N1 N -0.0385(3) 0.1623(2) 0.49717(19) 0.0325(5) Uani 1 1 d . . .
N2 N 0.0593(3) 0.2875(3) 0.5758(2) 0.0378(5) Uani 1 1 d . . .
N3 N 0.1576(5) 0.4006(3) 0.6481(3) 0.0725(10) Uani 1 1 d . . .
N4 N -0.2803(3) -0.0753(2) 0.33458(19) 0.0323(4) Uani 1 1 d . . .
N5 N -0.4202(3) -0.1741(3) 0.2596(2) 0.0353(5) Uani 1 1 d . . .
N6 N -0.5491(4) -0.2679(4) 0.1884(3) 0.0650(8) Uani 1 1 d . . .
N7 N -0.1433(4) 0.0531(3) 0.6954(2) 0.0426(6) Uani 1 1 d . . .
N8 N -0.0708(3) 0.1809(3) 0.7746(2) 0.0385(5) Uani 1 1 d . . .
N9 N -0.0019(5) 0.2968(3) 0.8561(3) 0.0611(8) Uani 1 1 d . . .
N10 N -0.4726(4) -0.1583(3) 0.5008(2) 0.0505(7) Uani 1 1 d . . .
N11 N -0.5322(3) -0.1858(2) 0.58068(19) 0.0333(4) Uani 1 1 d . . .
N12 N -0.5995(4) -0.2171(3) 0.6531(3) 0.0508(6) Uani 1 1 d . . .
N13 N 0.0551(3) 0.2902(2) 0.31049(19) 0.0317(4) Uani 1 1 d . . .
N14 N 0.0110(3) 0.3363(2) 0.2182(2) 0.0332(4) Uani 1 1 d . . .
C1 C -0.1813(4) 0.2746(3) 0.1403(3) 0.0366(5) Uani 1 1 d . . .
H1B H -0.194(4) 0.324(3) 0.082(3) 0.037(7) Uiso 1 1 d . . .
H1A H -0.260(4) 0.291(3) 0.193(3) 0.031(7) Uiso 1 1 d . . .
C2 C 0.1599(4) 0.4484(3) 0.2215(3) 0.0410(6) Uani 1 1 d . . .
H2 H 0.147(5) 0.493(4) 0.175(3) 0.056(10) Uiso 1 1 d . . .
C3 C 0.3054(4) 0.4751(3) 0.3169(3) 0.0449(7) Uani 1 1 d . . .
H3 H 0.421(6) 0.545(5) 0.339(4) 0.077(12) Uiso 1 1 d . . .
C4 C 0.2351(4) 0.3745(3) 0.3694(3) 0.0363(6) Uani 1 1 d . . .
H4 H 0.281(4) 0.359(3) 0.430(3) 0.034(8) Uiso 1 1 d . . .
N15 N -0.2123(3) 0.0193(2) 0.13065(19) 0.0312(4) Uani 1 1 d . . .
N16 N -0.2244(3) 0.1120(2) 0.07039(18) 0.0330(4) Uani 1 1 d . . .
C5 C -0.2796(4) 0.0314(4) -0.0524(2) 0.0418(6) Uani 1 1 d . . .
H5 H -0.288(5) 0.086(4) -0.100(3) 0.049(9) Uiso 1 1 d . . .
C6 C -0.3032(4) -0.1178(4) -0.0739(3) 0.0440(7) Uani 1 1 d . . .
H6 H -0.339(5) -0.188(4) -0.142(4) 0.064(11) Uiso 1 1 d . . .
C7 C -0.2592(4) -0.1206(3) 0.0423(2) 0.0366(6) Uani 1 1 d . . .
H7 H -0.262(4) -0.201(4) 0.062(3) 0.042(8) 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'
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
N4 Cu1 N13 174.60(8) . . ?
N4 Cu1 N15 95.53(9) . . ?
N13 Cu1 N15 89.60(9) . . ?
N4 Cu1 N1 77.89(9) . . ?
N13 Cu1 N1 96.97(9) . . ?
N15 Cu1 N1 173.42(8) . . ?
N4 Cu1 N12 85.20(9) . 2_456 ?
N13 Cu1 N12 93.10(8) . 2_456 ?
N15 Cu1 N12 90.43(9) . 2_456 ?
N1 Cu1 N12 88.83(9) . 2_456 ?
N4 Cu1 N7 83.51(8) . 2_556 ?
N13 Cu1 N7 97.75(8) . 2_556 ?
N15 Cu1 N7 94.94(8) . 2_556 ?
N1 Cu1 N7 84.60(8) . 2_556 ?
N12 Cu1 N7 167.92(8) 2_456 2_556 ?
N7 Cu2 N10 94.87(10) . . ?
N7 Cu2 N4 165.78(10) . . ?
N10 Cu2 N4 90.33(9) . . ?
N7 Cu2 N1 99.60(10) . . ?
N10 Cu2 N1 164.43(10) . . ?
N4 Cu2 N1 76.96(8) . . ?
N2 N1 Cu1 127.34(18) . . ?
N2 N1 Cu2 127.60(18) . . ?
Cu1 N1 Cu2 101.40(9) . . ?
N3 N2 N1 176.4(3) . . ?
N5 N4 Cu1 127.02(18) . . ?
N5 N4 Cu2 125.56(17) . . ?
Cu1 N4 Cu2 102.31(9) . . ?
N6 N5 N4 178.7(3) . . ?
N8 N7 Cu2 126.0(2) . . ?
N9 N8 N7 174.7(3) . . ?
N11 N10 Cu2 127.2(2) . . ?
N12 N11 N10 176.1(3) . . ?
C4 N13 N14 105.2(2) . . ?
C4 N13 Cu1 132.37(19) . . ?
N14 N13 Cu1 121.01(16) . . ?
C2 N14 N13 110.8(2) . . ?
C2 N14 C1 129.1(2) . . ?
N13 N14 C1 119.82(19) . . ?
N14 C1 N16 109.7(2) . . ?
N14 C2 C3 107.5(2) . . ?
C2 C3 C4 105.5(2) . . ?
N13 C4 C3 111.0(3) . . ?
C7 N15 N16 105.5(2) . . ?
C7 N15 Cu1 132.22(18) . . ?
N16 N15 Cu1 122.01(16) . . ?
C5 N16 N15 110.8(2) . . ?
C5 N16 C1 129.3(2) . . ?
N15 N16 C1 119.8(2) . . ?
N16 C5 C6 107.7(2) . . ?
C5 C6 C7 105.4(3) . . ?
N15 C7 C6 110.6(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
Cu1 N4 1.989(2) . ?
Cu1 N13 1.998(2) . ?
Cu1 N15 1.999(2) . ?
Cu1 N1 2.004(2) . ?
Cu1 N12 2.643(3) 2_456 ?
Cu1 N7 2.703(3) 2_556 ?
Cu2 N7 1.951(2) . ?
Cu2 N10 1.965(2) . ?
Cu2 N4 2.012(2) . ?
Cu2 N1 2.023(2) . ?
N1 N2 1.224(3) . ?
N2 N3 1.131(4) . ?
N4 N5 1.215(3) . ?
N5 N6 1.137(4) . ?
N7 N8 1.209(3) . ?
N8 N9 1.145(4) . ?
N10 N11 1.187(3) . ?
N11 N12 1.147(3) . ?
N13 C4 1.331(3) . ?
N13 N14 1.360(3) . ?
N14 C2 1.347(3) . ?
N14 C1 1.447(3) . ?
C1 N16 1.449(3) . ?
C2 C3 1.360(4) . ?
C3 C4 1.387(4) . ?
N15 C7 1.331(3) . ?
N15 N16 1.357(3) . ?
N16 C5 1.341(3) . ?
C5 C6 1.362(5) . ?
C6 C7 1.390(4) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168337395
