#------------------------------------------------------------------------------
#$Date: 2025-08-21 14:03:24 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301848 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/24/7022487.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_7022487
loop_
_publ_author_name
'Mukherjee, Sandip'
'Mukherjee, Partha Sarathi'
_publ_section_title
;
 Cu(II)-azide polynuclear complexes of Cu4 building clusters with
 Schiff-base co-ligands: synthesis, structures, magnetic behavior and DFT
 studies.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4019
_journal_page_last               4030
_journal_paper_doi               10.1039/c2dt32802j
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C9 H13 Cu2 N15'
_chemical_formula_sum            'C9 H13 Cu2 N15'
_chemical_formula_weight         458.42
_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                 103.475(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.4645(11)
_cell_length_b                   20.057(3)
_cell_length_c                   12.863(2)
_cell_measurement_reflns_used    3248
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      1.92
_cell_volume                     1621.9(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1999)'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0677
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15956
_diffrn_reflns_theta_full        26.21
_diffrn_reflns_theta_max         26.21
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    2.655
_exptl_absorpt_correction_T_max  0.5245
_exptl_absorpt_correction_T_min  0.4429
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0405P)²+1.9467P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0998
_reflns_number_gt                2447
_reflns_number_total             3248
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c2dt32802j.txt
_cod_data_source_block           complex1
_cod_original_cell_volume        1621.8(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7022487
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
Cu1 Cu -0.04684(9) 0.12053(3) 0.26224(4) 0.03074(17) Uani 1 1 d .
Cu2 Cu 0.53256(8) 0.07191(3) 0.46027(4) 0.02885(16) Uani 1 1 d .
N1 N -0.0856(5) 0.02901(18) 0.1943(3) 0.0300(8) Uani 1 1 d .
N2 N -0.2024(5) 0.14455(18) 0.1181(3) 0.0299(8) Uani 1 1 d .
N3 N -0.0572(6) 0.21973(18) 0.2879(3) 0.0324(9) Uani 1 1 d .
H3 H -0.0911 0.2253 0.3521 0.039 Uiso 1 1 calc R
N4 N 0.1456(6) 0.0959(2) 0.3957(3) 0.0349(9) Uani 1 1 d .
N5 N 0.0876(7) 0.1013(3) 0.4746(4) 0.0529(13) Uani 1 1 d .
N6 N 0.0389(10) 0.1080(4) 0.5548(5) 0.118(3) Uani 1 1 d .
N7 N 0.6074(6) 0.10699(19) 0.3281(3) 0.0318(9) Uani 1 1 d .
N8 N 0.4582(6) 0.11340(18) 0.2544(3) 0.0317(9) Uani 1 1 d .
N9 N 0.3174(7) 0.1209(2) 0.1816(3) 0.0520(12) Uani 1 1 d .
N10 N 0.5069(6) -0.02228(18) 0.4105(3) 0.0347(9) Uani 1 1 d .
N11 N 0.4949(6) -0.04318(18) 0.3213(3) 0.0314(9) Uani 1 1 d .
N12 N 0.4810(7) -0.0626(2) 0.2366(3) 0.0509(12) Uani 1 1 d .
N13 N 0.5787(7) 0.1564(2) 0.5370(3) 0.0436(11) Uani 1 1 d .
N14 N 0.6559(6) 0.2019(2) 0.5026(3) 0.0382(10) Uani 1 1 d .
N15 N 0.7273(8) 0.2486(2) 0.4708(4) 0.0542(12) Uani 1 1 d .
C1 C -0.0184(7) -0.0289(2) 0.2359(4) 0.0399(12) Uani 1 1 d .
H1 H 0.0561 -0.0306 0.3070 0.048 Uiso 1 1 calc R
C2 C -0.0541(8) -0.0880(3) 0.1779(5) 0.0457(13) Uani 1 1 d .
H2 H -0.0061 -0.1284 0.2102 0.055 Uiso 1 1 calc R
C3 C -0.1601(8) -0.0860(3) 0.0730(5) 0.0475(14) Uani 1 1 d .
H3A H -0.1854 -0.1249 0.0325 0.057 Uiso 1 1 calc R
C4 C -0.2292(8) -0.0249(3) 0.0282(4) 0.0428(12) Uani 1 1 d .
H4 H -0.3005 -0.0220 -0.0434 0.051 Uiso 1 1 calc R
C5 C -0.1916(7) 0.0314(2) 0.0903(4) 0.0322(11) Uani 1 1 d .
C6 C -0.2562(7) 0.0988(2) 0.0519(4) 0.0350(11) Uani 1 1 d .
H6 H -0.3327 0.1069 -0.0177 0.042 Uiso 1 1 calc R
C7 C -0.2415(8) 0.2156(2) 0.0987(4) 0.0412(12) Uani 1 1 d .
H7A H -0.3794 0.2226 0.0506 0.049 Uiso 1 1 calc R
H7B H -0.1332 0.2348 0.0668 0.049 Uiso 1 1 calc R
C8 C -0.2348(8) 0.2474(2) 0.2054(4) 0.0421(12) Uani 1 1 d .
H8A H -0.2168 0.2952 0.2002 0.051 Uiso 1 1 calc R
H8B H -0.3681 0.2394 0.2256 0.051 Uiso 1 1 calc R
C9 C 0.1445(8) 0.2547(3) 0.2937(4) 0.0514(14) Uani 1 1 d .
H9A H 0.2539 0.2349 0.3484 0.077 Uiso 1 1 calc R
H9B H 0.1288 0.3008 0.3104 0.077 Uiso 1 1 calc R
H9C H 0.1827 0.2514 0.2261 0.077 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'
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_3
N4 Cu1 N2 171.11(16) .
N4 Cu1 N3 98.38(16) .
N2 Cu1 N3 83.25(15) .
N4 Cu1 N1 98.10(16) .
N2 Cu1 N1 80.16(15) .
N3 Cu1 N1 163.40(14) .
N13 Cu2 N10 168.59(17) .
N13 Cu2 N7 94.93(16) .
N10 Cu2 N7 94.55(15) .
N13 Cu2 N10 92.64(16) 3_656
N10 Cu2 N10 77.15(16) 3_656
N7 Cu2 N10 169.17(15) 3_656
C1 N1 C5 118.5(4) .
C1 N1 Cu1 129.2(3) .
C5 N1 Cu1 112.2(3) .
C6 N2 C7 126.4(4) .
C6 N2 Cu1 117.9(3) .
C7 N2 Cu1 115.7(3) .
C9 N3 C8 112.9(4) .
C9 N3 Cu1 114.6(3) .
C8 N3 Cu1 107.6(3) .
N5 N4 Cu1 118.6(3) .
N6 N5 N4 176.9(7) .
N8 N7 Cu2 113.8(3) .
N9 N8 N7 177.9(5) .
N11 N10 Cu2 128.1(3) .
N11 N10 Cu2 128.6(3) 3_656
Cu2 N10 Cu2 102.85(16) 3_656
N12 N11 N10 179.1(5) .
N14 N13 Cu2 120.8(3) .
N15 N14 N13 177.0(5) .
N1 C1 C2 122.6(5) .
C3 C2 C1 119.2(5) .
C2 C3 C4 118.5(5) .
C5 C4 C3 119.4(5) .
N1 C5 C4 121.8(4) .
N1 C5 C6 113.8(4) .
C4 C5 C6 124.4(4) .
N2 C6 C5 115.9(4) .
N2 C7 C8 106.9(4) .
N3 C8 C7 110.3(4) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N4 1.934(4) .
Cu1 N2 1.952(4) .
Cu1 N3 2.021(4) .
Cu1 N1 2.023(4) .
Cu2 N13 1.949(4) .
Cu2 N10 1.989(4) .
Cu2 N7 2.001(4) .
Cu2 N10 2.004(4) 3_656
N1 C1 1.310(6) .
N1 C5 1.355(5) .
N2 C6 1.246(6) .
N2 C7 1.459(6) .
N3 C9 1.467(6) .
N3 C8 1.478(6) .
N4 N5 1.166(5) .
N5 N6 1.154(7) .
N7 N8 1.191(5) .
N8 N9 1.153(5) .
N10 N11 1.207(5) .
N10 Cu2 2.004(4) 3_656
N11 N12 1.141(5) .
N13 N14 1.175(5) .
N14 N15 1.160(5) .
C1 C2 1.390(7) .
C2 C3 1.364(7) .
C3 C4 1.384(7) .
C4 C5 1.371(6) .
C5 C6 1.467(6) .
C7 C8 1.504(7) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168347921
