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#$Date: 2025-08-21 01:01:10 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301838 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/41/4324174.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_4324174
loop_
_publ_author_name
'Nadia Marino'
'Oluwatayo. F. Ikotun'
'Miguel Julve'
'Francesc Lloret'
'Juan Cano'
'Robert P. Doyle'
_publ_section_title
;
 Pyrophosphate-Mediated Magnetic Interactions in Cu(II) Coordination
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              378
_journal_page_last               389
_journal_paper_doi               10.1021/ic1020884
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C20 H20 Cu2 N4 O14 P4'
_chemical_formula_sum            'C20 H20 Cu2 N4 O14 P4'
_chemical_formula_weight         791.36
_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                110.133(2)
_cell_angle_beta                 110.318(2)
_cell_angle_gamma                98.579(2)
_cell_formula_units_Z            1
_cell_length_a                   8.7298(9)
_cell_length_b                   9.0086(9)
_cell_length_c                   10.0823(10)
_cell_measurement_reflns_used    3511
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.38
_cell_volume                     664.83(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      98(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0147
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6174
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    1.922
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            light-blue
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             398
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.286
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0368
_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)+(0.0900P)²+0.2290P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                2632
_reflns_number_total             2893
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1020884_si_002_2.cif
_cod_data_source_block           1b
_cod_database_code               4324174
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 0.50059(4) -0.25353(4) -0.23723(4) 0.01395(14) Uani 1 1 d . . .
P1 P 0.67959(8) 0.12874(8) -0.02656(8) 0.01289(18) Uani 1 1 d . . .
P2 P 0.81855(8) -0.11545(8) 0.06992(8) 0.01350(18) Uani 1 1 d . . .
O1 O 0.5599(2) -0.0163(2) -0.1797(2) 0.0165(4) Uani 1 1 d . . .
O2 O 0.5938(2) 0.2389(2) 0.0508(2) 0.0166(4) Uani 1 1 d . . .
O3 O 0.8173(2) 0.2387(2) -0.0457(2) 0.0176(4) Uani 1 1 d . . .
H3A H 0.8660 0.1809 -0.0879 0.026 Uiso 1 1 calc R . .
O4 O 0.7847(2) 0.0612(2) 0.0942(2) 0.0167(4) Uani 1 1 d . . .
O5 O 0.7354(2) -0.2279(2) -0.1029(2) 0.0166(4) Uani 1 1 d . . .
O6 O 1.0055(2) -0.0832(2) 0.1564(2) 0.0179(4) Uani 1 1 d . . .
O7 O 0.7241(2) -0.1819(2) 0.1549(2) 0.0188(4) Uani 1 1 d . . .
H7A H 0.6205 -0.2007 0.1082 0.028 Uiso 1 1 calc R . .
N1 N 0.2818(3) -0.3044(3) -0.4198(3) 0.0153(5) Uani 1 1 d . . .
N2 N 0.4475(3) -0.4990(3) -0.3389(3) 0.0155(4) Uani 1 1 d . . .
C1 C 0.2054(4) -0.1933(3) -0.4492(3) 0.0181(5) Uani 1 1 d . . .
H1 H 0.2523 -0.0826 -0.3767 0.022 Uiso 1 1 calc R . .
C2 C 0.0584(4) -0.2391(4) -0.5849(3) 0.0226(6) Uani 1 1 d . . .
H2 H 0.0064 -0.1605 -0.6023 0.027 Uiso 1 1 calc R . .
C3 C -0.0098(4) -0.4029(4) -0.6939(4) 0.0252(6) Uani 1 1 d . . .
H3 H -0.1076 -0.4358 -0.7861 0.030 Uiso 1 1 calc R . .
C4 C 0.0699(4) -0.5183(4) -0.6638(3) 0.0232(6) Uani 1 1 d . . .
H4 H 0.0265 -0.6293 -0.7356 0.028 Uiso 1 1 calc R . .
C5 C 0.2151(3) -0.4645(3) -0.5249(3) 0.0169(5) Uani 1 1 d . . .
C6 C 0.3083(3) -0.5773(3) -0.4784(3) 0.0162(5) Uani 1 1 d . . .
C7 C 0.2595(4) -0.7453(3) -0.5667(3) 0.0201(6) Uani 1 1 d . . .
H7 H 0.1647 -0.7957 -0.6634 0.024 Uiso 1 1 calc R . .
C8 C 0.3529(4) -0.8389(4) -0.5102(4) 0.0230(6) Uani 1 1 d . . .
H8 H 0.3213 -0.9531 -0.5681 0.028 Uiso 1 1 calc R . .
C9 C 0.4948(4) -0.7598(4) -0.3656(4) 0.0233(6) Uani 1 1 d . . .
H9 H 0.5592 -0.8202 -0.3248 0.028 Uiso 1 1 calc R . .
C10 C 0.5383(4) -0.5899(4) -0.2837(3) 0.0207(6) Uani 1 1 d . . .
H10 H 0.6335 -0.5366 -0.1872 0.025 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'
P P 0.1023 0.0942 '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 O5 90.45(8) . . ?
O1 Cu1 N2 166.95(9) . . ?
O5 Cu1 N2 91.42(9) . . ?
O1 Cu1 N1 93.43(9) . . ?
O5 Cu1 N1 164.37(9) . . ?
N2 Cu1 N1 81.49(10) . . ?
O1 Cu1 O2 94.98(8) . 2_655 ?
O5 Cu1 O2 93.72(8) . 2_655 ?
N2 Cu1 O2 97.78(8) . 2_655 ?
N1 Cu1 O2 101.00(8) . 2_655 ?
O1 Cu1 Cu1 48.61(6) . 2_655 ?
O5 Cu1 Cu1 88.89(6) . 2_655 ?
N2 Cu1 Cu1 144.33(7) . 2_655 ?
N1 Cu1 Cu1 105.00(7) . 2_655 ?
O2 Cu1 Cu1 46.66(5) 2_655 2_655 ?
O2 P1 O1 114.91(11) . . ?
O2 P1 O3 107.79(11) . . ?
O1 P1 O3 111.35(11) . . ?
O2 P1 O4 107.60(11) . . ?
O1 P1 O4 109.29(10) . . ?
O3 P1 O4 105.41(11) . . ?
O6 P2 O5 117.49(12) . . ?
O6 P2 O7 108.32(11) . . ?
O5 P2 O7 110.27(12) . . ?
O6 P2 O4 107.81(11) . . ?
O5 P2 O4 108.54(11) . . ?
O7 P2 O4 103.48(11) . . ?
P1 O1 Cu1 130.75(12) . . ?
P1 O2 Cu1 134.40(11) . 2_655 ?
P1 O3 H3A 109.5 . . ?
P1 O4 P2 132.50(12) . . ?
P2 O5 Cu1 121.85(11) . . ?
P2 O7 H7A 109.5 . . ?
C1 N1 C5 119.3(2) . . ?
C1 N1 Cu1 125.9(2) . . ?
C5 N1 Cu1 114.65(18) . . ?
C10 N2 C6 118.7(2) . . ?
C10 N2 Cu1 126.3(2) . . ?
C6 N2 Cu1 115.01(18) . . ?
N1 C1 C2 121.7(3) . . ?
N1 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 119.1(3) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 118.7(3) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
N1 C5 C4 121.9(3) . . ?
N1 C5 C6 114.7(2) . . ?
C4 C5 C6 123.4(3) . . ?
N2 C6 C7 122.1(3) . . ?
N2 C6 C5 113.8(2) . . ?
C7 C6 C5 124.1(3) . . ?
C6 C7 C8 119.3(3) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
C7 C8 C9 119.0(3) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
C10 C9 C8 118.7(3) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
N2 C10 C9 122.2(3) . . ?
N2 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
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 1.9439(19) . ?
Cu1 O5 1.9508(19) . ?
Cu1 N2 1.990(2) . ?
Cu1 N1 1.991(2) . ?
Cu1 O2 2.273(2) 2_655 ?
Cu1 Cu1 5.3624(7) 2_655 ?
P1 O2 1.4992(19) . ?
P1 O1 1.5057(19) . ?
P1 O3 1.550(2) . ?
P1 O4 1.6109(19) . ?
P2 O6 1.485(2) . ?
P2 O5 1.509(2) . ?
P2 O7 1.571(2) . ?
P2 O4 1.6129(19) . ?
O2 Cu1 2.273(2) 2_655 ?
O3 H3A 0.8200 . ?
O7 H7A 0.8200 . ?
N1 C1 1.342(3) . ?
N1 C5 1.346(4) . ?
N2 C10 1.345(4) . ?
N2 C6 1.351(4) . ?
C1 C2 1.386(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.381(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.394(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.386(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.491(4) . ?
C6 C7 1.371(4) . ?
C7 C8 1.384(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.391(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.382(4) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139135323
