#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:43:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179344 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/41/4324173.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_4324173
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, 3(H2 O)'
_chemical_formula_sum            'C20 H26 Cu2 N4 O17 P4'
_chemical_formula_weight         845.41
_chemical_name_systematic
; 
 ? 
;
_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                93.399(2)
_cell_angle_beta                 110.835(2)
_cell_angle_gamma                104.247(2)
_cell_formula_units_Z            1
_cell_length_a                   8.4735(8)
_cell_length_b                   9.7033(9)
_cell_length_c                   9.8403(9)
_cell_measurement_reflns_used    3381
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.68
_cell_volume                     723.22(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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6795
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    1.781
_exptl_absorpt_correction_T_max  0.9007
_exptl_absorpt_correction_T_min  0.7761
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            light-blue
_exptl_crystal_density_diffrn    1.941
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.995
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3295
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0317
_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)+(0.0479P)²+0.7593P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0870
_reflns_number_gt                2994
_reflns_number_total             3295
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1020884_si_002_1.cif
_cod_data_source_block           1a
_cod_database_code               4324173
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 0.62413(4) 0.76598(3) -0.40798(3) 0.01239(10) Uani 1 1 d . . .
N2 N 0.8277(3) 0.9442(2) -0.3323(2) 0.0147(4) Uani 1 1 d . . .
N1 N 0.5674(3) 0.8622(2) -0.5869(2) 0.0152(4) Uani 1 1 d . . .
C10 C 0.9599(3) 0.9743(3) -0.1994(3) 0.0183(5) Uani 1 1 d . . .
H10 H 0.9588 0.9072 -0.1330 0.022 Uiso 1 1 calc R . .
C9 C 1.0975(4) 1.0997(3) -0.1562(3) 0.0241(6) Uani 1 1 d . . .
H9 H 1.1895 1.1187 -0.0615 0.029 Uiso 1 1 calc R . .
C8 C 1.0993(4) 1.1977(3) -0.2533(3) 0.0277(6) Uani 1 1 d . . .
H8 H 1.1923 1.2848 -0.2256 0.033 Uiso 1 1 calc R . .
C7 C 0.9638(4) 1.1669(3) -0.3909(3) 0.0245(6) Uani 1 1 d . . .
H7 H 0.9626 1.2322 -0.4592 0.029 Uiso 1 1 calc R . .
C6 C 0.8299(3) 1.0391(3) -0.4270(3) 0.0164(5) Uani 1 1 d . . .
C5 C 0.6794(3) 0.9935(3) -0.5718(3) 0.0160(5) Uani 1 1 d . . .
C4 C 0.6532(4) 1.0758(3) -0.6841(3) 0.0206(5) Uani 1 1 d . . .
H4 H 0.7315 1.1689 -0.6711 0.025 Uiso 1 1 calc R . .
C3 C 0.5100(4) 1.0191(3) -0.8159(3) 0.0215(5) Uani 1 1 d . . .
H3 H 0.4890 1.0735 -0.8942 0.026 Uiso 1 1 calc R . .
C2 C 0.3980(4) 0.8831(3) -0.8330(3) 0.0211(5) Uani 1 1 d . . .
H2 H 0.3010 0.8421 -0.9235 0.025 Uiso 1 1 calc R . .
C1 C 0.4304(3) 0.8078(3) -0.7147(3) 0.0178(5) Uani 1 1 d . . .
H1 H 0.3529 0.7150 -0.7251 0.021 Uiso 1 1 calc R . .
P2 P 0.57119(8) 0.59844(7) -0.15370(7) 0.01534(14) Uani 1 1 d . . .
P1 P 0.29243(8) 0.50684(6) -0.44311(7) 0.01289(14) Uani 1 1 d . . .
O1 O 0.3932(2) 0.63060(19) -0.49182(19) 0.0189(4) Uani 1 1 d . . .
O2 O 0.2222(2) 0.36566(18) -0.54513(18) 0.0162(4) Uani 1 1 d . . .
O3 O 0.1472(2) 0.5460(2) -0.4044(2) 0.0197(4) Uani 1 1 d D . .
H3A H 0.103(8) 0.573(13) -0.346(6) 0.300 Uiso 1 1 d D . .
O4 O 0.4268(2) 0.48035(18) -0.28876(18) 0.0148(3) Uani 1 1 d . . .
O5 O 0.6720(2) 0.71679(19) -0.20840(18) 0.0190(4) Uani 1 1 d . . .
O6 O 0.6785(2) 0.51602(19) -0.05250(19) 0.0197(4) Uani 1 1 d . . .
O7 O 0.4659(3) 0.66555(19) -0.0796(2) 0.0225(4) Uani 1 1 d . . .
H7A H 0.4242 0.6059 -0.0339 0.034 Uiso 1 1 calc R . .
O1W O 0.0428(3) 0.6435(3) -0.1840(2) 0.0381(5) Uani 1 1 d D . .
O2W O 0.0041(7) 0.5776(6) 0.0316(6) 0.0520(14) Uani 0.50 1 d P . .
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 94.10(7) . . ?
O1 Cu1 N2 164.89(8) . . ?
O5 Cu1 N2 91.84(8) . . ?
O1 Cu1 N1 89.96(8) . . ?
O5 Cu1 N1 164.96(8) . . ?
N2 Cu1 N1 80.94(8) . . ?
O1 Cu1 O2 99.95(7) . 2_664 ?
O5 Cu1 O2 92.61(7) . 2_664 ?
N2 Cu1 O2 93.65(7) . 2_664 ?
N1 Cu1 O2 100.96(7) . 2_664 ?
O1 Cu1 Cu1 43.85(6) . 2_664 ?
O5 Cu1 Cu1 86.51(5) . 2_664 ?
N2 Cu1 Cu1 150.67(6) . 2_664 ?
N1 Cu1 Cu1 106.24(6) . 2_664 ?
O2 Cu1 Cu1 57.24(4) 2_664 2_664 ?
C10 N2 C6 119.0(2) . . ?
C10 N2 Cu1 125.68(17) . . ?
C6 N2 Cu1 115.34(16) . . ?
C1 N1 C5 119.4(2) . . ?
C1 N1 Cu1 125.49(17) . . ?
C5 N1 Cu1 115.10(16) . . ?
N2 C10 C9 122.0(2) . . ?
N2 C10 H10 119.0 . . ?
C9 C10 H10 119.0 . . ?
C10 C9 C8 119.0(2) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
C7 C8 C9 119.2(2) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C8 C7 C6 118.7(2) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
N2 C6 C7 122.0(2) . . ?
N2 C6 C5 114.4(2) . . ?
C7 C6 C5 123.6(2) . . ?
N1 C5 C4 121.8(2) . . ?
N1 C5 C6 114.2(2) . . ?
C4 C5 C6 124.1(2) . . ?
C3 C4 C5 118.4(2) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
C2 C3 C4 119.9(2) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C2 C1 118.5(2) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
N1 C1 C2 121.9(2) . . ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
O5 P2 O6 115.90(11) . . ?
O5 P2 O7 107.67(11) . . ?
O6 P2 O7 111.21(10) . . ?
O5 P2 O4 110.39(10) . . ?
O6 P2 O4 105.35(10) . . ?
O7 P2 O4 105.87(10) . . ?
O2 P1 O1 115.58(11) . . ?
O2 P1 O3 111.28(10) . . ?
O1 P1 O3 111.25(11) . . ?
O2 P1 O4 105.95(9) . . ?
O1 P1 O4 107.43(9) . . ?
O3 P1 O4 104.52(10) . . ?
P1 O1 Cu1 135.55(11) . . ?
P1 O2 Cu1 126.62(10) . 2_664 ?
P1 O3 H3A 154(4) . . ?
P2 O4 P1 127.93(11) . . ?
P2 O5 Cu1 130.94(11) . . ?
P2 O7 H7A 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 O1 1.9215(17) . ?
Cu1 O5 1.9720(17) . ?
Cu1 N2 1.997(2) . ?
Cu1 N1 2.004(2) . ?
Cu1 O2 2.1720(17) 2_664 ?
Cu1 Cu1 5.0185(7) 2_664 ?
N2 C10 1.342(3) . ?
N2 C6 1.349(3) . ?
N1 C1 1.338(3) . ?
N1 C5 1.352(3) . ?
C10 C9 1.382(4) . ?
C10 H10 0.9500 . ?
C9 C8 1.388(4) . ?
C9 H9 0.9500 . ?
C8 C7 1.385(4) . ?
C8 H8 0.9500 . ?
C7 C6 1.386(4) . ?
C7 H7 0.9500 . ?
C6 C5 1.486(3) . ?
C5 C4 1.388(3) . ?
C4 C3 1.387(4) . ?
C4 H4 0.9500 . ?
C3 C2 1.383(4) . ?
C3 H3 0.9500 . ?
C2 C1 1.392(3) . ?
C2 H2 0.9500 . ?
C1 H1 0.9500 . ?
P2 O5 1.5021(18) . ?
P2 O6 1.5056(18) . ?
P2 O7 1.563(2) . ?
P2 O4 1.5965(17) . ?
P1 O2 1.4997(18) . ?
P1 O1 1.5020(18) . ?
P1 O3 1.5333(18) . ?
P1 O4 1.6216(17) . ?
O2 Cu1 2.1720(17) 2_664 ?
O3 H3A 0.850(5) . ?
O7 H7A 0.8400 . ?
O2W O2W 1.571(11) 2_565 ?
