#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/15/7211593.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_7211593
loop_
_publ_author_name
'DeBurgomaster, Paul'
'Ouellette, Wayne'
'Liu, Hongxue'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
 Hydrothermal chemistry of vanadium oxides with aromatic di- and
 tri-phosphonates in the presence of secondary metal copper(II) cationic
 complex subunits
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              446
_journal_paper_doi               10.1039/b910641c
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C32 H34 Cu2 N4 O20 P6'
_chemical_formula_sum            'C32 H34 Cu2 N4 O20 P6'
_chemical_formula_weight         1107.53
_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                114.17(3)
_cell_angle_beta                 105.57(3)
_cell_angle_gamma                104.01(3)
_cell_formula_units_Z            1
_cell_length_a                   10.114(2)
_cell_length_b                   10.753(2)
_cell_length_c                   11.130(2)
_cell_measurement_reflns_used    4759
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      3.18
_cell_volume                     974.8(6)
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9826
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         3.18
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0.001
_exptl_absorpt_coefficient_mu    1.430
_exptl_absorpt_correction_T_max  0.8702
_exptl_absorpt_correction_T_min  0.6736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         4759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0369
_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)+(0.0402P)²+1.3065P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                4482
_reflns_number_total             4759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b910641c.txt
_cod_data_source_block           17
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        974.7(3)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7211593
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
Cu1 Cu 0.32964(3) 1.03078(3) 0.63871(3) 0.00992(8) Uani 1 1 d .
P1 P 0.37230(6) 0.79014(6) 0.38268(6) 0.00936(12) Uani 1 1 d .
P2 P -0.12859(6) 0.25476(6) 0.10277(6) 0.01208(12) Uani 1 1 d .
P3 P 0.43751(6) 0.25250(6) 0.20176(6) 0.01130(12) Uani 1 1 d .
O1 O 0.37265(17) 0.85962(17) 0.53234(17) 0.0117(3) Uani 1 1 d .
O2 O 0.26335(19) 0.83265(19) 0.2932(2) 0.0143(3) Uani 1 1 d .
O3 O 0.52366(17) 0.82871(17) 0.37879(18) 0.0131(3) Uani 1 1 d .
O4 O -0.1666(2) 0.3360(2) 0.2314(2) 0.0222(4) Uani 1 1 d .
O5 O -0.21487(19) 0.2580(2) -0.02796(18) 0.0190(4) Uani 1 1 d .
O6 O -0.1418(2) 0.0998(2) 0.0752(2) 0.0280(5) Uani 1 1 d .
O7 O 0.59514(18) 0.35312(19) 0.2492(2) 0.0195(4) Uani 1 1 d .
O8 O 0.36576(18) 0.12553(18) 0.04510(18) 0.0158(3) Uani 1 1 d .
O9 O 0.4181(2) 0.1897(2) 0.3041(2) 0.0195(4) Uani 1 1 d .
O40 O 0.4765(2) 1.0623(2) 0.8415(2) 0.0176(4) Uani 1 1 d .
N1 N 0.2640(2) 1.1895(2) 0.7395(2) 0.0136(4) Uani 1 1 d .
N2 N 0.1275(2) 0.9021(2) 0.6064(2) 0.0123(4) Uani 1 1 d .
C1 C 0.2897(2) 0.5900(2) 0.2997(2) 0.0105(4) Uani 1 1 d .
C2 C 0.1346(2) 0.5116(2) 0.2412(2) 0.0114(4) Uani 1 1 d .
H2 H 0.0729 0.5634 0.2474 0.014 Uiso 1 1 calc R
C3 C 0.0707(2) 0.3560(2) 0.1732(2) 0.0114(4) Uani 1 1 d .
C4 C 0.1647(2) 0.2790(2) 0.1611(2) 0.0119(4) Uani 1 1 d .
H4 H 0.1232 0.1757 0.1132 0.014 Uiso 1 1 calc R
C5 C 0.3201(2) 0.3557(2) 0.2203(2) 0.0110(4) Uani 1 1 d .
C6 C 0.3813(2) 0.5105(2) 0.2912(2) 0.0117(4) Uani 1 1 d .
H6 H 0.4847 0.5621 0.3337 0.014 Uiso 1 1 calc R
C7 C 0.3472(3) 1.3364(3) 0.8132(3) 0.0173(5) Uani 1 1 d .
H7 H 0.4393 1.3698 0.8099 0.021 Uiso 1 1 calc R
C8 C 0.3015(3) 1.4400(3) 0.8938(3) 0.0187(5) Uani 1 1 d .
H8 H 0.3601 1.5413 0.9409 0.022 Uiso 1 1 calc R
C9 C 0.1673(3) 1.3902(3) 0.9029(3) 0.0190(5) Uani 1 1 d .
H9 H 0.1354 1.4575 0.9584 0.023 Uiso 1 1 calc R
C10 C 0.0809(3) 1.2389(3) 0.8286(3) 0.0185(5) Uani 1 1 d .
H10 H -0.0094 1.2034 0.8342 0.022 Uiso 1 1 calc R
C11 C 0.1307(3) 1.1407(3) 0.7453(2) 0.0138(4) Uani 1 1 d .
C12 C 0.0474(2) 0.9779(3) 0.6596(2) 0.0135(4) Uani 1 1 d .
C13 C -0.0997(3) 0.9056(3) 0.6338(3) 0.0183(5) Uani 1 1 d .
H13 H -0.1532 0.9594 0.6696 0.022 Uiso 1 1 calc R
C14 C -0.1650(3) 0.7514(3) 0.5534(3) 0.0212(5) Uani 1 1 d .
H14 H -0.2639 0.7005 0.5333 0.025 Uiso 1 1 calc R
C15 C -0.0823(3) 0.6733(3) 0.5031(3) 0.0198(5) Uani 1 1 d .
H15 H -0.1239 0.5699 0.4508 0.024 Uiso 1 1 calc R
C16 C 0.0644(3) 0.7534(3) 0.5327(3) 0.0161(4) Uani 1 1 d .
H16 H 0.1206 0.7015 0.5001 0.019 Uiso 1 1 calc R
H2' H 0.250(4) 0.802(4) 0.219(4) 0.030(10) Uiso 1 1 d .
H4' H -0.241(5) 0.324(5) 0.218(5) 0.049(13) Uiso 1 1 d .
H6' H -0.227(5) 0.018(5) 0.027(5) 0.068(14) Uiso 1 1 d .
H9' H 0.480(4) 0.165(4) 0.338(4) 0.034(10) Uiso 1 1 d .
H40A H 0.448(4) 1.080(4) 0.899(4) 0.026(9) Uiso 1 1 d .
H40B H 0.550(5) 1.110(4) 0.868(4) 0.032(11) 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'
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
O3 Cu1 O1 94.82(7) 2_676 .
O3 Cu1 N1 90.51(8) 2_676 .
O1 Cu1 N1 173.95(7) . .
O3 Cu1 N2 158.28(8) 2_676 .
O1 Cu1 N2 93.35(8) . .
N1 Cu1 N2 80.66(9) . .
O3 Cu1 O40 97.81(9) 2_676 .
O1 Cu1 O40 89.34(8) . .
N1 Cu1 O40 92.79(8) . .
N2 Cu1 O40 102.37(9) . .
O3 P1 O1 115.63(10) . .
O3 P1 O2 113.56(10) . .
O1 P1 O2 105.52(10) . .
O3 P1 C1 106.28(10) . .
O1 P1 C1 108.48(10) . .
O2 P1 C1 107.01(11) . .
O5 P2 O6 114.66(12) . .
O5 P2 O4 111.31(11) . .
O6 P2 O4 111.41(13) . .
O5 P2 C3 112.59(11) . .
O6 P2 C3 102.76(11) . .
O4 P2 C3 103.23(11) . .
O7 P3 O8 113.82(11) . .
O7 P3 O9 113.79(11) . .
O8 P3 O9 109.99(10) . .
O7 P3 C5 110.61(10) . .
O8 P3 C5 107.30(10) . .
O9 P3 C5 100.31(10) . .
P1 O1 Cu1 132.04(10) . .
P1 O2 H2' 116(3) . .
P1 O3 Cu1 143.13(10) . 2_676
P2 O4 H4' 118(4) . .
P2 O6 H6' 126(3) . .
P3 O9 H9' 120(3) . .
Cu1 O40 H40A 115(3) . .
Cu1 O40 H40B 114(3) . .
H40A O40 H40B 112(4) . .
C7 N1 C11 118.7(2) . .
C7 N1 Cu1 125.49(16) . .
C11 N1 Cu1 115.38(16) . .
C16 N2 C12 118.8(2) . .
C16 N2 Cu1 126.33(16) . .
C12 N2 Cu1 114.78(16) . .
C2 C1 C6 118.8(2) . .
C2 C1 P1 121.24(17) . .
C6 C1 P1 119.94(17) . .
C1 C2 C3 121.1(2) . .
C1 C2 H2 119.5 . .
C3 C2 H2 119.5 . .
C4 C3 C2 118.8(2) . .
C4 C3 P2 119.93(17) . .
C2 C3 P2 121.23(17) . .
C5 C4 C3 120.9(2) . .
C5 C4 H4 119.6 . .
C3 C4 H4 119.6 . .
C6 C5 C4 119.2(2) . .
C6 C5 P3 121.29(17) . .
C4 C5 P3 119.56(17) . .
C5 C6 C1 121.2(2) . .
C5 C6 H6 119.4 . .
C1 C6 H6 119.4 . .
N1 C7 C8 122.6(2) . .
N1 C7 H7 118.7 . .
C8 C7 H7 118.7 . .
C9 C8 C7 118.7(2) . .
C9 C8 H8 120.7 . .
C7 C8 H8 120.7 . .
C8 C9 C10 119.3(2) . .
C8 C9 H9 120.4 . .
C10 C9 H9 120.4 . .
C9 C10 C11 119.2(2) . .
C9 C10 H10 120.4 . .
C11 C10 H10 120.4 . .
N1 C11 C10 121.4(2) . .
N1 C11 C12 114.5(2) . .
C10 C11 C12 124.1(2) . .
N2 C12 C13 122.0(2) . .
N2 C12 C11 114.1(2) . .
C13 C12 C11 124.0(2) . .
C14 C13 C12 118.5(2) . .
C14 C13 H13 120.8 . .
C12 C13 H13 120.8 . .
C15 C14 C13 119.8(2) . .
C15 C14 H14 120.1 . .
C13 C14 H14 120.1 . .
C14 C15 C16 118.5(2) . .
C14 C15 H15 120.8 . .
C16 C15 H15 120.8 . .
N2 C16 C15 122.4(2) . .
N2 C16 H16 118.8 . .
C15 C16 H16 118.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O3 1.9578(17) 2_676
Cu1 O1 1.9643(17) .
Cu1 N1 1.998(2) .
Cu1 N2 2.013(2) .
Cu1 O40 2.178(2) .
P1 O3 1.5033(16) .
P1 O1 1.5195(17) .
P1 O2 1.5627(18) .
P1 C1 1.808(2) .
P2 O5 1.5013(19) .
P2 O6 1.5296(19) .
P2 O4 1.548(2) .
P2 C3 1.803(2) .
P3 O7 1.4954(19) .
P3 O8 1.524(2) .
P3 O9 1.5736(19) .
P3 C5 1.807(2) .
O2 H2' 0.71(4) .
O3 Cu1 1.9578(17) 2_676
O4 H4' 0.70(4) .
O6 H6' 0.89(5) .
O9 H9' 0.81(4) .
O40 H40A 0.74(4) .
O40 H40B 0.69(4) .
N1 C7 1.342(3) .
N1 C11 1.352(3) .
N2 C16 1.337(3) .
N2 C12 1.361(3) .
C1 C2 1.398(3) .
C1 C6 1.400(3) .
C2 C3 1.402(3) .
C2 H2 0.9300 .
C3 C4 1.402(3) .
C4 C5 1.399(3) .
C4 H4 0.9300 .
C5 C6 1.393(3) .
C6 H6 0.9300 .
C7 C8 1.383(3) .
C7 H7 0.9300 .
C8 C9 1.381(4) .
C8 H8 0.9300 .
C9 C10 1.384(4) .
C9 H9 0.9300 .
C10 C11 1.391(3) .
C10 H10 0.9300 .
C11 C12 1.474(3) .
C12 C13 1.388(3) .
C13 C14 1.388(4) .
C13 H13 0.9300 .
C14 C15 1.387(4) .
C14 H14 0.9300 .
C15 C16 1.392(3) .
C15 H15 0.9300 .
C16 H16 0.9300 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O3 P1 O1 Cu1 101.58(14) . .
O2 P1 O1 Cu1 -24.82(15) . .
C1 P1 O1 Cu1 -139.20(13) . .
O3 Cu1 O1 P1 -55.05(14) 2_676 .
N1 Cu1 O1 P1 96.4(7) . .
N2 Cu1 O1 P1 104.82(14) . .
O40 Cu1 O1 P1 -152.83(14) . .
O1 P1 O3 Cu1 -92.30(19) . 2_676
O2 P1 O3 Cu1 29.9(2) . 2_676
C1 P1 O3 Cu1 147.28(16) . 2_676
O3 Cu1 N1 C7 -24.3(2) 2_676 .
O1 Cu1 N1 C7 -175.9(6) . .
N2 Cu1 N1 C7 175.7(2) . .
O40 Cu1 N1 C7 73.6(2) . .
O3 Cu1 N1 C11 163.36(16) 2_676 .
O1 Cu1 N1 C11 11.8(8) . .
N2 Cu1 N1 C11 3.29(16) . .
O40 Cu1 N1 C11 -98.80(17) . .
O3 Cu1 N2 C16 111.1(2) 2_676 .
O1 Cu1 N2 C16 -0.9(2) . .
N1 Cu1 N2 C16 178.2(2) . .
O40 Cu1 N2 C16 -91.0(2) . .
O3 Cu1 N2 C12 -65.1(3) 2_676 .
O1 Cu1 N2 C12 -177.07(16) . .
N1 Cu1 N2 C12 2.04(16) . .
O40 Cu1 N2 C12 92.87(16) . .
O3 P1 C1 C2 -158.09(18) . .
O1 P1 C1 C2 77.0(2) . .
O2 P1 C1 C2 -36.4(2) . .
O3 P1 C1 C6 20.9(2) . .
O1 P1 C1 C6 -104.08(19) . .
O2 P1 C1 C6 142.51(18) . .
C6 C1 C2 C3 -0.8(3) . .
P1 C1 C2 C3 178.12(17) . .
C1 C2 C3 C4 -1.7(3) . .
C1 C2 C3 P2 177.94(17) . .
O5 P2 C3 C4 -110.64(19) . .
O6 P2 C3 C4 13.2(2) . .
O4 P2 C3 C4 129.21(19) . .
O5 P2 C3 C2 69.7(2) . .
O6 P2 C3 C2 -166.39(19) . .
O4 P2 C3 C2 -50.4(2) . .
C2 C3 C4 C5 2.3(3) . .
P2 C3 C4 C5 -177.32(17) . .
C3 C4 C5 C6 -0.4(3) . .
C3 C4 C5 P3 -179.71(17) . .
O7 P3 C5 C6 -9.2(2) . .
O8 P3 C5 C6 -133.87(19) . .
O9 P3 C5 C6 111.26(19) . .
O7 P3 C5 C4 170.14(17) . .
O8 P3 C5 C4 45.4(2) . .
O9 P3 C5 C4 -69.4(2) . .
C4 C5 C6 C1 -2.3(3) . .
P3 C5 C6 C1 177.06(17) . .
C2 C1 C6 C5 2.9(3) . .
P1 C1 C6 C5 -176.11(17) . .
C11 N1 C7 C8 -0.6(4) . .
Cu1 N1 C7 C8 -172.76(18) . .
N1 C7 C8 C9 2.3(4) . .
C7 C8 C9 C10 -1.6(4) . .
C8 C9 C10 C11 -0.6(4) . .
C7 N1 C11 C10 -1.7(3) . .
Cu1 N1 C11 C10 171.19(17) . .
C7 N1 C11 C12 179.4(2) . .
Cu1 N1 C11 C12 -7.7(2) . .
C9 C10 C11 N1 2.3(4) . .
C9 C10 C11 C12 -178.9(2) . .
C16 N2 C12 C13 -3.0(3) . .
Cu1 N2 C12 C13 173.42(18) . .
C16 N2 C12 C11 177.0(2) . .
Cu1 N2 C12 C11 -6.6(2) . .
N1 C11 C12 N2 9.3(3) . .
C10 C11 C12 N2 -169.5(2) . .
N1 C11 C12 C13 -170.6(2) . .
C10 C11 C12 C13 10.5(4) . .
N2 C12 C13 C14 1.1(4) . .
C11 C12 C13 C14 -178.9(2) . .
C12 C13 C14 C15 1.1(4) . .
C13 C14 C15 C16 -1.3(4) . .
C12 N2 C16 C15 2.8(3) . .
Cu1 N2 C16 C15 -173.24(18) . .
C14 C15 C16 N2 -0.6(4) . .
