#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/15/7211591.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_7211591
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         'C18 H18 Cu N2 O10 P2, O'
_chemical_formula_sum            'C18 H18 Cu N2 O11 P2'
_chemical_formula_weight         563.82
_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                92.437(2)
_cell_angle_beta                 98.233(2)
_cell_angle_gamma                92.697(2)
_cell_formula_units_Z            2
_cell_length_a                   6.4769(7)
_cell_length_b                   8.4915(9)
_cell_length_c                   18.798(2)
_cell_measurement_reflns_used    5380
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.59
_cell_volume                     1020.81(19)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10151
_diffrn_reflns_theta_full        28.07
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         2.59
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0.001
_exptl_absorpt_coefficient_mu    1.296
_exptl_absorpt_correction_T_max  0.7816
_exptl_absorpt_correction_T_min  0.6971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             574
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0415
_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)+(0.0510P)²+1.7726P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1071
_reflns_number_gt                4592
_reflns_number_total             4921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b910641c.txt
_cod_data_source_block           15
_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        1020.78(19)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7211591
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 0.5000 0.0000 1.0000 0.01339(11) Uani 1 2 d S
Cu2 Cu 0.5000 0.5000 0.5000 0.01544(11) Uani 1 2 d S
P1 P 0.71288(10) 0.03863(7) 0.83109(3) 0.01434(14) Uani 1 1 d .
P2 P 0.76016(10) 0.58931(7) 0.68682(3) 0.01392(14) Uani 1 1 d .
N1 N 0.5328(3) 0.2104(2) 1.05011(11) 0.0126(4) Uani 1 1 d .
N2 N 0.4709(3) 0.7108(2) 0.46228(11) 0.0155(4) Uani 1 1 d .
O1 O 0.4970(3) 0.0091(2) 0.79200(10) 0.0204(4) Uani 1 1 d .
O2 O 0.7075(3) 0.1133(2) 0.90719(10) 0.0167(4) Uani 1 1 d .
O3 O 0.8398(3) -0.1133(2) 0.84096(10) 0.0182(4) Uani 1 1 d .
O4 O 0.7589(3) 0.5925(2) 0.60409(10) 0.0178(4) Uani 1 1 d .
O5 O 0.8869(3) 0.7296(2) 0.72478(10) 0.0177(4) Uani 1 1 d .
O6 O 0.5331(3) 0.5708(2) 0.70125(11) 0.0213(4) Uani 1 1 d .
O7 O 0.2260(3) 0.0728(2) 0.95999(9) 0.0158(3) Uani 1 1 d .
O8 O 0.0149(3) 0.2694(2) 0.97345(10) 0.0179(4) Uani 1 1 d .
O9 O 0.2484(3) 0.5535(2) 0.54376(10) 0.0170(4) Uani 1 1 d .
O10 O 0.0150(3) 0.7410(2) 0.54250(10) 0.0197(4) Uani 1 1 d .
O90 O 0.2998(3) 0.7882(2) 0.70711(11) 0.0209(4) Uani 1 1 d .
C1 C 0.8719(4) 0.4103(3) 0.71641(13) 0.0140(4) Uani 1 1 d .
C2 C 0.7655(4) 0.3069(3) 0.75600(13) 0.0152(5) Uani 1 1 d .
H2 H 0.6278 0.3276 0.7642 0.018 Uiso 1 1 calc R
C3 C 0.8590(4) 0.1730(3) 0.78381(13) 0.0146(5) Uani 1 1 d .
C4 C 1.0624(4) 0.1464(3) 0.77313(14) 0.0169(5) Uani 1 1 d .
H4 H 1.1301 0.0587 0.7936 0.020 Uiso 1 1 calc R
C5 C 1.1675(4) 0.2475(3) 0.73263(14) 0.0183(5) Uani 1 1 d .
H5 H 1.3056 0.2267 0.7248 0.022 Uiso 1 1 calc R
C6 C 1.0735(4) 0.3787(3) 0.70341(14) 0.0170(5) Uani 1 1 d .
H6 H 1.1454 0.4460 0.6749 0.020 Uiso 1 1 calc R
C7 C 0.7013(4) 0.2757(3) 1.09228(13) 0.0166(5) Uani 1 1 d .
H7 H 0.8222 0.2165 1.1023 0.020 Uiso 1 1 calc R
C8 C 0.7027(4) 0.4294(3) 1.12192(14) 0.0194(5) Uani 1 1 d .
H8 H 0.8241 0.4752 1.1513 0.023 Uiso 1 1 calc R
C9 C 0.5258(4) 0.5141(3) 1.10803(14) 0.0188(5) Uani 1 1 d .
H9 H 0.5247 0.6189 1.1277 0.023 Uiso 1 1 calc R
C10 C 0.3485(4) 0.4448(3) 1.06500(13) 0.0163(5) Uani 1 1 d .
H10 H 0.2242 0.5001 1.0555 0.020 Uiso 1 1 calc R
C11 C 0.3601(4) 0.2930(3) 1.03667(13) 0.0134(4) Uani 1 1 d .
C12 C 0.1856(4) 0.2058(3) 0.98654(13) 0.0146(4) Uani 1 1 d .
C13 C 0.5951(4) 0.7856(3) 0.42231(14) 0.0177(5) Uani 1 1 d .
H13 H 0.7229 0.7417 0.4147 0.021 Uiso 1 1 calc R
C14 C 0.5405(5) 0.9272(3) 0.39147(14) 0.0210(5) Uani 1 1 d .
H14 H 0.6319 0.9809 0.3642 0.025 Uiso 1 1 calc R
C15 C 0.3523(5) 0.9881(3) 0.40104(15) 0.0231(6) Uani 1 1 d .
H15 H 0.3103 1.0820 0.3787 0.028 Uiso 1 1 calc R
C16 C 0.2247(4) 0.9115(3) 0.44350(14) 0.0195(5) Uani 1 1 d .
H16 H 0.0955 0.9525 0.4514 0.023 Uiso 1 1 calc R
C17 C 0.2910(4) 0.7735(3) 0.47395(13) 0.0155(5) Uani 1 1 d .
C18 C 0.1739(4) 0.6820(3) 0.52371(13) 0.0158(5) Uani 1 1 d .
H2' H 0.803(7) 0.154(5) 0.926(2) 0.048(13) Uiso 1 1 d .
H4' H 0.864(9) 0.631(7) 0.587(3) 0.085(19) 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
O7 Cu1 O7 179.998(1) 2_657 .
O7 Cu1 N1 83.23(8) 2_657 2_657
O7 Cu1 N1 96.77(8) . 2_657
O7 Cu1 N1 96.77(8) 2_657 .
O7 Cu1 N1 83.23(8) . .
N1 Cu1 N1 180.00(14) 2_657 .
N2 Cu2 N2 179.998(1) 2_666 .
N2 Cu2 O9 82.86(8) 2_666 2_666
N2 Cu2 O9 97.14(8) . 2_666
N2 Cu2 O9 97.14(8) 2_666 .
N2 Cu2 O9 82.86(8) . .
O9 Cu2 O9 180.000(1) 2_666 .
O1 P1 O2 110.42(11) . .
O1 P1 O3 114.11(11) . .
O2 P1 O3 106.87(10) . .
O1 P1 C3 110.23(11) . .
O2 P1 C3 107.88(11) . .
O3 P1 C3 107.08(11) . .
O5 P2 O6 115.69(11) . .
O5 P2 O4 110.57(11) . .
O6 P2 O4 108.30(11) . .
O5 P2 C1 110.02(11) . .
O6 P2 C1 103.99(11) . .
O4 P2 C1 107.85(11) . .
C7 N1 C11 119.7(2) . .
C7 N1 Cu1 127.89(17) . .
C11 N1 Cu1 112.41(16) . .
C13 N2 C17 119.6(2) . .
C13 N2 Cu2 127.55(18) . .
C17 N2 Cu2 112.44(17) . .
P1 O2 H2' 118(4) . .
P2 O4 H4' 121(4) . .
C12 O7 Cu1 113.92(16) . .
C18 O9 Cu2 113.51(16) . .
C2 C1 C6 119.6(2) . .
C2 C1 P2 120.81(19) . .
C6 C1 P2 119.47(19) . .
C1 C2 C3 120.9(2) . .
C1 C2 H2 119.5 . .
C3 C2 H2 119.5 . .
C4 C3 C2 118.9(2) . .
C4 C3 P1 121.59(19) . .
C2 C3 P1 119.47(19) . .
C3 C4 C5 120.3(2) . .
C3 C4 H4 119.8 . .
C5 C4 H4 119.8 . .
C4 C5 C6 120.9(2) . .
C4 C5 H5 119.5 . .
C6 C5 H5 119.5 . .
C5 C6 C1 119.2(2) . .
C5 C6 H6 120.4 . .
C1 C6 H6 120.4 . .
N1 C7 C8 121.1(2) . .
N1 C7 H7 119.5 . .
C8 C7 H7 119.5 . .
C9 C8 C7 119.3(2) . .
C9 C8 H8 120.4 . .
C7 C8 H8 120.4 . .
C8 C9 C10 119.7(2) . .
C8 C9 H9 120.2 . .
C10 C9 H9 120.2 . .
C11 C10 C9 117.7(2) . .
C11 C10 H10 121.1 . .
C9 C10 H10 121.1 . .
N1 C11 C10 122.6(2) . .
N1 C11 C12 113.5(2) . .
C10 C11 C12 123.9(2) . .
O8 C12 O7 125.1(2) . .
O8 C12 C11 118.4(2) . .
O7 C12 C11 116.5(2) . .
N2 C13 C14 121.2(2) . .
N2 C13 H13 119.4 . .
C14 C13 H13 119.4 . .
C15 C14 C13 119.2(2) . .
C15 C14 H14 120.4 . .
C13 C14 H14 120.4 . .
C14 C15 C16 119.6(2) . .
C14 C15 H15 120.2 . .
C16 C15 H15 120.2 . .
C17 C16 C15 118.1(2) . .
C17 C16 H16 120.9 . .
C15 C16 H16 120.9 . .
N2 C17 C16 122.2(2) . .
N2 C17 C18 113.8(2) . .
C16 C17 C18 124.0(2) . .
O10 C18 O9 126.1(2) . .
O10 C18 C17 117.5(2) . .
O9 C18 C17 116.4(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O7 1.9644(17) 2_657
Cu1 O7 1.9644(17) .
Cu1 N1 1.972(2) 2_657
Cu1 N1 1.972(2) .
Cu2 N2 1.960(2) 2_666
Cu2 N2 1.960(2) .
Cu2 O9 1.9901(18) 2_666
Cu2 O9 1.9901(18) .
P1 O1 1.488(2) .
P1 O2 1.5456(19) .
P1 O3 1.5656(18) .
P1 C3 1.792(3) .
P2 O5 1.5066(19) .
P2 O6 1.5356(19) .
P2 O4 1.5555(19) .
P2 C1 1.790(2) .
N1 C7 1.336(3) .
N1 C11 1.347(3) .
N2 C13 1.335(3) .
N2 C17 1.346(3) .
O2 H2' 0.73(5) .
O4 H4' 0.85(6) .
O7 C12 1.269(3) .
O8 C12 1.250(3) .
O9 C18 1.265(3) .
O10 C18 1.254(3) .
C1 C2 1.395(3) .
C1 C6 1.399(3) .
C2 C3 1.399(3) .
C2 H2 0.9500 .
C3 C4 1.389(3) .
C4 C5 1.389(4) .
C4 H4 0.9500 .
C5 C6 1.391(4) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C8 1.397(4) .
C7 H7 0.9500 .
C8 C9 1.380(4) .
C8 H8 0.9500 .
C9 C10 1.396(4) .
C9 H9 0.9500 .
C10 C11 1.384(3) .
C10 H10 0.9500 .
C11 C12 1.506(3) .
C13 C14 1.395(4) .
C13 H13 0.9500 .
C14 C15 1.378(4) .
C14 H14 0.9500 .
C15 C16 1.388(4) .
C15 H15 0.9500 .
C16 C17 1.385(3) .
C16 H16 0.9500 .
C17 C18 1.504(3) .
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
O7 Cu1 N1 C7 4.5(2) 2_657
O7 Cu1 N1 C7 -175.5(2) .
N1 Cu1 N1 C7 161(6) 2_657
O7 Cu1 N1 C11 -176.91(16) 2_657
O7 Cu1 N1 C11 3.09(16) .
N1 Cu1 N1 C11 -21(6) 2_657
N2 Cu2 N2 C13 -55(3) 2_666
O9 Cu2 N2 C13 -2.0(2) 2_666
O9 Cu2 N2 C13 178.0(2) .
N2 Cu2 N2 C17 118(3) 2_666
O9 Cu2 N2 C17 170.89(17) 2_666
O9 Cu2 N2 C17 -9.11(17) .
O7 Cu1 O7 C12 -119(6) 2_657
N1 Cu1 O7 C12 174.35(17) 2_657
N1 Cu1 O7 C12 -5.65(17) .
N2 Cu2 O9 C18 -173.65(17) 2_666
N2 Cu2 O9 C18 6.34(17) .
O9 Cu2 O9 C18 -21(15) 2_666
O5 P2 C1 C2 113.2(2) .
O6 P2 C1 C2 -11.3(2) .
O4 P2 C1 C2 -126.1(2) .
O5 P2 C1 C6 -62.9(2) .
O6 P2 C1 C6 172.6(2) .
O4 P2 C1 C6 57.8(2) .
C6 C1 C2 C3 1.0(4) .
P2 C1 C2 C3 -175.14(19) .
C1 C2 C3 C4 1.7(4) .
C1 C2 C3 P1 -177.36(19) .
O1 P1 C3 C4 -135.3(2) .
O2 P1 C3 C4 104.1(2) .
O3 P1 C3 C4 -10.7(2) .
O1 P1 C3 C2 43.8(2) .
O2 P1 C3 C2 -76.9(2) .
O3 P1 C3 C2 168.42(19) .
C2 C3 C4 C5 -2.9(4) .
P1 C3 C4 C5 176.1(2) .
C3 C4 C5 C6 1.4(4) .
C4 C5 C6 C1 1.3(4) .
C2 C1 C6 C5 -2.5(4) .
P2 C1 C6 C5 173.7(2) .
C11 N1 C7 C8 -1.0(4) .
Cu1 N1 C7 C8 177.50(18) .
N1 C7 C8 C9 0.9(4) .
C7 C8 C9 C10 0.3(4) .
C8 C9 C10 C11 -1.2(4) .
C7 N1 C11 C10 0.0(4) .
Cu1 N1 C11 C10 -178.76(19) .
C7 N1 C11 C12 178.3(2) .
Cu1 N1 C11 C12 -0.5(2) .
C9 C10 C11 N1 1.1(4) .
C9 C10 C11 C12 -177.0(2) .
Cu1 O7 C12 O8 -174.1(2) .
Cu1 O7 C12 C11 6.9(3) .
N1 C11 C12 O8 176.6(2) .
C10 C11 C12 O8 -5.1(4) .
N1 C11 C12 O7 -4.3(3) .
C10 C11 C12 O7 173.9(2) .
C17 N2 C13 C14 -0.8(4) .
Cu2 N2 C13 C14 171.64(19) .
N2 C13 C14 C15 -1.7(4) .
C13 C14 C15 C16 2.7(4) .
C14 C15 C16 C17 -1.1(4) .
C13 N2 C17 C16 2.5(4) .
Cu2 N2 C17 C16 -171.0(2) .
C13 N2 C17 C18 -176.3(2) .
Cu2 N2 C17 C18 10.2(3) .
C15 C16 C17 N2 -1.5(4) .
C15 C16 C17 C18 177.1(2) .
Cu2 O9 C18 O10 179.0(2) .
Cu2 O9 C18 C17 -2.5(3) .
N2 C17 C18 O10 173.5(2) .
C16 C17 C18 O10 -5.3(4) .
N2 C17 C18 O9 -5.2(3) .
C16 C17 C18 O9 176.0(2) .
