#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:17:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179783 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/79/7007929.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_7007929
loop_
_publ_author_name
'Ouellette, Wayne'
'Golub, Vladimir'
'O'Connor, Charles J'
'Zubieta, Jon'
_publ_section_title
;
 Solid state coordination chemistry of metal oxides: structural
 consequences of fluoride incorporation into the
 oxovanadium-copper-bisterpy-{O3P(CH2)nPO3}4- system, n= 1-5 (bisterpy
 = 2,2':4',4":2",2"'-quaterpyridyl-6', 6"-di-2-pyridine).
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              291
_journal_page_last               309
_journal_paper_doi               10.1039/b412808g
_journal_year                    2005
_chemical_formula_moiety
;
[{Cu2(bisterpy)}V2F2O2(H2O)2{O3P(CH2)2PO3}2]*2H2O (2*2H2O)
;
_chemical_formula_sum            'C17 H19 Cu F N3 O9 P2 V'
_chemical_formula_weight         604.77
_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                108.9150(10)
_cell_angle_beta                 109.9160(10)
_cell_angle_gamma                100.4530(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2116(6)
_cell_length_b                   10.7482(6)
_cell_length_c                   11.0667(6)
_cell_measurement_reflns_used    6622
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.51
_cell_measurement_theta_min      2.12
_cell_volume                     1020.51(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL and CrystalMaker 5.x'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  '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  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13210
_diffrn_reflns_theta_full        31.51
_diffrn_reflns_theta_max         31.51
_diffrn_reflns_theta_min         2.12
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0.001
_exptl_absorpt_coefficient_mu    1.727
_exptl_absorpt_correction_T_max  0.7697
_exptl_absorpt_correction_T_min  0.6254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELXL-97 (SHELDRICK, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.968
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.192
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0454
_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)+(0.0651P)²+2.4469P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1250
_reflns_number_gt                5736
_reflns_number_total             6622
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b412808g.txt
_cod_data_source_block           compound_2
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7007929
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 0.13930(3) 0.13751(3) 0.25237(3) 0.00854(8) Uani 1 1 d . . .
V1 V 0.13388(5) 0.46182(4) 0.70865(4) 0.00976(9) Uani 1 1 d . . .
P1 P 0.29373(7) 0.02094(7) 0.49960(7) 0.01093(13) Uani 1 1 d . . .
P2 P -0.07744(7) 0.27485(7) 0.36448(7) 0.00922(12) Uani 1 1 d . . .
O1 O -0.0328(2) 0.17595(19) 0.26447(19) 0.0111(3) Uani 1 1 d . . .
O2 O 0.0555(2) 0.37427(19) 0.50287(19) 0.0122(3) Uani 1 1 d . . .
O3 O 0.1627(2) 0.64564(19) 0.7077(2) 0.0123(3) Uani 1 1 d . . .
O4 O -0.0054(2) 0.4213(2) 0.7396(2) 0.0152(4) Uani 1 1 d . . .
O5 O 0.2339(2) 0.12839(19) 0.4571(2) 0.0121(3) Uani 1 1 d . . .
O6 O 0.3041(2) -0.0892(2) 0.3721(2) 0.0148(4) Uani 1 1 d . . .
H6 H 0.3645 -0.0506 0.3513 0.022 Uiso 1 1 calc R . .
O7 O 0.4406(2) 0.0845(2) 0.6296(2) 0.0140(3) Uani 1 1 d . . .
O90 O 0.4460(2) 0.2730(2) 0.8711(2) 0.0203(4) Uani 1 1 d . . .
O91 O 0.2251(2) 0.3089(2) 0.6892(2) 0.0152(4) Uani 1 1 d . . .
N1 N 0.0320(2) -0.0720(2) 0.1324(2) 0.0096(4) Uani 1 1 d . . .
N2 N 0.2708(2) 0.0871(2) 0.1657(2) 0.0093(4) Uani 1 1 d . . .
N3 N 0.2767(2) 0.3322(2) 0.3052(2) 0.0111(4) Uani 1 1 d . . .
C1 C -0.0957(3) -0.1462(3) 0.1208(3) 0.0120(4) Uani 1 1 d . . .
C2 C -0.1523(3) -0.2905(3) 0.0483(3) 0.0127(4) Uani 1 1 d . . .
C3 C -0.0738(3) -0.3599(3) -0.0135(3) 0.0132(4) Uani 1 1 d . . .
C4 C 0.0585(3) -0.2834(3) -0.0024(3) 0.0114(4) Uani 1 1 d . . .
C5 C 0.1077(3) -0.1401(2) 0.0707(2) 0.0095(4) Uani 1 1 d . . .
C6 C 0.2434(3) -0.0465(3) 0.0853(3) 0.0093(4) Uani 1 1 d . . .
C7 C 0.3320(3) -0.0849(3) 0.0185(3) 0.0095(4) Uani 1 1 d . . .
C8 C 0.4511(3) 0.0179(2) 0.0353(2) 0.0087(4) Uani 1 1 d . . .
C9 C 0.4749(3) 0.1570(3) 0.1173(3) 0.0106(4) Uani 1 1 d . . .
C10 C 0.3811(3) 0.1879(2) 0.1803(3) 0.0100(4) Uani 1 1 d . . .
C11 C 0.3834(3) 0.3290(3) 0.2588(3) 0.0111(4) Uani 1 1 d . . .
C12 C 0.4788(3) 0.4487(3) 0.2747(3) 0.0186(5) Uani 1 1 d . . .
C13 C 0.4656(4) 0.5766(3) 0.3405(4) 0.0226(6) Uani 1 1 d . . .
C14 C 0.3568(4) 0.5798(3) 0.3868(4) 0.0234(6) Uani 1 1 d . . .
C15 C 0.2646(3) 0.4563(3) 0.3689(3) 0.0165(5) Uani 1 1 d . . .
C16 C 0.1550(3) -0.0789(3) 0.5302(3) 0.0124(4) Uani 1 1 d . . .
C17 C 0.2084(3) -0.1732(3) 0.6003(3) 0.0141(5) Uani 1 1 d . . .
F1 F 0.30002(18) 0.55678(17) 0.88977(17) 0.0156(3) Uani 1 1 d . . .
H1 H -0.146(4) -0.103(4) 0.153(4) 0.012(8) Uiso 1 1 d . . .
H2 H -0.250(4) -0.342(4) 0.033(4) 0.019(10) Uiso 1 1 d . . .
H3 H -0.111(4) -0.463(3) -0.067(3) 0.004(7) Uiso 1 1 d . . .
H4 H 0.109(4) -0.321(4) -0.042(4) 0.013(8) Uiso 1 1 d . . .
H7 H 0.307(4) -0.172(4) -0.040(4) 0.017(9) Uiso 1 1 d . . .
H9 H 0.546(4) 0.223(4) 0.130(4) 0.017(9) Uiso 1 1 d . . .
H12 H 0.555(5) 0.448(5) 0.236(5) 0.034(12) Uiso 1 1 d . . .
H13 H 0.527(6) 0.657(5) 0.350(5) 0.040(13) Uiso 1 1 d . . .
H14 H 0.344(5) 0.659(5) 0.423(5) 0.033(12) Uiso 1 1 d . . .
H15 H 0.194(6) 0.447(6) 0.397(6) 0.050(15) Uiso 1 1 d . . .
H16A H 0.070(5) -0.138(4) 0.438(4) 0.022(10) Uiso 1 1 d . . .
H17A H 0.238(5) -0.245(4) 0.537(4) 0.022(10) Uiso 1 1 d . . .
H16B H 0.127(5) -0.018(4) 0.593(4) 0.022(10) Uiso 1 1 d . . .
H17B H 0.299(5) -0.117(5) 0.697(5) 0.028(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'
F F 0.0171 0.0103 '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'
V V 0.3005 0.5294 '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 N2 157.97(9) . . ?
O1 Cu1 N1 94.21(8) . . ?
N2 Cu1 N1 78.80(8) . . ?
O1 Cu1 N3 102.31(8) . . ?
N2 Cu1 N3 79.13(8) . . ?
N1 Cu1 N3 155.42(8) . . ?
O1 Cu1 O5 97.21(8) . . ?
N2 Cu1 O5 104.36(8) . . ?
N1 Cu1 O5 97.39(8) . . ?
N3 Cu1 O5 98.42(8) . . ?
O4 V1 F1 105.82(9) . . ?
O4 V1 O3 109.01(9) . . ?
F1 V1 O3 84.49(8) . . ?
O4 V1 O2 104.25(9) . . ?
F1 V1 O2 149.46(8) . . ?
O3 V1 O2 90.81(8) . . ?
O4 V1 O91 109.89(10) . . ?
F1 V1 O91 83.58(8) . . ?
O3 V1 O91 141.07(9) . . ?
O2 V1 O91 81.30(8) . . ?
O7 P1 O5 113.81(11) . . ?
O7 P1 O6 110.54(11) . . ?
O5 P1 O6 110.77(11) . . ?
O7 P1 C16 110.29(12) . . ?
O5 P1 C16 106.80(12) . . ?
O6 P1 C16 104.12(12) . . ?
O1 P2 O2 111.57(10) . . ?
O1 P2 O3 110.82(11) . 2_566 ?
O2 P2 O3 111.45(11) . 2_566 ?
O1 P2 C17 108.52(12) . 2_556 ?
O2 P2 C17 109.86(12) . 2_556 ?
O3 P2 C17 104.34(12) 2_566 2_556 ?
P2 O1 Cu1 140.53(12) . . ?
P2 O2 V1 145.97(12) . . ?
P2 O3 V1 140.09(12) 2_566 . ?
P1 O5 Cu1 131.63(11) . . ?
C1 N1 C5 118.7(2) . . ?
C1 N1 Cu1 126.35(17) . . ?
C5 N1 Cu1 114.63(16) . . ?
C6 N2 C10 121.0(2) . . ?
C6 N2 Cu1 119.58(16) . . ?
C10 N2 Cu1 119.25(16) . . ?
C15 N3 C11 118.2(2) . . ?
C15 N3 Cu1 127.67(18) . . ?
C11 N3 Cu1 113.90(17) . . ?
N1 C1 C2 122.1(2) . . ?
C3 C2 C1 119.0(2) . . ?
C2 C3 C4 119.3(2) . . ?
C5 C4 C3 118.6(2) . . ?
N1 C5 C4 122.4(2) . . ?
N1 C5 C6 113.7(2) . . ?
C4 C5 C6 123.9(2) . . ?
N2 C6 C7 120.9(2) . . ?
N2 C6 C5 112.7(2) . . ?
C7 C6 C5 126.3(2) . . ?
C6 C7 C8 119.4(2) . . ?
C9 C8 C7 118.4(2) . . ?
C9 C8 C8 120.2(3) . 2_655 ?
C7 C8 C8 121.4(3) . 2_655 ?
C10 C9 C8 119.1(2) . . ?
N2 C10 C9 121.2(2) . . ?
N2 C10 C11 113.1(2) . . ?
C9 C10 C11 125.5(2) . . ?
N3 C11 C12 122.2(2) . . ?
N3 C11 C10 114.5(2) . . ?
C12 C11 C10 123.1(2) . . ?
C11 C12 C13 119.2(3) . . ?
C14 C13 C12 118.5(3) . . ?
C13 C14 C15 119.8(3) . . ?
N3 C15 C14 122.0(3) . . ?
C17 C16 P1 113.68(18) . . ?
C16 C17 P2 116.40(18) . 2_556 ?
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 1.9142(18) . ?
Cu1 N2 1.955(2) . ?
Cu1 N1 2.051(2) . ?
Cu1 N3 2.067(2) . ?
Cu1 O5 2.1828(19) . ?
V1 O4 1.592(2) . ?
V1 F1 1.9147(17) . ?
V1 O3 1.9478(19) . ?
V1 O2 1.9513(19) . ?
V1 O91 2.0197(19) . ?
P1 O7 1.519(2) . ?
P1 O5 1.5299(19) . ?
P1 O6 1.571(2) . ?
P1 C16 1.813(3) . ?
P2 O1 1.5231(19) . ?
P2 O2 1.5252(19) . ?
P2 O3 1.5383(19) 2_566 ?
P2 C17 1.799(3) 2_556 ?
O3 P2 1.5383(19) 2_566 ?
N1 C1 1.340(3) . ?
N1 C5 1.357(3) . ?
N2 C6 1.337(3) . ?
N2 C10 1.338(3) . ?
N3 C15 1.342(3) . ?
N3 C11 1.355(3) . ?
C1 C2 1.391(4) . ?
C2 C3 1.387(4) . ?
C3 C4 1.391(3) . ?
C4 C5 1.384(3) . ?
C5 C6 1.481(3) . ?
C6 C7 1.389(3) . ?
C7 C8 1.400(3) . ?
C8 C9 1.399(3) . ?
C8 C8 1.494(5) 2_655 ?
C9 C10 1.390(3) . ?
C10 C11 1.474(3) . ?
C11 C12 1.384(4) . ?
C12 C13 1.387(4) . ?
C13 C14 1.374(4) . ?
C14 C15 1.391(4) . ?
C16 C17 1.532(4) . ?
C17 P2 1.799(3) 2_556 ?
