#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:17:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179783 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/79/7007930.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_7007930
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_sum            'C16 H13 Cu F2 N3 O5 P V'
_chemical_formula_weight         510.74
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.3650(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2914(4)
_cell_length_b                   18.1119(10)
_cell_length_c                   12.9448(7)
_cell_measurement_reflns_used    21868
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.50
_cell_measurement_theta_min      1.95
_cell_volume                     1691.32(16)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21868
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         31.50
_diffrn_reflns_theta_min         1.95
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0.001
_exptl_absorpt_coefficient_mu    1.964
_exptl_absorpt_correction_T_max  0.7984
_exptl_absorpt_correction_T_min  0.4718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELXL-97 (SHELDRICK, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.006
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         5620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0291
_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)+(0.0370P)²+1.3030P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                5083
_reflns_number_total             5620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b412808g.txt
_cod_data_source_block           p21_n
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      P21/n
_cod_database_code               7007930
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.68674(3) 0.234891(10) 0.560358(14) 0.00817(5) Uani 1 1 d . . .
V1 V 0.97014(3) 0.130211(14) 0.75232(2) 0.00860(6) Uani 1 1 d . . .
P1 P 0.57956(5) 0.07903(2) 0.62952(3) 0.00790(7) Uani 1 1 d . . .
O1 O 0.85205(16) 0.20522(6) 0.71191(9) 0.0121(2) Uani 1 1 d . . .
O2 O 0.54314(15) 0.14660(6) 0.56048(9) 0.0113(2) Uani 1 1 d . . .
O3 O 0.78311(15) 0.06227(6) 0.66496(9) 0.0102(2) Uani 1 1 d . . .
O4 O 0.48364(16) 0.08377(7) 0.73013(9) 0.0128(2) Uani 1 1 d . . .
H4' H 0.3683 0.0868 0.7129 0.019 Uiso 1 1 calc R . .
O5 O 0.91310(16) 0.10563(6) 0.86432(9) 0.0120(2) Uani 1 1 d . . .
F1 F 1.13032(13) 0.06872(6) 0.68556(8) 0.0168(2) Uani 1 1 d . . .
F2 F 1.19061(14) 0.17794(6) 0.79972(8) 0.0174(2) Uani 1 1 d . . .
N1 N 0.50486(18) 0.30241(7) 0.61799(10) 0.0095(2) Uani 1 1 d . . .
N2 N 0.79016(18) 0.32944(7) 0.53263(10) 0.0089(2) Uani 1 1 d . . .
N3 N 0.89502(18) 0.20179(7) 0.48035(10) 0.0097(2) Uani 1 1 d . . .
C1 C 0.3585(2) 0.28127(9) 0.66217(12) 0.0114(3) Uani 1 1 d . . .
H1 H 0.3308 0.2301 0.6651 0.014 Uiso 1 1 calc R . .
C2 C 0.2452(2) 0.33181(9) 0.70409(13) 0.0124(3) Uani 1 1 d . . .
H2 H 0.1424 0.3155 0.7354 0.015 Uiso 1 1 calc R . .
C3 C 0.2862(2) 0.40646(9) 0.69904(13) 0.0126(3) Uani 1 1 d . . .
H3 H 0.2107 0.4421 0.7264 0.015 Uiso 1 1 calc R . .
C4 C 0.4392(2) 0.42869(9) 0.65348(12) 0.0115(3) Uani 1 1 d . . .
H4 H 0.4694 0.4795 0.6494 0.014 Uiso 1 1 calc R . .
C5 C 0.5462(2) 0.37533(8) 0.61440(12) 0.0089(3) Uani 1 1 d . . .
C6 C 0.7148(2) 0.39083(8) 0.56612(12) 0.0094(3) Uani 1 1 d . . .
C7 C 0.7941(2) 0.45958(8) 0.55496(12) 0.0106(3) Uani 1 1 d . . .
H7 H 0.7418 0.5029 0.5801 0.013 Uiso 1 1 calc R . .
C8 C 0.9534(2) 0.46383(8) 0.50562(12) 0.0092(3) Uani 1 1 d . . .
C9 C 1.0236(2) 0.39900(8) 0.46762(12) 0.0100(3) Uani 1 1 d . . .
H9 H 1.1282 0.4007 0.4317 0.012 Uiso 1 1 calc R . .
C10 C 0.9382(2) 0.33215(8) 0.48307(12) 0.0091(3) Uani 1 1 d . . .
C11 C 0.9980(2) 0.25856(8) 0.45200(12) 0.0094(3) Uani 1 1 d . . .
C12 C 1.1494(2) 0.24711(9) 0.40001(12) 0.0116(3) Uani 1 1 d . . .
H12 H 1.2195 0.2876 0.3804 0.014 Uiso 1 1 calc R . .
C13 C 1.1961(2) 0.17508(9) 0.37736(13) 0.0122(3) Uani 1 1 d . . .
H13 H 1.2988 0.1658 0.3417 0.015 Uiso 1 1 calc R . .
C14 C 1.0920(2) 0.11674(9) 0.40705(12) 0.0119(3) Uani 1 1 d . . .
H14 H 1.1223 0.0672 0.3924 0.014 Uiso 1 1 calc R . .
C15 C 0.9424(2) 0.13266(8) 0.45871(12) 0.0113(3) Uani 1 1 d . . .
H15 H 0.8710 0.0929 0.4795 0.014 Uiso 1 1 calc R . .
C16 C 0.4714(2) 0.00301(8) 0.55467(12) 0.0106(3) Uani 1 1 d . . .
H16A H 0.5045 -0.0435 0.5932 0.013 Uiso 1 1 calc R . .
H16B H 0.3352 0.0088 0.5475 0.013 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'
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'
H H 0.0000 0.0000 '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
O2 Cu1 N2 166.76(5) . . ?
O2 Cu1 N1 96.71(5) . . ?
N2 Cu1 N1 80.03(5) . . ?
O2 Cu1 N3 101.66(5) . . ?
N2 Cu1 N3 80.02(5) . . ?
N1 Cu1 N3 159.50(5) . . ?
O2 Cu1 O1 91.37(5) . . ?
N2 Cu1 O1 101.74(5) . . ?
N1 Cu1 O1 96.97(5) . . ?
N3 Cu1 O1 91.66(5) . . ?
O5 V1 O1 108.54(6) . . ?
O5 V1 F2 98.90(5) . . ?
O1 V1 F2 96.23(5) . . ?
O5 V1 F1 119.75(5) . . ?
O1 V1 F1 131.40(5) . . ?
F2 V1 F1 82.15(5) . . ?
O5 V1 O3 95.25(5) . . ?
O1 V1 O3 92.57(5) . . ?
F2 V1 O3 160.00(5) . . ?
F1 V1 O3 78.57(4) . . ?
O2 P1 O3 114.78(6) . . ?
O2 P1 O4 112.62(7) . . ?
O3 P1 O4 107.12(7) . . ?
O2 P1 C16 105.96(7) . . ?
O3 P1 C16 110.01(7) . . ?
O4 P1 C16 106.01(7) . . ?
V1 O1 Cu1 132.18(6) . . ?
P1 O2 Cu1 128.82(7) . . ?
P1 O3 V1 126.07(7) . . ?
C1 N1 C5 119.21(13) . . ?
C1 N1 Cu1 126.21(11) . . ?
C5 N1 Cu1 114.50(10) . . ?
C10 N2 C6 121.57(13) . . ?
C10 N2 Cu1 119.23(10) . . ?
C6 N2 Cu1 119.17(10) . . ?
C15 N3 C11 118.86(13) . . ?
C15 N3 Cu1 127.75(11) . . ?
C11 N3 Cu1 113.31(10) . . ?
N1 C1 C2 122.19(14) . . ?
C3 C2 C1 118.51(14) . . ?
C2 C3 C4 119.46(15) . . ?
C5 C4 C3 118.76(14) . . ?
N1 C5 C4 121.86(14) . . ?
N1 C5 C6 113.58(13) . . ?
C4 C5 C6 124.56(14) . . ?
N2 C6 C7 120.91(14) . . ?
N2 C6 C5 112.52(13) . . ?
C7 C6 C5 126.57(14) . . ?
C6 C7 C8 118.68(14) . . ?
C9 C8 C7 118.84(14) . . ?
C9 C8 C8 120.50(17) . 3_766 ?
C7 C8 C8 120.66(17) . 3_766 ?
C10 C9 C8 119.13(14) . . ?
N2 C10 C9 120.79(14) . . ?
N2 C10 C11 112.91(13) . . ?
C9 C10 C11 126.28(14) . . ?
N3 C11 C12 121.91(14) . . ?
N3 C11 C10 114.47(13) . . ?
C12 C11 C10 123.60(14) . . ?
C11 C12 C13 118.57(15) . . ?
C14 C13 C12 119.73(14) . . ?
C13 C14 C15 118.31(14) . . ?
N3 C15 C14 122.61(14) . . ?
C16 C16 P1 113.23(14) 3_656 . ?
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 O2 1.9116(11) . ?
Cu1 N2 1.9258(13) . ?
Cu1 N1 2.0246(13) . ?
Cu1 N3 2.0484(13) . ?
Cu1 O1 2.2141(12) . ?
V1 O5 1.6275(12) . ?
V1 O1 1.6522(12) . ?
V1 F2 1.8496(10) . ?
V1 F1 1.9091(10) . ?
V1 O3 2.0504(11) . ?
P1 O2 1.5159(12) . ?
P1 O3 1.5190(11) . ?
P1 O4 1.5677(12) . ?
P1 C16 1.7983(15) . ?
N1 C1 1.338(2) . ?
N1 C5 1.3570(19) . ?
N2 C10 1.3346(19) . ?
N2 C6 1.3400(19) . ?
N3 C15 1.339(2) . ?
N3 C11 1.3548(19) . ?
C1 C2 1.394(2) . ?
C2 C3 1.388(2) . ?
C3 C4 1.395(2) . ?
C4 C5 1.383(2) . ?
C5 C6 1.485(2) . ?
C6 C7 1.389(2) . ?
C7 C8 1.407(2) . ?
C8 C9 1.399(2) . ?
C8 C8 1.493(3) 3_766 ?
C9 C10 1.389(2) . ?
C10 C11 1.476(2) . ?
C11 C12 1.389(2) . ?
C12 C13 1.390(2) . ?
C13 C14 1.387(2) . ?
C14 C15 1.390(2) . ?
C16 C16 1.536(3) 3_656 ?
