#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/85/2018553.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2018553
loop_
_publ_author_name
'Venegas-Yazigi, Diego'
'Vega, Andres'
'Valdes de la Barra, Karen'
'Saldias, Marianela'
'Le Fur, Eric'
_publ_section_title
;
 A new hybrid organic--inorganic chain:
 [(phen)Cu--μ-(κ²O:O'-VP₂O₁₀H₃)₂--Cu(phen)]ₙ
;
_journal_coeditor_code           YP3013
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m200
_journal_page_last               m202
_journal_paper_doi               10.1107/S0108270112026005
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Cu V (H P O4) (H2 P O4) O2 (C12 H8 N2)]'
_chemical_formula_moiety         'C12 H11 Cu N2 O10 P2 V'
_chemical_formula_sum            'C12 H11 Cu N2 O10 P2 V'
_chemical_formula_weight         519.66
_chemical_name_systematic
;
poly[(dihydrogenphosphato-κO)(μ₃-hydrogenphosphato)di-μ-oxido-
(1,10-phenanthroline)copper(II)vanadium(V)]
;
_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           SHELXL97
_cell_angle_alpha                75.25(3)
_cell_angle_beta                 82.58(3)
_cell_angle_gamma                84.91(3)
_cell_formula_units_Z            2
_cell_length_a                   7.2350(14)
_cell_length_b                   10.705(2)
_cell_length_c                   11.624(2)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.1
_cell_measurement_theta_min      2.50
_cell_volume                     861.9(3)
_computing_cell_refinement       'SAINT-NT (Bruker, 1999)'
_computing_data_collection       'SMART-NT (Bruker, 2001)'
_computing_data_reduction        'SAINT-NT (Bruker, 1999)'
_computing_molecular_graphics
;
SHELXTL-NT (Sheldrick, 2008) and ORTEPIII (Farrugia 1997)
;
_computing_publication_material  'SHELXTL-NT (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL-NT (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL-NT (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16352
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.20
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.021
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.493
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0264
_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+1.0381P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0757
_reflns_number_gt                2737
_reflns_number_total             3031
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            yp3013.cif
_cod_data_source_block           I
_cod_database_code               2018553
_cod_database_fobs_code          2018553
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu1 1.12123(4) 0.63888(3) 0.79354(3) 0.02349(11) Uani d . 1 1 . .
V V1 0.64322(6) 0.62598(4) 0.83604(4) 0.02653(13) Uani d . 1 1 . .
P P1 0.92146(9) 0.38207(6) 0.92512(6) 0.02031(15) Uani d . 1 1 . .
P P2 0.57687(10) 0.80389(6) 1.03196(7) 0.02956(18) Uani d . 1 1 . .
O O1 0.7417(3) 0.46947(19) 0.91659(19) 0.0348(5) Uani d . 1 1 A .
O O2 1.0856(2) 0.45305(17) 0.85199(17) 0.0276(4) Uani d . 1 1 A .
O O3 0.9501(3) 0.32515(19) 1.05341(16) 0.0327(4) Uani d . 1 1 . .
O O4 0.9004(3) 0.2714(2) 0.86304(19) 0.0357(5) Uani d . 1 1 A .
O O5 0.7869(3) 0.6841(2) 0.7222(2) 0.0448(5) Uani d . 1 1 A .
O O6 0.4540(3) 0.6055(2) 0.7902(2) 0.0509(6) Uani d . 1 1 . .
O O7 0.3863(3) 0.86317(18) 1.0534(2) 0.0390(5) Uani d . 1 1 A .
O O8 0.6202(3) 0.7018(2) 1.1470(2) 0.0576(7) Uani d . 1 1 A .
O O9 0.7233(3) 0.9043(2) 1.0087(3) 0.0721(10) Uani d . 1 1 A .
O O10A 0.5764(11) 0.7266(9) 0.9405(9) 0.0552(19) Uani d P 0.60 1 A 1
O O10B 0.6308(15) 0.7593(12) 0.9169(12) 0.041(2) Uani d P 0.40 1 A 2
N N1 1.1515(3) 0.8276(2) 0.7169(2) 0.0276(5) Uani d . 1 1 . .
N N2 1.1869(3) 0.6241(2) 0.62461(19) 0.0262(5) Uani d . 1 1 . .
C C1 1.2038(4) 0.5192(3) 0.5823(3) 0.0361(7) Uani d . 1 1 . .
H H1 1.1742 0.4401 0.6341 0.043 Uiso calc R 1 1 . .
C C2 1.2648(5) 0.5238(3) 0.4622(3) 0.0456(8) Uani d . 1 1 . .
H H2 1.2780 0.4485 0.4353 0.055 Uiso calc R 1 1 . .
C C3 1.3049(5) 0.6395(4) 0.3851(3) 0.0450(8) Uani d . 1 1 . .
H H3 1.3452 0.6432 0.3051 0.054 Uiso calc R 1 1 . .
C C4 1.2855(4) 0.7532(3) 0.4258(3) 0.0376(7) Uani d . 1 1 . .
C C5 1.2264(3) 0.7394(3) 0.5481(2) 0.0272(6) Uani d . 1 1 . .
C C6 1.2054(4) 0.8496(3) 0.5976(2) 0.0287(6) Uani d . 1 1 . .
C C7 1.2380(4) 0.9737(3) 0.5238(3) 0.0396(7) Uani d . 1 1 . .
C C8 1.2105(5) 1.0770(3) 0.5791(3) 0.0508(9) Uani d . 1 1 . .
H H8 1.2286 1.1610 0.5340 0.061 Uiso calc R 1 1 . .
C C9 1.1571(5) 1.0542(3) 0.6992(4) 0.0499(9) Uani d . 1 1 . .
H H9 1.1403 1.1224 0.7363 0.060 Uiso calc R 1 1 . .
C C10 1.1278(4) 0.9276(3) 0.7663(3) 0.0379(7) Uani d . 1 1 . .
H H10 1.0906 0.9132 0.8480 0.046 Uiso calc R 1 1 . .
C C11 1.2959(5) 0.9847(4) 0.3989(3) 0.0529(9) Uani d . 1 1 . .
H H11 1.3176 1.0659 0.3485 0.063 Uiso calc R 1 1 . .
C C12 1.3195(5) 0.8801(4) 0.3532(3) 0.0514(9) Uani d . 1 1 . .
H H12 1.3590 0.8907 0.2721 0.062 Uiso calc R 1 1 . .
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 Cu1 O2 2_767 . 94.30(9) y
O3 Cu1 N2 2_767 . 172.94(9) y
O2 Cu1 N2 . . 92.16(9) y
O3 Cu1 N1 2_767 . 91.00(9) y
O2 Cu1 N1 . . 173.99(9) y
N2 Cu1 N1 . . 82.42(10) y
O3 Cu1 O6 2_767 1_655 102.09(10) y
O2 Cu1 O6 . 1_655 92.22(9) y
N2 Cu1 O6 . 1_655 80.48(10) y
N1 Cu1 O6 . 1_655 89.43(9) y
O6 V1 O5 . . 108.35(14) ?
O6 V1 O10A . . 104.9(3) ?
O5 V1 O10A . . 116.4(2) ?
O6 V1 O1 . . 109.28(12) ?
O5 V1 O1 . . 108.71(11) ?
O10A V1 O1 . . 109.0(3) ?
O6 V1 O10B . . 115.1(4) ?
O5 V1 O10B . . 99.8(3) ?
O1 V1 O10B . . 114.9(4) ?
O3 P1 O2 . . 113.73(12) ?
O3 P1 O1 . . 109.99(12) ?
O2 P1 O1 . . 111.08(11) ?
O3 P1 O4 . . 109.67(12) ?
O2 P1 O4 . . 104.23(11) ?
O1 P1 O4 . . 107.83(12) ?
O7 P2 O10A . . 108.8(4) ?
O7 P2 O10B . . 118.8(5) ?
O10A P2 O10B . . 20.8(3) ?
O7 P2 O9 . . 110.99(12) ?
O10A P2 O9 . . 117.6(3) ?
O10B P2 O9 . . 96.8(3) ?
O7 P2 O8 . . 108.39(13) ?
O10A P2 O8 . . 104.2(4) ?
O10B P2 O8 . . 114.4(5) ?
O9 P2 O8 . . 106.33(18) ?
P1 O2 Cu1 . . 130.63(12) ?
P1 O1 V1 . . 142.85(13) ?
P1 O3 Cu1 . 2_767 139.25(13) ?
C1 N2 C5 . . 118.6(2) ?
C1 N2 Cu1 . . 129.1(2) ?
C5 N2 Cu1 . . 112.23(18) ?
C10 N1 C6 . . 118.6(2) ?
C10 N1 Cu1 . . 129.4(2) ?
C6 N1 Cu1 . . 111.98(18) ?
V1 O6 Cu1 . 1_455 150.57(16) ?
P2 O10A V1 . . 164.2(6) ?
P2 O10B V1 . . 148.6(6) ?
N1 C6 C7 . . 123.0(3) ?
N1 C6 C5 . . 116.6(2) ?
C7 C6 C5 . . 120.4(3) ?
N2 C1 C2 . . 122.1(3) ?
N2 C1 H1 . . 119.0 ?
C2 C1 H1 . . 119.0 ?
N2 C5 C4 . . 123.1(3) ?
N2 C5 C6 . . 116.7(2) ?
C4 C5 C6 . . 120.3(3) ?
C8 C7 C6 . . 116.7(3) ?
C8 C7 C11 . . 125.4(3) ?
C6 C7 C11 . . 117.9(3) ?
C3 C4 C5 . . 116.5(3) ?
C3 C4 C12 . . 125.4(3) ?
C5 C4 C12 . . 118.1(3) ?
C3 C2 C1 . . 119.4(3) ?
C3 C2 H2 . . 120.3 ?
C1 C2 H2 . . 120.3 ?
N1 C10 C9 . . 122.0(3) ?
N1 C10 H10 . . 119.0 ?
C9 C10 H10 . . 119.0 ?
C8 C9 C10 . . 119.7(3) ?
C8 C9 H9 . . 120.2 ?
C10 C9 H9 . . 120.2 ?
C2 C3 C4 . . 120.3(3) ?
C2 C3 H3 . . 119.9 ?
C4 C3 H3 . . 119.9 ?
C9 C8 C7 . . 120.0(3) ?
C9 C8 H8 . . 120.0 ?
C7 C8 H8 . . 120.0 ?
C11 C12 C4 . . 121.8(3) ?
C11 C12 H12 . . 119.1 ?
C4 C12 H12 . . 119.1 ?
C12 C11 C7 . . 121.5(3) ?
C12 C11 H11 . . 119.3 ?
C7 C11 H11 . . 119.3 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 N1 . 2.009(2) y
Cu1 N2 . 2.003(2) y
Cu1 O2 . 1.9603(19) y
Cu1 O3 2_767 1.9122(19) y
Cu1 O5 . 2.632(2) y
Cu1 O6 1_655 2.399(2) y
V1 O6 . 1.584(2) ?
V1 O5 . 1.600(2) ?
V1 O10A . 1.814(9) ?
V1 O1 . 1.831(2) ?
V1 O10B . 1.888(14) ?
P1 O3 . 1.494(2) ?
P1 O2 . 1.5103(19) ?
P1 O1 . 1.532(2) ?
P1 O4 . 1.563(2) ?
P2 O7 . 1.484(2) ?
P2 O10A . 1.505(9) ?
P2 O10B . 1.526(14) ?
P2 O9 . 1.527(2) ?
P2 O8 . 1.544(2) ?
O3 Cu1 2_767 1.9122(19) ?
N2 C1 . 1.326(4) ?
N2 C5 . 1.354(3) ?
N1 C10 . 1.327(4) ?
N1 C6 . 1.357(4) ?
O6 Cu1 1_455 2.399(2) ?
C6 C7 . 1.407(4) ?
C6 C5 . 1.428(4) ?
C1 C2 . 1.398(4) ?
C1 H1 . 0.9300 ?
C5 C4 . 1.405(4) ?
C7 C8 . 1.402(5) ?
C7 C11 . 1.436(5) ?
C4 C3 . 1.404(5) ?
C4 C12 . 1.428(5) ?
C2 C3 . 1.361(5) ?
C2 H2 . 0.9300 ?
C10 C9 . 1.400(4) ?
C10 H10 . 0.9300 ?
C9 C8 . 1.364(5) ?
C9 H9 . 0.9300 ?
C3 H3 . 0.9300 ?
C8 H8 . 0.9300 ?
C12 C11 . 1.345(6) ?
C12 H12 . 0.9300 ?
C11 H11 . 0.9300 ?
