#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/23/7022314.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_7022314
loop_
_publ_author_name
'Orive, Joseba'
'Larrea, Edurne S.'
'Fernández de Luis, Roberto'
'Iglesias, Marta'
'Mesa, José L'
'Rojo, Teófilo'
'Arriortua, María I'
_publ_section_title
;
 Amine templated open-framework vanadium(III) phosphites with catalytic
 properties.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4500
_journal_page_last               4512
_journal_paper_doi               10.1039/c2dt32286b
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C2.5 H10.5 N O7 P2 V'
_chemical_formula_weight         279.5
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2012-04-16T16:49:36-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                112.901(4)
_cell_angle_beta                 95.506(2)
_cell_angle_gamma                90.995(2)
_cell_formula_units_Z            2
_cell_length_a                   5.24030(10)
_cell_length_b                   9.2240(3)
_cell_length_c                   10.8060(4)
_cell_measurement_reflns_used    9567
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.5464
_cell_measurement_theta_min      3.7149
_cell_volume                     478.08(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.3504
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_orient_matrix_UB_11      0.0132506412
_diffrn_orient_matrix_UB_12      -0.0192230465
_diffrn_orient_matrix_UB_13      0.0576192233
_diffrn_orient_matrix_UB_21      -0.0001198122
_diffrn_orient_matrix_UB_22      0.0809968604
_diffrn_orient_matrix_UB_23      0.0424675843
_diffrn_orient_matrix_UB_31      -0.1354766776
_diffrn_orient_matrix_UB_32      -0.0070071974
_diffrn_orient_matrix_UB_33      -0.0024915687
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13363
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         3.73
_exptl_absorpt_coefficient_mu    1.382
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_meas      1.931(2)
_exptl_crystal_density_method    flotation
_exptl_crystal_F_000             283
_exptl_crystal_size_max          0.5462
_exptl_crystal_size_mid          0.1048
_exptl_crystal_size_min          0.0795
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2012
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0671P)²+0.1791P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                1730
_reflns_number_total             2012
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c2dt32286b.txt
_cod_data_source_block           compound_1
_cod_original_formula_sum        'C2.50 H10.50 N O7 P2 V'
_cod_database_code               7022314
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
V1 V 0.5 0.5 0.5 0.01282(16) Uani 1 2 d S . .
V2 V 0 0 0.5 0.01433(17) Uani 1 2 d S . .
P1 P 1.04034(11) 0.62842(7) 0.70789(6) 0.01581(17) Uani 1 1 d . . .
P2 P 0.47321(11) 0.10863(7) 0.37619(6) 0.01463(17) Uani 1 1 d D . .
O1 O 0.7627(3) 0.5636(2) 0.66072(18) 0.0217(4) Uani 1 1 d . . .
O2 O 0.5219(3) 0.27363(19) 0.48676(19) 0.0223(4) Uani 1 1 d . . .
O3 O 0.7736(3) 0.4800(2) 0.38032(19) 0.0224(4) Uani 1 1 d . . .
O4 O 0.2104(3) 0.0343(2) 0.37089(19) 0.0216(4) Uani 1 1 d . . .
O5 O 0.6863(3) 0.00311(19) 0.38604(18) 0.0206(4) Uani 1 1 d . . .
O6W O -0.0078(3) 0.2407(2) 0.6103(2) 0.0215(4) Uani 1 1 d D . .
O7 O 1.1036(4) 0.6556(4) 0.8534(2) 0.0510(7) Uani 1 1 d . . .
N N 0.5669(6) 0.5532(6) 0.9014(4) 0.0675(12) Uani 1 1 d . B .
H0A H 0.4155 0.5864 0.879 0.081 Uiso 1 1 calc R . .
H0B H 0.6822 0.5714 0.8517 0.081 Uiso 1 1 calc R . .
C1 C 0.6511(7) 0.6465(7) 1.0467(5) 0.0641(13) Uani 1 1 d . . .
H1 H 0.8189 0.6127 1.0696 0.077 Uiso 1 1 calc R A 1
C2 C 0.5384(7) 0.3832(7) 0.8672(5) 0.0629(12) Uani 1 1 d . . .
H2A H 0.7032 0.3441 0.884 0.075 Uiso 1 1 calc R B .
H2B H 0.4765 0.3284 0.7722 0.075 Uiso 1 1 calc R . .
C3 C 0.6770(18) 0.7963(11) 1.0648(9) 0.068(3) Uani 0.5 1 d P B 1
H3A H 0.759 0.8049 0.992 0.102 Uiso 0.5 1 calc PR B 1
H3B H 0.78 0.8542 1.1489 0.102 Uiso 0.5 1 calc PR B 1
H3C H 0.5108 0.8388 1.0665 0.102 Uiso 0.5 1 calc PR B 1
H1P H 1.069(5) 0.770(3) 0.718(3) 0.017(7) Uiso 1 1 d . . .
H6B H 0.115(4) 0.295(3) 0.600(4) 0.039(9) Uiso 1 1 d D . .
H6A H -0.143(3) 0.282(3) 0.596(3) 0.028(8) Uiso 1 1 d D . .
H2P H 0.473(5) 0.113(3) 0.2507(15) 0.02 Uiso 1 1 d 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 0 '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 0.006 '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'
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 V1 O3 180 2_666 .
O3 V1 O1 89.44(7) 2_666 .
O3 V1 O1 90.56(7) . .
O3 V1 O1 90.56(7) 2_666 2_666
O3 V1 O1 89.44(7) . 2_666
O1 V1 O1 180 . 2_666
O3 V1 O2 93.39(7) 2_666 2_666
O3 V1 O2 86.61(7) . 2_666
O1 V1 O2 92.48(7) . 2_666
O1 V1 O2 87.52(7) 2_666 2_666
O3 V1 O2 86.61(7) 2_666 .
O3 V1 O2 93.39(7) . .
O1 V1 O2 87.52(7) . .
O1 V1 O2 92.48(7) 2_666 .
O2 V1 O2 180 2_666 .
O5 V2 O5 180 2_656 1_455
O5 V2 O4 90.02(7) 2_656 .
O5 V2 O4 89.98(7) 1_455 .
O5 V2 O4 89.98(7) 2_656 2_556
O5 V2 O4 90.02(7) 1_455 2_556
O4 V2 O4 180 . 2_556
O5 V2 O6W 90.56(7) 2_656 2_556
O5 V2 O6W 89.44(7) 1_455 2_556
O4 V2 O6W 88.32(7) . 2_556
O4 V2 O6W 91.68(7) 2_556 2_556
O5 V2 O6W 89.44(7) 2_656 .
O5 V2 O6W 90.56(7) 1_455 .
O4 V2 O6W 91.68(7) . .
O4 V2 O6W 88.32(7) 2_556 .
O6W V2 O6W 180 2_556 .
O7 P1 O1 109.82(13) . .
O7 P1 O3 111.49(12) . 2_766
O1 P1 O3 111.57(10) . 2_766
O7 P1 H1P 98.8(13) . .
O1 P1 H1P 111.7(12) . .
O3 P1 H1P 112.8(13) 2_766 .
O4 P2 O5 112.01(10) . .
O4 P2 O2 113.28(10) . .
O5 P2 O2 111.19(10) . .
O4 P2 H2P 103.6(12) . .
O5 P2 H2P 105.5(12) . .
O2 P2 H2P 110.7(12) . .
P1 O1 V1 141.52(11) . .
P2 O2 V1 136.76(11) . .
P1 O3 V1 146.38(11) 2_766 .
P2 O4 V2 136.85(11) . .
P2 O5 V2 141.79(11) . 1_655
V2 O6W H6B 114(2) . .
V2 O6W H6A 116(2) . .
H6B O6W H6A 106(2) . .
C2 N C1 113.3(3) . .
C2 N H0A 108.9 . .
C1 N H0A 108.9 . .
C2 N H0B 108.9 . .
C1 N H0B 108.9 . .
H0A N H0B 107.7 . .
C3 C1 N 108.0(5) . .
C3 C1 C2 113.0(6) . 2_667
N C1 C2 110.1(4) . 2_667
C3 C1 H1 108.6 . .
N C1 H1 108.6 . .
C2 C1 H1 108.6 2_667 .
N C2 C1 108.8(4) . 2_667
N C2 H2A 109.9 . .
C1 C2 H2A 109.9 2_667 .
N C2 H2B 109.9 . .
C1 C2 H2B 109.9 2_667 .
H2A C2 H2B 108.3 . .
C1 C3 H3A 109.5 . .
C1 C3 H3B 109.5 . .
C1 C3 H3C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O3 1.9855(17) 2_666
V1 O3 1.9855(17) .
V1 O1 1.9939(18) .
V1 O1 1.9939(18) 2_666
V1 O2 2.0427(16) 2_666
V1 O2 2.0427(16) .
V2 O5 1.9646(17) 2_656
V2 O5 1.9646(17) 1_455
V2 O4 1.9720(17) .
V2 O4 1.9720(17) 2_556
V2 O6W 2.0745(17) 2_556
V2 O6W 2.0745(17) .
P1 O7 1.495(2) .
P1 O1 1.5245(17) .
P1 O3 1.5263(18) 2_766
P1 H1P 1.27(3) .
P2 O4 1.5138(17) .
P2 O5 1.5171(17) .
P2 O2 1.5238(18) .
P2 H2P 1.373(10) .
O3 P1 1.5263(18) 2_766
O5 V2 1.9646(17) 1_655
O6W H6B 0.844(10) .
O6W H6A 0.838(10) .
N C2 1.466(7) .
N C1 1.484(6) .
N H0A 0.9 .
N H0B 0.9 .
C1 C3 1.321(11) .
C1 C2 1.515(5) 2_667
C1 H1 0.98 .
C2 C1 1.515(5) 2_667
C2 H2A 0.97 .
C2 H2B 0.97 .
C3 H3A 0.96 .
C3 H3B 0.96 .
C3 H3C 0.96 .
