#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:40:30 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301839 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/05/4330517.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_4330517
loop_
_publ_author_name
'Nadia Marino'
'Susan K. Hanson'
'Peter Müller'
'Robert P. Doyle'
_publ_section_title
;
 Pyro without Fire: Synthesis, Structure, and Reactivity of a Dimeric
 Vanadyl Pyrophosphate Coordination Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10077
_journal_page_last               10079
_journal_paper_doi               10.1021/ic3015767
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C20 H20 N4 O11 P2 V2, 3(H2 O)'
_chemical_formula_sum            'C20 H26 N4 O14 P2 V2'
_chemical_formula_weight         710.27
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 102.586(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0648(6)
_cell_length_b                   12.3888(7)
_cell_length_c                   20.0121(11)
_cell_measurement_reflns_used    5197
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      67.12
_cell_measurement_theta_min      4.53
_cell_volume                     2677.3(3)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2011)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2011)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2011)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL(Bruker,2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8048
_diffrn_reflns_theta_full        65.07
_diffrn_reflns_theta_max         65.07
_diffrn_reflns_theta_min         4.53
_exptl_absorpt_coefficient_mu    7.698
_exptl_absorpt_correction_T_max  0.9270
_exptl_absorpt_correction_T_min  0.6995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2287
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0310
_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)+(0.0531P)²+5.3451P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0871
_reflns_number_gt                2156
_reflns_number_total             2287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3015767_si_002_1.cif
_cod_data_source_block           vpo22
_cod_database_code               4330517
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
V1 V 0.81927(4) 0.56904(3) 0.673014(19) 0.01604(14) Uani 1 1 d .
O1 O 0.89117(15) 0.45541(14) 0.68233(8) 0.0217(4) Uani 1 1 d .
P1 P 0.94237(5) 0.71496(4) 0.80612(3) 0.01468(16) Uani 1 1 d .
O2 O 0.85170(14) 0.63362(13) 0.76495(8) 0.0178(4) Uani 1 1 d .
O3 O 1.05035(14) 0.65935(13) 0.85386(8) 0.0174(4) Uani 1 1 d .
O4 O 0.87925(15) 0.79674(13) 0.84143(8) 0.0205(4) Uani 1 1 d .
O5 O 1.0000 0.77991(17) 0.7500 0.0167(5) Uani 1 2 d S
C1 C 0.6894(2) 0.8037(2) 0.67034(12) 0.0211(5) Uani 1 1 d .
H1 H 0.7245 0.8024 0.7181 0.025 Uiso 1 1 calc R
C2 C 0.6323(2) 0.8974(2) 0.64214(13) 0.0240(5) Uani 1 1 d .
H2 H 0.6286 0.9593 0.6696 0.029 Uiso 1 1 calc R
C3 C 0.5809(2) 0.8984(2) 0.57277(14) 0.0278(6) Uani 1 1 d .
H3 H 0.5410 0.9616 0.5519 0.033 Uiso 1 1 calc R
C4 C 0.5873(2) 0.8072(2) 0.53367(13) 0.0256(6) Uani 1 1 d .
H4 H 0.5518 0.8067 0.4860 0.031 Uiso 1 1 calc R
C5 C 0.6473(2) 0.7162(2) 0.56597(12) 0.0195(5) Uani 1 1 d .
C6 C 0.6621(2) 0.6146(2) 0.52988(12) 0.0201(5) Uani 1 1 d .
C7 C 0.6009(2) 0.5950(2) 0.46235(13) 0.0278(6) Uani 1 1 d .
H7 H 0.5484 0.6482 0.4369 0.033 Uiso 1 1 calc R
C8 C 0.6179(2) 0.4970(2) 0.43314(13) 0.0316(6) Uani 1 1 d .
H8 H 0.5773 0.4821 0.3872 0.038 Uiso 1 1 calc R
C9 C 0.6941(3) 0.4207(2) 0.47107(14) 0.0299(6) Uani 1 1 d .
H9 H 0.7067 0.3527 0.4517 0.036 Uiso 1 1 calc R
C10 C 0.7517(2) 0.4451(2) 0.53761(13) 0.0244(5) Uani 1 1 d .
H10 H 0.8038 0.3922 0.5637 0.029 Uiso 1 1 calc R
N1 N 0.69765(17) 0.71473(16) 0.63381(10) 0.0179(4) Uani 1 1 d .
N2 N 0.73736(18) 0.54008(16) 0.56712(10) 0.0188(4) Uani 1 1 d .
O1W O 0.66134(15) 0.50365(14) 0.69238(9) 0.0222(4) Uani 1 1 d D
H1W H 0.611(2) 0.5321(19) 0.7121(15) 0.033 Uiso 1 1 d D
H2W H 0.641(3) 0.4397(10) 0.6847(16) 0.033 Uiso 1 1 d D
O2W O 0.86538(17) 0.23798(15) 0.65843(10) 0.0280(4) Uani 1 1 d D
H3W H 0.889(2) 0.3025(11) 0.6644(17) 0.042 Uiso 1 1 d D
H4W H 0.7893(11) 0.242(2) 0.6590(17) 0.042 Uiso 1 1 d D
O3W O 1.0000 0.1053(2) 0.7500 0.0286(6) Uani 1 2 d SD
H5W H 0.955(2) 0.1463(13) 0.7215(10) 0.043 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 '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
O1 V1 O2 105.24(8) . .
O1 V1 O3 98.86(8) . 2_756
O2 V1 O3 91.66(6) . 2_756
O1 V1 O1W 93.04(8) . .
O2 V1 O1W 88.46(7) . .
O3 V1 O1W 167.63(7) 2_756 .
O1 V1 N2 93.44(8) . .
O2 V1 N2 160.71(7) . .
O3 V1 N2 90.12(7) 2_756 .
O1W V1 N2 85.77(7) . .
O1 V1 N1 166.10(8) . .
O2 V1 N1 88.49(7) . .
O3 V1 N1 82.56(7) 2_756 .
O1W V1 N1 85.07(7) . .
N2 V1 N1 72.70(7) . .
O4 P1 O3 113.22(9) . .
O4 P1 O2 112.48(9) . .
O3 P1 O2 111.89(9) . .
O4 P1 O5 106.63(10) . .
O3 P1 O5 106.62(7) . .
O2 P1 O5 105.34(8) . .
P1 O2 V1 137.43(10) . .
P1 O3 V1 126.93(9) . 2_756
P1 O5 P1 120.47(14) . 2_756
N1 C1 C2 123.3(2) . .
N1 C1 H1 118.4 . .
C2 C1 H1 118.4 . .
C3 C2 C1 118.0(2) . .
C3 C2 H2 121.0 . .
C1 C2 H2 121.0 . .
C2 C3 C4 120.0(2) . .
C2 C3 H3 120.0 . .
C4 C3 H3 120.0 . .
C3 C4 C5 118.4(2) . .
C3 C4 H4 120.8 . .
C5 C4 H4 120.8 . .
N1 C5 C4 121.9(2) . .
N1 C5 C6 114.5(2) . .
C4 C5 C6 123.7(2) . .
N2 C6 C7 121.7(2) . .
N2 C6 C5 115.6(2) . .
C7 C6 C5 122.7(2) . .
C8 C7 C6 118.9(3) . .
C8 C7 H7 120.6 . .
C6 C7 H7 120.6 . .
C7 C8 C9 119.6(2) . .
C7 C8 H8 120.2 . .
C9 C8 H8 120.2 . .
C10 C9 C8 118.7(3) . .
C10 C9 H9 120.6 . .
C8 C9 H9 120.6 . .
N2 C10 C9 122.9(2) . .
N2 C10 H10 118.6 . .
C9 C10 H10 118.6 . .
C1 N1 C5 118.4(2) . .
C1 N1 V1 124.66(16) . .
C5 N1 V1 116.04(15) . .
C10 N2 C6 118.3(2) . .
C10 N2 V1 121.09(17) . .
C6 N2 V1 120.44(16) . .
V1 O1W H1W 127.8(18) . .
V1 O1W H2W 123.7(18) . .
H1W O1W H2W 108.2(16) . .
H3W O2W H4W 103.3(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O1 1.6077(17) .
V1 O2 1.9662(16) .
V1 O3 1.9902(16) 2_756
V1 O1W 2.0384(17) .
V1 N2 2.1457(19) .
V1 N1 2.286(2) .
P1 O4 1.4929(17) .
P1 O3 1.5223(16) .
P1 O2 1.5299(16) .
P1 O5 1.6211(12) .
O3 V1 1.9902(16) 2_756
O5 P1 1.6211(12) 2_756
C1 N1 1.336(3) .
C1 C2 1.382(4) .
C1 H1 0.9500 .
C2 C3 1.381(4) .
C2 H2 0.9500 .
C3 C4 1.385(4) .
C3 H3 0.9500 .
C4 C5 1.394(3) .
C4 H4 0.9500 .
C5 N1 1.351(3) .
C5 C6 1.478(3) .
C6 N2 1.353(3) .
C6 C7 1.395(4) .
C7 C8 1.377(4) .
C7 H7 0.9500 .
C8 C9 1.379(4) .
C8 H8 0.9500 .
C9 C10 1.378(4) .
C9 H9 0.9500 .
C10 N2 1.342(3) .
C10 H10 0.9500 .
O1W H1W 0.824(10) .
O1W H2W 0.830(10) .
O2W H3W 0.841(10) .
O2W H4W 0.846(10) .
O3W H5W 0.839(9) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W O3W 0.824(10) 1.824(10) 2.646(2) 175(3) 3_455
O1W H2W O4 0.830(10) 1.846(10) 2.664(2) 169(3) 4_646
O2W H3W O1 0.841(10) 1.928(14) 2.740(2) 162(3) .
O2W H4W O4 0.846(10) 1.984(14) 2.804(2) 163(3) 4_646
O3W H5W O2W 0.839(9) 1.825(10) 2.663(2) 177(3) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168337800
