#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/64/4326449.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_4326449
loop_
_publ_author_name
'Diego Solis-Ibarra'
'Jared S. Silvia'
'Vojtech Jancik'
'Christopher C. Cummins'
_publ_contact_author_name        'Christopher C. Cummins'
_publ_section_title
;
 Facile Synthesis of Zero-, One-, and Two-Dimensional Vanadyl
 Pyrophosphates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9980
_journal_page_last               9984
_journal_paper_doi               10.1021/ic200510y
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'H19 Li8 O41.5 P8 V4'
_chemical_formula_weight         1191.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 130.0070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.3531(4)
_cell_length_b                   14.0324(3)
_cell_length_c                   11.9795(3)
_cell_measurement_reflns_used    2764
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.72
_cell_measurement_theta_min      4.45
_cell_volume                     2363.14(10)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.9.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2212
_diffrn_reflns_theta_full        67.60
_diffrn_reflns_theta_max         67.60
_diffrn_reflns_theta_min         4.45
_exptl_absorpt_coefficient_mu    9.963
_exptl_absorpt_correction_T_max  0.2406
_exptl_absorpt_correction_T_min  0.1897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1174
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         1.144
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2212
_refine_ls_number_restraints     229
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0791P)²+31.1502P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.1802
_reflns_number_gt                2038
_reflns_number_total             2212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200510y_si_001_2.cif
_cod_data_source_block           d8_10077
_cod_original_cell_volume        2363.14(9)
_cod_original_formula_sum        'H19 Li8 O41.50 P8 V4'
_cod_database_code               4326449
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
P1 P 0.18007(9) 0.89933(9) 0.69166(14) 0.0206(3) Uani 1 1 d U . .
P2 P 0.49577(9) 0.89942(9) 0.71283(13) 0.0187(3) Uani 1 1 d U . .
V1 V 0.31530(15) 1.0000 1.0055(2) 0.0207(5) Uani 0.7489(19) 2 d SPDU . 1
V2 V 0.31079(17) 1.0000 0.6351(3) 0.0242(5) Uani 0.7489(19) 2 d SPDU . 1
O1 O 0.2662(14) 1.0000 1.073(2) 0.029(2) Uani 0.7489(19) 2 d SPDU . 1
O9 O 0.2543(11) 1.0000 0.4685(11) 0.036(2) Uani 0.7489(19) 2 d SPDU . 1
O4 O 0.394(2) 1.0000 0.899(2) 0.029(4) Uani 0.2489(19) 1 d PDU A 1
H4A H 0.4360(12) 1.0000 0.8918(15) 0.044 Uiso 0.2489(19) 1 d PD A 1
H4B H 0.410(8) 1.0000 0.982(6) 0.044 Uiso 0.2489(19) 1 d PD A 1
V1A V 0.3417(5) 1.0000 0.9868(7) 0.0183(12) Uani 0.2511(19) 2 d SPDU . 2
O1A O 0.391(3) 1.0000 0.919(5) 0.022(3) Uani 0.2511(19) 2 d SPDU . 2
V2A V 0.3383(4) 1.0000 0.7060(7) 0.0170(11) Uani 0.2511(19) 2 d SPDU . 2
O9A O 0.387(3) 1.0000 0.870(2) 0.023(3) Uani 0.2511(19) 2 d SPDU . 2
O4A O 0.245(5) 1.0000 1.061(9) 0.036(9) Uani 0.2511(19) 2 d SPDU . 2
H4C H 0.225(11) 1.0000 0.975(9) 0.053 Uiso 0.2511(19) 2 d SPD . 2
H4D H 0.304(5) 1.0000 1.128(10) 0.053 Uiso 0.2511(19) 2 d SPD . 2
O4B O 0.258(4) 1.0000 0.445(3) 0.045(5) Uani 0.2511(19) 2 d SPDU . 2
H4E H 0.312(12) 1.0000 0.527(19) 0.068 Uiso 0.2511(19) 2 d SPD . 2
H4F H 0.211(17) 1.0000 0.44(4) 0.068 Uiso 0.2511(19) 2 d SPD . 2
O5 O 0.2422(2) 0.8981(2) 0.8570(4) 0.0222(7) Uani 1 1 d U . .
O2 O 0.4090(3) 0.8981(3) 0.7027(5) 0.0310(8) Uani 1 1 d U . .
O3 O 0.5867(3) 0.8988(3) 0.8724(4) 0.0315(9) Uani 1 1 d U . .
O7 O 0.1261(3) 1.0000 0.6374(5) 0.0235(10) Uani 1 2 d SU . .
O6 O 0.1048(3) 0.8245(3) 0.6170(4) 0.0285(8) Uani 1 1 d U . .
O11 O 0.4947(4) 1.0000 0.6471(5) 0.0206(10) Uani 1 2 d SU . .
O10 O 0.2406(3) 0.8976(3) 0.6452(4) 0.0246(8) Uani 1 1 d U . .
O8 O 0.4943(3) 0.8247(3) 0.6240(4) 0.0292(8) Uani 1 1 d U . .
O12 O 0.1972(5) 0.6135(5) 0.6918(7) 0.0694(17) Uani 1 1 d DU . .
H12A H 0.224(7) 0.659(6) 0.685(12) 0.104 Uiso 1 1 d D . .
H12B H 0.230(5) 0.5748(7) 0.760(3) 0.104 Uiso 1 1 d D . .
O13 O 0.4661(7) 0.6037(5) 0.6992(9) 0.086(2) Uani 1 1 d DU . .
H13A H 0.431(9) 0.652(6) 0.677(13) 0.129 Uiso 1 1 d D . .
H13B H 0.483(8) 0.5748(7) 0.776(5) 0.129 Uiso 1 1 d D . .
Li1 Li 0.4923(10) 0.6860(8) 0.6036(17) 0.052(3) Uani 1 1 d U . .
Li2 Li 0.0894(10) 0.6832(9) 0.5882(16) 0.058(3) Uani 1 1 d U . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li Li 0.0008 0.0003 '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'
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
O6 P1 O5 113.8(2) . .
O6 P1 O10 112.4(2) . .
O5 P1 O10 111.2(2) . .
O6 P1 O7 106.5(2) . .
O5 P1 O7 106.7(2) . .
O10 P1 O7 105.7(2) . .
O5 P1 Li1 147.5(3) . 7_566
O10 P1 Li1 91.5(3) . 7_566
O7 P1 Li1 88.1(3) . 7_566
O8 P2 O2 113.6(2) . .
O8 P2 O3 113.3(2) . .
O2 P2 O3 110.2(2) . .
O8 P2 O11 106.2(2) . .
O2 P2 O11 106.8(2) . .
O3 P2 O11 106.1(2) . .
O2 P2 Li2 100.6(3) . 7_566
O3 P2 Li2 141.6(3) . 7_566
O11 P2 Li2 85.4(3) . 7_566
O1 V1 O5 100.6(6) . .
O1 V1 O5 100.6(6) . 6_575
O5 V1 O5 92.2(2) . 6_575
O1 V1 O3 99.7(6) . 5_677
O5 V1 O3 159.7(2) . 5_677
O5 V1 O3 85.18(15) 6_575 5_677
O1 V1 O3 99.7(6) . 2_657
O5 V1 O3 85.17(15) . 2_657
O5 V1 O3 159.7(2) 6_575 2_657
O3 V1 O3 90.4(2) 5_677 2_657
O1 V1 O4 179.8(11) . .
O5 V1 O4 79.5(4) . .
O5 V1 O4 79.5(4) 6_575 .
O3 V1 O4 80.2(5) 5_677 .
O3 V1 O4 80.2(5) 2_657 .
O9 V2 O10 99.0(4) . 6_575
O9 V2 O10 99.0(4) . .
O10 V2 O10 92.8(2) 6_575 .
O9 V2 O2 101.7(4) . .
O10 V2 O2 159.4(2) 6_575 .
O10 V2 O2 84.85(15) . .
O9 V2 O2 101.7(4) . 6_575
O10 V2 O2 84.85(15) 6_575 6_575
O10 V2 O2 159.4(2) . 6_575
O2 V2 O2 90.2(2) . 6_575
O1A V1A O3 99.0(13) . 5_677
O1A V1A O3 99.0(13) . 2_657
O3 V1A O3 94.5(3) 5_677 2_657
O1A V1A O5 98.0(13) . .
O3 V1A O5 162.7(4) 5_677 .
O3 V1A O5 85.60(17) 2_657 .
O1A V1A O5 98.0(13) . 6_575
O3 V1A O5 85.60(16) 5_677 6_575
O3 V1A O5 162.7(4) 2_657 6_575
O5 V1A O5 89.2(3) . 6_575
O1A V1A O9A 8(2) . .
O3 V1A O9A 104.4(7) 5_677 .
O3 V1A O9A 104.4(7) 2_657 .
O5 V1A O9A 92.2(7) . .
O5 V1A O9A 92.2(7) 6_575 .
O1A V1A O4A 173(3) . .
O3 V1A O4A 85.9(13) 5_677 .
O3 V1A O4A 85.9(14) 2_657 .
O5 V1A O4A 76.9(14) . .
O5 V1A O4A 76.9(14) 6_575 .
O9A V1A O4A 165(2) . .
O9A O1A V1A 148(7) . .
V1A O1A V2A 132(3) . .
O9A V2A O2 100.0(10) . .
O9A V2A O2 100.0(10) . 6_575
O2 V2A O2 94.4(3) . 6_575
O9A V2A O10 96.6(11) . 6_575
O2 V2A O10 163.2(4) . 6_575
O2 V2A O10 85.41(16) 6_575 6_575
O9A V2A O10 96.6(11) . .
O2 V2A O10 85.41(16) . .
O2 V2A O10 163.2(4) 6_575 .
O10 V2A O10 89.9(3) 6_575 .
O9A V2A O1A 5.4(16) . .
O2 V2A O1A 103.5(7) . .
O2 V2A O1A 103.5(7) 6_575 .
O10 V2A O1A 92.8(7) 6_575 .
O10 V2A O1A 92.8(7) . .
O9A V2A O4B 179(2) . .
O2 V2A O4B 80.7(10) . .
O2 V2A O4B 80.7(10) 6_575 .
O10 V2A O4B 82.7(10) 6_575 .
O10 V2A O4B 82.7(10) . .
O1A V2A O4B 173.6(18) . .
O1A O9A V2A 159(7) . .
V2A O9A V1A 135(2) . .
P1 O5 V1 131.8(2) . .
P1 O5 V1A 122.7(3) . .
P2 O2 V2A 131.9(3) . .
P2 O2 V2 130.1(2) . .
P2 O3 V1A 132.1(3) . 5_677
P2 O3 V1 130.9(2) . 5_677
P1 O7 P1 123.5(3) . 6_575
P1 O6 Li1 128.3(4) . 8_465
P1 O6 Li2 140.8(5) . .
Li1 O6 Li2 83.6(6) 8_465 .
P1 O6 Li1 122.1(4) . 7_566
Li1 O6 Li1 83.8(6) 8_465 7_566
Li2 O6 Li1 78.2(5) . 7_566
P2 O11 P2 122.4(3) . 6_575
P1 O10 V2 131.5(2) . .
P1 O10 V2A 122.6(3) . .
P2 O8 Li2 127.6(4) . 7_566
P2 O8 Li1 141.5(5) . .
Li2 O8 Li1 81.1(6) 7_566 .
P2 O8 Li2 124.3(5) . 8_565
Li2 O8 Li2 77.8(7) 7_566 8_565
Li1 O8 Li2 82.6(5) . 8_565
O13 Li1 O8 121.6(7) . .
O13 Li1 O6 124.4(7) . 8_565
O8 Li1 O6 97.4(5) . 8_565
O13 Li1 O6 113.0(7) . 7_566
O8 Li1 O6 99.5(6) . 7_566
O6 Li1 O6 95.6(6) 8_565 7_566
O13 Li1 Li2 139.1(7) . 7_566
O8 Li1 Li2 49.3(4) . 7_566
O6 Li1 Li2 96.1(6) 8_565 7_566
O6 Li1 Li2 50.4(4) 7_566 7_566
O13 Li1 Li2 155.5(9) . 8_565
O8 Li1 Li2 50.2(4) . 8_565
O6 Li1 Li2 48.7(4) 8_565 8_565
O6 Li1 Li2 91.5(6) 7_566 8_565
Li2 Li1 Li2 57.9(6) 7_566 8_565
O13 Li1 Li1 141.4(5) . 2_656
O8 Li1 Li1 96.3(4) . 2_656
O6 Li1 Li1 49.0(4) 8_565 2_656
O6 Li1 Li1 47.2(5) 7_566 2_656
Li2 Li1 Li1 60.9(5) 7_566 2_656
Li2 Li1 Li1 57.1(5) 8_565 2_656
O13 Li1 P1 89.2(5) . 7_566
O8 Li1 P1 116.8(6) . 7_566
O6 Li1 P1 108.2(5) 8_565 7_566
O6 Li1 P1 24.1(2) 7_566 7_566
Li2 Li1 P1 70.8(5) 7_566 7_566
Li2 Li1 P1 115.3(6) 8_565 7_566
Li1 Li1 P1 65.1(5) 2_656 7_566
O12 Li2 O8 117.6(7) . 7_566
O12 Li2 O6 116.6(7) . .
O8 Li2 O6 100.8(7) 7_566 .
O12 Li2 O8 122.0(8) . 8_465
O8 Li2 O8 101.9(6) 7_566 8_465
O6 Li2 O8 93.6(6) . 8_465
O12 Li2 Li2 147.1(5) . 2_556
O8 Li2 Li2 52.9(5) 7_566 2_556
O6 Li2 Li2 96.2(4) . 2_556
O8 Li2 Li2 49.4(5) 8_465 2_556
O12 Li2 Li1 139.7(8) . 7_566
O8 Li2 Li1 49.6(5) 7_566 7_566
O6 Li2 Li1 51.4(4) . 7_566
O8 Li2 Li1 98.1(6) 8_465 7_566
Li2 Li2 Li1 63.1(5) 2_556 7_566
O12 Li2 Li1 144.8(8) . 8_465
O8 Li2 Li1 97.4(6) 7_566 8_465
O6 Li2 Li1 47.7(4) . 8_465
O8 Li2 Li1 47.2(4) 8_465 8_465
Li2 Li2 Li1 59.0(5) 2_556 8_465
Li1 Li2 Li1 62.0(6) 7_566 8_465
O12 Li2 P2 96.2(5) . 7_566
O8 Li2 P2 22.3(2) 7_566 7_566
O6 Li2 P2 118.9(6) . 7_566
O8 Li2 P2 111.3(5) 8_465 7_566
Li2 Li2 P2 67.1(6) 2_556 7_566
Li1 Li2 P2 69.8(5) 7_566 7_566
Li1 Li2 P2 118.9(6) 8_465 7_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 O6 1.490(4) .
P1 O5 1.523(4) .
P1 O10 1.530(4) .
P1 O7 1.603(3) .
P1 Li1 3.093(14) 7_566
P2 O8 1.482(4) .
P2 O2 1.517(4) .
P2 O3 1.529(4) .
P2 O11 1.611(2) .
P2 Li2 3.089(14) 7_566
V1 O1 1.553(9) .
V1 O5 1.984(4) .
V1 O5 1.984(4) 6_575
V1 O3 2.002(4) 5_677
V1 O3 2.002(4) 2_657
V1 O4 2.463(15) .
V2 O9 1.549(9) .
V2 O10 1.984(4) 6_575
V2 O10 1.984(4) .
V2 O2 2.019(4) .
V2 O2 2.019(4) 6_575
V1A O1A 1.563(16) .
V1A O3 1.934(6) 5_677
V1A O3 1.934(6) 2_657
V1A O5 2.035(6) .
V1A O5 2.035(6) 6_575
V1A O9A 2.04(3) .
V1A O4A 2.443(19) .
O1A O9A 0.54(4) .
O1A V2A 2.06(4) .
V2A O9A 1.548(17) .
V2A O2 1.948(5) .
V2A O2 1.948(5) 6_575
V2A O10 2.032(5) 6_575
V2A O10 2.032(5) .
V2A O4B 2.456(19) .
O3 V1A 1.934(6) 5_677
O3 V1 2.002(4) 5_677
O7 P1 1.603(3) 6_575
O6 Li1 1.972(12) 8_465
O6 Li2 2.002(13) .
O6 Li1 2.031(16) 7_566
O11 P2 1.611(2) 6_575
O8 Li2 1.952(15) 7_566
O8 Li1 1.960(11) .
O8 Li2 2.051(16) 8_565
O12 Li2 1.803(15) .
O13 Li1 1.892(14) .
Li1 O6 1.972(12) 8_565
Li1 O6 2.031(16) 7_566
Li1 Li2 2.543(19) 7_566
Li1 Li2 2.648(17) 8_565
Li1 Li1 2.67(3) 2_656
Li1 P1 3.092(14) 7_566
Li2 O8 1.952(15) 7_566
Li2 O8 2.051(15) 8_465
Li2 Li2 2.51(3) 2_556
Li2 Li1 2.543(19) 7_566
Li2 Li1 2.648(17) 8_465
Li2 P2 3.089(14) 7_566
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 276 101 ' '
2 0.500 0.500 0.000 267 96 ' '
3 0.250 0.250 0.500 18 8 ' '
4 0.750 0.250 0.500 18 8 ' '
5 0.750 0.750 0.500 18 8 ' '
6 0.250 0.750 0.500 18 8 ' '
