#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:22:40 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180136 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/33/7103387.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_7103387
loop_
_publ_author_name
'Berrocal, Teresa'
'Mesa, José L'
'Pizarro, José L'
'Bazán, Begoña'
'Iglesias, Marta'
'Aguayo, Andrés T'
'Arriortua, María I'
'Rojo, Teófilo'
_publ_section_title
;
 Microporous vanadyl-arsenate with the template incorporated exhibiting
 sorption and catalytic properties.
;
_journal_issue                   39
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4738
_journal_page_last               4740
_journal_paper_doi               10.1039/b807250g
_journal_year                    2008
_chemical_formula_sum            'C5 H23 As3 N2 O19 V3'
_chemical_formula_weight         792.83
_chemical_name_systematic
;
?
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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      2.3
_audit_creation_date             2008-06-05T09:51:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   19.0945(16)
_cell_length_b                   19.0945(16)
_cell_length_c                   11.0133(9)
_cell_measurement_reflns_used    1248
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      4.443
_cell_measurement_theta_min      45.562
_cell_volume                     3477.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'BRUKER SMART APEX CCD System'
_diffrn_measurement_method       'ω rotations with narrow frame'
_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  0.1566
_diffrn_reflns_av_unetI/netI     0.0973
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            30908
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         2.82
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.519
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2322
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.331
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.876
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.876
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0134P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0725
_reflns_number_gt                1673
_reflns_number_total             2367
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b807250g.txt
_cod_data_source_block           fjl25atci
_cod_database_code               7103387
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -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
V1 V 0.60527(6) 0.15124(5) 0.10030(8) 0.0074(2) Uani 1 1 d . . .
V2 V 0.50653(8) -0.02355(8) 0.2500 0.0083(3) Uani 1 2 d S . .
As1 As 0.41373(3) 0.01341(3) 0.01242(5) 0.00815(15) Uani 1 1 d . . .
As2 As 0.50366(5) 0.22713(5) 0.2500 0.0085(2) Uani 1 2 d S . .
O1 O 0.4939(2) 0.0447(2) 0.1105(3) 0.0088(9) Uani 1 1 d . . .
O2 O 0.3587(2) -0.0866(2) 0.0020(3) 0.0106(9) Uani 1 1 d . . .
O3 O 0.4435(2) 0.0589(2) -0.1240(3) 0.0091(9) Uiso 1 1 d . . .
O4 O 0.3532(2) 0.0455(2) 0.0754(3) 0.0153(9) Uani 1 1 d . . .
H2 H 0.3138 0.0323 0.0317 0.018 Uiso 1 1 calc R . .
O5 O 0.5758(3) 0.1984(3) 0.2500 0.0089(12) Uiso 1 2 d S . .
O6 O 0.4109(3) 0.1432(3) 0.2500 0.0100(13) Uani 1 2 d S . .
O7 O 0.7217(2) 0.2321(2) 0.1229(3) 0.0098(9) Uiso 1 1 d . . .
O8 O 0.5794(2) 0.1931(2) -0.0018(4) 0.0151(9) Uani 1 1 d . . .
O9 O 0.4139(3) -0.0936(3) 0.2500 0.0183(14) Uani 1 2 d S . .
O10 O 0.6154(3) 0.0877(3) 0.2500 0.0077(13) Uani 1 2 d S . .
H1 H 0.649(6) 0.074(6) 0.2500 0.050 Uiso 1 2 d S . .
O11A O 0.2138(8) 0.2157(9) 0.4081(12) 0.069(4) Uani 0.50 1 d P . .
O11B O 0.2429(10) 0.1936(8) 0.4786(13) 0.090(5) Uani 0.50 1 d P . .
O12 O 0.3264(4) 0.2345(4) 0.2500 0.0316(17) Uani 1 2 d S . .
C1 C 0.7342(5) 0.2656(6) 0.8129(7) 0.064(3) Uani 1 1 d . . .
H1A H 0.7621 0.3216 0.8391 0.077 Uiso 1 1 calc R . .
H1B H 0.6784 0.2422 0.8391 0.077 Uiso 1 1 calc R . .
C2 C 0.8053(5) 0.1866(6) 0.8192(6) 0.056(3) Uani 1 1 d . . .
H2A H 0.8576 0.2369 0.8202 0.067 Uiso 1 1 calc R . .
C3 C 0.8373(11) 0.1480(10) 0.8824(18) 0.071(6) Uani 0.50 1 d P . .
H1C H 0.8465 0.1667 0.9649 0.107 Uiso 0.50 1 calc PR . .
H1D H 0.8875 0.1593 0.8460 0.107 Uiso 0.50 1 calc PR . .
H1E H 0.8002 0.0908 0.8808 0.107 Uiso 0.50 1 calc PR . .
N1 N 0.7669(5) 0.2272(4) 0.8744(5) 0.062(2) Uani 1 1 d . . .
H1F H 0.7271 0.1902 0.9215 0.075 Uiso 1 1 calc R . .
H1G H 0.8038 0.2643 0.9252 0.075 Uiso 1 1 calc R . .
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
O8 V1 O7 101.84(17) . . ?
O8 V1 O2 101.34(17) . 7_655 ?
O7 V1 O2 87.38(14) . 7_655 ?
O8 V1 O1 96.11(16) . . ?
O7 V1 O1 161.74(15) . . ?
O2 V1 O1 85.81(14) 7_655 . ?
O8 V1 O5 97.09(18) . . ?
O7 V1 O5 90.24(17) . . ?
O2 V1 O5 161.52(15) 7_655 . ?
O1 V1 O5 90.87(17) . . ?
O8 V1 O10 168.2(2) . . ?
O7 V1 O10 87.74(18) . . ?
O2 V1 O10 85.88(15) 7_655 . ?
O1 V1 O10 74.89(17) . . ?
O5 V1 O10 75.71(15) . . ?
O9 V2 O3 103.59(18) . 4_655 ?
O9 V2 O3 103.59(18) . 7_655 ?
O3 V2 O3 88.8(2) 4_655 7_655 ?
O9 V2 O10 165.4(3) . . ?
O3 V2 O10 86.74(15) 4_655 . ?
O3 V2 O10 86.74(15) 7_655 . ?
O9 V2 O1 95.53(17) . 10_556 ?
O3 V2 O1 85.62(14) 4_655 10_556 ?
O3 V2 O1 160.84(15) 7_655 10_556 ?
O10 V2 O1 74.68(14) . 10_556 ?
O9 V2 O1 95.53(17) . . ?
O3 V2 O1 160.84(15) 4_655 . ?
O3 V2 O1 85.62(14) 7_655 . ?
O10 V2 O1 74.68(14) . . ?
O1 V2 O1 93.8(2) 10_556 . ?
O2 As1 O3 112.78(17) . . ?
O2 As1 O4 106.84(18) . . ?
O3 As1 O4 106.99(17) . . ?
O2 As1 O1 112.62(17) . . ?
O3 As1 O1 111.65(17) . . ?
O4 As1 O1 105.40(17) . . ?
O7 As2 O7 113.4(2) 8_666 5_665 ?
O7 As2 O6 106.90(15) 8_666 . ?
O7 As2 O6 106.90(15) 5_665 . ?
O7 As2 O5 110.25(15) 8_666 . ?
O7 As2 O5 110.25(15) 5_665 . ?
O6 As2 O5 108.9(2) . . ?
As1 O1 V1 127.05(19) . . ?
As1 O1 V2 126.97(19) . . ?
V1 O1 V2 105.44(15) . . ?
As1 O2 V1 121.77(19) . 7_655 ?
As1 O3 V2 122.95(19) . 7_655 ?
As1 O4 H2 109.5 . . ?
As2 O5 V1 124.76(13) . 10_556 ?
As2 O5 V1 124.76(13) . . ?
V1 O5 V1 104.4(2) 10_556 . ?
As2 O7 V1 129.8(2) 3_655 . ?
V2 O10 V1 104.63(17) . 10_556 ?
V2 O10 V1 104.63(17) . . ?
V1 O10 V1 102.6(2) 10_556 . ?
V2 O10 H1 102(7) . . ?
V1 O10 H1 120(3) 10_556 . ?
V1 O10 H1 120(3) . . ?
N1 C1 C1 119.9(4) . 10_557 ?
N1 C1 H1A 107.3 . . ?
C1 C1 H1A 107.3 10_557 . ?
N1 C1 H1B 107.3 . . ?
C1 C1 H1B 107.3 10_557 . ?
H1A C1 H1B 106.9 . . ?
C3 C2 N1 124.2(11) . . ?
C3 C2 C2 120.8(9) . 10_557 ?
N1 C2 C2 114.9(4) . 10_557 ?
C3 C2 H2A 90.7 . . ?
N1 C2 H2A 90.7 . . ?
C2 C2 H2A 90.7 10_557 . ?
C2 C3 H1C 109.5 . . ?
C2 C3 H1D 109.5 . . ?
H1C C3 H1D 109.5 . . ?
C2 C3 H1E 109.5 . . ?
H1C C3 H1E 109.5 . . ?
H1D C3 H1E 109.5 . . ?
C1 N1 C2 125.1(6) . . ?
C1 N1 H1F 106.0 . . ?
C2 N1 H1F 106.0 . . ?
C1 N1 H1G 106.0 . . ?
C2 N1 H1G 106.0 . . ?
H1F N1 H1G 106.3 . . ?
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
V1 O8 1.594(4) . ?
V1 O7 1.990(4) . ?
V1 O2 2.028(4) 7_655 ?
V1 O1 2.085(4) . ?
V1 O5 2.087(3) . ?
V1 O10 2.112(3) . ?
V2 O9 1.597(5) . ?
V2 O3 1.983(4) 4_655 ?
V2 O3 1.983(4) 7_655 ?
V2 O10 2.102(5) . ?
V2 O1 2.106(4) 10_556 ?
V2 O1 2.106(4) . ?
As1 O2 1.661(4) . ?
As1 O3 1.686(3) . ?
As1 O4 1.703(4) . ?
As1 O1 1.718(3) . ?
As2 O7 1.675(4) 8_666 ?
As2 O7 1.675(4) 5_665 ?
As2 O6 1.693(5) . ?
As2 O5 1.718(5) . ?
O2 V1 2.028(4) 7_655 ?
O3 V2 1.983(4) 7_655 ?
O4 H2 0.8200 . ?
O5 V1 2.087(3) 10_556 ?
O7 As2 1.675(4) 3_655 ?
O10 V1 2.112(3) 10_556 ?
O10 H1 0.80(9) . ?
O11A O11B 1.151(16) . ?
C1 N1 1.359(9) . ?
C1 C1 1.385(15) 10_557 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.359(17) . ?
C2 N1 1.442(9) . ?
C2 C2 1.524(14) 10_557 ?
C2 H2A 0.9800 . ?
C3 H1C 0.9600 . ?
C3 H1D 0.9600 . ?
C3 H1E 0.9600 . ?
N1 H1F 0.9000 . ?
N1 H1G 0.9000 . ?
