#------------------------------------------------------------------------------
#$Date: 2016-01-09 12:24:32 +0200 (Sat, 09 Jan 2016) $
#$Revision: 173743 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/16/7221631.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_7221631
loop_
_publ_author_name
'Martín-Caballero, Jagoba'
'Wéry, Ana San José'
'Artetxe, Beñat'
'Reinoso, Santiago'
'Felices, Leire San'
'Vilas, José Luis'
'Gutiérrez-Zorrilla, Juan M.'
_publ_section_title
;
 Sequential single-crystal-to-single-crystal transformations promoted by
 gradual thermal dehydration in a porous metavanadate hybrid
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              8915
_journal_paper_doi               10.1039/C5CE01076D
_journal_volume                  17
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C10 H26.67 Cu N4 O7.33 V2'
_chemical_formula_sum            'C10 H26.67 Cu N4 O7.33 V2'
_chemical_formula_weight         485.77
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_update_record
;
2015-07-14 deposited with the CCDC.
2015-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                103.208(14)
_cell_angle_beta                 106.557(12)
_cell_angle_gamma                95.595(11)
_cell_formula_units_Z            3
_cell_length_a                   8.6253(10)
_cell_length_b                   12.890(2)
_cell_length_c                   13.368(2)
_cell_measurement_reflns_used    1438
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.88
_cell_measurement_theta_min      2.479
_cell_volume                     1365.7(4)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'OLEX2 (Dolomanov, 2009)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2439
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0429004
_diffrn_orient_matrix_UB_12      -0.0004858
_diffrn_orient_matrix_UB_13      0.0536807
_diffrn_orient_matrix_UB_21      -0.0481645
_diffrn_orient_matrix_UB_22      -0.0508663
_diffrn_orient_matrix_UB_23      -0.0080755
_diffrn_orient_matrix_UB_31      0.0585697
_diffrn_orient_matrix_UB_32      -0.0265949
_diffrn_orient_matrix_UB_33      -0.0188539
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.1383
_diffrn_reflns_laue_measured_fraction_full 0.995
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8860
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    2.203
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
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)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             745
_exptl_crystal_size_max          0.2659
_exptl_crystal_size_mid          0.0649
_exptl_crystal_size_min          0.0371
_refine_diff_density_max         1.334
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.15
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.0886
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0366P)²+9.9777P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1621
_refine_ls_wR_factor_ref         0.1828
_reflns_number_gt                3280
_reflns_number_total             4794
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce01076d2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7221629--7221632.cif.'
_cod_database_code               7221631
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_calc_flag
V1 V 0.03494(19) 0.27302(13) 0.65599(13) 0.0217(4) Uani 1 d
V2 V 0.44851(19) 0.34661(13) 0.70848(14) 0.0213(4) Uani 1 d
V3 V 0.76858(19) 0.19969(13) 0.79161(14) 0.0234(4) Uani 1 d
Cu1A Cu 0.5 0.5 1 0.0275(5) Uani 1 d
Cu1B Cu 0 0 0.5 0.0230(4) Uani 1 d
Cu1C Cu 0.5 0.5 0.5 0.0277(5) Uani 1 d
O1 O -0.0008(8) 0.3955(5) 0.6651(6) 0.0338(18) Uani 1 d
O2 O 0.4990(8) 0.4655(6) 0.7972(6) 0.0360(19) Uani 1 d
O3 O 0.8467(8) 0.2510(6) 0.9221(6) 0.0376(19) Uani 1 d
O12 O 0.2569(7) 0.2765(5) 0.7117(5) 0.0229(15) Uani 1 d
O23 O 0.6010(8) 0.2664(6) 0.7409(7) 0.046(2) Uani 1 d
O13 O -0.0692(8) 0.2081(6) 0.7311(6) 0.0358(19) Uani 1 d
O1M O -0.0316(8) 0.2013(6) 0.5299(5) 0.0331(18) Uani 1 d
O2M O 0.4317(8) 0.3639(6) 0.5888(5) 0.0304(17) Uani 1 d
O3M O 0.6978(8) 0.0710(5) 0.7662(5) 0.0302(17) Uani 1 d
N1C N 0.2597(10) 0.5056(7) 0.4444(7) 0.028(2) Uani 1 d
H1C H 0.2497 0.5546 0.3974 0.034 Uiso 1 calc
N1B N 0.2297(9) 0.0371(6) 0.6073(6) 0.0234(19) Uani 1 d
H1B H 0.2446 0.1132 0.6471 0.028 Uiso 1 calc
N4C N 0.4984(9) 0.3907(7) 0.3627(7) 0.029(2) Uani 1 d
H4C H 0.5068 0.432 0.3107 0.035 Uiso 1 calc
N4B N 0.1058(9) 0.0238(6) 0.3899(6) 0.0211(18) Uani 1 d
H4B H 0.1158 -0.0478 0.3499 0.025 Uiso 1 calc
C3B C 0.2777(11) 0.0830(8) 0.4533(8) 0.025(2) Uani 1 d
H3BA H 0.3465 0.0772 0.4068 0.03 Uiso 1 calc
H3BB H 0.2769 0.159 0.4825 0.03 Uiso 1 calc
C2B C 0.3422(11) 0.0320(8) 0.5430(8) 0.022(2) Uani 1 d
H2BA H 0.3496 -0.0427 0.5135 0.026 Uiso 1 calc
H2BB H 0.451 0.0703 0.5883 0.026 Uiso 1 calc
C6C C 0.1967(13) 0.3533(9) 0.2829(8) 0.032(3) Uani 1 d
H6CA H 0.2106 0.4076 0.2451 0.038 Uiso 1 calc
H6CB H 0.1074 0.2964 0.2341 0.038 Uiso 1 calc
C5B C 0.0203(11) 0.0772(7) 0.3083(8) 0.021(2) Uani 1 d
H5BA H 0.082 0.0806 0.2584 0.025 Uiso 1 calc
H5BB H 0.016 0.1507 0.3444 0.025 Uiso 1 calc
C7B C 0.2706(12) -0.0239(8) 0.6896(8) 0.028(2) Uani 1 d
H7BA H 0.3812 0.0053 0.7384 0.034 Uiso 1 calc
H7BB H 0.2674 -0.0991 0.6541 0.034 Uiso 1 calc
C7C C 0.1492(11) 0.4031(8) 0.3783(9) 0.031(3) Uani 1 d
H7CA H 0.0378 0.4166 0.3542 0.037 Uiso 1 calc
H7CB H 0.1513 0.3529 0.4227 0.037 Uiso 1 calc
C5C C 0.3518(11) 0.3059(9) 0.3080(9) 0.031(3) Uani 1 d
H5CA H 0.3451 0.2585 0.3541 0.037 Uiso 1 calc
H5CB H 0.3618 0.2628 0.2412 0.037 Uiso 1 calc
C6B C -0.1512(11) 0.0176(8) 0.2459(8) 0.028(2) Uani 1 d
H6BA H -0.1464 -0.0579 0.2176 0.034 Uiso 1 calc
H6BB H -0.1938 0.0465 0.1845 0.034 Uiso 1 calc
C3C C 0.6521(12) 0.3475(8) 0.3915(9) 0.032(3) Uani 1 d
H3CA H 0.6764 0.3133 0.3264 0.038 Uiso 1 calc
H3CB H 0.6415 0.2937 0.4305 0.038 Uiso 1 calc
C2C C 0.2125(12) 0.5601(9) 0.5388(9) 0.031(3) Uani 1 d
H2CA H 0.1958 0.5094 0.5799 0.038 Uiso 1 calc
H2CB H 0.1108 0.5868 0.5144 0.038 Uiso 1 calc
N4A N 0.2922(9) 0.3907(7) 0.9446(7) 0.030(2) Uani 1 d
H4A H 0.276 0.3581 0.8678 0.036 Uiso 1 calc
N1A N 0.3538(9) 0.6102(7) 0.9766(7) 0.027(2) Uani 1 d
H1A H 0.3433 0.6445 1.0473 0.032 Uiso 1 calc
C5A C 0.2843(12) 0.3007(9) 0.9943(9) 0.036(3) Uani 1 d
H5AA H 0.1799 0.2524 0.9565 0.043 Uiso 1 calc
H5AB H 0.2887 0.3292 1.069 0.043 Uiso 1 calc
C3A C 0.1560(11) 0.4530(8) 0.9486(9) 0.031(3) Uani 1 d
H3AA H 0.1532 0.4762 1.0223 0.037 Uiso 1 calc
H3AB H 0.0512 0.4084 0.9034 0.037 Uiso 1 calc
C7A C 0.4100(12) 0.6984(9) 0.9346(8) 0.035(3) Uani 1 d
H7AA H 0.3297 0.7462 0.9275 0.042 Uiso 1 calc
H7AB H 0.4175 0.6678 0.8631 0.042 Uiso 1 calc
C2A C 0.1893(12) 0.5504(8) 0.9071(9) 0.034(3) Uani 1 d
H2AA H 0.1867 0.5273 0.8322 0.041 Uiso 1 calc
H2AB H 0.107 0.596 0.9114 0.041 Uiso 1 calc
C6A C 0.4234(12) 0.2363(8) 0.9917(9) 0.032(3) Uani 1 d
H6AA H 0.4016 0.1714 1.0141 0.038 Uiso 1 calc
H6AB H 0.4265 0.2142 0.918 0.038 Uiso 1 calc
O1W O -0.0534(10) 0.1364(6) 0.0703(6) 0.045(2) Uani 1 d
O2W O 0.2423(10) 0.0532(6) 0.0853(7) 0.048(2) Uani 1 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'
Cu Cu 0.3201 1.2651 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-12 6 2 0.1202
0 -7 -14 0.0127
12 0 -2 0.1326
-12 1 3 0.1175
0 12 9 0.0421
0 -12 16 0.0129
0 14 -15 0.0235
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 O1M 110.4(4) . .
O1 V1 O13 110.6(4) . .
O1M V1 O13 107.9(4) . .
O1 V1 O12 109.4(3) . .
O1M V1 O12 109.6(3) . .
O13 V1 O12 108.9(3) . .
O2M V2 O2 108.7(4) . .
O2M V2 O23 109.0(4) . .
O2 V2 O23 110.6(4) . .
O2M V2 O12 111.5(3) . .
O2 V2 O12 109.3(3) . .
O23 V2 O12 107.8(3) . .
O3 V3 O3M 109.1(4) . .
O3 V3 O23 108.8(4) . .
O3M V3 O23 108.7(3) . .
O3 V3 O13 108.9(3) . 1_655
O3M V3 O13 106.3(3) . 1_655
O23 V3 O13 114.9(4) . 1_655
N4A Cu1A N4A 180 . 2_667
N4A Cu1A N1A 86.0(3) . .
N4A Cu1A N1A 94.0(3) 2_667 .
N4A Cu1A N1A 94.0(3) . 2_667
N4A Cu1A N1A 86.0(3) 2_667 2_667
N1A Cu1A N1A 180 . 2_667
N4B Cu1B N4B 180 . 2_556
N4B Cu1B N1B 93.7(3) . 2_556
N4B Cu1B N1B 86.3(3) 2_556 2_556
N4B Cu1B N1B 86.3(3) . .
N4B Cu1B N1B 93.7(3) 2_556 .
N1B Cu1B N1B 180 2_556 .
N1C Cu1C N1C 180 . 2_666
N1C Cu1C N4C 85.9(3) . 2_666
N1C Cu1C N4C 94.1(3) 2_666 2_666
N1C Cu1C N4C 94.1(3) . .
N1C Cu1C N4C 85.9(3) 2_666 .
N4C Cu1C N4C 180 2_666 .
V2 O12 V1 138.7(4) . .
V2 O23 V3 171.9(6) . .
V1 O13 V3 149.6(5) . 1_455
C7C N1C C2C 113.7(8) . .
C7C N1C Cu1C 116.9(6) . .
C2C N1C Cu1C 106.8(6) . .
C2B N1B C7B 112.6(7) . .
C2B N1B Cu1B 106.3(6) . .
C7B N1B Cu1B 118.1(6) . .
C5C N4C C3C 113.3(8) . .
C5C N4C Cu1C 117.1(6) . .
C3C N4C Cu1C 106.0(6) . .
C5B N4B C3B 112.2(7) . .
C5B N4B Cu1B 117.9(6) . .
C3B N4B Cu1B 105.9(6) . .
C2B C3B N4B 107.3(8) . .
N1B C2B C3B 108.4(8) . .
C7C C6C C5C 114.9(9) . .
N4B C5B C6B 111.7(8) . .
N1B C7B C6B 111.2(8) . 2_556
N1C C7C C6C 112.1(8) . .
N4C C5C C6C 111.7(9) . .
C5B C6B C7B 115.0(8) . 2_556
N4C C3C C2C 108.1(8) . 2_666
N1C C2C C3C 108.3(8) . 2_666
C5A N4A C3A 112.2(8) . .
C5A N4A Cu1A 118.3(6) . .
C3A N4A Cu1A 106.4(6) . .
C2A N1A C7A 111.7(8) . .
C2A N1A Cu1A 107.1(6) . .
C7A N1A Cu1A 117.2(6) . .
N4A C5A C6A 113.0(9) . .
N4A C3A C2A 106.9(8) . .
N1A C7A C6A 112.1(9) . 2_667
N1A C2A C3A 106.7(8) . .
C7A C6A C5A 112.2(8) 2_667 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O1 1.622(7) .
V1 O1M 1.630(7) .
V1 O13 1.807(7) .
V1 O12 1.838(6) .
V2 O2M 1.634(7) .
V2 O2 1.640(7) .
V2 O23 1.770(7) .
V2 O12 1.821(6) .
V3 O3 1.628(7) .
V3 O3M 1.633(7) .
V3 O23 1.799(7) .
V3 O13 1.811(7) 1_655
Cu1A N4A 2.005(8) .
Cu1A N4A 2.005(8) 2_667
Cu1A N1A 2.009(8) .
Cu1A N1A 2.009(8) 2_667
Cu1B N4B 2.003(8) .
Cu1B N4B 2.003(8) 2_556
Cu1B N1B 2.023(8) 2_556
Cu1B N1B 2.023(8) .
Cu1C N1C 2.007(8) .
Cu1C N1C 2.007(8) 2_666
Cu1C N4C 2.038(8) 2_666
Cu1C N4C 2.038(8) .
O13 V3 1.812(7) 1_455
N1C C7C 1.476(12) .
N1C C2C 1.482(12) .
N1B C2B 1.464(11) .
N1B C7B 1.477(12) .
N4C C5C 1.472(12) .
N4C C3C 1.473(12) .
N4B C5B 1.480(11) .
N4B C3B 1.506(11) .
C3B C2B 1.494(13) .
C6C C7C 1.477(14) .
C6C C5C 1.507(13) .
C5B C6B 1.502(12) .
C7B C6B 1.518(13) 2_556
C6B C7B 1.518(13) 2_556
C3C C2C 1.501(14) 2_666
C2C C3C 1.501(14) 2_666
N4A C5A 1.467(14) .
N4A C3A 1.493(12) .
N1A C2A 1.476(12) .
N1A C7A 1.478(13) .
C5A C6A 1.528(14) .
C3A C2A 1.519(15) .
C7A C6A 1.524(13) 2_667
C6A C7A 1.524(13) 2_667
