#------------------------------------------------------------------------------
#$Date: 2016-01-09 12:24:32 +0200 (Sat, 09 Jan 2016) $
#$Revision: 173743 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/16/7221630.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_7221630
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 H30 Cu N4 O9 V2'
_chemical_formula_sum            'C10 H30 Cu N4 O9 V2'
_chemical_formula_weight         515.8
_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                102.032(3)
_cell_angle_beta                 101.742(3)
_cell_angle_gamma                97.560(3)
_cell_formula_units_Z            3
_cell_length_a                   8.0199(2)
_cell_length_b                   13.9524(6)
_cell_length_c                   14.2588(5)
_cell_measurement_reflns_used    5724
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.087
_cell_measurement_theta_min      2.372
_cell_volume                     1502.38(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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      0.0897824
_diffrn_orient_matrix_UB_12      0.0108259
_diffrn_orient_matrix_UB_13      0.0229175
_diffrn_orient_matrix_UB_21      -0.0134114
_diffrn_orient_matrix_UB_22      0.040479
_diffrn_orient_matrix_UB_23      0.0352752
_diffrn_orient_matrix_UB_31      -0.0140622
_diffrn_orient_matrix_UB_32      -0.0322228
_diffrn_orient_matrix_UB_33      0.0311928
_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  0.0169
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9271
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    2.014
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.958
_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            purple
_exptl_crystal_density_diffrn    1.71
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             795
_exptl_crystal_size_max          0.1213
_exptl_crystal_size_mid          0.1012
_exptl_crystal_size_min          0.0602
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0366P)²+1.8005P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                4751
_reflns_number_total             5290
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce01076d2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7221629--7221632.cif.'
_cod_original_cell_volume        1502.39(10)
_cod_database_code               7221630
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 0.85344(5) 0.72421(3) 0.14391(3) 0.01114(11) Uani 1 d
V2 V 0.25620(5) 0.84299(3) 0.13405(3) 0.00902(11) Uani 1 d
V3 V 0.61300(6) 0.82388(3) 0.28768(3) 0.01096(11) Uani 1 d
Cu1A Cu 0.5 1 0.5 0.01304(11) Uani 1 d
Cu1B Cu 0.5 0.5 0 0.01923(13) Uani 1 d
Cu1C Cu 0.5 1 0 0.01098(11) Uani 1 d
O1 O 0.9037(2) 0.64355(14) 0.21019(15) 0.0196(4) Uani 1 d
O12 O 1.0385(2) 0.77404(14) 0.10424(14) 0.0155(4) Uani 1 d
O13 O 0.7731(2) 0.82430(14) 0.21506(14) 0.0155(4) Uani 1 d
O2 O 0.2657(2) 0.95636(13) 0.19976(13) 0.0144(4) Uani 1 d
O23 O 0.4015(2) 0.78064(14) 0.20437(13) 0.0154(4) Uani 1 d
O3 O 0.6394(3) 0.74897(15) 0.36307(14) 0.0186(4) Uani 1 d
O1M O 0.6978(2) 0.66479(14) 0.04725(14) 0.0184(4) Uani 1 d
O2M O 0.3220(2) 0.85389(14) 0.03435(13) 0.0170(4) Uani 1 d
O3M O 0.6224(2) 0.93682(14) 0.35407(13) 0.0157(4) Uani 1 d
N4A N 0.2719(3) 0.9865(2) 0.40576(18) 0.0272(6) Uani 1 d
H4A H 0.2861 0.9554 0.3403 0.033 Uiso 1 calc
N1A N 0.4589(4) 0.85758(19) 0.51289(18) 0.0302(7) Uani 1 d
H1A H 0.4866 0.8168 0.4553 0.036 Uiso 1 calc
C5A C 0.1225(4) 0.9234(4) 0.4217(3) 0.0563(14) Uani 1 d
H5AA H 0.0212 0.9204 0.3699 0.068 Uiso 1 calc
H5AB H 0.0992 0.954 0.4842 0.068 Uiso 1 calc
C2A C 0.5908(7) 0.8526(3) 0.5998(3) 0.0506(12) Uani 1 d
H2AA H 0.6027 0.7839 0.5977 0.061 Uiso 1 calc
H2AB H 0.5571 0.8798 0.66 0.061 Uiso 1 calc
C6A C 0.1507(6) 0.8204(4) 0.4224(3) 0.0636(16) Uani 1 d
H6AA H 0.1899 0.7934 0.3641 0.076 Uiso 1 calc
H6AB H 0.041 0.7793 0.4188 0.076 Uiso 1 calc
C3A C 0.2434(6) 1.0885(3) 0.4028(3) 0.0509(12) Uani 1 d
H3AA H 0.2057 1.1185 0.4608 0.061 Uiso 1 calc
H3AB H 0.1547 1.0866 0.3447 0.061 Uiso 1 calc
C7A C 0.2821(6) 0.8140(3) 0.5135(3) 0.0599(14) Uani 1 d
H7AA H 0.2521 0.8489 0.5723 0.072 Uiso 1 calc
H7AB H 0.2776 0.7447 0.5157 0.072 Uiso 1 calc
N4B N 0.3326(3) 0.56868(18) 0.06561(19) 0.0218(6) Uani 1 d
H4B H 0.3927 0.6368 0.0992 0.026 Uiso 1 calc
N1B N 0.3765(3) 0.53140(18) -0.12491(19) 0.0211(5) Uani 1 d
H1B H 0.2949 0.4706 -0.1629 0.025 Uiso 1 calc
C2B C 0.2707(4) 0.6059(2) -0.0948(2) 0.0255(7) Uani 1 d
H2BA H 0.1805 0.6077 -0.1509 0.031 Uiso 1 calc
H2BB H 0.3425 0.6716 -0.0697 0.031 Uiso 1 calc
C3B C 0.1915(4) 0.5762(2) -0.0157(2) 0.0242(7) Uani 1 d
H3BA H 0.1259 0.6256 0.0085 0.029 Uiso 1 calc
H3BB H 0.1134 0.5125 -0.0423 0.029 Uiso 1 calc
C5B C 0.2664(4) 0.5248(2) 0.1404(2) 0.0274(7) Uani 1 d
H5BA H 0.1981 0.459 0.1085 0.033 Uiso 1 calc
H5BB H 0.1911 0.5659 0.1678 0.033 Uiso 1 calc
C6B C 0.4109(4) 0.5165(2) 0.2231(2) 0.0292(7) Uani 1 d
H6BA H 0.3613 0.4998 0.2756 0.035 Uiso 1 calc
H6BB H 0.4866 0.581 0.2497 0.035 Uiso 1 calc
C7B C 0.4815(4) 0.5609(2) -0.1920(3) 0.0281(7) Uani 1 d
H7BA H 0.5579 0.624 -0.1591 0.034 Uiso 1 calc
H7BB H 0.4052 0.5701 -0.2503 0.034 Uiso 1 calc
N4C N 0.7211(3) 0.96138(17) 0.06585(16) 0.0131(5) Uani 1 d
H4C H 0.6883 0.91 0.0996 0.016 Uiso 1 calc
N1C N 0.5163(3) 0.90645(16) -0.12493(16) 0.0123(5) Uani 1 d
H1C H 0.5646 0.9476 -0.1644 0.015 Uiso 1 calc
C5C C 0.8527(3) 1.0412(2) 0.1395(2) 0.0171(6) Uani 1 d
H5CA H 0.8967 1.0897 0.1065 0.021 Uiso 1 calc
H5CB H 0.949 1.0123 0.1675 0.021 Uiso 1 calc
C2C C 0.6466(3) 0.8460(2) -0.0948(2) 0.0155(6) Uani 1 d
H2CA H 0.6888 0.8161 -0.151 0.019 Uiso 1 calc
H2CB H 0.5952 0.7931 -0.0693 0.019 Uiso 1 calc
C3C C 0.7937(3) 0.9136(2) -0.0160(2) 0.0156(6) Uani 1 d
H3CA H 0.8788 0.8754 0.0078 0.019 Uiso 1 calc
H3CB H 0.8501 0.964 -0.0427 0.019 Uiso 1 calc
C6C C 0.7798(4) 1.0935(2) 0.2218(2) 0.0172(6) Uani 1 d
H6CA H 0.8745 1.1363 0.2731 0.021 Uiso 1 calc
H6CB H 0.7258 1.0438 0.2502 0.021 Uiso 1 calc
C7C C 0.6475(4) 1.1559(2) 0.1889(2) 0.0159(6) Uani 1 d
H7CA H 0.623 1.1967 0.2467 0.019 Uiso 1 calc
H7CB H 0.696 1.2002 0.1532 0.019 Uiso 1 calc
O1W O 0.8133(8) 0.6317(4) 0.4665(4) 0.0663(14) Uani 0.7 d
O2W O 0.657(3) 0.6190(8) 0.4828(9) 0.103(6) Uani 0.3 d
O3W O 0.3864(14) 0.6296(8) 0.4346(8) 0.045(3) Uani 0.25 d
O4W O 0.382(4) 0.555(2) 0.503(3) 0.181(15) Uani 0.25 d
O5W O 0.2499(13) 0.5541(6) 0.5134(7) 0.096(3) Uani 0.5 d
O6W O 1.0454(9) 0.6415(5) 0.6353(6) 0.121(2) Uani 0.75 d
O7W O 0.877(4) 0.6804(11) 0.6909(12) 0.179(15) Uani 0.25 d
O8W O 0.926(3) 0.7206(13) 0.861(2) 0.109(8) Uani 0.2 d
O9W O 0.565(4) 0.558(2) 0.5598(14) 0.197(12) Uani 0.3 d
O10W O 1.0191(6) 0.5478(3) 0.3532(3) 0.1016(15) 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
3 -17 13 0.043
-2 -15 16 0.0435
5 12 -16 0.046
0 -4 -17 0.0293
-2 -12 -11 0.0279
-11 8 4 0.0439
11 -8 -4 0.0568
1 11 12 0.0299
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
O1M V1 O1 107.60(10) . .
O1M V1 O12 109.75(9) . .
O1 V1 O12 110.58(9) . .
O1M V1 O13 108.32(9) . .
O1 V1 O13 110.21(9) . .
O12 V1 O13 110.31(9) . .
O2M V2 O2 107.26(9) . .
O2M V2 O12 111.70(9) . 1_455
O2 V2 O12 110.00(9) . 1_455
O2M V2 O23 108.95(9) . .
O2 V2 O23 109.21(9) . .
O12 V2 O23 109.66(8) 1_455 .
O3M V3 O3 108.27(10) . .
O3M V3 O13 110.36(9) . .
O3 V3 O13 112.36(9) . .
O3M V3 O23 109.50(9) . .
O3 V3 O23 108.02(9) . .
O13 V3 O23 108.28(9) . .
N4A Cu1A N4A 180 . 2_676
N4A Cu1A N1A 94.64(12) . .
N4A Cu1A N1A 85.36(12) 2_676 .
N4A Cu1A N1A 85.36(12) . 2_676
N4A Cu1A N1A 94.64(12) 2_676 2_676
N1A Cu1A N1A 180 . 2_676
N1B Cu1B N1B 180 2_665 .
N1B Cu1B N4B 93.63(10) 2_665 .
N1B Cu1B N4B 86.37(10) . .
N1B Cu1B N4B 86.37(10) 2_665 2_665
N1B Cu1B N4B 93.63(10) . 2_665
N4B Cu1B N4B 180 . 2_665
N1C Cu1C N1C 180 . 2_675
N1C Cu1C N4C 86.49(9) . .
N1C Cu1C N4C 93.51(9) 2_675 .
N1C Cu1C N4C 93.50(9) . 2_675
N1C Cu1C N4C 86.50(9) 2_675 2_675
N4C Cu1C N4C 180 . 2_675
V1 O12 V2 149.66(12) . 1_655
V3 O13 V1 132.19(11) . .
V3 O23 V2 132.44(11) . .
C5A N4A C3A 113.3(3) . .
C5A N4A Cu1A 116.8(2) . .
C3A N4A Cu1A 106.9(2) . .
C7A N1A C2A 113.4(3) . .
C7A N1A Cu1A 117.2(3) . .
C2A N1A Cu1A 106.5(2) . .
N4A C5A C6A 113.0(3) . .
N1A C2A C3A 107.6(3) . 2_676
C5A C6A C7A 113.7(3) . .
N4A C3A C2A 107.9(3) . 2_676
N1A C7A C6A 111.6(3) . .
C3B N4B C5B 112.3(2) . .
C3B N4B Cu1B 105.69(18) . .
C5B N4B Cu1B 117.42(19) . .
C2B N1B C7B 112.4(2) . .
C2B N1B Cu1B 106.43(19) . .
C7B N1B Cu1B 118.12(19) . .
N1B C2B C3B 107.7(2) . .
N4B C3B C2B 108.4(2) . .
N4B C5B C6B 112.2(2) . .
C5B C6B C7B 113.9(3) . 2_665
N1B C7B C6B 112.1(3) . 2_665
C3C N4C C5C 111.4(2) . .
C3C N4C Cu1C 105.48(16) . .
C5C N4C Cu1C 117.55(17) . .
C2C N1C C7C 112.3(2) . 2_675
C2C N1C Cu1C 106.28(16) . .
C7C N1C Cu1C 116.98(17) 2_675 .
N4C C5C C6C 112.3(2) . .
N1C C2C C3C 108.1(2) . .
N4C C3C C2C 107.9(2) . .
C5C C6C C7C 113.9(2) . .
N1C C7C C6C 112.2(2) 2_675 .
O1W O2W O9W 133.3(12) . .
O5W O4W O9W 141(3) . .
O5W O4W O3W 99.7(18) . .
O9W O4W O3W 109.0(19) . .
O5W O4W O9W 119(2) . 2_666
O9W O4W O9W 77(2) . 2_666
O3W O4W O9W 107(2) . 2_666
O4W O9W O2W 93.0(15) . .
O4W O9W O4W 103(2) . 2_666
O2W O9W O4W 88.3(15) . 2_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O1M 1.6422(19) .
V1 O1 1.6522(19) .
V1 O12 1.7998(18) .
V1 O13 1.8185(19) .
V2 O2M 1.6424(18) .
V2 O2 1.6452(18) .
V2 O12 1.8003(18) 1_455
V2 O23 1.8096(18) .
V3 O3M 1.6440(19) .
V3 O3 1.6512(19) .
V3 O13 1.8061(19) .
V3 O23 1.8067(18) .
Cu1A N4A 1.998(2) .
Cu1A N4A 1.998(2) 2_676
Cu1A N1A 2.024(3) .
Cu1A N1A 2.024(3) 2_676
Cu1B N1B 2.017(3) 2_665
Cu1B N1B 2.017(3) .
Cu1B N4B 2.018(2) .
Cu1B N4B 2.018(2) 2_665
Cu1C N1C 2.016(2) .
Cu1C N1C 2.016(2) 2_675
Cu1C N4C 2.025(2) .
Cu1C N4C 2.025(2) 2_675
O12 V2 1.8003(18) 1_655
N4A C5A 1.476(5) .
N4A C3A 1.479(5) .
N1A C7A 1.470(5) .
N1A C2A 1.476(5) .
C5A C6A 1.486(7) .
C2A C3A 1.480(6) 2_676
C6A C7A 1.523(7) .
C3A C2A 1.480(6) 2_676
N4B C3B 1.478(4) .
N4B C5B 1.488(4) .
N1B C2B 1.477(4) .
N1B C7B 1.481(4) .
C2B C3B 1.505(4) .
C5B C6B 1.511(5) .
C6B C7B 1.520(5) 2_665
C7B C6B 1.520(5) 2_665
N4C C3C 1.484(3) .
N4C C5C 1.486(3) .
N1C C2C 1.479(3) .
N1C C7C 1.482(3) 2_675
C5C C6C 1.512(4) .
C2C C3C 1.506(4) .
C6C C7C 1.522(4) .
C7C N1C 1.482(3) 2_675
O1W O2W 1.32(2) .
O2W O9W 1.74(3) .
O3W O4W 1.57(3) .
O4W O5W 1.10(3) .
O4W O9W 1.51(3) .
O4W O9W 1.79(4) 2_666
O6W O7W 1.79(3) .
O9W O4W 1.79(4) 2_666
