#------------------------------------------------------------------------------
#$Date: 2016-01-09 12:24:32 +0200 (Sat, 09 Jan 2016) $
#$Revision: 173743 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/16/7221632.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_7221632
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 H24 Cu N4 O6 V2'
_chemical_formula_sum            'C10 H24 Cu N4 O6 V2'
_chemical_formula_weight         461.75
_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                102.449(18)
_cell_angle_beta                 101.653(19)
_cell_angle_gamma                101.148(19)
_cell_formula_units_Z            3
_cell_length_a                   8.751(2)
_cell_length_b                   13.094(3)
_cell_length_c                   13.363(3)
_cell_measurement_reflns_used    690
_cell_measurement_temperature    393(2)
_cell_measurement_theta_max      17.408
_cell_measurement_theta_min      2.447
_cell_volume                     1418.8(6)
_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      393(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2439
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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      -0.0817958
_diffrn_orient_matrix_UB_12      -0.029399
_diffrn_orient_matrix_UB_13      -0.0193224
_diffrn_orient_matrix_UB_21      0.0103739
_diffrn_orient_matrix_UB_22      -0.0128493
_diffrn_orient_matrix_UB_23      -0.0521486
_diffrn_orient_matrix_UB_31      0.0223456
_diffrn_orient_matrix_UB_32      -0.0474276
_diffrn_orient_matrix_UB_33      0.008125
_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  0.0969
_diffrn_reflns_av_unetI/netI     0.354
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_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       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8399
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.975
_exptl_absorpt_coefficient_mu    2.111
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.895
_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    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             705
_exptl_crystal_size_max          0.1255
_exptl_crystal_size_mid          0.0853
_exptl_crystal_size_min          0.0304
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.2426
_refine_ls_R_factor_gt           0.1078
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0545P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.2511
_reflns_number_gt                2116
_reflns_number_total             4991
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce01076d2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7221629--7221632.cif.'
_cod_original_cell_volume        1418.7(6)
_cod_database_code               7221632
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
Cu1A Cu 0.5 0.5 0.5 0.0558(8) Uani 1 d
Cu1B Cu 1 1 1 0.0525(8) Uani 1 d
Cu1C Cu 1 0.5 1 0.0586(8) Uani 1 d
V1 V 0.9538(3) 0.71468(19) 0.85150(19) 0.0416(7) Uani 1 d
V2 V 0.5651(3) 0.6472(2) 0.7896(2) 0.0472(8) Uani 1 d
V3 V 0.2672(3) 0.7796(2) 0.7300(2) 0.0557(9) Uani 1 d
O1 O 1.0010(11) 0.7946(8) 0.9715(7) 0.061(3) Uani 1 d
O1M O 0.9525(11) 0.5925(7) 0.8626(8) 0.060(3) Uani 1 d
O2 O 0.5995(11) 0.6135(10) 0.8988(8) 0.086(4) Uani 1 d
O2M O 0.4944(11) 0.5434(9) 0.6901(8) 0.081(4) Uani 1 d
O3 O 0.2113(14) 0.7244(11) 0.6068(10) 0.113(5) Uani 1 d
O3M O 0.3334(12) 0.9089(9) 0.7495(9) 0.079(4) Uani 1 d
O12 O 0.7575(10) 0.7200(7) 0.7774(7) 0.052(3) Uani 1 d
O23 O 0.4328(13) 0.7316(10) 0.7952(11) 0.111(5) Uani 1 d
O31 O 0.1015(11) 0.7609(9) 0.7863(9) 0.079(4) Uani 1 d
N1B N 0.8787(14) 0.9843(9) 1.1096(11) 0.055(4) Uani 1 d
H1B H 0.8706 1.0575 1.1404 0.066 Uiso 1 calc
N4B N 0.7842(12) 0.9543(9) 0.8967(10) 0.050(3) Uani 1 d
H4B H 0.7665 0.8769 0.8641 0.06 Uiso 1 calc
C3B C 0.6629(18) 0.9641(14) 0.9557(14) 0.074(6) Uani 1 d
H3BA H 0.5579 0.9206 0.9129 0.089 Uiso 1 calc
H3BB H 0.6572 1.0387 0.9765 0.089 Uiso 1 calc
N1C N 0.7746(14) 0.4859(10) 1.0158(10) 0.058(4) Uani 1 d
H1C H 0.7247 0.5256 0.9696 0.07 Uiso 1 calc
C3A C 0.7884(19) 0.4566(15) 0.5861(13) 0.077(6) Uani 1 d
H3AA H 0.8651 0.4122 0.5844 0.092 Uiso 1 calc
H3AB H 0.7863 0.4835 0.6592 0.092 Uiso 1 calc
C2B C 0.7139(17) 0.9249(12) 1.0515(13) 0.062(5) Uani 1 d
H2BA H 0.6417 0.9354 1.097 0.074 Uiso 1 calc
H2BB H 0.7084 0.8483 1.03 0.074 Uiso 1 calc
N1A N 0.7107(14) 0.6108(12) 0.5417(11) 0.071(4) Uani 1 d
H1A H 0.7257 0.6478 0.6163 0.085 Uiso 1 calc
N4C N 0.9060(14) 0.3535(10) 0.8967(9) 0.058(4) Uani 1 d
H4C H 0.9327 0.3006 0.9348 0.07 Uiso 1 calc
C7B C 1.055(2) 1.0521(14) 0.8020(14) 0.077(5) Uani 1 d
H7BA H 1.1203 1.0439 0.7517 0.093 Uiso 1 calc
H7BB H 1.0607 1.1285 0.8263 0.093 Uiso 1 calc
C2A C 0.8385(19) 0.5507(16) 0.5399(14) 0.081(6) Uani 1 d
H2AA H 0.9421 0.5969 0.5823 0.097 Uiso 1 calc
H2AB H 0.8464 0.5246 0.4679 0.097 Uiso 1 calc
C2C C 0.6857(18) 0.3753(13) 0.9738(15) 0.076(6) Uani 1 d
H2CA H 0.571 0.3698 0.9616 0.091 Uiso 1 calc
H2CB H 0.7156 0.3333 1.0228 0.091 Uiso 1 calc
C5C C 0.970(2) 0.3340(13) 0.8010(14) 0.085(6) Uani 1 d
H5CA H 0.9392 0.3818 0.7586 0.101 Uiso 1 calc
H5CB H 0.9213 0.2603 0.7587 0.101 Uiso 1 calc
C6A C 0.397(2) 0.2420(13) 0.5040(16) 0.093(6) Uani 1 d
H6AA H 0.3677 0.178 0.5283 0.111 Uiso 1 calc
H6AB H 0.3991 0.2185 0.4304 0.111 Uiso 1 calc
C3C C 0.7278(19) 0.3346(14) 0.8705(14) 0.082(6) Uani 1 d
H3CA H 0.677 0.2582 0.8403 0.099 Uiso 1 calc
H3CB H 0.692 0.3735 0.8199 0.099 Uiso 1 calc
C7C C 1.241(2) 0.4672(14) 0.8788(16) 0.090(6) Uani 1 d
H7CA H 1.3545 0.4719 0.8831 0.108 Uiso 1 calc
H7CB H 1.2065 0.511 0.8329 0.108 Uiso 1 calc
C6B C 0.880(2) 0.9929(13) 0.7446(14) 0.071(5) Uani 1 d
H6BA H 0.8486 1.019 0.6828 0.085 Uiso 1 calc
H6BB H 0.8747 0.9167 0.7197 0.085 Uiso 1 calc
N4A N 0.6281(15) 0.3924(11) 0.5233(11) 0.068(4) Uani 1 d
H4A H 0.6405 0.3572 0.4539 0.081 Uiso 1 calc
C5A C 0.564(3) 0.3060(17) 0.5685(17) 0.114(8) Uani 1 d
H5AA H 0.5597 0.3372 0.6403 0.137 Uiso 1 calc
H5AB H 0.6353 0.258 0.5714 0.137 Uiso 1 calc
C6C C 1.1493(19) 0.3521(14) 0.8275(13) 0.071(5) Uani 1 d
H6CA H 1.181 0.3269 0.7629 0.086 Uiso 1 calc
H6CB H 1.1799 0.3085 0.8747 0.086 Uiso 1 calc
C7A C 0.269(2) 0.3062(16) 0.5115(16) 0.097(7) Uani 1 d
H7AA H 0.1631 0.2578 0.4804 0.116 Uiso 1 calc
H7AB H 0.2767 0.3382 0.5855 0.116 Uiso 1 calc
C5B C 0.7603(19) 1.0048(15) 0.8096(13) 0.072(5) Uani 1 d
H5BA H 0.7689 1.0809 0.8381 0.086 Uiso 1 calc
H5BB H 0.6525 0.9726 0.7642 0.086 Uiso 1 calc
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
-4 -16 8 0.0426
5 -15 -7 0.0276
-11 8 -1 0.0566
-1 3 17 0.0108
1 -3 -17 0.0197
-12 -1 4 0.0658
0 18 -7 0.0385
12 -1 -3 0.0574
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
N4A Cu1A N4A 180 . 2_666
N4A Cu1A N1A 86.9(6) . .
N4A Cu1A N1A 93.1(6) 2_666 .
N4A Cu1A N1A 93.1(6) . 2_666
N4A Cu1A N1A 86.9(6) 2_666 2_666
N1A Cu1A N1A 180 . 2_666
N4B Cu1B N4B 180 . 2_777
N4B Cu1B N1B 85.7(5) . .
N4B Cu1B N1B 94.3(5) 2_777 .
N4B Cu1B N1B 94.3(5) . 2_777
N4B Cu1B N1B 85.7(5) 2_777 2_777
N1B Cu1B N1B 180 . 2_777
N1C Cu1C N1C 180 2_767 .
N1C Cu1C N4C 96.3(5) 2_767 .
N1C Cu1C N4C 83.7(5) . .
N1C Cu1C N4C 83.7(5) 2_767 2_767
N1C Cu1C N4C 96.3(5) . 2_767
N4C Cu1C N4C 180 . 2_767
N1C Cu1C O1M 92.2(4) 2_767 2_767
N1C Cu1C O1M 87.8(4) . 2_767
N4C Cu1C O1M 87.3(4) . 2_767
N4C Cu1C O1M 92.7(4) 2_767 2_767
N1C Cu1C O1M 87.8(4) 2_767 .
N1C Cu1C O1M 92.2(4) . .
N4C Cu1C O1M 92.7(4) . .
N4C Cu1C O1M 87.3(4) 2_767 .
O1M Cu1C O1M 180 2_767 .
O1M V1 O1 107.3(5) . .
O1M V1 O31 111.6(5) . 1_655
O1 V1 O31 107.9(5) . 1_655
O1M V1 O12 110.9(4) . .
O1 V1 O12 110.5(4) . .
O31 V1 O12 108.5(5) 1_655 .
O2M V2 O2 111.4(7) . .
O2M V2 O23 111.4(6) . .
O2 V2 O23 108.6(6) . .
O2M V2 O12 108.1(5) . .
O2 V2 O12 107.2(5) . .
O23 V2 O12 110.1(5) . .
O3 V3 O3M 109.0(7) . .
O3 V3 O31 110.1(6) . .
O3M V3 O31 106.8(5) . .
O3 V3 O23 111.7(6) . .
O3M V3 O23 106.9(6) . .
O31 V3 O23 112.2(6) . .
V1 O1M Cu1C 139.2(5) . .
V1 O12 V2 124.5(5) . .
V2 O23 V3 150.2(8) . .
V3 O31 V1 165.5(7) . 1_455
C7B N1B C2B 114.8(13) 2_777 .
C7B N1B Cu1B 119.9(10) 2_777 .
C2B N1B Cu1B 106.1(10) . .
C3B N4B C5B 111.2(13) . .
C3B N4B Cu1B 108.2(10) . .
C5B N4B Cu1B 118.1(9) . .
N4B C3B C2B 106.2(13) . .
C2C N1C C7C 112.5(13) . 2_767
C2C N1C Cu1C 109.5(10) . .
C7C N1C Cu1C 116.1(10) 2_767 .
N4A C3A C2A 108.8(14) . .
N1B C2B C3B 109.8(13) . .
C7A N1A C2A 112.3(14) 2_666 .
C7A N1A Cu1A 119.5(12) 2_666 .
C2A N1A Cu1A 106.7(11) . .
C3C N4C C5C 113.0(13) . .
C3C N4C Cu1C 107.7(9) . .
C5C N4C Cu1C 115.7(10) . .
N1B C7B C6B 114.5(13) 2_777 .
N1A C2A C3A 105.9(13) . .
N1C C2C C3C 106.4(14) . .
N4C C5C C6C 112.9(15) . .
C5A C6A C7A 113.0(15) . .
N4C C3C C2C 106.2(13) . .
N1C C7C C6C 116.2(14) 2_767 .
C5B C6B C7B 115.3(15) . .
C3A N4A C5A 112.4(16) . .
C3A N4A Cu1A 105.2(9) . .
C5A N4A Cu1A 118.5(12) . .
N4A C5A C6A 111.7(18) . .
C5C C6C C7C 114.8(14) . .
N1A C7A C6A 111.3(16) 2_666 .
N4B C5B C6B 112.6(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1A N4A 2.000(12) .
Cu1A N4A 2.000(12) 2_666
Cu1A N1A 2.005(12) .
Cu1A N1A 2.005(12) 2_666
Cu1B N4B 1.996(11) .
Cu1B N4B 1.996(11) 2_777
Cu1B N1B 1.996(12) .
Cu1B N1B 1.996(12) 2_777
Cu1C N1C 2.003(11) 2_767
Cu1C N1C 2.003(11) .
Cu1C N4C 2.013(12) .
Cu1C N4C 2.013(12) 2_767
Cu1C O1M 2.420(10) 2_767
Cu1C O1M 2.420(10) .
V1 O1M 1.636(9) .
V1 O1 1.637(9) .
V1 O31 1.781(10) 1_655
V1 O12 1.823(9) .
V2 O2M 1.601(10) .
V2 O2 1.602(11) .
V2 O23 1.750(10) .
V2 O12 1.825(9) .
V3 O3 1.580(12) .
V3 O3M 1.625(11) .
V3 O31 1.764(9) .
V3 O23 1.825(11) .
O31 V1 1.781(10) 1_455
N1B C7B 1.428(18) 2_777
N1B C2B 1.463(16) .
N4B C3B 1.453(17) .
N4B C5B 1.456(18) .
C3B C2B 1.50(2) .
N1C C2C 1.434(17) .
N1C C7C 1.456(19) 2_767
C3A N4A 1.463(18) .
C3A C2A 1.52(2) .
N1A C7A 1.42(2) 2_666
N1A C2A 1.49(2) .
N4C C3C 1.486(17) .
N4C C5C 1.489(18) .
C7B N1B 1.428(18) 2_777
C7B C6B 1.53(2) .
C2C C3C 1.51(2) .
C5C C6C 1.50(2) .
C6A C5A 1.51(2) .
C6A C7A 1.53(2) .
C7C N1C 1.456(19) 2_767
C7C C6C 1.50(2) .
C6B C5B 1.50(2) .
N4A C5A 1.46(2) .
C7A N1A 1.42(2) 2_666
