Sequential single-crystal-to-single-crystal transformations promoted by gradual thermal dehydration in a porous metavanadate hybrid
Martín-Caballero, Jagoba; Wéry, Ana San José; Artetxe, Beñat; Reinoso, Santiago; Felices, Leire San; Vilas, José Luis; Gutiérrez-Zorrilla, Juan M.; CrystEngComm 17 (2015) 8915–; doi:10.1039/C5CE01076D

data_7221629
_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 H34 Cu N4 O11 V2'
_chemical_formula_sum            'C10 H34 Cu N4 O11 V2'
_chemical_formula_weight         551.83
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    Heat-sensitive
_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_creation_date             2015-07-08T20:05:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-07-14 deposited with the CCDC.
2015-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                79.513(2)
_cell_angle_beta                 98.024(2)
_cell_angle_gamma                105.156(2)
_cell_formula_units_Z            12
_cell_length_a                   16.4455(3)
_cell_length_b                   15.0098(5)
_cell_length_c                   27.8995(7)
_cell_measurement_reflns_used    13498
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.992
_cell_measurement_theta_min      1.887
_cell_volume                     6505.5(3)
_computing_cell_refinement
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
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_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
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_computing_data_reduction
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        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)'
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_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 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.024691
_diffrn_orient_matrix_UB_12      -0.0043702
_diffrn_orient_matrix_UB_13      -0.0240898
_diffrn_orient_matrix_UB_21      -0.040847
_diffrn_orient_matrix_UB_22      -0.0038886
_diffrn_orient_matrix_UB_23      -0.0079479
_diffrn_orient_matrix_UB_31      -0.0132561
_diffrn_orient_matrix_UB_32      0.0445132
_diffrn_orient_matrix_UB_33      -0.0055991
_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  0.0357
_diffrn_reflns_av_unetI/netI     0.072
_diffrn_reflns_laue_measured_fraction_full 1
_diffrn_reflns_laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            46122
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.672
_exptl_absorpt_coefficient_mu    1.873
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.95956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.69
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3420
_refine_diff_density_max         0.997
_refine_diff_density_min         -1.075
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1558
_refine_ls_number_reflns         22908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+13.3392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                17910
_reflns_number_total             22908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01076d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7221629--7221632.cif.'
_cod_database_code               7221629