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_7221632
_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
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_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
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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)
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_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       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w 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
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_diffrn_reflns_limit_k_min       -15
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_diffrn_reflns_number            8399
_diffrn_reflns_point_group_measured_fraction_full 0.997
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_diffrn_reflns_theta_full        24.999
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_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/[\s^2^(Fo^2^)+(0.0545P)^2^] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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