Single-Crystal to Single-Crystal Reversible Transformations Induced by Thermal Dehydration in Keggin-Type Polyoxometalates Decorated with Copper(II)-Picolinate Complexes: The Structure Directing Role of Guanidinium
Pache, Aroa; Reinoso, Santiago; Felices, Leire; Iturrospe, Amaia; Lezama, Luis; Gutiérrez-Zorrilla, Juan; Inorganics 3 (2015) 194–; doi:10.3390/inorganics3020194

data_1520326
_publ_section_title
;
 Single-Crystal to Single-Crystal Reversible Transformations Induced by
 Thermal Dehydration in Keggin-Type Polyoxometalates Decorated with
 Copper(II)-Picolinate Complexes: The Structure Directing Role of
 Guanidinium
;
_journal_issue                   2
_journal_name_full               Inorganics
_journal_page_first              194
_journal_paper_doi               10.3390/inorganics3020194
_journal_volume                  3
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'C4 H24 N12, C48 H36 Cu4 N8 O18, C24 H16 Cu2 N4 O48 Si W12, 6 (H2 O)'
_chemical_formula_sum            'C76 H88 Cu6 N24 O72 Si W12'
_chemical_formula_weight         5105.23
_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_creation_date             2014-04-08T09:54:26-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                107.102(3)
_cell_angle_beta                 94.393(3)
_cell_angle_gamma                101.008(3)
_cell_formula_units_Z            1
_cell_length_a                   11.7014(4)
_cell_length_b                   15.9523(5)
_cell_length_c                   17.0285(5)
_cell_measurement_reflns_used    13438
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.156
_cell_measurement_theta_min      2.7403
_cell_measurement_wavelength     1.54184
_cell_volume                     2952.16(18)
_computing_cell_refinement
'CrysAlis Pro (Oxford Diffraction Ltd., 2011)'
_computing_data_collection
'CrysAlis Pro (Oxford Diffraction Ltd., 2011)'
_computing_data_reduction
'CrysAlis Pro (Oxford Diffraction Ltd., 2011)'
_computing_molecular_graphics    'Diamond v.3.2f (Crystal Impact GbR, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'OLEX2 (Dolomanov et al, 2010)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4023
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   31.00   89.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.7631 -124.0000  117.0000 58

  2 omega   29.00   90.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.7631 -125.0000  -60.0000 61

  3 omega  -24.00   55.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.7631  -38.0000  -60.0000 79

  4 omega   -6.00  108.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.7631    0.0000  150.0000 114

  5 omega    7.00   61.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.7631 -125.0000 -150.0000 54

  6 omega   79.00  145.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   90.0000 66

  7 omega   85.00  158.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000    0.0000 73

  8 omega   86.00  114.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -107.0000  -83.0000 28

  9 omega   94.00  156.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  -60.0000 62

 10 omega   50.00   83.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000 -150.0000 33

 11 omega   45.00   71.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  150.0000 26

 12 omega   96.00  136.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  -90.0000 40

 13 omega   40.00   65.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -30.0000 25

 14 omega  114.00  150.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   60.0000 36

 15 omega   38.00   64.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000    0.0000 26

 16 omega   70.00  146.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000    0.0000 76

 17 omega   80.00  106.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -124.0000  163.0000 26

 18 omega   39.00   74.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  120.0000 35

 19 omega   86.00  149.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000 -120.0000 63

 20 omega  109.00  136.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000 -150.0000 27

 21 omega   49.00   82.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -148.0000  132.0000 33

 22 omega  109.00  134.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -148.0000  132.0000 25

 23 omega   93.00  119.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  150.0000 26

 24 omega  132.00  157.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  150.0000 25

 25 omega   44.00  112.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -104.0000 -177.0000 68

 26 omega   49.00   76.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -120.0000 27

 27 omega   86.00  113.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -180.0000 27

 28 omega  124.00  157.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -180.0000 33

 29 omega   32.00  107.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -99.0000  -72.0000 75

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.036164
_diffrn_orient_matrix_UB_12      0.0241861
_diffrn_orient_matrix_UB_13      0.0875932
_diffrn_orient_matrix_UB_21      -0.1260987
_diffrn_orient_matrix_UB_22      -0.0048331
_diffrn_orient_matrix_UB_23      -0.0374502
_diffrn_orient_matrix_UB_31      -0.0338811
_diffrn_orient_matrix_UB_32      -0.1006985
_diffrn_orient_matrix_UB_33      -0.0082134
_diffrn_radiation_monochromator  'Multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Nova (Cu) X-ray micro-source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22568
_diffrn_reflns_theta_full        71.5
_diffrn_reflns_theta_max         71.5
_diffrn_reflns_theta_min         2.74
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    23.180
_exptl_absorpt_correction_T_max  0.333
_exptl_absorpt_correction_T_min  0.072
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
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)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2364
_exptl_crystal_size_max          0.1754
_exptl_crystal_size_mid          0.1342
_exptl_crystal_size_min          0.0705
_refine_diff_density_max         1.533
_refine_diff_density_min         -3.35
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.278
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         11493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.278
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+55.3485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1168
_reflns_number_gt                10892
_reflns_number_total             11493
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            s2.cif
_cod_data_source_block           1
_cod_original_cell_volume        2952.16(16)
_cod_database_code               1520326