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_1520324
_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 Ge W12, 6 (H2 O)'
_chemical_formula_sum            'C76 H88 Cu6 Ge N24 O72 W12'
_chemical_formula_weight         5149.73
_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             2014-04-09T09:43:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                107.057(3)
_cell_angle_beta                 94.372(2)
_cell_angle_gamma                100.971(2)
_cell_formula_units_Z            1
_cell_length_a                   11.7110(3)
_cell_length_b                   15.9628(6)
_cell_length_c                   17.0341(5)
_cell_measurement_reflns_used    14826
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2458
_cell_measurement_theta_min      1.5432
_cell_measurement_wavelength     0.71073
_cell_volume                     2958.92(17)
_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 16.2439
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_details
;
  1 omega  -18.00   14.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1517  -99.0000  -30.0000 32

  2 omega -104.00   -5.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1517  -38.0000   90.0000 99

  3 omega  -35.00    8.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1517  -57.0000    0.0000 43

  4 omega  -10.00   25.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1517  -99.0000   60.0000 35

  5 omega  -53.00   51.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1517   38.0000   30.0000 104

  6 omega -100.00   -8.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1517  -57.0000 -120.0000 92

  7 omega   49.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6986  178.0000  -60.0000 60

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0044857
_diffrn_orient_matrix_UB_12      -0.0397134
_diffrn_orient_matrix_UB_13      0.0095613
_diffrn_orient_matrix_UB_21      -0.0220503
_diffrn_orient_matrix_UB_22      0.0163793
_diffrn_orient_matrix_UB_23      0.0378592
_diffrn_orient_matrix_UB_31      -0.0581097
_diffrn_orient_matrix_UB_32      -0.0206887
_diffrn_orient_matrix_UB_33      -0.0202656
_diffrn_radiation_monochromator  'Multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Nova (Mo) X-ray micro-source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19292
_diffrn_reflns_theta_full        25.5
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         1.54
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    13.025
_exptl_absorpt_correction_T_max  0.409
_exptl_absorpt_correction_T_min  0.115
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
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    2.890
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2382
_exptl_crystal_size_max          0.4358
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.0962
_refine_diff_density_max         1.578
_refine_diff_density_min         -3.235
_refine_diff_density_rms         0.24
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.28
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         11018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.28
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0001P)^2^+65.2649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                10485
_reflns_number_total             11018
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            s5.cif
_cod_data_source_block           3
_cod_original_cell_volume        2958.92(16)
_cod_database_code               1520324