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_1520322
_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 H32 Cu4 N8 O16, C24 H16 Cu2 N4 O48 Ge W12'
_chemical_formula_sum            'C76 H72 Cu6 Ge N24 O64 W12'
_chemical_formula_weight         5005.61
_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             2014-04-09T10:00:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                104.371(5)
_cell_angle_beta                 91.222(5)
_cell_angle_gamma                100.534(5)
_cell_formula_units_Z            1
_cell_length_a                   11.6025(7)
_cell_length_b                   15.9736(9)
_cell_length_c                   15.9849(10)
_cell_measurement_reflns_used    4607
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.252
_cell_measurement_theta_min      4.637
_cell_measurement_wavelength     1.54184
_cell_volume                     2814.5(3)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega -106.00  -16.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5756  -38.0000   60.0000 90

  2 omega  -65.00   35.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5756   38.0000 -120.0000 100

  3 omega   16.00  113.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5756   38.0000  -30.0000 97

  4 omega    4.00   89.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5756 -125.0000   60.0000 85

  5 omega  -87.00  -50.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  125.0000  150.0000 37

  6 omega   79.00  156.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109   30.0000 -150.0000 77

  7 omega   32.00   57.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -30.0000    0.0000 25

  8 omega   35.00   74.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -45.0000 -180.0000 39

  9 omega   58.00  115.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109 -125.0000   60.0000 57

 10 omega   45.00  108.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -94.0000 -180.0000 63

 11 omega   25.00  104.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -94.0000  -60.0000 79

 12 omega   34.00   69.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -30.0000  -60.0000 35

 13 omega   42.00   69.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -30.0000 -120.0000 27

 14 omega   37.00   62.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -94.0000 -120.0000 25

 15 omega   48.00  158.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109   15.0000  150.0000 110

 16 omega   38.00   66.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -45.0000  -60.0000 28

 17 omega   40.00   65.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -45.0000  150.0000 25

 18 omega   38.00  138.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -61.0000   30.0000 100

 19 omega   33.00   62.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -30.0000  -30.0000 29

 20 omega   48.00   76.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -45.0000  -90.0000 28

 21 omega   63.00  122.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109 -125.0000  -60.0000 59

 22 omega   67.00  109.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -94.0000   90.0000 42

 23 omega   90.00  135.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109   45.0000  -90.0000 45

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.051678
_diffrn_orient_matrix_UB_12      -0.0225076
_diffrn_orient_matrix_UB_13      0.0794186
_diffrn_orient_matrix_UB_21      -0.0189262
_diffrn_orient_matrix_UB_22      -0.0976574
_diffrn_orient_matrix_UB_23      -0.0503472
_diffrn_orient_matrix_UB_31      0.1236973
_diffrn_orient_matrix_UB_32      0.0160381
_diffrn_orient_matrix_UB_33      -0.0332372
_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  0.0531
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20323
_diffrn_reflns_theta_full        71.49
_diffrn_reflns_theta_max         71.49
_diffrn_reflns_theta_min         2.86
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    24.412
_exptl_absorpt_correction_T_max  0.551
_exptl_absorpt_correction_T_min  0.18
_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    2.953
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2302
_exptl_crystal_size_max          0.1297
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.033
_refine_diff_density_max         6.499
_refine_diff_density_min         -2.961
_refine_diff_density_rms         0.457
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         10854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.112
_refine_ls_R_factor_gt           0.0789
_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^)+(0.1221P)^2^+74.0459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1979
_refine_ls_wR_factor_ref         0.2308
_reflns_number_gt                7649
_reflns_number_total             10854
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            s6.cif
_cod_data_source_block           3a
_cod_database_code               1520322