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_1520323
_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, C42 H30 Cu3.5 N7 O55 Si W12, 4 (H2 O)'
_chemical_formula_sum            'C46 H62 Cu3.5 N19 O59 Si W12'
_chemical_formula_weight         4281.83
_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             2014-04-10T10:57:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                101.508(2)
_cell_angle_beta                 90.346(2)
_cell_angle_gamma                105.544(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9426(2)
_cell_length_b                   12.8151(3)
_cell_length_c                   30.0533(6)
_cell_measurement_reflns_used    18119
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2463
_cell_measurement_theta_min      1.6842
_cell_measurement_wavelength     0.71073
_cell_volume                     4333.58(16)
_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   23.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1517  -99.0000  120.0000 41

  2 omega    1.00   98.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6986   57.0000  120.0000 97

  3 omega   71.00  112.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6986  178.0000    0.0000 41

  4 omega  -53.00   39.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6986  -38.0000 -120.0000 92

  5 omega  -51.00   47.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6986  -38.0000  -30.0000 98

  6 omega   72.00  108.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6986  178.0000   90.0000 36

  7 omega   24.00  100.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6986   77.0000 -180.0000 76

  8 omega  -22.00   57.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6986   38.0000    0.0000 79

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0175038
_diffrn_orient_matrix_UB_12      -0.0532241
_diffrn_orient_matrix_UB_13      0.0053826
_diffrn_orient_matrix_UB_21      0.0040272
_diffrn_orient_matrix_UB_22      -0.0247044
_diffrn_orient_matrix_UB_23      -0.0230403
_diffrn_orient_matrix_UB_31      0.0591009
_diffrn_orient_matrix_UB_32      0.0027859
_diffrn_orient_matrix_UB_33      0.0047539
_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  0.0232
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            34946
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         1.68
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    16.822
_exptl_absorpt_correction_T_max  0.496
_exptl_absorpt_correction_T_min  0.178
_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            lightblue
_exptl_crystal_density_diffrn    3.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3893
_exptl_crystal_size_max          0.2066
_exptl_crystal_size_mid          0.0748
_exptl_crystal_size_min          0.0529
_refine_diff_density_max         6.115
_refine_diff_density_min         -6.737
_refine_diff_density_rms         0.422
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.273
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         17052
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.272
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.086
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+532.2190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1732
_refine_ls_wR_factor_ref         0.1763
_reflns_number_gt                15317
_reflns_number_total             17052
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            s4.cif
_cod_data_source_block           2
_cod_original_cell_volume        4333.58(15)
_cod_original_formula_sum        'C46 H62 Cu3.50 N19 O59 Si W12'
_cod_database_code               1520323