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_1520325
_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 O18, C24 H16 Cu2 N4 O48 Si W12'
_chemical_formula_sum            'C76 H72 Cu6 N24 O64 Si W12'
_chemical_formula_weight         4961.11
_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             2014-04-08T11:17:16-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                104.292(2)
_cell_angle_beta                 91.168(2)
_cell_angle_gamma                100.599(2)
_cell_formula_units_Z            1
_cell_length_a                   11.6039(3)
_cell_length_b                   15.9379(5)
_cell_length_c                   15.9984(5)
_cell_measurement_reflns_used    9109
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.049
_cell_measurement_theta_min      2.102
_cell_measurement_wavelength     0.71073
_cell_volume                     2811.55(15)
_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   84.00  112.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  178.0000 -180.0000 28

  2 omega    5.00   94.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329   57.0000 -150.0000 89

  3 omega   72.00  113.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  178.0000   90.0000 41

  4 omega  -47.00   31.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  -38.0000  -30.0000 78

  5 omega  -44.00   21.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  -57.0000   60.0000 65

  6 omega  -13.00   34.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  -99.0000  150.0000 47

  7 omega   50.00   76.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  -99.0000  150.0000 26

  8 omega    6.00  107.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329   77.0000  -90.0000 101

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.020153
_diffrn_orient_matrix_UB_12      -0.0355363
_diffrn_orient_matrix_UB_13      -0.0279242
_diffrn_orient_matrix_UB_21      -0.0113232
_diffrn_orient_matrix_UB_22      -0.0251133
_diffrn_orient_matrix_UB_23      0.0309139
_diffrn_orient_matrix_UB_31      -0.0578916
_diffrn_orient_matrix_UB_32      -0.017293
_diffrn_orient_matrix_UB_33      -0.0191786
_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  0.0206
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19291
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         1.79
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    13.447
_exptl_absorpt_correction_T_max  0.61
_exptl_absorpt_correction_T_min  0.475
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
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    2.930
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2284
_exptl_crystal_size_max          0.0737
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.0447
_refine_diff_density_max         1.541
_refine_diff_density_min         -1.982
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.363
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         11071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.363
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0461
_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^+42.5066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.083
_refine_ls_wR_factor_ref         0.0848
_reflns_number_gt                10022
_reflns_number_total             11071
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            s3.cif
_cod_data_source_block           1a
_cod_original_cell_volume        2811.55(14)
_cod_database_code               1520325