Reversible Dehydration in Polyoxometalate-Based Hybrid Compounds: A Study of Single-Crystal to Single-Crystal Transformations in Keggin-Type Germanotungstates Decorated with Copper(II) Complexes of Tetradentate N-Donor Ligands
Iturrospe, Amaia; San Felices, Leire; Reinoso, Santiago; Artetxe, Beñat; Lezama, Luis; Gutiérrez-Zorrilla, Juan M.; Crystal Growth & Design 14 (2014) 2318–; doi:10.1021/cg500027f

data_4510249
_publ_section_title
;
 Reversible Dehydration in Polyoxometalate-Based Hybrid Compounds: A Study
 of Single-Crystal to Single-Crystal Transformations in Keggin-Type
 Germanotungstates Decorated with Copper(II) Complexes of Tetradentate
 N-Donor Ligands
;
_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2318
_journal_paper_doi               10.1021/cg500027f
_journal_volume                  14
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C34 H52 Cu2 Ge N8 O42  W12, 3(H2 O)'
_chemical_formula_sum            'C34 H58 Cu2 Ge N8 O45 W12'
_chemical_formula_weight         3704.66
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-12-27T16:02:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.305(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0268(3)
_cell_length_b                   12.1249(3)
_cell_length_c                   24.7245(6)
_cell_measurement_reflns_used    12727
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3264
_cell_measurement_theta_min      1.6539
_cell_measurement_wavelength     0.71073
_cell_volume                     3285.64(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  -92.00   -6.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3079  -57.0000   60.0000 86

  2 omega    8.00   93.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8548   57.0000    0.0000 85

  3 omega  -47.00   59.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8548  -57.0000 -150.0000 106

  4 omega  -59.00  -32.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3079   77.0000   90.0000 27

  5 omega  -17.00   26.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3079  -99.0000  -60.0000 43

  6 omega   24.00  104.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8548  -19.0000    0.0000 80

  7 omega   35.00  110.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8548  178.0000  -90.0000 75

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0401275
_diffrn_orient_matrix_UB_12      0.0125399
_diffrn_orient_matrix_UB_13      -0.0196749
_diffrn_orient_matrix_UB_21      -0.0464826
_diffrn_orient_matrix_UB_22      0.0316926
_diffrn_orient_matrix_UB_23      -0.0147982
_diffrn_orient_matrix_UB_31      0.0204117
_diffrn_orient_matrix_UB_32      0.0475942
_diffrn_orient_matrix_UB_33      0.0150329
_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  0.0385
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22415
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         1.66
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    22.095
_exptl_absorpt_correction_T_max  0.208
_exptl_absorpt_correction_T_min  0.052
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
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            orange
_exptl_crystal_density_diffrn    3.745
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.1304
_exptl_crystal_size_min          0.0772
_refine_diff_density_max         1.822
_refine_diff_density_min         -2.654
_refine_diff_density_rms         0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6460
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.221
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0137P)^2^+80.1410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0859
_reflns_number_gt                5916
_reflns_number_total             6460
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg500027f_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4510247--4510251.cif.'
_cod_original_cell_volume        3285.64(14)
_cod_original_formula_sum        'C34 H58 Cu2 Ge N8 O45  W12'
_cod_database_code               4510249