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_4510250
_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 H48 Cu2 Ge1 N8 O40 W12'
_chemical_formula_sum            'C34 H48 Cu2 Ge N8 O40 W12'
_chemical_formula_weight         3614.67
_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             2013-12-27T16:05:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 97.9366(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8619(2)
_cell_length_b                   11.9467(2)
_cell_length_c                   24.0621(5)
_cell_measurement_reflns_used    6487
_cell_measurement_temperature    423(2)
_cell_measurement_theta_max      74.1590
_cell_measurement_theta_min      4.1050
_cell_measurement_wavelength     1.54184
_cell_volume                     3092.48(10)
_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      423(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2012
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega -115.00  -16.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5756  -38.0000 -120.0000 99

  2 omega -110.00  -82.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5756  -87.0000   33.0000 28

  3 omega  -73.00   31.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5756   77.0000   30.0000 104

  4 omega   36.00   63.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000 -180.0000 27

  5 omega   37.00   77.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000  150.0000 40

  6 omega   31.00   59.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000  -60.0000 28

  7 omega   39.00   66.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000    0.0000 27

  8 omega   39.00   76.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000  -30.0000 37

  9 omega   31.00   59.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000  120.0000 28

 10 omega   37.00  122.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609 -125.0000  150.0000 85

 11 omega   34.00   62.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000   60.0000 28

 12 omega   47.00  151.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   15.0000  -30.0000 104

 13 omega   78.00  132.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   30.0000   90.0000 54

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1413236000
_diffrn_orient_matrix_UB_12      -0.0160675000
_diffrn_orient_matrix_UB_13      -0.0020691000
_diffrn_orient_matrix_UB_21      -0.0057502000
_diffrn_orient_matrix_UB_22      -0.0568694000
_diffrn_orient_matrix_UB_23      -0.0577541000
_diffrn_orient_matrix_UB_31      0.0227896000
_diffrn_orient_matrix_UB_32      -0.1146097000
_diffrn_orient_matrix_UB_33      0.0289189000
_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  0.0358
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11512
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         4.14
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    42.126
_exptl_absorpt_correction_T_max  0.623
_exptl_absorpt_correction_T_min  0.225
_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. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.882
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3212
_exptl_crystal_size_max          0.1171
_exptl_crystal_size_mid          0.0881
_exptl_crystal_size_min          0.0243
_refine_diff_density_max         3.113
_refine_diff_density_min         -2.129
_refine_diff_density_rms         0.296
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5505
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+80.3115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1321
_reflns_number_gt                5066
_reflns_number_total             5505
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg500027f_si_002.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 4510247--4510251.cif.'
_cod_original_cell_volume        3092.51(10)
_cod_database_code               4510250