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_4510251
_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
'C17 H24 Cu N4 O40 Ge W12, C17 H26 Cu N4 O, 8(H2O)'
_chemical_formula_sum            'C34 H66 Cu2 Ge N8 O49 W12'
_chemical_formula_weight         3776.82
_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             2013-12-27T17:04:26-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                79.433(2)
_cell_angle_beta                 78.0316(18)
_cell_angle_gamma                76.0427(18)
_cell_formula_units_Z            2
_cell_length_a                   12.7695(2)
_cell_length_b                   13.0603(3)
_cell_length_c                   21.2588(5)
_cell_measurement_reflns_used    10964
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.0500
_cell_measurement_theta_min      3.4760
_cell_measurement_wavelength     1.54184
_cell_volume                     3332.56(13)
_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 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  -85.00   38.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.5756   19.0000  -90.0000 123

  2 omega  -67.00   30.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.5756   38.0000    0.0000 97

  3 omega  -33.00   63.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5756  -57.0000   60.0000 96

  4 omega   43.00   92.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5756 -125.0000   30.0000 49

  5 omega   42.00   79.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5756 -125.0000 -120.0000 37

  6 omega   88.00  120.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   45.0000  -30.0000 32

  7 omega   38.00   66.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000    0.0000 28

  8 omega   35.00   77.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000  -60.0000 42

  9 omega   48.00  108.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000   30.0000 60

 10 omega   47.00  158.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   15.0000 -180.0000 111

 11 omega   81.00  152.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   45.0000 -150.0000 71

 12 omega   25.00  109.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000 -180.0000 84

 13 omega   35.00   64.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000 -120.0000 29

 14 omega   49.00  126.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -77.0000 -120.0000 77

 15 omega  108.00  136.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -61.0000   90.0000 28

 16 omega   42.00   67.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000    0.0000 25

 17 omega   33.00   68.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000 -150.0000 35

 18 omega   29.00  109.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000   90.0000 80

 19 omega   30.00   59.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000  -30.0000 29

 20 omega   81.00  146.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   61.0000 -120.0000 65

 21 omega   35.00   75.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -61.0000   90.0000 40

 22 omega   97.00  122.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609 -125.0000  -30.0000 25

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0032349000
_diffrn_orient_matrix_UB_12      -0.0866689000
_diffrn_orient_matrix_UB_13      0.0598274000
_diffrn_orient_matrix_UB_21      -0.0073227000
_diffrn_orient_matrix_UB_22      0.0837527000
_diffrn_orient_matrix_UB_23      0.0440742000
_diffrn_orient_matrix_UB_31      -0.1259184000
_diffrn_orient_matrix_UB_32      0.0233443000
_diffrn_orient_matrix_UB_33      0.0087201000
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23435
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.52
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    39.256
_exptl_absorpt_correction_T_max  0.398
_exptl_absorpt_correction_T_min  0.049
_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            blue
_exptl_crystal_density_diffrn    3.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.1575
_exptl_crystal_size_mid          0.0989
_exptl_crystal_size_min          0.0327
_refine_diff_density_max         3.742
_refine_diff_density_min         -3.845
_refine_diff_density_rms         0.415
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         11880
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0704
_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^)+(0.1465P)^2^+17.9009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1968
_refine_ls_wR_factor_ref         0.2200
_reflns_number_gt                9565
_reflns_number_total             11880
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg500027f_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4510247--4510251.cif.'
_cod_original_cell_volume        3332.55(13)
_cod_database_code               4510251