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_4510247
_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
'C16 H22 Cu Ge N4 O40 W12, C16 H24 Cu N4 O, 3.5(H2 O)'
_chemical_formula_sum            'C32 H53 Cu2 Ge N8 O44.5 W12'
_chemical_formula_weight         3667.69
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-12-27T16:55:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.4494(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.54269(8)
_cell_length_b                   22.41402(14)
_cell_length_c                   25.84917(16)
_cell_measurement_reflns_used    35707
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.1310
_cell_measurement_theta_min      2.6000
_cell_measurement_wavelength     1.54184
_cell_volume                     6530.40(8)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega -105.00  -14.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.5756  -38.0000   90.0000 91

  2 omega  -63.00  -13.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.5756  125.0000 -150.0000 50

  3 omega -114.00  -49.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.5756 -162.0000 -112.0000 65

  4 omega  -28.00   10.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5756  -38.0000   60.0000 38

  5 omega   29.00   67.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5756  -38.0000   60.0000 38

  6 omega   34.00  124.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -61.0000  -90.0000 90

  7 omega   94.00  151.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   45.0000  -30.0000 57

  8 omega   85.00  132.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   30.0000  150.0000 47

  9 omega   43.00   69.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000  120.0000 26

 10 omega   34.00   65.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000 -150.0000 31

 11 omega   89.00  154.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   61.0000    0.0000 65

 12 omega   34.00   60.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000  120.0000 26

 13 omega   77.00  146.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   77.0000   30.0000 69

 14 omega   50.00   77.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000 -180.0000 27

 15 omega   37.00   98.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5756 -125.0000   90.0000 61

 16 omega   11.00  118.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5756   77.0000 -150.0000 107

 17 omega   78.00  108.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5756   38.0000    0.0000 30

 18 omega   30.00   56.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5756   38.0000    0.0000 26

 19 omega   46.00  135.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -77.0000   30.0000 89

 20 omega   86.00  155.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   45.0000   90.0000 69

 21 omega   96.00  122.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609 -125.0000  150.0000 26

 22 omega   30.00   57.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000    0.0000 27

 23 omega   36.00   68.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000 -120.0000 32

 24 omega   79.00  115.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609 -117.0000   38.0000 36

 25 omega   51.00   91.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000 -180.0000 40

 26 omega   39.00   65.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000  150.0000 26

 27 omega   33.00   64.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000 -180.0000 31

 28 omega   47.00  104.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000  -90.0000 57

 29 omega   47.00  103.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000 -150.0000 56

 30 omega   34.00   69.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609 -125.0000  150.0000 35

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0718582000
_diffrn_orient_matrix_UB_12      0.0584179000
_diffrn_orient_matrix_UB_13      -0.0088914000
_diffrn_orient_matrix_UB_21      -0.0357646000
_diffrn_orient_matrix_UB_22      -0.0136480000
_diffrn_orient_matrix_UB_23      -0.0597393000
_diffrn_orient_matrix_UB_31      -0.1106198000
_diffrn_orient_matrix_UB_32      -0.0335658000
_diffrn_orient_matrix_UB_33      0.0087941000
_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  0.0665
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            53179
_diffrn_reflns_theta_full        69.00
_diffrn_reflns_theta_max         69.00
_diffrn_reflns_theta_min         2.64
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    39.970
_exptl_absorpt_correction_T_max  0.171
_exptl_absorpt_correction_T_min  0.023
_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    3.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6540
_exptl_crystal_size_max          0.2953
_exptl_crystal_size_mid          0.1306
_exptl_crystal_size_min          0.0988
_refine_diff_density_max         3.651
_refine_diff_density_min         -4.040
_refine_diff_density_rms         0.513
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         12121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0824P)^2^+159.5773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1456
_reflns_number_gt                11844
_reflns_number_total             12121
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg500027f_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4510247--4510251.cif.'
_cod_original_cell_volume        6530.40(7)
_cod_original_formula_sum        'C32 H53 Cu2 Ge N8 O44.50 W12'
_cod_database_code               4510247