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_4510248
_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         'C32 H44 Cu2 Ge1 N8 O40 W12'
_chemical_formula_sum            'C32 H44 Cu2 Ge N8 O40 W12'
_chemical_formula_weight         3586.53
_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             2013-12-27T15:56:06-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.3723(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.46769(14)
_cell_length_b                   22.5699(3)
_cell_length_c                   25.3959(3)
_cell_measurement_reflns_used    9526
_cell_measurement_temperature    423(2)
_cell_measurement_theta_max      25.6770
_cell_measurement_theta_min      1.9730
_cell_measurement_wavelength     0.71073
_cell_volume                     6420.43(14)
_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 16.2439
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega   74.00  114.50   0.7500    7.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  178.0000 -120.0000 54

  2 omega  -36.00   86.25   0.7500    7.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767   19.0000  -90.0000 163

  3 omega  -15.00   15.00   0.7500    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  -99.0000  150.0000 40

  4 omega   60.00  115.50   0.7500    7.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  178.0000    0.0000 74

  5 omega   40.00  113.50   0.7500    7.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  178.0000  120.0000 98

  6 omega  -26.00   61.00   0.7500    7.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  -57.0000   60.0000 116

  7 omega  -39.00   31.50   0.7500    7.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  -57.0000  -60.0000 94

  8 omega  -51.00  -15.75   0.7500    7.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  -37.0000  -90.0000 47

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0050440000
_diffrn_orient_matrix_UB_12      -0.0114492000
_diffrn_orient_matrix_UB_13      -0.0264183000
_diffrn_orient_matrix_UB_21      0.0085182000
_diffrn_orient_matrix_UB_22      -0.0291094000
_diffrn_orient_matrix_UB_23      0.0106307000
_diffrn_orient_matrix_UB_31      -0.0625325000
_diffrn_orient_matrix_UB_32      -0.0030398000
_diffrn_orient_matrix_UB_33      -0.0026188000
_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  0.0577
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            43638
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.64
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    22.602
_exptl_absorpt_correction_T_max  0.183
_exptl_absorpt_correction_T_min  0.055
_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    3.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6360
_exptl_crystal_size_max          0.2629
_exptl_crystal_size_mid          0.1400
_exptl_crystal_size_min          0.0959
_refine_diff_density_max         1.654
_refine_diff_density_min         -1.468
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         11313
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0317P)^2^+44.1748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                8503
_reflns_number_total             11313
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg500027f_si_002.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 4510247--4510251.cif.'
_cod_original_cell_volume        6420.44(15)
_cod_database_code               4510248