Copper(II) Complexes of Tetradentate Pyridyl Ligands Supported on Keggin Polyoxometalates: Single-Crystal to Single-Crystal Transformations Promoted by Reversible Dehydration Processes
Amaia Iturrospe; Beñat Artetxe; Santiago Reinoso; Leire San Felices; Pablo Vitoria; Luis Lezama; Juan M. Gutiérrez-Zorrilla; Inorganic Chemistry 52 (2013) 3084–3093; doi:10.1021/ic302499f

data_4334157
_publ_section_title
;
 Copper(II) Complexes of Tetradentate Pyridyl Ligands Supported on Keggin
 Polyoxometalates: Single-Crystal to Single-Crystal Transformations
 Promoted by Reversible Dehydration Processes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3084
_journal_page_last               3093
_journal_paper_doi               10.1021/ic302499f
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C16 H22 Cu N4 O40 Si W12, C16 H24 Cu N4 O'
_chemical_formula_sum            'C32 H46 Cu2 N8 O41 Si W12'
_chemical_formula_weight         3559.99
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-11-09T15:22:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.3953(6)
_cell_length_b                   23.6891(7)
_cell_length_c                   26.5521(10)
_cell_measurement_reflns_used    19686
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.3313
_cell_measurement_theta_min      2.8597
_cell_measurement_wavelength     0.71073
_cell_volume                     12199.6(7)
_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 8.3504
_diffrn_detector_type            Sapphire2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   -9.00  112.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7729   77.0000  -30.0000 121

  2 omega   48.00  100.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7729   77.0000 -150.0000 52

  3 omega   -6.00   51.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7729   77.0000 -150.0000 57

  4 omega   98.00  124.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7729   77.0000 -150.0000 26

  5 omega   -8.00   24.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7729   77.0000   90.0000 32

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0316783
_diffrn_orient_matrix_UB_12      0.0068784
_diffrn_orient_matrix_UB_13      -0.0116966
_diffrn_orient_matrix_UB_21      -0.0150283
_diffrn_orient_matrix_UB_22      -0.0045754
_diffrn_orient_matrix_UB_23      -0.0239159
_diffrn_orient_matrix_UB_31      -0.0100285
_diffrn_orient_matrix_UB_32      0.0286972
_diffrn_orient_matrix_UB_33      -0.0010229
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0876
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            74996
_diffrn_reflns_theta_full        30.5
_diffrn_reflns_theta_max         30.5
_diffrn_reflns_theta_min         2.87
_diffrn_source_current           40
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    23.329
_exptl_absorpt_correction_T_max  0.58
_exptl_absorpt_correction_T_min  0.07
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
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            Blue
_exptl_crystal_density_diffrn    3.875
_exptl_crystal_description       prism
_exptl_crystal_F_000             12640
_exptl_crystal_size_max          0.1895
_exptl_crystal_size_mid          0.1077
_exptl_crystal_size_min          0.0232
_refine_diff_density_max         5.507
_refine_diff_density_min         -9.589
_refine_diff_density_rms         0.471
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         18587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.059
_refine_ls_shift/su_max          0.55
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+435.8749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1119
_reflns_number_gt                12734
_reflns_number_total             18587
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302499f_si_002_1.cif
_cod_data_source_block           1
_cod_database_code               4334157