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_4334159
_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         'C32 H40 Cu2 N8 O40 Si1 W12'
_chemical_formula_sum            'C32 H40 Cu2 N8 O40 Si W12'
_chemical_formula_weight         3538.09
_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             2012-11-10T09:41:55-00:00
_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                   19.2671(3)
_cell_length_b                   23.9764(4)
_cell_length_c                   26.6345(5)
_cell_measurement_reflns_used    22344
_cell_measurement_temperature    423(2)
_cell_measurement_theta_max      28.2808
_cell_measurement_theta_min      1.525
_cell_measurement_wavelength     0.71073
_cell_volume                     12304.0(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega   -9.00   21.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1517  -99.0000   90.0000 30

  2 omega  -91.00    5.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1517  -57.0000  150.0000 96

  3 omega    6.00   36.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6986  -23.0000  -29.0000 30

  4 omega  -18.00   15.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1517  -99.0000   30.0000 33

  5 omega -114.00  -38.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1517 -178.0000  150.0000 76

  6 omega  -19.00   21.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1517  -99.0000  -30.0000 40

  7 omega   62.00   93.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6986  178.0000 -150.0000 31

  8 omega  -31.00   27.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6986  -57.0000  -60.0000 58

  9 omega   36.00  108.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6986   19.0000  120.0000 72

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0067089
_diffrn_orient_matrix_UB_12      -0.0176122
_diffrn_orient_matrix_UB_13      0.0208179
_diffrn_orient_matrix_UB_21      0.0086509
_diffrn_orient_matrix_UB_22      -0.0220421
_diffrn_orient_matrix_UB_23      -0.0166258
_diffrn_orient_matrix_UB_31      0.0350972
_diffrn_orient_matrix_UB_32      0.0087678
_diffrn_orient_matrix_UB_33      0.0001022
_diffrn_radiation_monochromator  'Multilayer optics'
_diffrn_radiation_source         'Nova (Cu) x-ray micro-source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            84001
_diffrn_reflns_theta_full        27
_diffrn_reflns_theta_max         27
_diffrn_reflns_theta_min         1.53
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    23.129
_exptl_absorpt_correction_T_max  0.509
_exptl_absorpt_correction_T_min  0.046
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
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    3.82
_exptl_crystal_description       prism
_exptl_crystal_F_000             12544
_exptl_crystal_size_max          0.2692
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.0296
_refine_diff_density_max         3.036
_refine_diff_density_min         -2.945
_refine_diff_density_rms         0.337
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.31
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         13367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.31
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+754.8865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1334
_reflns_number_gt                11442
_reflns_number_total             13367
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302499f_si_002_3.cif
_cod_data_source_block           1a
_cod_database_code               4334159