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_4334161
_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             2012-11-14T17:39:00-00:00
_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                   19.4645(2)
_cell_length_b                   23.7700(3)
_cell_length_c                   26.6287(3)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3067
_cell_measurement_theta_min      1.5503
_cell_measurement_wavelength     0.71073
_cell_volume                     12320.3(2)
_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 16.2439
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_details
;
  1 omega  -76.00   44.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1517  -19.0000 -180.0000 120

  2 omega   71.00  113.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6986  178.0000    0.0000 42

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0312892
_diffrn_orient_matrix_UB_12      0.0012229
_diffrn_orient_matrix_UB_13      0.0136337
_diffrn_orient_matrix_UB_21      -0.0184228
_diffrn_orient_matrix_UB_22      0.0030195
_diffrn_orient_matrix_UB_23      -0.0228226
_diffrn_orient_matrix_UB_31      -0.0031538
_diffrn_orient_matrix_UB_32      -0.0296517
_diffrn_orient_matrix_UB_33      -0.0017346
_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  0.0391
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            28380
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         1.55
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    23.101
_exptl_absorpt_correction_T_max  0.359
_exptl_absorpt_correction_T_min  0.141
_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            'dark blue'
_exptl_crystal_density_diffrn    3.843
_exptl_crystal_description       prism
_exptl_crystal_F_000             12688
_exptl_crystal_size_max          0.3022
_exptl_crystal_size_mid          0.0872
_exptl_crystal_size_min          0.0457
_refine_diff_density_max         5.503
_refine_diff_density_min         -7.439
_refine_diff_density_rms         0.417
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         12559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.258
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.206
_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^+675.9532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.106
_refine_ls_wR_factor_ref         0.1101
_reflns_number_gt                10768
_reflns_number_total             12559
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic302499f_si_002_5.cif
_cod_data_source_block           1_rehydrated
_cod_database_code               4334161