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_4334158
_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         'C34 H52 Cu2 N8 O42 Si W12, 3(H2 O)'
_chemical_formula_sum            'C34 H58 Cu2 N8 O45 Si W12'
_chemical_formula_weight         3660.11
_chemical_name_systematic
;
 ?
;
_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             2012-11-15T10:48:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.104(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9853(2)
_cell_length_b                   12.0992(3)
_cell_length_c                   24.7010(6)
_cell_measurement_reflns_used    10289
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.6378
_cell_measurement_theta_min      2.8934
_cell_measurement_wavelength     0.71073
_cell_volume                     3264.48(13)
_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  -99.00   14.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.3955  -77.0000  -60.0000 113

  2 omega  -55.00   65.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3330  -77.0000   60.0000 120

  3 omega   55.00   86.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3330   77.0000  -30.0000 31

  4 omega -108.00    3.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.3955  -77.0000 -180.0000 111

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0620157
_diffrn_orient_matrix_UB_12      -0.0142148
_diffrn_orient_matrix_UB_13      -0.0079289
_diffrn_orient_matrix_UB_21      -0.0147796
_diffrn_orient_matrix_UB_22      0.0123173
_diffrn_orient_matrix_UB_23      0.0265814
_diffrn_orient_matrix_UB_31      -0.0126115
_diffrn_orient_matrix_UB_32      0.055505
_diffrn_orient_matrix_UB_33      -0.0079861
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23034
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.9
_diffrn_source_current           40
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    21.805
_exptl_absorpt_correction_T_max  0.554
_exptl_absorpt_correction_T_min  0.138
_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            Brown
_exptl_crystal_density_diffrn    3.713
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             3256
_exptl_crystal_size_max          0.1314
_exptl_crystal_size_mid          0.1094
_exptl_crystal_size_min          0.028
_refine_diff_density_max         2.811
_refine_diff_density_min         -2.531
_refine_diff_density_rms         0.318
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         8067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.041
_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^)+(0.0355P)^2^+13.8571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0847
_reflns_number_gt                6449
_reflns_number_total             8067
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302499f_si_002_2.cif
_cod_data_source_block           2
_cod_database_code               4334158