The first crystallographic observation of up to the third hydration layer of Cu(II) ion in an unusual ‘water-cation layer’ templated by an Anderson polyoxometallate
Ali, Mahammad; Dutta, Daipayan; Biswas, Surajit; Marek, Jaromir; Jana, Atish Dipankar; CrystEngComm 11 (2009) 2608–; doi:10.1039/b910732k

data_7201411
_publ_section_title
;
 The first crystallographic observation of up to the third hydration
 layer of Cu(II) ion in an unusual &#x2018;water-cation layer&#x2019;
 templated by an Anderson polyoxometallate
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              2608
_journal_paper_doi               10.1039/b910732k
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety
'2(C36 H24 Cu N6), Mo6 O24 Te, Cu H12 O6, 27(H2 O) '
_chemical_formula_sum            'C72 H114 Cu3 Mo6 N12 O57 Te'
_chemical_formula_weight         2953.61
_space_group_IT_number           163
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   17.2848(6)
_cell_length_b                   17.2848(6)
_cell_length_c                   19.2560(11)
_cell_measurement_reflns_used    25262
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.1316
_cell_measurement_theta_min      2.7176
_cell_volume                     4982.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.4353
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'KUMA KM4 + CCD'
_diffrn_measurement_method       'rotation method, \w--scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0079
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37123
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    1.754
_exptl_absorpt_correction_T_max  1.04437
_exptl_absorpt_correction_T_min  0.94010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
(compiled Mar 23 2006,23:39:28)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2954
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.645
_refine_diff_density_min         -3.151
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         2951
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+45.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1351
_reflns_number_gt                2580
_reflns_number_total             2951
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b910732k.txt
_cod_data_source_block           in72
_cod_database_code               7201411