Unsymmetrical surface modification of a heteropolyoxotungstate via in-situ generation of monomeric and dimeric copper(II) species.
Ritchie, Chris; Burkholder, Eric; Kögerler, Paul; Cronin, Leroy; Dalton transactions (Cambridge, England : 2003)  (2006) 1712–1714; doi:10.1039/b518316b

data_7007147
_publ_section_title
;
 Unsymmetrical surface modification of a heteropolyoxotungstate via
 in-situ generation of monomeric and dimeric copper(II) species.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1712
_journal_page_last               1714
_journal_paper_doi               10.1039/b518316b
_journal_year                    2006
_chemical_formula_sum            'C52 H54 Cu3 N8 O44 Si W12'
_chemical_formula_weight         3919.94
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.888(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0816(19)
_cell_length_b                   21.908(3)
_cell_length_c                   25.635(3)
_cell_measurement_reflns_used    19095
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      1.24
_cell_volume                     7677.2(17)
_computing_cell_refinement       'Bruker-AXS APEX2 v2'
_computing_data_collection       'Bruker-AXS APEX2 v2'
_computing_data_reduction        'Bruker-AXS APEX2 v2'
_computing_molecular_graphics    'Bruker-AXS APEX2 v2'
_computing_publication_material  'Bruker-AXS APEX2 v2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker-AXS X8 APEX II'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0791
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            88894
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.24
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    18.823
_exptl_absorpt_correction_T_max  0.2547
_exptl_absorpt_correction_T_min  0.0705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    3.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7052
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.413
_refine_diff_density_min         -2.360
_refine_diff_density_rms         0.367
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1091
_refine_ls_number_reflns         19095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.056
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+34.5251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0930
_reflns_number_gt                13633
_reflns_number_total             19095
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b518316b.txt
_cod_data_source_block           p21-n
_cod_original_cell_volume        7677.2(18)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7007147