Combination of Lacunary Polyoxometalates and High-Nuclear Transition Metal Clusters under Hydrothermal Conditions. 3. Structure and Characterization of [Cu(enMe)2]2{[Cu(enMe)2(H2O)]2[Cu6(enMe)2(B-a-SiW9O34)2]}.4H2O
Shou-Tian Zheng; Da-Qiang Yuan; Jie Zhang; Guo-Yu Yang; Inorganic Chemistry 46 (2007) 4569–4574; doi:10.1021/ic070160c

data_4308154
_publ_section_title
;
Combination of Lacunary Polyoxometalates and High-Nuclear Transition Metal
Clusters under Hydrothermal Conditions. 3. Structure and Characterization
of [Cu(enMe)2]2{[Cu(enMe)2(H2O)]2[Cu6(enMe)2(B-a-SiW9O34)2]}.4H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4569
_journal_page_last               4574
_journal_paper_doi               10.1021/ic070160c
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C30 H112 Cu10 N20 O74 Si2 W18'
_chemical_formula_weight         5938.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.8340(10)
_cell_angle_beta                 110.7440(10)
_cell_angle_gamma                104.7110(10)
_cell_formula_units_Z            1
_cell_length_a                   12.5105(2)
_cell_length_b                   14.3710(2)
_cell_length_c                   17.2687(2)
_cell_measurement_temperature    273(2)
_cell_volume                     2704.58(7)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14633
_diffrn_reflns_theta_full        25.70
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.091
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2673
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.709
_refine_diff_density_min         -3.377
_refine_diff_density_rms         0.371
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         9956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+89.7160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1250
_reflns_number_gt                8387
_reflns_number_total             9956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070160c-file003.cif
_cod_data_source_block           1
_cod_original_cell_volume        2704.57(7)
_cod_database_code               4308154