Synthesis, Characterization, and Crystal Structures of Double-Cubane-Substituted and Asymmetric Penta-Ni-Substituted Dimeric Polyoxometalates
Zhang, Zhiming; Wang, Enbo; Qi, Yanfei; Li, Yangguang; Mao, Baodong; Su, Zhongmin; Crystal Growth & Design 7 (2007) 1305–; doi:10.1021/cg060868m

data_4504172
_publ_section_title
;
 Synthesis, Characterization, and Crystal Structures of
 Double-Cubane-Substituted and Asymmetric Penta-Ni-Substituted Dimeric
 Polyoxometalates
;
_journal_issue                   7
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1305
_journal_paper_doi               10.1021/cg060868m
_journal_volume                  7
_journal_year                    2007
_chemical_formula_sum            'H60 K12 Ni7 O95 Si2 W16'
_chemical_formula_weight         5458.43
_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                107.62(3)
_cell_angle_beta                 91.67(3)
_cell_angle_gamma                102.37(3)
_cell_formula_units_Z            1
_cell_length_a                   11.442(2)
_cell_length_b                   11.905(2)
_cell_length_c                   17.169(3)
_cell_measurement_reflns_used    16589
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3.07
_cell_volume                     2166.1(8)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.1459
_diffrn_reflns_av_sigmaI/netI    0.1971
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16589
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    23.357
_exptl_absorpt_correction_T_max  0.311
_exptl_absorpt_correction_T_min  0.153
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    4.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.147
_refine_diff_density_min         -3.000
_refine_diff_density_rms         0.688
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         7559
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1562
_refine_ls_R_factor_gt           0.0865
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1921
_refine_ls_wR_factor_ref         0.2339
_reflns_number_gt                4302
_reflns_number_total             7559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg060868msi20070205_100709.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               4504172