Synthesis, Characterization, and Crystal Structures of Two Novel High-Nuclear Nickel-Substituted Dimeric Polyoxometalates
Zhang, Zhiming; Li, Yangguang; Wang, Enbo; Wang, Xinlong; Qin, Chao; An, Haiyan; Inorganic Chemistry 45 (2006) 4313–4315; doi:10.1021/ic052149n

data_4332082
_publ_section_title
;
 Synthesis, Characterization, and Crystal Structures of Two Novel
 High-Nuclear Nickel-Substituted Dimeric Polyoxometalates
;
_journal_issue                   11
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4313
_journal_page_last               4315
_journal_paper_doi               10.1021/ic052149n
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C3 H58 K Na9 Ni7 O108 Si2 W19'
_chemical_formula_weight         6028.80
_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                113.35(3)
_cell_angle_beta                 94.50(3)
_cell_angle_gamma                92.09(3)
_cell_formula_units_Z            2
_cell_length_a                   12.462(3)
_cell_length_b                   20.616(4)
_cell_length_c                   23.966(5)
_cell_measurement_reflns_used    42202
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.00
_cell_volume                     5620(2)
_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 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotation anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0985
_diffrn_reflns_av_sigmaI/netI    0.1238
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            42202
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    20.699
_exptl_absorpt_correction_T_max  0.0786
_exptl_absorpt_correction_T_min  0.0627
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5376
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         4.180
_refine_diff_density_min         -3.501
_refine_diff_density_rms         0.511
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1384
_refine_ls_number_reflns         19105
_refine_ls_number_restraints     780
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0738
_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^)+(0.0873P)^2^+272.8875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1829
_refine_ls_wR_factor_ref         0.2159
_reflns_number_gt                11934
_reflns_number_total             19105
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic052149nsup1.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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        5620.4(19)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4332082