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_4332083
_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            'H53 K6 Na4 Ni6 O95.5 Si2 W18'
_chemical_formula_weight         5625.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 101.22(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.580(4)
_cell_length_b                   22.550(5)
_cell_length_c                   22.521(5)
_cell_measurement_reflns_used    71788
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.99
_cell_volume                     9754(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1214
_diffrn_reflns_av_sigmaI/netI    0.1036
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            71788
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    22.669
_exptl_absorpt_correction_T_max  0.0669
_exptl_absorpt_correction_T_min  0.0466
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.831
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10012
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.26
_refine_diff_density_max         5.183
_refine_diff_density_min         -2.353
_refine_diff_density_rms         0.487
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1231
_refine_ls_number_reflns         17139
_refine_ls_number_restraints     672
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0720P)^2^+129.7468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1643
_reflns_number_gt                10875
_reflns_number_total             17139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic052149nsup2.cif
_cod_data_source_block           zzm2
_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 

2024-01-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'H212 K24 Na16 Ni24 O382 Si8 W72'
_cod_original_formula_weight         22502.90
_cod_original_formula_units_Z            1
_cod_original_cell_volume        9753(3)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4332083