A Novel Dimeric Ni-Substituted β-Keggin Silicotungstate: Structure and Magnetic Properties of K12[{β-SiNi2W10O36(OH)2(H2O)}2].20H2O
Ulrich Kortz; Yves P. Jeannin; André Tézé; Gilbert Hervé; Samih Isber; Inorganic Chemistry 38 (1999) 3670–3675; doi:10.1021/ic990008d

data_4322177
_publ_contact_author
;
KORTZ U.                 
Department of Chemistry
American University of Beirut
Bliss street, POB 11-0236
Beirut, Lebanon
;
_publ_contact_author_email       ' ulrich.kortz@aub.edu.lb'
_publ_contact_author_fax         ' 961 1 74 44 61'
_publ_contact_author_phone       ' 961 3 77 64 39'
_publ_section_title
;
 A Novel Dimeric Ni-Substituted \b-Keggin Silicotungstate: Structure and
 Magnetic Properties of K12[{\b-SiNi2W10O36(OH)2(H2O)}2].20H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3670
_journal_page_last               3675
_journal_paper_doi               10.1021/ic990008d
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source
;
'synthesis described in the paper'
;
_chemical_formula_moiety
' (K 1+)12 (H4 Ni2 W10 Si1 O39 6-)2  20(H2 O) '
_chemical_formula_sum            'H48 K12 Ni4 O98 Si2 W20'
_chemical_formula_weight         6053.43
_chemical_name_systematic
;
'bis-\m-hydroxo-bis[aquahydroxodotriacontaoxo-\m12-(tetraoxosilicato)-'
'(\b-4,10-dinickeldecatungsten)ate](12-)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   no
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 99.62(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.701(4)
_cell_length_b                   24.447(11)
_cell_length_c                   13.995(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      12.08
_cell_measurement_theta_min      11.96
_cell_volume                     4622(3)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
;
RC85 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       '  Enraf-nonius CAD4 '
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.11
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8704
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.00
_diffrn_standards_decay_%        13.29
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    26.81
_exptl_absorpt_correction_T_max  1.45
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   DIFABS
_exptl_absorpt_process_details   'refined from delta-F'
_exptl_crystal_colour            ' green '
_exptl_crystal_density_diffrn    4.31
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' box '
_exptl_crystal_F_000             5213.42
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         3.66
_refine_diff_density_min         -2.52
_refine_ls_extinction_coef       27.5(15)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   9.4654
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         5390
_refine_ls_R_factor_obs          0.0460
_refine_ls_shift/esd_max         0.004737
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      ?
_refine_ls_wR_factor_obs         0.0542
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_observed          5390
_reflns_number_total             8119
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ic990008d.cif
_cod_data_source_block           H48W20Ni4Si2K12O98
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'no' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct_Methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' H48 W20 Ni4 Si2 K12 O98 '
_cod_database_code               4322177