Synthesis, Magnetism, and Electrochemistry of the Ni14- and Ni5-Containing Heteropolytungstates [Ni14(OH)6(H2O)10(HPO4)4(P2W15O56)4]34- and [Ni5(OH)4(H2O)4(β-GeW9O34)(β-GeW8O30(OH))]13-
Masooma Ibrahim; Yixian Xiang; Bassem S. Bassil; Yanhua Lan; Annie K. Powell; Pedro de Oliveira; Bineta Keita; Ulrich Kortz; Inorganic Chemistry 52 (2013) 8399–8408; doi:10.1021/ic400943j

data_4335572
_publ_contact_author_address
;
Jacobs University, School of Engineering and Science, 
P.O. Box 750 561, 28725 Bremen, Germany
;
_publ_contact_author_email       u.kortz@jacobs-university.de
_publ_contact_author_fax         '+49 421 200 3229'
_publ_contact_author_name        'Ulrich Kortz '
_publ_contact_author_phone       '+49 421 200 3235'
_publ_section_title
;
 Synthesis, Magnetism, and Electrochemistry of the Ni14- and
 Ni5-Containing Heteropolytungstates
 [Ni14(OH)6(H2O)10(HPO4)4(P2W15O56)4]34- and
 [Ni5(OH)4(H2O)4(\b-GeW9O34)(\b-GeW8O30(OH))]13-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8399
_journal_page_last               8408
_journal_paper_doi               10.1021/ic400943j
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'H248 Na32.5 Ni14 O365 P12 Rb1.5 W60'
_chemical_formula_weight         19189.94
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.601(3)
_cell_angle_beta                 92.688(2)
_cell_angle_gamma                90.439(2)
_cell_formula_units_Z            2
_cell_length_a                   15.6062(5)
_cell_length_b                   24.9652(9)
_cell_length_c                   49.490(2)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.91
_cell_measurement_theta_min      2.78
_cell_volume                     19259.0(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.1449
_diffrn_reflns_av_sigmaI/netI    0.1025
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            271892
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    18.888
_exptl_absorpt_correction_T_max  0.2200
_exptl_absorpt_correction_T_min  0.0494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    3.309
_exptl_crystal_description       rod
_exptl_crystal_F_000             17186
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.785
_refine_diff_density_min         -2.963
_refine_diff_density_rms         0.401
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2212
_refine_ls_number_reflns         39724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1807
_refine_ls_R_factor_gt           0.1067
_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^)+(0.0460P)^2^+6000.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2262
_refine_ls_wR_factor_ref         0.2772
_reflns_number_gt                23300
_reflns_number_total             39724
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400943j_si_002.cif
_cod_data_source_block           try
_cod_original_cell_volume        19258.9(12)
_cod_original_formula_sum        'H248 Na32.50 Ni14 O365 P12 Rb1.50 W60'
_cod_database_code               4335572