Synthesis, Structure, and Magnetic Properties of (n-Bu4N)2[{Ni(MeOH)2}2{Mo(NO)}2(μ3-OH)2(μ-OMe)4{Mo5O13(OMe)4(NO)}2], a New Type of Polyoxometalate Incorporating a Rhomb-like Cluster
Richard Villanneau; Anna Proust; Francis Robert; Pierre Veillet; Pierre Gouzerh; Inorganic Chemistry 38 (1999) 4981–4985; doi:10.1021/ic990480z

data_4322348
_publ_contact_author
;
Pr Pierre Gouzerh
Laboratoire de chimie Inorganique et Mat\'eriaux Mol\'eculaires, CNRS ESA 7071,
Universit\'e Pierre et Marie Curie, 4 place Jussieu, 75252 Paris Cedex 05
;
_publ_contact_author_email       ' pg@ccr.jussieu.fr '
_publ_contact_author_fax         ' 33 1 44 27 38 41 '
_publ_contact_author_phone       ' 33 1 44 27 30 34 '
_publ_section_title
;
 Synthesis, Structure, and Magnetic Properties of
 (n-Bu4N)2[{Ni(MeOH)2}2{Mo(NO)}2(\m3-OH)2(\m-OMe)4{Mo5O13(OMe)4(NO)}2], a
 New Type of Polyoxometalate Incorporating a Rhomb-like Cluster
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4981
_journal_page_last               4985
_journal_paper_doi               10.1021/ic990480z
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source
;

?

;
_chemical_formula_moiety         ' C48 H126 Mo12 Ni2 N6 O48 '
_chemical_formula_sum            'C48 H126 Mo12 N6 Ni2 O48'
_chemical_formula_weight         2824.16
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             98-09-18
_audit_creation_method           CRYSTALS
_cell_angle_alpha                90
_cell_angle_beta                 109.58(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.960(7)
_cell_length_b                   25.990(15)
_cell_length_c                   20.669(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      10.4
_cell_measurement_theta_min      10.0
_cell_volume                     9596(7)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
;

RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)

;
_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)

;
_computing_structure_solution
;
SHELXS86 (Sheldrick, 1986)
SIR92 (Giacovazzo et al, 1992)
;
_diffrn_ambient_temperature      295
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.16
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17754
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1
_diffrn_standards_decay_%        10
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.953
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.37
_exptl_absorpt_correction_type   DIFABS
_exptl_absorpt_process_details   'refined from delta-F'
_exptl_crystal_colour            ' deep green '
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_description       ' box '
_exptl_crystal_F_000             5640
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.01
_refine_diff_density_min         -1.02
_refine_ls_extinction_coef       No
_refine_ls_goodness_of_fit_obs   3.1584
_refine_ls_matrix_type
'block diagonal approximation to the full matrix'
_refine_ls_number_parameters     536
_refine_ls_number_reflns         4130
_refine_ls_R_factor_obs          0.0869
_refine_ls_shift/esd_max         0.053331
_refine_ls_structure_factor_coef F
_refine_ls_wR_factor_obs         0.0942
_reflns_limit_h_max              21
_reflns_limit_h_min              -22
_reflns_limit_k_max              30
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_observed          4130
_reflns_number_total             16389
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ic990480z.cif
_cod_data_source_block           CRYSTALS_cif
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C48 H126 Mo12 Ni2 N6 O48 '
_cod_database_code               4322348