Tetraammonium hexahydrogen hexamolybdonickelate(II) tetrahydrate, (NH~4~)~4~[H~6~NiMo~6~O~24~]·4H~2~O
Lee, Uk; Joo, Hea-Chung; Kwon, Jae-Sam; Acta Crystallographica Section E 58 (2002) i6–i8; doi:10.1107/S1600536801021109

data_2200815
_publ_section_title
;
 Tetraammonium hexahydrogen hexamolybdonickelate(II) tetrahydrate,
 (NH~4~)~4~[H~6~NiMo~6~O~24~]&#x00B7;4H~2~O
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i6
_journal_page_last               i8
_journal_paper_doi               10.1107/S1600536801021109
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '(N H4)4 [H6 Ni Mo6 O24], 4H2 O'
_chemical_formula_moiety         'H30 Mo6 N4 Ni O28'
_chemical_formula_structural     '(N H4)4 (H6 Ni Mo6 O24) (H2 O)4'
_chemical_formula_sum            'H30 Mo6 N4 Ni O28'
_chemical_formula_weight         1168.63
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.31(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.994(3)
_cell_length_b                   11.131(2)
_cell_length_c                   11.384(9)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      10.5
_cell_measurement_theta_min      9.5
_cell_volume                     1434.3(14)
_computing_cell_refinement       STADI4
_computing_data_collection       'STADI4 (Stoe & Cie, 1996)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1996)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL97-2 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97-2 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full .993
_diffrn_measured_fraction_theta_max .993
_diffrn_measurement_device_type  'Stoe STADI4'
_diffrn_measurement_method       \w/2-\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71069
_diffrn_reflns_av_R_equivalents  .0000
_diffrn_reflns_av_sigmaI/netI    .0405
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3290
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        4.9
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.288
_exptl_absorpt_correction_T_max  .8494
_exptl_absorpt_correction_T_min  .5422
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 1996)'
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    2.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'octagonal plate'
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .19
_exptl_crystal_size_min          .10
_refine_diff_density_max         1.112
_refine_diff_density_min         -1.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          .0813
_refine_ls_R_factor_gt           .0526
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0508P)^2^+13.3268P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .1170
_refine_ls_wR_factor_ref         .1371
_reflns_number_gt                2448
_reflns_number_total             3290
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br6038.cif
_cod_data_source_block           I
_cod_original_cell_volume        1434.3(12)
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               2200815
_cod_database_fobs_code          2200815