Tris(piperazinediium) phosphatododecamolybo(V,VI)phosphate
Lu, Yu-kun; Xu, Ji-qing; Yu, Hai-hui; Acta Crystallographica Section E 66 (2010) m263–m264; doi:10.1107/S1600536810002473

data_2225366
_publ_section_title
;
 Tris(piperazinediium) phosphatododecamolybo(V,VI)phosphate
;
_journal_coeditor_code           SI2235
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m263
_journal_page_last               m264
_journal_paper_doi               10.1107/S1600536810002473
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '(C4 H12 N2)3 [P Mo12 O40]'
_chemical_formula_moiety         '3(C4 H12 N2 2+, Mo12 O40 P 6-'
_chemical_formula_sum            'C12 H36 Mo12 N6 O40 P'
_chemical_formula_weight         2086.72
_chemical_name_systematic
;
Tris(piperazinediium) phosphatododecamolybdo(V,VI)phosphate
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   17.890(3)
_cell_length_b                   17.890(3)
_cell_length_c                   23.600(6)
_cell_measurement_reflns_used    7741
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.91
_cell_measurement_theta_min      2.28
_cell_volume                     6541(2)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'RAPID-AUTO (Rigaku, 1998)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       '\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  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11291
_diffrn_reflns_theta_full        25.90
_diffrn_reflns_theta_max         25.90
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.485
_exptl_absorpt_correction_T_max  0.682
_exptl_absorpt_correction_T_min  0.517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             5934
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.609
_refine_ls_extinction_coef       0.000246(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+29.6980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0528
_reflns_number_gt                1363
_reflns_number_total             1413
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            si2235.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               2225366
_cod_database_fobs_code          2225366