Bis[4,4'-(propane-1,3-diyl)dipiperidinium] β-octamolybdate(VI)
Driss, Mohamed; Ksiksi, Rekaya; Ben Amor, Fatma; Zid, Mohamed Faouzi; Acta Crystallographica Section E 66 (2010) m533–m534; doi:10.1107/S1600536810013632

data_2225820
_publ_section_title
;
 Bis[4,4'-(propane-1,3-diyl)dipiperidinium] \b-octamolybdate(VI)
;
_journal_coeditor_code           DN2553
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m533
_journal_page_last               m534
_journal_paper_doi               10.1107/S1600536810013632
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '(C13 H28 N2)2 [Mo8 O26]'
_chemical_formula_moiety         '2C13 H28 N2 2+ , Mo8 O26 4-'
_chemical_formula_structural     '(C13 N2 H28)2 [Mo8 O26]'
_chemical_formula_sum            'C26 H56 Mo8 N4 O26'
_chemical_formula_weight         1608.26
_chemical_name_systematic
;
bis[4,4'-(propane-1,3-diyl)dipiperidinium] \b-octamolybdate(VI)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   23.975(5)
_cell_length_b                   13.935(4)
_cell_length_c                   13.647(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      12
_cell_volume                     4559(3)
_computing_cell_refinement
;
CAD-4 EXPRESS (Duisenberg, 1992; Mac\'i\<cek & Yordanov, 1992)
;
_computing_data_collection
;
CAD-4 EXPRESS (Duisenberg, 1992; Mac\'i\<cek & Yordanov, 1992)
;
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996), ORTEP-3 for Windows (Farrugia,
1997)
and DIAMOND (Brandenburg, 2001)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            5810
_diffrn_reflns_theta_full        26.98
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        4
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.216
_exptl_absorpt_correction_T_max  0.642
_exptl_absorpt_correction_T_min  0.556
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>,  1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.046
_refine_diff_density_min         -1.269
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0500P)^2^+9.1911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                3996
_reflns_number_total             4960
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn2553.cif
_cod_data_source_block           I
_cod_database_code               2225820
_cod_database_fobs_code          2225820