Tetrakis[4-amino-<i>N</i>-(2-hydroxyethyl)pyridinium] hexacosaoxooctamolybdate
Ying Yan; Chuan-De Wu; Jiu-Hui Liu; Quan-Zheng Zhang; Can-Zhong Lu; Acta Crystallographica Section E 59 (2003) m102–m104; doi:10.1107/S1600536803003155

data_2201907
_publ_section_title
;
 Tetrakis[4-amino-<i>N</i>-(2-hydroxyethyl)pyridinium]
 hexacosaoxooctamolybdate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m102
_journal_page_last               m104
_journal_paper_doi               10.1107/S1600536803003155
_journal_volume                  59
_journal_year                    2003
_chemical_formula_moiety         '(C7 H11 N2 O)4 [Mo8 O26]'
_chemical_formula_sum            'C28 H44 Mo8 N8 O30'
_chemical_formula_weight         1740.23
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 111.150(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.657(3)
_cell_length_b                   13.816(3)
_cell_length_c                   14.892(3)
_cell_measurement_reflns_used    4440
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.08
_cell_volume                     2428.7(9)
_computing_cell_refinement       'SMART and SAINT (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SMART and SAINT'
_computing_molecular_graphics    SHELXL97
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'SMART 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  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7194
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.098
_exptl_absorpt_correction_T_max  0.568
_exptl_absorpt_correction_T_min  0.363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.102
_refine_diff_density_min         -0.818
_refine_ls_extinction_coef       0.000240(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4280
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0471P)^2^+9.0016P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                3561
_reflns_number_total             4280
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cm6029.cif
_cod_data_source_block           I
_cod_original_cell_volume        2428.8(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2201907
_cod_database_fobs_code          2201907