Bis(2-ammonio-5-chloropyridine) tetradecachlorohexamolybdate
Flemström, Andreas; Acta Crystallographica Section E 60 (2004) m1303–m1305; doi:10.1107/S160053680401935X

data_2204170
_publ_section_title
;
 Bis(2-ammonio-5-chloropyridine) tetradecachlorohexamolybdate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1303
_journal_page_last               m1305
_journal_paper_doi               10.1107/S160053680401935X
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '(C5 H6 Cl N2)~2~ [Mo6 Cl14]'
_chemical_formula_moiety         '2C5 H6 Cl N2 + , Cl14 Mo6 2-'
_chemical_formula_sum            'C10 H12 Cl16 Mo6 N4'
_chemical_formula_weight         1331.08
_chemical_name_systematic
;
Bis(2-ammonio-5-chloropyridine) tetradecachlorohexamolybdate
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.81(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.186(6)
_cell_length_b                   18.238(8)
_cell_length_c                   9.614(6)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293
_cell_measurement_theta_max      52.0
_cell_measurement_theta_min      4.3
_cell_volume                     1582.1(16)
_computing_cell_refinement       IPDS
_computing_data_collection       'IPDS (Stoe & Cie, 1997)'
_computing_data_reduction        IPDS
_computing_publication_material  'SHELXL97 and JANA2000'
_computing_structure_refinement  'SHELXL97 and JANA2000'
_computing_structure_solution
'SHELXS97 (Sheldrick, 1997) and JANA2000 (Pet\<r\'i\<cek & Du\<sek, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Stoe IPDS CCD area-detector'
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12075
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.673
_exptl_absorpt_correction_T_max  0.652
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.794
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.101
_refine_diff_density_max         1.040
_refine_diff_density_min         -1.642
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2926
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0245
_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^)+(0.052P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0871
_reflns_number_gt                2486
_reflns_number_total             2926
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6059.cif
_cod_data_source_block           I
_cod_original_cell_volume        1582.0(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2204170
_cod_database_fobs_code          2204170