Dianilinium tetradecachlorohexamolybdate dihydrate, (PhNH~3~)~2~[(Mo~6~Cl~8~)Cl~6~]·2H~2~O
Andreas Flemström; Acta Crystallographica Section E 59 (2003) m162–m164; doi:10.1107/S1600536803004884

data_2202252
_publ_section_title
;
 Dianilinium tetradecachlorohexamolybdate dihydrate,
 (PhNH~3~)~2~[(Mo~6~Cl~8~)Cl~6~]&#x00B7;2H~2~O
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m162
_journal_page_last               m164
_journal_paper_doi               10.1107/S1600536803004884
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '2C6 H8 N 1+, Mo6 Cl14 2-, 2H2 O1'
_chemical_formula_moiety         '2C6 H8 N 1+, Mo6 Cl14 2-, 2H2 O1'
_chemical_formula_structural     '((Mo6 Cl8) Cl6) (C6 H5 NH3)2 (H2 O)2'
_chemical_formula_sum            'C12 H20 Cl14 Mo6 N2 O2'
_chemical_formula_weight         1296.24
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 126.21(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.665(8)
_cell_length_b                   11.335(3)
_cell_length_c                   17.347(6)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      4.1
_cell_volume                     3279(3)
_computing_cell_refinement       'IPDS Software'
_computing_data_collection       'IPDS Software (Stoe & Cie, 1997)'
_computing_data_reduction        'IPDS Software'
_computing_publication_material  'SHELXL97 and JANA2000'
_computing_structure_refinement  'SHELXL97 and JANA2000'
_computing_structure_solution
'SHELXS97 (Sheldrick, 1997) and JANA2000 (Petricek & Dusek, 2000)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 6.0
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'Area-detector \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_sigmaI/netI    0.030
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8558
_diffrn_reflns_theta_full        23.9
_diffrn_reflns_theta_max         23.9
_diffrn_reflns_theta_min         3.5
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.38
_exptl_absorpt_correction_T_max  0.634
_exptl_absorpt_correction_T_min  0.463
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 1996)'
_exptl_crystal_colour            'Cognac brown'
_exptl_crystal_density_diffrn    2.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.37
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2368
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.35
_refine_ls_R_factor_all          0.038
_refine_ls_R_factor_gt           0.029
_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^)+(0.02P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.060
_refine_ls_wR_factor_ref         0.062
_reflns_number_gt                1908
_reflns_number_total             2368
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ya6150.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_hbond_publ_flag' value 'Yes' changed to 'yes' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (5 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3279.(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2202252