Two new inorganic-organic hybrid salts: [NH2Me2]4[NMe4]2-[Mo0.5O4⊂(Mo12O36)]·1.5H2O and [NMe4]2[NH4]2[Mo8O26]·2H2O
Duraisamy, T.; Ramanan, A.; Vittal, J. J.; Journal of Materials Chemistry 9 (1999) 763–; doi:10.1039/a806073h

data_7212958
_publ_section_title
;
 Two new inorganic-organic hybrid salts:
 [NH2Me2]4[NMe4]2-[Mo0.5O4&#x2282;(Mo12O36)]&#x00B7;1.5H2O and
 [NMe4]2[NH4]2[Mo8O26]&#x00B7;2H2O
;
_journal_issue                   3
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              763
_journal_paper_doi               10.1039/a806073h
_journal_volume                  9
_journal_year                    1999
_chemical_compound_source        'see text'
_chemical_formula_structural     (Me2NH2)4(Me4N)2[Mo12.5O40].1.5H2O
_chemical_formula_sum            'C16 H57.5 Mo12.5 N6 O41.5'
_chemical_formula_weight         2197.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.4037(2)
_cell_length_b                   19.5153(2)
_cell_length_c                   12.7108(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.26
_cell_measurement_theta_min      1.82
_cell_volume                     5557.35(12)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  'SHELXTL (Siemens, 1996)'
_computing_structure_refinement  'SHELXTL (Siemens, 1996)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens SMART CCD System'
_diffrn_measurement_method       'frames \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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            33763
_diffrn_reflns_theta_max         29.26
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    2.820
_exptl_absorpt_correction_T_max  0.5834
_exptl_absorpt_correction_T_min  0.4516
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    2.626
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'rhombohedral type'
_exptl_crystal_F_000             4210
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.880
_refine_diff_density_min         -3.816
_refine_diff_density_rms         0.209
_refine_ls_extinction_coef       0.00017(3)
_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_all   1.119
_refine_ls_goodness_of_fit_obs   1.155
_refine_ls_hydrogen_treatment
;
the H-stoms were not included for the disordered atoms. 
riding models were used for the rest.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7272
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.124
_refine_ls_restrained_S_obs      1.155
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_obs          0.0472
_refine_ls_shift/esd_max         -0.024
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+41.5492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1326
_refine_ls_wR_factor_obs         0.1250
_reflns_number_observed          6152
_reflns_number_total             7273
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            806073hsup1.cif
_cod_data_source_block           jjv5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+41.5492P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+41.5492P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      Pnma
_cod_original_formula_sum        'C16 H57.50 Mo12.50 N6 O41.50'
_cod_database_code               7212958