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_7212959
_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
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_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_sum            'C8 H36 Mo8 N4 O28'
_chemical_formula_weight         1403.93
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_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                 110.242(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.2641(1)
_cell_length_b                   16.3815(1)
_cell_length_c                   10.0775(1)
_cell_measurement_reflns_used    4878
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.24
_cell_measurement_theta_min      2.15
_cell_volume                     1744.68(3)
_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  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5644
_diffrn_reflns_theta_max         29.24
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    2.878
_exptl_absorpt_correction_T_max  0.6494
_exptl_absorpt_correction_T_min  0.4774
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.672
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'rectangular plates'
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.00293(14)
_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   1.101
_refine_ls_goodness_of_fit_obs   1.126
_refine_ls_hydrogen_treatment
; 
all the H atoms were located.  The positional parameters of H atoms 
attached
to N(2) and O(1s) were refined. Individual isotropic thermal parameter 
was
refined for H atoms attached to O(1s) and a common isotropic thermal 
parameter was refined for ammonium H atoms.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         2213
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.100
_refine_ls_restrained_S_obs      1.125
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_obs          0.0241
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+2.2691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0640
_refine_ls_wR_factor_obs         0.0622
_reflns_number_observed          2010
_reflns_number_total             2213
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            806073hsup1.cif
_cod_data_source_block           jjv6
_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^)+(0.0345P)^2^+2.2691P] 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^)+(0.0345P)^2^+2.2691P] 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      C2/m
_cod_database_code               7212959