The first polyoxomolybdenum carbonate compound: Synthesis and crystal structure of (NH4)5[(Mo2VO4)3(µ6-CO3)(µ-CO3)3(µ-OH)3]·0.5CH3OH 1
Manos, Manolis J.; Keramidas, Anastasios D.; Woollins, J. Derek; Slawin, Alexandra M. Z.; Kabanos, Themistoklis A.; Journal of the Chemical Society, Dalton Transactions  (2001) 3419–; doi:10.1039/b108430p

data_7011171
_publ_section_title
;
 The first polyoxomolybdenum carbonate compound: Synthesis and crystal
 structure of
 (NH4)5[(Mo2VO4)3(&#x00B5;6-CO3)(&#x00B5;-CO3)3(&#x00B5;-OH)3]&#x00B7;0.5CH3OH
 1
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_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3419
_journal_paper_doi               10.1039/b108430p
_journal_year                    2001
_chemical_formula_analytical     'C4.50 H25 Mo6 N5 O27.50'
_chemical_formula_moiety         'Mo6 O12(OH)3(CO3)4.(NH4)5.(C H3 OH)0.5'
_chemical_formula_structural     'C4.50 H25 Mo6 N5 O27.50'
_chemical_formula_sum            'C4.5 H25 Mo6 N5 O27.5'
_chemical_formula_weight         1164.94
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   21.9946(4)
_cell_length_b                   21.9946(4)
_cell_length_c                   12.4171(4)
_cell_measurement_reflns_used    104
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      168
_cell_measurement_theta_min      12
_cell_volume                     5202.2(2)
_computing_cell_refinement       SMART/SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       CCD
_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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7650
_diffrn_reflns_theta_max         23.23
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    2.198
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.711663
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.231
_exptl_crystal_description       prism
_exptl_crystal_F_000             3354
_exptl_crystal_size_max          .1
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .1
_refine_diff_density_max         1.596
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       0.00016(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   1.059
_refine_ls_goodness_of_fit_obs   1.080
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1604
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.552
_refine_ls_restrained_S_obs      1.079
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_obs          0.0445
_refine_ls_shift/esd_max         -0.279
_refine_ls_shift/esd_mean        0.042
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+65.1722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1831
_refine_ls_wR_factor_obs         0.1238
_reflns_number_observed          1501
_reflns_number_total             1654
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b108430p.txt
_cod_data_source_block           amtk13
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+65.1722P] 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^)+(0.0858P)^2^+65.1722P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5202.1(2)
_cod_original_sg_symbol_H-M      R-3
_cod_original_formula_sum        'C4.50 H25 Mo6 N5 O27.50'
_cod_database_code               7011171