Rerefinement of tris(dimethylammonium) dodecamolybdophosphate in the space group <i>R</i>øverline 3<i>m</i>
Ng, Seik Weng; Acta Crystallographica Section E 60 (2004) m1786–m1787; doi:10.1107/S1600536804027941

data_2204804
_publ_section_title
;
 Rerefinement of tris(dimethylammonium) dodecamolybdophosphate in the
 space group <i>R</i>\/overline 3<i>m</i>
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1786
_journal_page_last               m1787
_journal_paper_doi               10.1107/S1600536804027941
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '(C2 H8 N)3 [Mo12 O40 P]'
_chemical_formula_moiety         '3C2 H8 N +, O40 P Mo12 3-'
_chemical_formula_sum            'C6 H24 Mo12 N3 O40 P'
_chemical_formula_weight         1960.53
_chemical_name_systematic
;
tris(dimethylammonium) dodecamolybdophosphate
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   16.541(2)
_cell_length_b                   16.541
_cell_length_c                   25.154(7)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      12.9
_cell_measurement_theta_min      5.0
_cell_volume                     5960.2(18)
_computing_cell_refinement       'LEAST SQUARES in XSCANS (Bruker, 1994)'
_computing_data_collection       'XSCANS (Bruker, 1994)'
_computing_data_reduction        'REDUCE in XSCANS (Bruker, 1994)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Siemens P4 four-circle'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'medium-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_av_sigmaI/netI    0.040
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            3044
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.6
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.811
_exptl_absorpt_correction_T_max  0.484
_exptl_absorpt_correction_T_min  0.295
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'via \y scan (North et al., 1968)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    3.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             5520
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.35
_refine_diff_density_min         -0.91
_refine_ls_extinction_coef       0.00054(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1304
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.08
_refine_ls_R_factor_all          0.033
_refine_ls_R_factor_gt           0.027
_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^)+(0.038P)^2^+0.2473P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.067
_refine_ls_wR_factor_ref         0.069
_reflns_number_gt                1150
_reflns_number_total             1304
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk6195.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        5960(2)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               2204804
_cod_database_fobs_code          2204804