#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/25/2212527.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2212527
loop_
_publ_author_name
'Zong-Jun Ku'
'Zhong-Hai Zhang'
'Ke-Li Zhang'
_publ_section_title
;
 Tris(dimethylammonium) hydrogen α-dodecamolybdosilicate
;
_journal_coeditor_code           DN2123
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m878
_journal_page_last               m880
_journal_paper_doi               10.1107/S1600536807007192
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C2 H8 N)3 [H Si Mo12 O40 ]'
_chemical_formula_moiety         '3(C2 H8 N +), Mo12 O40 Si 3-'
_chemical_formula_sum            'C6 H24 Mo12 N3 O40 Si'
_chemical_formula_weight         1957.65
_chemical_name_systematic
;
Tris(dimethylammonium) hydrogen a-dodecamolybdosilicate
;
_space_group_IT_number           166
_symmetry_cell_setting           hexagonal
_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           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   16.4365(8)
_cell_length_b                   16.4365(8)
_cell_length_c                   25.142(2)
_cell_measurement_reflns_used    5375
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.53
_cell_measurement_theta_min      2.43
_cell_volume                     5882.3(6)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.1095
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            13145
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.851
_exptl_absorpt_correction_T_max  0.485
_exptl_absorpt_correction_T_min  0.288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5514
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.545
_refine_diff_density_min         -0.614
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.341
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.341
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0312
_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/[σ²(Fo²)+(0.014P)²+41.0665P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                1735
_reflns_number_total             1752
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            dn2123.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
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 'Hexagonal' changed to 'hexagonal'
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_sg_symbol_H-M      'R -3 m'
_cod_database_code               2212527
_cod_database_fobs_code          2212527
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'-x, -x+y, -z'
'x-y, -y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'x, x-y, z'
'-x+y, y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Si Si1 0.0000 0.0000 0.23511(8) 0.0104(4) Uani d S 1
Mo Mo1 0.13563(3) 0.067815(16) 0.117155(17) 0.01844(13) Uani d S 1
Mo Mo2 0.21176(2) 0.21820(2) 0.237178(13) 0.02002(12) Uani d . 1
Mo Mo3 0.074905(16) 0.14981(3) 0.345728(16) 0.01944(13) Uani d S 1
O O1 0.0000 0.0000 0.1706(2) 0.0132(11) Uani d S 1
O O2 0.05390(12) 0.1078(2) 0.25660(12) 0.0133(6) Uani d S 1
O O3 0.2206(3) 0.11032(15) 0.07109(14) 0.0274(9) Uani d S 1
O O4 0.05455(14) 0.1091(3) 0.08785(13) 0.0194(7) Uani d S 1
O O5 0.18181(19) 0.1705(2) 0.16659(10) 0.0207(5) Uani d . 1
O O6 0.2337(3) 0.11686(13) 0.25148(13) 0.0199(7) Uani d S 1
O O7 0.3208(2) 0.3106(2) 0.22980(10) 0.0268(6) Uani d . 1
O O8 0.14036(13) 0.2807(3) 0.22515(14) 0.0204(7) Uani d S 1
O O9 0.19610(18) 0.22909(19) 0.31299(9) 0.0209(5) Uani d . 1
O O10 0.1056(3) 0.05279(13) 0.35292(13) 0.0180(7) Uani d S 1
O O11 0.09746(15) 0.1949(3) 0.40743(14) 0.0253(8) Uani d S 1
C C1 0.2084(2) 0.4168(4) 0.1248(2) 0.0358(14) Uani d S 1
H H1A 0.2064 0.4128 0.1629 0.054 Uiso d SR 1
H H1B 0.1773 0.4498 0.1129 0.054 Uiso d R 1
N N2 0.16039(18) 0.3208(4) 0.10237(17) 0.0291(11) Uani d S 1
H H2A 0.1892 0.2901 0.1145 0.035 Uiso d R 1
C C3 0.1584(3) 0.3167(5) 0.0436(2) 0.0395(16) Uani d S 1
H H3A 0.1261 0.2522 0.0323 0.059 Uiso d SR 1
H H3B 0.2215 0.3476 0.0302 0.059 Uiso d R 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Si1 O2 . . 109.40(13)
O2 Si1 O2 . 2 109.55(13)
O3 Mo1 O4 . . 99.73(13)
O4 Mo1 O4 3 . 89.0(2)
O3 Mo1 O5 . . 101.55(13)
O4 Mo1 O5 3 . 158.69(12)
O4 Mo1 O5 . . 88.67(14)
O5 Mo1 O5 . 23 85.88(17)
O3 Mo1 O1 . . 171.09(18)
O4 Mo1 O1 . . 74.08(11)
O5 Mo1 O1 . . 84.91(11)
O7 Mo2 O5 . . 102.03(12)
O7 Mo2 O6 . . 103.18(15)
O5 Mo2 O6 . . 86.50(13)
O7 Mo2 O8 . . 99.12(14)
O5 Mo2 O8 . . 88.41(13)
O6 Mo2 O8 . . 157.69(15)
O7 Mo2 O9 . . 98.94(12)
O5 Mo2 O9 . . 159.02(11)
O6 Mo2 O9 . . 89.27(13)
O8 Mo2 O9 . . 87.76(14)
O7 Mo2 O2 . . 169.56(12)
O5 Mo2 O2 . . 85.27(11)
O6 Mo2 O2 . . 84.53(13)
O8 Mo2 O2 . . 73.40(11)
O9 Mo2 O2 . . 73.87(11)
O11 Mo3 O10 . . 100.92(14)
O10 Mo3 O10 2 . 86.1(2)
O11 Mo3 O9 . . 99.79(13)
O10 Mo3 O9 2 . 159.29(13)
O10 Mo3 O9 . . 89.42(14)
O11 Mo3 O9 . 24 99.79(13)
O9 Mo3 O9 . 24 87.64(17)
O11 Mo3 O2 . . 172.46(17)
O10 Mo3 O2 2 . 84.54(12)
O10 Mo3 O2 . . 84.54(12)
O9 Mo3 O2 . . 74.90(9)
Si1 O1 Mo1 . . 124.83(10)
Mo1 O1 Mo1 3 . 90.61(15)
Si1 O1 Mo1 . 2 124.83(10)
Mo1 O1 Mo1 . 2 90.61(15)
Si1 O2 Mo3 . . 124.34(18)
Si1 O2 Mo2 . . 124.06(10)
Mo3 O2 Mo2 . . 91.62(10)
Mo2 O2 Mo2 . 24 91.43(12)
Mo1 O4 Mo1 2 . 121.18(18)
Mo2 O5 Mo1 . . 150.79(16)
Mo2 O6 Mo2 23 . 151.1(2)
Mo2 O8 Mo2 24 . 121.76(19)
Mo3 O9 Mo2 . . 119.61(13)
Mo3 O10 Mo3 3 . 151.3(2)
N2 C1 H1A . . 109.0
N2 C1 H1B . . 109.5
H1A C1 H1B . . 109.9
C3 N2 C1 . . 114.7(5)
C3 N2 H2A . . 108.6
C1 N2 H2A . . 108.6
N2 C3 H3A . . 109.4
N2 C3 H3B . . 109.5
H3A C3 H3B . . 109.4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Si1 O1 . 1.622(5)
Si1 O2 . 1.627(3)
Si1 O2 2 1.627(3)
Si1 O2 3 1.627(3)
Mo1 O3 . 1.675(4)
Mo1 O4 3 1.9193(17)
Mo1 O4 . 1.9193(17)
Mo1 O5 . 1.921(3)
Mo1 O5 23 1.921(3)
Mo1 O1 . 2.352(3)
Mo2 O7 . 1.682(3)
Mo2 O5 . 1.903(3)
Mo2 O6 . 1.907(4)
Mo2 O8 . 1.931(4)
Mo2 O9 . 1.943(2)
Mo2 O2 . 2.357(2)
Mo3 O11 . 1.679(3)
Mo3 O10 . 1.906(4)
Mo3 O9 . 1.936(3)
Mo3 O2 . 2.319(3)
C1 N2 . 1.478(8)
C1 H1A . 0.9604
C1 H1B . 0.9599
N2 C3 . 1.478(7)
N2 H2A . 0.9000
C3 H3A . 0.9614
C3 H3B . 0.9600
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N2 H2A O5 . 0.90 2.31 3.115(5) 148.0
N2 H2A O7 11 0.90 2.37 3.030(3) 130.5
