#------------------------------------------------------------------------------
#$Date: 2016-02-20 21:30:07 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/49/2224947.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_2224947
loop_
_publ_author_name
'Hill, Björn'
'Lerner, Hans-Wolfram'
'Bolte, Michael'
_publ_section_title
;
 Redetermination of diammonium thiomolybdate
;
_journal_coeditor_code           FB2179
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i13
_journal_paper_doi               10.1107/S1600536810003016
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '(N H4)2 [Mo S4]'
_chemical_formula_moiety         'Mo S4 2-, 2(H4 N +)'
_chemical_formula_sum            'H8 Mo N2 S4'
_chemical_formula_weight         260.26
_chemical_name_systematic
;
diammonium thiomolybdate
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5867(4)
_cell_length_b                   6.9451(4)
_cell_length_c                   12.2005(5)
_cell_measurement_reflns_used    14093
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.7
_cell_volume                     812.32(7)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2001)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS II two-circle diffractometer'
_diffrn_measurement_method       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  0.0722
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14872
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.90
_diffrn_reflns_theta_min         2.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.547
_exptl_absorpt_correction_T_max  0.7670
_exptl_absorpt_correction_T_min  0.5685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS; Spek, 2009; Blessing, 1995)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.883
_refine_ls_extinction_coef       0.0173(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         859
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0377P)²+0.2462P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0596
_reflns_number_gt                833
_reflns_number_total             859
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fb2179.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 'Orthorhombic' changed to
'orthorhombic' 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_database_code               2224947
_cod_database_fobs_code          2224947
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo Mo1 0.25414(2) 0.7500 0.42734(2) 0.01490(16) Uani d S 1 . .
S S1 0.03014(7) 0.7500 0.38769(6) 0.0229(2) Uani d S 1 . .
S S2 0.28425(9) 0.7500 0.60460(7) 0.0246(2) Uani d S 1 . .
S S3 0.35338(5) 0.49616(7) 0.35742(5) 0.0259(2) Uani d . 1 . .
N N1 0.6660(3) 0.7500 0.3880(2) 0.0257(6) Uani d SD 1 . .
H H1A 0.746(4) 0.7500 0.355(5) 0.072(19) Uiso d SD 1 . .
H H1B 0.590(4) 0.7500 0.347(4) 0.089(19) Uiso d SD 1 . .
H H1C 0.665(5) 0.850(5) 0.433(3) 0.114(18) Uiso d D 1 . .
N N2 -0.0471(3) 0.7500 0.6609(2) 0.0223(5) Uani d SD 1 . .
H H2A -0.002(5) 0.7500 0.723(3) 0.09(2) Uiso d SD 1 . .
H H2B 0.003(6) 0.7500 0.600(3) 0.10(2) Uiso d SD 1 . .
H H2C -0.097(5) 0.644(5) 0.656(4) 0.114(16) Uiso d D 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Mo1 0.0146(2) 0.0149(2) 0.0152(2) 0.000 0.00038(8) 0.000
S1 0.0161(4) 0.0297(4) 0.0228(4) 0.000 -0.0034(3) 0.000
S2 0.0214(4) 0.0349(4) 0.0175(4) 0.000 -0.0024(3) 0.000
S3 0.0235(3) 0.0196(3) 0.0346(3) 0.00079(18) 0.0062(2) -0.0074(2)
N1 0.0235(14) 0.0268(14) 0.0267(15) 0.000 -0.0028(11) 0.000
N2 0.0219(13) 0.0258(13) 0.0193(13) 0.000 0.0030(10) 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mo Mo -1.6832 0.6857 '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'
S S 0.1246 0.1234 '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
_geom_angle_publ_flag
S3 Mo1 S3 8_575 . 108.13(3) ?
S3 Mo1 S2 8_575 . 109.30(2) ?
S3 Mo1 S2 . . 109.30(2) ?
S3 Mo1 S1 8_575 . 109.885(19) ?
S3 Mo1 S1 . . 109.885(19) ?
S2 Mo1 S1 . . 110.30(3) ?
H1A N1 H1B . . 118(6) ?
H1A N1 H1C . . 107(4) ?
H1B N1 H1C . . 110(3) ?
H2A N2 H2B . . 117(5) ?
H2A N2 H2C . . 109(3) ?
H2B N2 H2C . . 103(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mo1 S3 8_575 2.1773(5) ?
Mo1 S3 . 2.1773(5) ?
Mo1 S2 . 2.1818(9) ?
Mo1 S1 . 2.2013(8) ?
N1 H1A . 0.86(2) ?
N1 H1B . 0.88(2) ?
N1 H1C . 0.883(19) ?
N2 H2A . 0.88(2) ?
N2 H2B . 0.88(2) ?
N2 H2C . 0.879(19) ?
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
N1 H1A S1 1_655 0.86(2) 2.76(4) 3.491(3) 144(6)
N1 H1B S1 6_656 0.88(2) 2.92(5) 3.607(3) 135(5)
N1 H1B S3 . 0.88(2) 2.87(3) 3.497(3) 129(3)
N1 H1B S3 8_575 0.88(2) 2.87(3) 3.497(3) 129(3)
N1 H1C S3 4_656 0.883(19) 2.76(3) 3.550(3) 150(4)
N1 H1C S3 4_656 0.883(19) 2.76(3) 3.550(3) 150(4)
N2 H2C S3 5_566 0.879(19) 2.65(3) 3.405(2) 144(4)
N2 H2A S3 7_666 0.88(2) 2.762(17) 3.481(2) 140.3(12)
N2 H2A S3 2_565 0.88(2) 2.762(17) 3.481(2) 140.3(12)
N2 H2B S1 . 0.88(2) 2.61(4) 3.414(3) 153(6)
N2 H2B S2 . 0.88(2) 2.70(6) 3.250(3) 122(5)
