#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/87/2018761.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_2018761
loop_
_publ_author_name
'Takehara, Masaki'
'Hashimoto, Masato'
_publ_section_title
;
 Potassium, rubidium and ammonium salts of
 μ-(formato-κ²O:O')-μ-oxido-bis[oxidobis(peroxido-κ²O,O')molybdate(VI)]
;
_journal_coeditor_code           SF3186
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              37
_journal_page_last               40
_journal_paper_doi               10.1107/S0108270112049803
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '(NH4)3 [Mo2 (C H O2) O3 (O2)4]'
_chemical_formula_moiety         '3(H4 N +), C H Mo2 O13 3-'
_chemical_formula_sum            'C H13 Mo2 N3 O13'
_chemical_formula_weight         467.02
_chemical_name_common            'Triammonium formatotetraperoxidodimolybdate'
_chemical_name_systematic
;
Triammonium μ-(formato-κ²O:O')-μ-oxido-
bis[oxidobis(peroxido-κ²O,O')molybdate(VI)]
;
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.091(2)
_cell_length_b                   11.622(4)
_cell_length_c                   16.800(5)
_cell_measurement_reflns_used    4358
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      30.0628
_cell_measurement_theta_min      2.9922
_cell_volume                     1189.3(7)
_computing_cell_refinement       'CrystalClear (Rigaku, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'CrystalClear (Rigaku, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93.0(10)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku SATURN724+'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0153
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10346
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    2.187
_exptl_absorpt_correction_T_max  0.9239
_exptl_absorpt_correction_T_min  0.8303
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.755
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0176
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0207P)²+0.6740P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0427
_refine_ls_wR_factor_ref         0.0434
_reflns_number_gt                1704
_reflns_number_total             1779
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sf3186.cif
_cod_data_source_block           III
_cod_database_code               2018761
_cod_database_fobs_code          2018761
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y-1/2, z'
'x, -y-1/2, z-1/2'
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_symmetry_multiplicity
Mo Mo1 0.698345(18) 0.242596(10) 0.360801(7) 0.00715(5) Uani d . 1 1
O O1 0.46989(17) 0.18126(9) 0.39877(6) 0.0130(2) Uani d . 1 1
O O2 0.59493(18) 0.39874(9) 0.33975(6) 0.0132(2) Uani d . 1 1
O O3 0.69480(16) 0.38790(9) 0.42001(6) 0.0130(2) Uani d . 1 1
O O4 0.91788(18) 0.18305(10) 0.43521(6) 0.0182(2) Uani d . 1 1
O O5 0.90316(19) 0.11118(9) 0.36274(7) 0.0160(2) Uani d . 1 1
O O6 0.6451(2) 0.20824(13) 0.2500 0.0113(3) Uani d S 1 2
O O7 1.02448(17) 0.33003(9) 0.31653(6) 0.0136(2) Uani d . 1 1
C C1 1.1010(3) 0.35695(16) 0.2500 0.0099(3) Uani d S 1 2
H H1 1.239(5) 0.404(3) 0.2500 0.015 Uiso d S 1 2
N N1 0.2325(2) 0.41385(11) 0.45589(8) 0.0122(2) Uani d . 1 1
N N2 0.2423(3) 0.08963(16) 0.2500 0.0138(3) Uani d S 1 2
H H2 0.375(4) 0.401(2) 0.4593(15) 0.035(6) Uiso d . 1 1
H H3 0.180(4) 0.380(2) 0.4118(17) 0.036(7) Uiso d . 1 1
H H4 0.209(4) 0.486(2) 0.4511(16) 0.038(7) Uiso d . 1 1
H H5 0.162(4) 0.385(2) 0.5008(13) 0.028(7) Uiso d . 1 1
H H6 0.161(4) 0.108(2) 0.2909(13) 0.023(6) Uiso d . 1 1
H H7 0.368(5) 0.130(3) 0.2500 0.023(8) Uiso d S 1 2
H H8 0.279(7) 0.016(4) 0.2500 0.049(11) Uiso d S 1 2
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'
O O 0.0106 0.0060 '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'
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'
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
O1 Mo1 O6 . . 97.96(6) n
O1 Mo1 O2 . . 101.23(5) n
O6 Mo1 O2 . . 87.90(6) n
O1 Mo1 O4 . . 99.94(5) n
O6 Mo1 O4 . . 131.10(6) n
O2 Mo1 O4 . . 131.65(5) n
O1 Mo1 O3 . . 99.38(5) n
O6 Mo1 O3 . . 131.72(5) n
O2 Mo1 O3 . . 44.59(5) n
O4 Mo1 O3 . . 89.31(5) n
O1 Mo1 O5 . . 100.84(5) n
O6 Mo1 O5 . . 87.83(6) n
O2 Mo1 O5 . . 157.89(5) n
O4 Mo1 O5 . . 44.23(5) n
O3 Mo1 O5 . . 131.74(5) n
O1 Mo1 O7 . . 176.24(4) n
O6 Mo1 O7 . . 85.78(5) n
O2 Mo1 O7 . . 79.26(5) n
O4 Mo1 O7 . . 77.15(5) n
O3 Mo1 O7 . . 78.32(4) n
O5 Mo1 O7 . . 78.79(5) n
O3 O2 Mo1 . . 67.95(6) n
O2 O3 Mo1 . . 67.46(6) n
O5 O4 Mo1 . . 68.44(6) n
O4 O5 Mo1 . . 67.34(6) n
Mo1 O6 Mo1 . 6_556 149.10(8) y
C1 O7 Mo1 . . 134.87(10) y
O7 C1 O7 6_556 . 126.65(18) y
O7 C1 H1 6_556 . 116.67(9) n
O7 C1 H1 . . 116.67(9) n
H2 N1 H3 . . 110(2) n
H2 N1 H4 . . 109(2) n
H3 N1 H4 . . 107(2) n
H2 N1 H5 . . 110(2) n
H3 N1 H5 . . 110(2) n
H4 N1 H5 . . 111(2) n
H6 N2 H7 . . 110.4(18) n
H6 N2 H8 . . 113(2) n
H7 N2 H8 . . 107(3) n
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 O1 . 1.6886(11) y
Mo1 O6 . 1.9312(7) y
Mo1 O2 . 1.9532(12) y
Mo1 O4 . 1.9569(11) y
Mo1 O3 . 1.9600(12) y
Mo1 O5 . 1.9723(12) y
Mo1 O7 . 2.3520(12) y
O2 O3 . 1.4845(15) y
O4 O5 . 1.4792(16) y
O6 Mo1 6_556 1.9312(7) y
O7 C1 . 1.2508(13) y
C1 O7 6_556 1.2508(13) y
C1 H1 . 1.00(3) n
N1 H2 . 0.88(3) n
N1 H3 . 0.90(3) n
N1 H4 . 0.85(3) n
N1 H5 . 0.93(2) n
N2 H6 . 0.87(2) n
N2 H7 . 0.90(3) n
N2 H8 . 0.88(4) n
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
_geom_hbond_publ_flag
N1 H2 O3 . 0.88(2) 2.06(2) 2.8954(19) 157(2) n
N1 H2 O2 . 0.88(2) 2.41(2) 2.9515(19) 120(2) n
N1 H3 O7 1_455 0.90(3) 1.95(3) 2.8348(19) 170 n
N1 H4 O5 7_665 0.85(2) 2.19(3) 2.897(2) 140 n
N1 H4 O4 7_665 0.85(2) 2.43(2) 3.278(2) 171 n
N1 H5 O4 3_456 0.93(2) 2.00(2) 2.8789(19) 157 n
N2 H6 O5 1_455 0.87(2) 1.98(2) 2.814(2) 159 n
N2 H7 O6 . 0.90(3) 1.92(3) 2.814(2) 177(3) n
N2 H8 O2 4_645 0.88(5) 2.17(3) 2.860(2) 134 n
N2 H8 O2 7_655 0.88(5) 2.17(3) 2.860(2) 134 n
