#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/08/4320813.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4320813
loop_
_publ_author_name
'Michael Brorson'
'Alan Hazell'
'Claus J. H. Jacobsen'
'Iver Schmidt'
'Jørgen Villadsen'
_publ_contact_author
;
Michael Brorson
Haldor Topsøe Research Laboratories
Nymøllevej 55
DK-2800 Lyngby
Denmark
;
_publ_section_title
;
 Preparation and Crystal Structures of Formato Complexes of the
 [MIV₃O₄]⁴⁺ and [MIV₃S₄]⁴⁺ (M = Mo,W) Clusters. Convenient
 Precursors to the Corresponding Aqua Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1346
_journal_page_last               1350
_journal_paper_doi               10.1021/ic9906656
_journal_volume                  39
_journal_year                    2000
_chemical_formula_structural     (NH4)3.20K0.80H3O[Mo3O4(HCO2)8]HCO2.H2O
_chemical_formula_sum            'C9 H26.8 K0.8 Mo3 N3.2 O24'
_chemical_formula_weight         883.06
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                106.817(7)
_cell_angle_beta                 91.651(9)
_cell_angle_gamma                88.340(9)
_cell_formula_units_Z            2
_cell_length_a                   11.011(2)
_cell_length_b                   13.310(2)
_cell_length_c                   9.993(1)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    294
_cell_measurement_theta_max      14.3
_cell_measurement_theta_min      10.1
_cell_volume                     1401.0(4)
_computing_cell_refinement       MAD
_computing_data_collection       'MAD (Allibon, 1995)'
_computing_data_reduction        'KRYSTAL (Hazell, 1995)'
_computing_molecular_graphics
;                                  
      ORTEP-III (Burnett & Johnson, 1996), KRYSTAL                    
;
_computing_publication_material  KRYSTAL
_computing_structure_refinement  'modified ORFLS(1962), KRYSTAL'
_computing_structure_solution
;                                  
      SIR92 (Altomare et al., 1994) KRYSTAL                           
;
_diffrn_ambient_temperature      294
_diffrn_measurement_device       'Huber four-circle diffractometer'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5370
_diffrn_reflns_reduction_process 5161
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.6
_diffrn_standards_decay_%        11
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.507
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   'integration, DATAP,KRYSTAL(Hazell,1995)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    2.093
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             872.80
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.81(9)
_refine_diff_density_min         -0.87(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   0.887
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    20
_refine_ls_number_parameters     451
_refine_ls_number_reflns         3972
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.026
_refine_ls_shift/esd_max         0.121
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/{[σcs(F²)+1.03F²]^1/2^-|F|}²'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.034
_reflns_number_observed          3972
_reflns_number_total             4926
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            ic9906656_2.cif
_cod_data_source_block           compound(1)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value
'1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^' was changed to 'calc'. New
tag '_refine_ls_weighting_details' was created. The value of the new
tag was set to 'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1401.0(3)
_cod_original_formula_sum        'C9 H26.80 K0.80 Mo3 N3.20 O24'
_cod_database_code               4320813
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
Mo1 0.14826(3) 0.17155(3) 0.76162(3) 0.0205(2) Uij 1.
Mo2 0.24333(3) 0.34452(3) 0.78338(3) 0.0222(2) Uij 1.
Mo3 0.04488(3) 0.30074(3) 0.65734(3) 0.0207(2) Uij 1.
O1 0.0832(2) 0.3177(2) 0.8615(3) 0.023(1) Uij 1.
O2 0.0832(2) 0.1555(2) 0.5744(3) 0.024(1) Uij 1.
O3 0.1938(2) 0.3473(2) 0.5989(3) 0.027(2) Uij 1.
O4 0.3120(2) 0.2066(2) 0.7289(3) 0.026(2) Uij 1.
O5 -0.0167(2) 0.1147(2) 0.8089(3) 0.029(2) Uij 1.
C6 -0.0917(4) 0.0562(4) 0.7245(5) 0.037(3) Uij 1.
O7 -0.1856(3) 0.0258(3) 0.7588(3) 0.058(2) Uij 1.
O8 0.2012(3) 0.0109(2) 0.6949(3) 0.033(2) Uij 1.
C9 0.2771(4) -0.0389(3) 0.6026(5) 0.035(3) Uij 1.
O10 0.3391(3) -0.0036(2) 0.5294(3) 0.044(2) Uij 1.
O11 0.1922(3) 0.1561(2) 0.9573(3) 0.031(2) Uij 1.
C12 0.1308(5) 0.1959(4) 1.0705(5) 0.040(3) Uij 1.
O13 0.1659(4) 0.2036(4) 1.1861(4) 0.087(4) Uij 1.
O14 0.3158(2) 0.3910(2) 0.9845(3) 0.036(2) Uij 1.
C15 0.2622(4) 0.4206(4) 1.1023(5) 0.039(3) Uij 1.
O16 0.3155(3) 0.4396(3) 1.2126(3) 0.060(3) Uij 1.
O17 0.4121(3) 0.4049(2) 0.7504(3) 0.040(2) Uij 1.
C18 0.4785(5) 0.3812(4) 0.6428(6) 0.050(3) Uij 1.
O19 0.4632(4) 0.3135(4) 0.5342(4) 0.082(3) Uij 1.
O20 0.1809(3) 0.5091(2) 0.8433(3) 0.034(2) Uij 1.
C21 0.0794(4) 0.5332(3) 0.8019(5) 0.037(3) Uij 1.
O22 0.0030(3) 0.4702(2) 0.7275(3) 0.034(2) Uij 1.
O23 -0.0302(3) 0.3128(2) 0.4648(3) 0.036(2) Uij 1.
C24 -0.0633(4) 0.2378(3) 0.3614(4) 0.033(2) Uij 1.
O25 -0.1309(3) 0.2466(3) 0.2647(3) 0.049(2) Uij 1.
O26 -0.1358(2) 0.2896(2) 0.6956(3) 0.033(2) Uij 1.
C27 -0.1872(4) 0.3124(4) 0.8133(5) 0.038(3) Uij 1.
O28 -0.2918(3) 0.2927(3) 0.8316(4) 0.060(3) Uij 1.
O29 0.5522(3) 0.1633(3) 1.0461(4) 0.065(3) Uij 1.
C30 0.4752(5) 0.1366(5) 1.1162(6) 0.061(4) Uij 1.
O31 0.4878(4) 0.0880(3) 1.2021(4) 0.073(3) Uij 1.
K1 0.5712(2) 0.3797(2) 1.0748(2) 0.043(2) Uij 0.291(8)
K2 0.2973(1) 0.1595(1) 1.4014(1) 0.036(1) Uij 0.509(7)
K1' 0.5712 0.3797 1.0748 0.043 Uij 0.709
K2' 0.2973 0.1595 1.4014 0.036 Uij 0.491
O32 0.4513(3) -0.1091(3) 1.2721(4) 0.045(2) Uij 1.
O33 0.6295(6) 0.3495(5) 1.3481(6) 0.068(4) Uij 1.
N34 0.7779(5) 0.0715(4) 1.0502(5) 0.043(3) Uij 1.
N35 0.2054(5) 0.5080(5) 0.4708(6) 0.048(3) Uij 1.
H6 -0.072(4) 0.031(4) 0.626(5) 0.037(12) Uiso 1.
H9 0.280(4) -0.116(4) 0.598(5) 0.042(13) Uiso 1.
H12 0.037(6) 0.214(5) 1.052(6) 0.086(20) Uiso 1.
H15 0.167(5) 0.428(4) 1.093(6) 0.066(17) Uiso 1.
H18 0.542(6) 0.423(5) 0.659(7) 0.090(22) Uiso 1.
H21 0.049(4) 0.603(4) 0.834(4) 0.033(11) Uiso 1.
H24 -0.038(4) 0.162(4) 0.364(5) 0.047(13) Uiso 1.
H27 -0.146(4) 0.358(4) 0.893(5) 0.039(12) Uiso 1.
H30 0.380(4) 0.163(3) 1.091(4) 0.035(11) Uiso 1.
H32a 0.520(6) -0.145(5) 1.266(7) 0.081(21) Uiso 1.
H32b 0.398(6) -0.162(5) 1.217(7) 0.078(20) Uiso 1.
H32c 0.421(8) -0.081(8) 1.353(10) 0.132(34) Uiso 1.
H33a 0.590(8) 0.324(8) 1.392(10) 0.119(39) Uiso 1.
H33b 0.666(7) 0.317(6) 1.345(8) 0.057(31) Uiso 1.
H34a 0.803(4) 0.056(4) 0.972(6) 0.039(14) Uiso 1.
H34b 0.783(7) 0.019(7) 1.078(8) 0.110(30) Uiso 1.
H34c 0.708(6) 0.091(5) 1.058(6) 0.060(20) Uiso 1.
H34d 0.818(6) 0.128(5) 1.120(7) 0.072(19) Uiso 1.
H35a 0.203(5) 0.467(4) 0.500(6) 0.038(16) Uiso 1.
H35b 0.240(5) 0.480(5) 0.386(7) 0.065(18) Uiso 1.
H35c 0.127(7) 0.555(6) 0.484(7) 0.091(22) Uiso 1.
H35d 0.251(7) 0.541(5) 0.518(7) 0.073(29) Uiso 1.
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
0 0 2
1 -5 0
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
Mo2 Mo1 Mo3 59.76(2)
Mo2 Mo1 O1 51.88(7)
Mo2 Mo1 O2 94.53(8)
Mo2 Mo1 O4 48.53(8)
Mo2 Mo1 O5 138.55(8)
Mo2 Mo1 O8 137.13(8)
Mo2 Mo1 O11 99.65(8)
Mo3 Mo1 O1 51.89(7)
Mo3 Mo1 O2 49.22(7)
Mo3 Mo1 O4 95.82(8)
Mo3 Mo1 O5 93.19(8)
Mo3 Mo1 O8 137.17(8)
Mo3 Mo1 O11 138.75(8)
O1 Mo1 O2 100.4(1)
O1 Mo1 O4 99.2(1)
O1 Mo1 O5 86.9(1)
O1 Mo1 O8 167.7(1)
O1 Mo1 O11 87.0(1)
O2 Mo1 O4 97.3(1)
O2 Mo1 O5 88.0(1)
O2 Mo1 O8 88.0(1)
O2 Mo1 O11 165.7(1)
O4 Mo1 O5 171.0(1)
O4 Mo1 O8 88.7(1)
O4 Mo1 O11 93.6(1)
O5 Mo1 O11 80.0(1)
O5 Mo1 O8 84.3(1)
O8 Mo1 O11 83.0(1)
Mo1 Mo2 Mo3 59.78(1)
Mo1 Mo2 O1 51.94(7)
Mo1 Mo2 O3 94.33(8)
Mo1 Mo2 O4 49.83(8)
Mo1 Mo2 O14 104.83(9)
Mo1 Mo2 O17 139.58(9)
Mo1 Mo2 O20 135.58(8)
Mo3 Mo2 O1 51.92(7)
Mo3 Mo2 O3 50.02(8)
Mo3 Mo2 O4 96.83(8)
Mo3 Mo2 O14 140.49(8)
Mo3 Mo2 O17 137.97(9)
Mo3 Mo2 O20 87.30(7)
O1 Mo2 O3 101.4(1)
O1 Mo2 O4 100.5(1)
O1 Mo2 O14 89.3(1)
O1 Mo2 O17 165.1(1)
O1 Mo2 O20 84.8(1)
O3 Mo2 O20 83.8(1)
O3 Mo2 O4 96.1(1)
O3 Mo2 O14 160.7(1)
O3 Mo2 O17 88.1(1)
O4 Mo2 O14 97.6(1)
O4 Mo2 O17 89.8(1)
O4 Mo2 O20 174.6(1)
O14 Mo2 O17 78.6(1)
O14 Mo2 O20 81.2(1)
O17 Mo2 O20 84.8(1)
Mo1 Mo3 Mo2 60.46(1)
Mo1 Mo3 O1 52.32(7)
Mo1 Mo3 O2 50.22(7)
Mo1 Mo3 O3 94.49(8)
Mo1 Mo3 O22 135.68(8)
Mo1 Mo3 O23 140.91(8)
Mo1 Mo3 O26 104.00(8)
Mo2 Mo3 O1 52.28(7)
Mo2 Mo3 O2 95.83(8)
Mo2 Mo3 O3 49.49(8)
Mo2 Mo3 O22 86.25(8)
Mo2 Mo3 O23 134.92(9)
Mo2 Mo3 O26 140.75(8)
O1 Mo3 O2 101.8(1)
O1 Mo3 O3 101.2(1)
O1 Mo3 O22 84.7(1)
O1 Mo3 O23 165.2(1)
O1 Mo3 O26 89.1(1)
O2 Mo3 O3 93.7(1)
O2 Mo3 O22 173.1(1)
O2 Mo3 O23 90.7(1)
O2 Mo3 O26 99.3(1)
O3 Mo3 O22 82.6(1)
O3 Mo3 O23 85.7(1)
O3 Mo3 O26 161.4(1)
O22 Mo3 O26 83.0(1)
O22 Mo3 O23 83.2(1)
O23 Mo3 O26 81.0(1)
Mo1 O1 Mo2 76.18(9)
Mo1 O1 Mo3 75.79(8)
Mo2 O1 Mo3 75.80(8)
Mo1 O2 Mo3 80.56(9)
Mo1 O4 Mo2 81.6(1)
Mo2 O3 Mo3 80.5(1)
Mo1 O5 C6 127.8(3)
Mo1 O8 C9 131.2(3)
Mo1 O11 C12 125.9(3)
Mo2 O14 C15 129.9(3)
Mo2 O17 C18 130.2(3)
Mo2 O20 C21 119.9(3)
Mo3 O22 C21 120.3(3)
Mo3 O23 C24 126.6(3)
Mo3 O26 C27 127.9(3)
O5 C6 O7 124.5(4)
O8 C9 O10 127.9(4)
O11 C12 O13 125.9(5)
O14 C15 O16 123.1(4)
O17 C18 O19 128.2(5)
O20 C21 O22 126.3(4)
O26 C27 O28 125.3(4)
O23 C24 O25 125.1(4)
O29 C30 O31 129.9(6)
O5 C6 H6 119(3)
O7 C6 H6 117(2)
O8 C9 H9 110(2)
O10 C9 H9 122(2)
O11 C12 H12 114(3)
O13 C12 H12 119(3)
O14 C15 H15 114(3)
O16 C15 H15 123(3)
O17 C18 H18 109(4)
O19 C18 H18 123(4)
O20 C21 H21 120(3)
O22 C21 H21 113(3)
O23 C24 H24 117(3)
O25 C24 H24 118(3)
O26 C27 H27 118(3)
O28 C27 H27 116(3)
O29 C30 H30 111(2)
O31 C30 H30 119(2)
H32a O32 H32b 101(5)
H32a O32 H32c 119(7)
H32b O32 H32c 110(7)
H33a O33 H33b 90(10)
H34a N34 H34b 108(6)
H34a N34 H34c 115(5)
H34a N34 H34d 117(5)
H34b N34 H34c 106(7)
H34b N34 H34d 108(6)
H34c N34 H34d 102(6)
H35a N35 H35b 105(6)
H35a N35 H35c 115(6)
H35a N35 H35d 100(7)
H35b N35 H35c 122(5)
H35b N35 H35d 108(7)
H35c N35 H35d 104(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mo1 Mo2 2.506(1)
Mo1 Mo3 2.489(1)
Mo2 Mo3 2.488(1)
Mo1 O1 2.032(3)
Mo1 O2 1.939(2)
Mo1 O4 1.936(3)
Mo1 O5 2.105(3)
Mo1 O8 2.117(3)
Mo1 O11 2.067(3)
Mo2 O1 2.030(2)
Mo2 O3 1.918(3)
Mo2 O4 1.898(3)
Mo2 O14 2.068(3)
Mo2 O17 2.118(3)
Mo2 O20 2.193(3)
Mo3 O1 2.020(3)
Mo3 O2 1.910(3)
Mo3 O3 1.933(3)
Mo3 O26 2.054(3)
Mo3 O23 2.118(3)
Mo3 O22 2.199(3)
O5 C6 1.272(5)
C6 O7 1.215(5)
O8 C9 1.283(5)
C9 O10 1.211(5)
O11 C12 1.301(5)
C12 O13 1.184(6)
O14 C15 1.284(5)
C15 O16 1.197(5)
O17 C18 1.275(6)
C18 O19 1.205(6)
O20 C21 1.245(5)
C21 O22 1.268(5)
O23 C24 1.265(5)
C24 O25 1.233(5)
O26 C27 1.272(5)
C27 O28 1.219(5)
O29 C30 1.238(6)
C30 O31 1.218(7)
C6 H6 0.98(5)
C9 H9 1.01(5)
C12 H12 1.08(6)
C15 H15 1.05(6)
C18 H18 0.89(7)
C21 H21 0.95(5)
C24 H24 1.04(5)
C27 H27 0.96(5)
C30 H30 1.14(4)
O32 H32a 0.87(7)
O32 H32b 0.96(7)
O32 H32c 0.86(10)
O33 H33a 0.78(9)
O33 H33b 0.58(7)
N34 H34a 0.80(5)
N34 H34b 0.83(9)
N34 H34c 0.80(6)
N34 H34d 0.98(7)
N35 H35a 0.69(5)
N35 H35b 0.91(7)
N35 H35c 1.04(8)
N35 H35d 0.74(7)
