#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/89/4318937.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_4318937
loop_
_publ_author_name
'Haruo Naruke'
'Toshihiro Yamase'
_publ_contact_author_address
; Chemical Resources Laboratory
Tokyo Institute of Technology
4259 Nagatsuta, Midori-ku, Yokohama 226-8503
Japan
;
_publ_contact_author_email       ' hnaruke@res.titech.ac.jp'
_publ_contact_author_fax         ' +81-(0)45-924-5276 '
_publ_contact_author_name        ' Haruo Naruke'
_publ_contact_author_phone       ' +81-(0)45-924-5271 '
_publ_section_title
;
 Structures of Novel R₂Mo₅O₁₈ and R₆Mo₁₂O₄₅ (R= Eu and Gd)
 Prepared by Thermal Decomposition of Polyoxomolybdate Precursor
 [R₂(H₂O)₁₂Mo₈O₂₇].nH₂O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6514
_journal_page_last               6520
_journal_paper_doi               10.1021/ic025697z
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'Eu6 Mo12 O45 '
_chemical_formula_sum            'Eu6 Mo12 O45'
_chemical_formula_weight         2783.01
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                104.194(2)
_cell_angle_beta                 109.567(3)
_cell_angle_gamma                108.998(2)
_cell_formula_units_Z            1
_cell_length_a                   9.3867(4)
_cell_length_b                   10.9408(5)
_cell_length_c                   11.4817(5)
_cell_measurement_reflns_used    3850
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.1
_cell_volume                     963.93(8)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.11'
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9864
_diffrn_measured_fraction_theta_max 0.9864
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7502
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_exptl_absorpt_coefficient_mu    13.444
_exptl_absorpt_correction_T_max  0.577
_exptl_absorpt_correction_T_min  0.259
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Higashi, 1999a,b)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.794
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.100
_refine_diff_density_max         3.03
_refine_diff_density_min         -2.82
_refine_ls_extinction_coef       0.0087(4)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.350
_refine_ls_number_parameters     287
_refine_ls_number_reflns         5526
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.0006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.05000(Max(Fo²,0) + 2Fc²)/3)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                4739
_reflns_number_total             5532
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic025697z_4.cif
_cod_data_source_block           eu6mo12
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'Eu6 Mo12 O45 '
_cod_database_code               4318937
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.21554(5) 0.05626(4) 0.59007(4) 0.00903(9) Uani 1.00 d . . .
Eu2 Eu -0.23542(4) -0.22283(4) 0.82465(4) 0.00830(9) Uani 1.00 d . . .
Eu3 Eu -0.33645(4) -0.65973(4) 0.20121(4) 0.00785(8) Uani 1.00 d . . .
Mo1 Mo 0.58456(8) 0.22330(7) 0.48106(6) 0.0089(1) Uani 1.00 d . . .
Mo2 Mo 0.06688(8) -0.13229(6) 0.20279(6) 0.0092(1) Uani 1.00 d . . .
Mo3 Mo -0.08584(8) -0.31165(6) 0.55226(6) 0.0085(1) Uani 1.00 d . . .
Mo4 Mo 0.91123(8) 0.46753(6) 0.81830(6) 0.0076(1) Uani 1.00 d . . .
Mo5 Mo -0.26694(8) -0.98154(6) 0.07984(6) 0.0085(1) Uani 1.00 d . . .
Mo6 Mo -0.47338(8) -0.56609(6) -0.13302(6) 0.0082(1) Uani 1.00 d . . .
O1 O 0.4169(7) 0.1637(6) 0.5211(6) 0.018(1) Uani 1.00 d . . .
O2 O 0.3341(7) 0.2865(6) 0.7550(6) 0.014(1) Uani 1.00 d . . .
O3 O 0.2897(8) 0.0154(7) 0.7841(6) 0.020(1) Uani 1.00 d . . .
O4 O -0.0349(7) -0.1588(6) 0.5120(6) 0.015(1) Uani 1.00 d . . .
O5 O 0.0305(8) -0.0662(6) 0.3412(6) 0.017(1) Uani 1.00 d . . .
O6 O 0.6595(8) 0.0984(7) 0.4518(6) 0.021(2) Uani 1.00 d . . .
O7 O 0.5240(7) 0.2654(6) 0.3380(6) 0.014(1) Uani 1.00 d . . .
O8 O 0.7532(8) 0.3824(6) 0.6180(6) 0.019(1) Uani 1.00 d . . .
O9 O 1.0000 0.5000 1.0000 0.019(2) Uani 1.00 d S . .
O10 O 0.2189(7) 0.0092(6) 0.1985(6) 0.018(1) Uani 1.00 d . . .
O11 O 0.1508(7) -0.2543(6) 0.2262(6) 0.017(1) Uani 1.00 d . . .
O12 O -0.1187(8) -0.2140(6) 0.0511(6) 0.017(1) Uani 1.00 d . . .
O13 O 0.1003(7) -0.3025(6) 0.6638(6) 0.018(1) Uani 1.00 d . . .
O14 O -0.2238(8) -0.3079(7) 0.6229(6) 0.019(2) Uani 1.00 d . . .
O15 O -0.1068(7) -0.3785(6) 0.8338(6) 0.015(1) Uani 1.00 d . . .
O16 O -0.1897(8) -0.4639(6) 0.4046(6) 0.019(1) Uani 1.00 d . . .
O17 O -0.0899(7) -0.5016(6) 0.2006(7) 0.018(2) Uani 1.00 d . . .
O18 O -0.4080(7) -0.5559(6) 0.0416(6) 0.016(1) Uani 1.00 d . . .
O19 O -0.3323(7) -0.8538(6) 0.0534(5) 0.012(1) Uani 1.00 d . . .
O20 O -0.0540(7) -0.9219(6) 0.1126(6) 0.016(1) Uani 1.00 d . . .
O21 O -0.3852(7) -1.1444(6) -0.0663(5) 0.011(1) Uani 1.00 d . . .
O22 O -0.3264(7) -0.6123(7) -0.1677(7) 0.019(2) Uani 1.00 d . . .
O23 O -0.4506(7) -0.4255(5) -0.1933(6) 0.010(1) Uani 1.00 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Eu Eu -0.158 3.668
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Mo Mo -1.683 0.686
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 EU1 O1 122.4(2) . . . yes
O3 EU1 O2 79.2(2) . . . yes
O3 EU1 O6 77.8(2) . . 2_656 yes
O3 EU1 O4 82.1(2) . . . yes
O3 EU1 O4 134.8(2) . . 2_556 yes
O3 EU1 O5 142.1(2) . . . yes
O3 EU1 O5 77.9(2) . . 2_556 yes
O1 EU1 O2 83.5(2) . . . yes
O1 EU1 O6 73.3(2) . . 2_656 yes
O1 EU1 O4 140.6(2) . . . yes
O1 EU1 O4 91.5(2) . . 2_556 yes
O1 EU1 O5 82.2(2) . . . yes
O1 EU1 O5 147.0(2) . . 2_556 yes
O2 EU1 O6 130.7(2) . . 2_656 yes
O2 EU1 O4 134.4(2) . . . yes
O2 EU1 O4 75.9(2) . . 2_556 yes
O2 EU1 O5 136.0(2) . . . yes
O2 EU1 O5 74.7(2) . . 2_556 yes
O6 EU1 O4 84.2(2) 2_656 . . yes
O6 EU1 O4 145.4(2) 2_656 . 2_556 yes
O6 EU1 O5 83.7(2) 2_656 . . yes
O6 EU1 O5 139.5(2) 2_656 . 2_556 yes
O4 EU1 O4 89.1(2) . . 2_556 yes
O4 EU1 O5 63.1(2) . . . yes
O4 EU1 O5 60.7(2) . . 2_556 yes
O4 EU1 O5 63.1(2) 2_556 . . yes
O4 EU1 O5 59.6(2) 2_556 . 2_556 yes
O5 EU1 O5 96.4(2) . . 2_556 yes
O14 EU2 O23 101.3(2) . . 1_556 yes
O14 EU2 O10 91.9(2) . . 2_556 yes
O14 EU2 O15 70.2(2) . . . yes
O14 EU2 O21 147.0(2) . . 1_566 yes
O14 EU2 O20 79.0(2) . . 2_546 yes
O14 EU2 O12 139.1(2) . . 1_556 yes
O14 EU2 O7 80.9(2) . . 2_556 yes
O23 EU2 O10 135.0(2) 1_556 . 2_556 yes
O23 EU2 O15 77.8(2) 1_556 . . yes
O23 EU2 O21 72.5(2) 1_556 . 1_566 yes
O23 EU2 O20 151.7(2) 1_556 . 2_546 yes
O23 EU2 O12 78.5(2) 1_556 . 1_556 yes
O23 EU2 O7 69.1(2) 1_556 . 2_556 yes
O10 EU2 O15 146.2(2) 2_556 . . yes
O10 EU2 O21 73.4(2) 2_556 . 1_566 yes
O10 EU2 O20 72.9(2) 2_556 . 2_546 yes
O10 EU2 O12 117.5(2) 2_556 . 1_556 yes
O10 EU2 O7 70.9(2) 2_556 . 2_556 yes
O15 EU2 O21 135.8(2) . . 1_566 yes
O15 EU2 O20 75.7(2) . . 2_546 yes
O15 EU2 O12 69.9(2) . . 1_556 yes
O15 EU2 O7 130.3(2) . . 2_556 yes
O21 EU2 O20 122.0(2) 1_566 . 2_546 yes
O21 EU2 O12 72.7(2) 1_566 . 1_556 yes
O21 EU2 O7 66.6(2) 1_566 . 2_556 yes
O20 EU2 O12 83.1(2) 2_546 . 1_556 yes
O20 EU2 O7 137.6(2) 2_546 . 2_556 yes
O12 EU2 O7 133.6(2) 1_556 . 2_556 yes
O16 EU3 O19 147.1(2) . . . yes
O16 EU3 O17 72.3(2) . . . yes
O16 EU3 O18 101.6(2) . . . yes
O16 EU3 O21 138.8(2) . . 2_435 yes
O16 EU3 O23 78.6(2) . . 2_445 yes
O16 EU3 O13 75.9(2) . . 2_546 yes
O16 EU3 O7 76.7(2) . . 1_445 yes
O19 EU3 O17 89.6(2) . . . yes
O19 EU3 O18 96.4(2) . . . yes
O19 EU3 O21 68.3(2) . . 2_435 yes
O19 EU3 O23 134.3(2) . . 2_445 yes
O19 EU3 O13 72.8(2) . . 2_546 yes
O19 EU3 O7 111.3(2) . . 1_445 yes
O17 EU3 O18 68.2(2) . . . yes
O17 EU3 O21 146.1(2) . . 2_435 yes
O17 EU3 O23 115.0(2) . . 2_445 yes
O17 EU3 O13 74.2(2) . . 2_546 yes
O17 EU3 O7 146.9(2) . . 1_445 yes
O18 EU3 O21 88.3(2) . . 2_435 yes
O18 EU3 O23 62.7(2) . . 2_445 yes
O18 EU3 O13 141.0(2) . . 2_546 yes
O18 EU3 O7 130.5(2) . . 1_445 yes
O21 EU3 O23 70.7(2) 2_435 . 2_445 yes
O21 EU3 O13 119.7(2) 2_435 . 2_546 yes
O21 EU3 O7 67.0(2) 2_435 . 1_445 yes
O23 EU3 O13 148.4(2) 2_445 . 2_546 yes
O23 EU3 O7 68.7(2) 2_445 . 1_445 yes
O13 EU3 O7 87.5(2) 2_546 . 1_445 yes
O6 MO1 O1 111.2(3) . . . yes
O6 MO1 O7 109.4(3) . . . yes
O6 MO1 O8 108.9(3) . . . yes
O1 MO1 O7 111.4(3) . . . yes
O1 MO1 O8 109.2(3) . . . yes
O7 MO1 O8 106.5(3) . . . yes
O12 MO2 O10 109.8(3) . . . yes
O12 MO2 O5 111.3(3) . . . yes
O12 MO2 O11 110.0(3) . . . yes
O10 MO2 O5 108.2(3) . . . yes
O10 MO2 O11 107.9(3) . . . yes
O5 MO2 O11 109.6(3) . . . yes
O13 MO3 O16 111.0(3) . . . yes
O13 MO3 O14 112.3(3) . . . yes
O13 MO3 O4 108.7(3) . . . yes
O16 MO3 O14 109.0(3) . . . yes
O16 MO3 O4 109.5(3) . . . yes
O14 MO3 O4 106.3(3) . . . yes
O17 MO4 O15 102.5(3) 2_656 . 1_665 yes
O17 MO4 O9 99.1(2) 2_656 . . yes
O17 MO4 O8 95.1(3) 2_656 . . yes
O17 MO4 O11 93.6(3) 2_656 . 2_656 yes
O17 MO4 O22 170.7(3) 2_656 . 1_666 yes
O15 MO4 O9 97.5(2) 1_665 . . yes
O15 MO4 O8 90.3(3) 1_665 . . yes
O15 MO4 O11 161.6(3) 1_665 . 2_656 yes
O15 MO4 O22 86.6(2) 1_665 . 1_666 yes
O9 MO4 O8 161.9(2) . . . yes
O9 MO4 O11 88.4(2) . . 2_656 yes
O9 MO4 O22 81.4(2) . . 1_666 yes
O8 MO4 O11 79.5(2) . . 2_656 yes
O8 MO4 O22 82.8(2) . . 1_666 yes
O11 MO4 O22 77.1(2) 2_656 . 1_666 yes
O19 MO5 O3 111.1(3) . . 2_546 yes
O19 MO5 O20 109.1(3) . . . yes
O19 MO5 O21 111.8(2) . . . yes
O3 MO5 O20 109.5(3) 2_546 . . yes
O3 MO5 O21 108.3(3) 2_546 . . yes
O20 MO5 O21 107.0(2) . . . yes
O22 MO6 O2 103.3(3) . . 1_444 yes
O22 MO6 O23 98.1(3) . . . yes
O22 MO6 O18 99.7(3) . . . yes
O22 MO6 O18 162.4(3) . . 2_445 yes
O2 MO6 O23 109.9(3) 1_444 . . yes
O2 MO6 O18 111.2(3) 1_444 . . yes
O2 MO6 O18 94.3(2) 1_444 . 2_445 yes
O23 MO6 O18 129.5(2) . . . yes
O23 MO6 O18 75.3(2) . . 2_445 yes
O18 MO6 O18 73.6(3) . . 2_445 yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
EU1 O3 2.302(7) . . yes
EU1 O1 2.365(6) . . yes
EU1 O2 2.365(5) . . yes
EU1 O6 2.396(6) . 2_656 yes
EU1 O4 2.413(5) . . yes
EU1 O4 2.462(6) . 2_556 yes
EU1 O5 2.502(6) . . yes
EU1 O5 2.703(6) . 2_556 yes
EU2 O14 2.328(6) . . yes
EU2 O23 2.371(5) . 1_556 yes
EU2 O10 2.378(6) . 2_556 yes
EU2 O15 2.390(5) . . yes
EU2 O21 2.391(5) . 1_566 yes
EU2 O20 2.395(5) . 2_546 yes
EU2 O12 2.423(6) . 1_556 yes
EU2 O7 2.531(6) . 2_556 yes
EU3 O16 2.326(6) . . yes
EU3 O19 2.392(5) . . yes
EU3 O17 2.400(6) . . yes
EU3 O18 2.406(6) . . yes
EU3 O21 2.415(5) . 2_435 yes
EU3 O23 2.451(5) . 2_445 yes
EU3 O13 2.469(6) . 2_546 yes
EU3 O7 2.483(6) . 1_445 yes
MO1 O6 1.742(6) . . yes
MO1 O1 1.754(6) . . yes
MO1 O7 1.775(6) . . yes
MO1 O8 1.790(6) . . yes
MO2 O12 1.748(6) . . yes
MO2 O10 1.755(6) . . yes
MO2 O5 1.769(6) . . yes
MO2 O11 1.787(6) . . yes
MO3 O13 1.740(6) . . yes
MO3 O16 1.747(6) . . yes
MO3 O14 1.749(6) . . yes
MO3 O4 1.801(6) . . yes
MO4 O17 1.696(6) . 2_656 yes
MO4 O15 1.719(6) . 1_665 yes
MO4 O9 1.8580(6) . . yes
MO4 O8 2.030(6) . . yes
MO4 O11 2.091(6) . 2_656 yes
MO4 O22 2.192(6) . 1_666 yes
MO5 O19 1.750(6) . . yes
MO5 O3 1.754(6) . 2_546 yes
MO5 O20 1.757(6) . . yes
MO5 O21 1.795(5) . . yes
MO6 O22 1.744(6) . . yes
MO6 O2 1.746(5) . 1_444 yes
MO6 O23 1.816(5) . . yes
MO6 O18 1.853(6) . . yes
MO6 O18 2.278(6) . 2_445 yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
EU1 EU1 3.4741(7) . 2_556 yes
EU1 EU2 5.5371(5) . 2_556 yes
EU1 EU3 5.6864(5) . 2_546 yes
EU1 EU3 6.0136(5) . 2_556 yes
EU1 EU3 6.1328(5) . 1_666 yes
EU1 EU2 6.1441(5) . . yes
EU1 EU2 6.4379(5) . 2_557 yes
EU1 EU1 6.6890(7) . 2_656 yes
EU1 EU2 6.9368(6) . 1_655 yes
EU1 EU3 7.0051(5) . . yes
EU1 EU2 7.0600(5) . 1_665 yes
EU1 EU2 7.6147(5) . 1_554 yes
EU1 EU3 7.6254(5) . 1_665 yes
EU1 EU3 7.6307(5) . 1_565 yes
EU1 EU3 8.7523(5) . 2_445 yes
EU1 EU2 8.9259(6) . 2_657 yes
EU1 EU2 9.2307(5) . 2_446 yes
EU1 EU2 9.2879(5) . 2_546 yes
EU1 EU3 9.3644(6) . 2_446 yes
EU1 EU1 9.3867(4) . 1_655 yes
EU1 EU1 9.3867(4) . 1_455 yes
EU1 EU3 9.4953(6) . 2_656 yes
EU1 EU3 9.6662(5) . 2_545 yes
EU1 EU1 9.7436(8) . 2_657 yes
EU1 EU2 9.8217(6) . 2_456 yes
EU1 EU1 9.9575(7) . 2_667 yes
EU2 EU3 3.6798(5) . 2_446 yes
EU2 EU2 4.8930(7) . 2_557 yes
EU2 EU3 5.9938(5) . 2_546 yes
EU2 EU2 7.1024(7) . 2_446 yes
EU2 EU3 7.1211(5) . . yes
EU2 EU3 7.1439(5) . 1_566 yes
EU2 EU3 7.2368(5) . 1_556 yes
EU2 EU3 7.5171(5) . 1_666 yes
EU2 EU3 9.0777(6) . 1_455 yes
EU2 EU2 9.1339(7) . 2_447 yes
EU2 EU2 9.1758(7) . 2_457 yes
EU2 EU2 9.3867(4) . 1_655 yes
EU2 EU2 9.3867(4) . 1_455 yes
EU2 EU2 9.4889(8) . 2_547 yes
EU2 EU3 9.5323(5) . 2_556 yes
EU3 EU3 6.6353(7) . 2_546 yes
EU3 EU3 6.7049(7) . 2_435 yes
EU3 EU3 6.9567(8) . 2_445 yes
EU3 EU3 8.8351(7) . 2_446 yes
EU3 EU3 9.3034(7) . 2_545 yes
EU3 EU3 9.3867(4) . 1_655 yes
EU3 EU3 9.3867(4) . 1_455 yes
