#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/89/4318934.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_4318934
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         'Gd6 Mo12 O45 '
_chemical_formula_sum            'Gd6 Mo12 O45'
_chemical_formula_weight         2814.75
_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                104.170(1)
_cell_angle_beta                 109.288(4)
_cell_angle_gamma                109.266(2)
_cell_formula_units_Z            1
_cell_length_a                   9.3409(3)
_cell_length_b                   10.8826(5)
_cell_length_c                   11.4377(5)
_cell_measurement_reflns_used    3439
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.5
_cell_volume                     950.79(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    none
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9977
_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  0.039
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9215
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    14.248
_exptl_absorpt_correction_T_max  0.643
_exptl_absorpt_correction_T_min  0.344
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Higashi, 1999a,b)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.916
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.07
_refine_diff_density_min         -1.87
_refine_ls_extinction_coef       0.0041(2)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4328
_refine_ls_R_factor_gt           0.0249
_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         0.0670
_reflns_number_gt                3802
_reflns_number_total             4329
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic025697z_1.cif
_cod_data_source_block           gd6mo12
_cod_original_cell_volume        950.80(8)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'Gd6 Mo12 O45 '
_cod_database_code               4318934
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
Gd1 Gd 0.21477(4) 0.05605(3) 0.58977(3) 0.00886(7) Uani 1.00 d . . .
Gd2 Gd -0.23581(4) -0.22320(3) 0.82440(3) 0.00802(7) Uani 1.00 d . . .
Gd3 Gd -0.33719(4) -0.66004(3) 0.20121(3) 0.00772(7) Uani 1.00 d . . .
Mo1 Mo 0.58451(7) 0.22318(5) 0.48091(5) 0.0087(1) Uani 1.00 d . . .
Mo2 Mo 0.06660(6) -0.13193(5) 0.20232(5) 0.0090(1) Uani 1.00 d . . .
Mo3 Mo -0.08582(6) -0.31164(5) 0.55209(5) 0.0084(1) Uani 1.00 d . . .
Mo4 Mo 0.91160(6) 0.46778(5) 0.81811(5) 0.0076(1) Uani 1.00 d . . .
Mo5 Mo -0.26655(6) -0.98136(5) 0.08020(5) 0.0082(1) Uani 1.00 d . . .
Mo6 Mo -0.47441(6) -0.56625(5) -0.13336(5) 0.0080(1) Uani 1.00 d . . .
O1 O 0.4163(6) 0.1648(5) 0.5213(5) 0.017(1) Uani 1.00 d . . .
O2 O 0.3334(6) 0.2862(4) 0.7547(4) 0.015(1) Uani 1.00 d . . .
O3 O 0.2890(6) 0.0142(5) 0.7826(5) 0.017(1) Uani 1.00 d . . .
O4 O -0.0331(5) -0.1579(4) 0.5127(4) 0.012(1) Uani 1.00 d . . .
O5 O 0.0289(6) -0.0663(4) 0.3406(4) 0.017(1) Uani 1.00 d . . .
O6 O 0.6582(6) 0.0970(5) 0.4513(5) 0.020(1) Uani 1.00 d . . .
O7 O 0.5250(5) 0.2654(4) 0.3381(4) 0.013(1) Uani 1.00 d . . .
O8 O 0.7549(6) 0.3822(4) 0.6178(4) 0.016(1) Uani 1.00 d . . .
O9 O 1.0000 0.5000 1.0000 0.019(2) Uani 1.00 d S . .
O10 O 0.2209(6) 0.0104(5) 0.1994(5) 0.017(1) Uani 1.00 d . . .
O11 O 0.1508(6) -0.2542(4) 0.2258(5) 0.016(1) Uani 1.00 d . . .
O12 O -0.1192(6) -0.2151(4) 0.0506(4) 0.015(1) Uani 1.00 d . . .
O13 O 0.1023(6) -0.3031(5) 0.6637(5) 0.018(1) Uani 1.00 d . . .
O14 O -0.2249(6) -0.3073(5) 0.6230(4) 0.016(1) Uani 1.00 d . . .
O15 O -0.1075(6) -0.3792(4) 0.8327(4) 0.016(1) Uani 1.00 d . . .
O16 O -0.1900(6) -0.4642(5) 0.4049(4) 0.016(1) Uani 1.00 d . . .
O17 O -0.0939(6) -0.5031(5) 0.1997(5) 0.017(1) Uani 1.00 d . . .
O18 O -0.4107(6) -0.5574(4) 0.0408(4) 0.014(1) Uani 1.00 d . . .
O19 O -0.3323(6) -0.8525(4) 0.0542(4) 0.013(1) Uani 1.00 d . . .
O20 O -0.0535(6) -0.9203(5) 0.1126(5) 0.018(1) Uani 1.00 d . . .
O21 O -0.3837(5) -1.1450(4) -0.0666(4) 0.011(1) Uani 1.00 d . . .
O22 O -0.3282(6) -0.6131(5) -0.1673(5) 0.018(1) Uani 1.00 d . . .
O23 O -0.4505(5) -0.4255(4) -0.1956(4) 0.011(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
O O 0.011 0.006
;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)
;
Gd Gd -0.165 3.904
;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 GD1 O1 122.2(2) . . . yes
O3 GD1 O2 79.3(2) . . . yes
O3 GD1 O4 82.1(2) . . . yes
O3 GD1 O6 77.4(2) . . 2_656 yes
O3 GD1 O4 135.3(2) . . 2_556 yes
O3 GD1 O5 142.1(1) . . . yes
O3 GD1 O5 78.1(2) . . 2_556 yes
O1 GD1 O2 83.4(2) . . . yes
O1 GD1 O4 140.6(2) . . . yes
O1 GD1 O6 73.2(2) . . 2_656 yes
O1 GD1 O4 91.5(1) . . 2_556 yes
O1 GD1 O5 82.3(2) . . . yes
O1 GD1 O5 146.7(1) . . 2_556 yes
O2 GD1 O4 134.4(2) . . . yes
O2 GD1 O6 130.2(2) . . 2_656 yes
O2 GD1 O4 76.2(1) . . 2_556 yes
O2 GD1 O5 135.9(1) . . . yes
O2 GD1 O5 74.4(1) . . 2_556 yes
O4 GD1 O6 84.5(2) . . 2_656 yes
O4 GD1 O4 89.0(1) . . 2_556 yes
O4 GD1 O5 63.2(1) . . . yes
O4 GD1 O5 61.1(1) . . 2_556 yes
O6 GD1 O4 145.4(1) 2_656 . 2_556 yes
O6 GD1 O5 84.3(2) 2_656 . . yes
O6 GD1 O5 139.9(1) 2_656 . 2_556 yes
O4 GD1 O5 62.7(1) 2_556 . . yes
O4 GD1 O5 59.6(1) 2_556 . 2_556 yes
O5 GD1 O5 96.4(1) . . 2_556 yes
O14 GD2 O23 100.7(2) . . 1_556 yes
O14 GD2 O10 91.6(2) . . 2_556 yes
O14 GD2 O21 146.9(1) . . 1_566 yes
O14 GD2 O20 79.3(2) . . 2_546 yes
O14 GD2 O15 70.4(1) . . . yes
O14 GD2 O12 139.2(1) . . 1_556 yes
O14 GD2 O7 80.6(1) . . 2_556 yes
O23 GD2 O10 134.5(1) 1_556 . 2_556 yes
O23 GD2 O21 73.0(1) 1_556 . 1_566 yes
O23 GD2 O20 151.4(1) 1_556 . 2_546 yes
O23 GD2 O15 77.9(1) 1_556 . . yes
O23 GD2 O12 79.0(1) 1_556 . 1_556 yes
O23 GD2 O7 68.9(1) 1_556 . 2_556 yes
O10 GD2 O21 73.1(1) 2_556 . 1_566 yes
O10 GD2 O20 73.8(2) 2_556 . 2_546 yes
O10 GD2 O15 146.5(2) 2_556 . . yes
O10 GD2 O12 117.8(2) 2_556 . 1_556 yes
O10 GD2 O7 70.3(1) 2_556 . 2_556 yes
O21 GD2 O20 121.9(1) 1_566 . 2_546 yes
O21 GD2 O15 136.0(1) 1_566 . . yes
O21 GD2 O12 72.8(1) 1_566 . 1_556 yes
O21 GD2 O7 66.7(1) 1_566 . 2_556 yes
O20 GD2 O15 75.2(2) 2_546 . . yes
O20 GD2 O12 82.7(2) 2_546 . 1_556 yes
O20 GD2 O7 137.9(1) 2_546 . 2_556 yes
O15 GD2 O12 69.8(1) . . 1_556 yes
O15 GD2 O7 130.4(1) . . 2_556 yes
O12 GD2 O7 133.8(1) 1_556 . 2_556 yes
O16 GD3 O17 72.5(2) . . . yes
O16 GD3 O19 146.9(2) . . . yes
O16 GD3 O18 102.2(1) . . . yes
O16 GD3 O21 138.6(2) . . 2_435 yes
O16 GD3 O23 78.4(1) . . 2_445 yes
O16 GD3 O13 75.4(2) . . 2_546 yes
O16 GD3 O7 76.3(2) . . 1_445 yes
O17 GD3 O19 89.4(2) . . . yes
O17 GD3 O18 68.5(2) . . . yes
O17 GD3 O21 145.8(1) . . 2_435 yes
O17 GD3 O23 114.9(1) . . 2_445 yes
O17 GD3 O13 74.5(2) . . 2_546 yes
O17 GD3 O7 146.8(2) . . 1_445 yes
O19 GD3 O18 96.2(1) . . . yes
O19 GD3 O21 68.8(1) . . 2_435 yes
O19 GD3 O23 134.7(1) . . 2_445 yes
O19 GD3 O13 73.1(1) . . 2_546 yes
O19 GD3 O7 111.6(1) . . 1_445 yes
O18 GD3 O21 87.4(1) . . 2_435 yes
O18 GD3 O23 62.8(1) . . 2_445 yes
O18 GD3 O13 141.6(2) . . 2_546 yes
O18 GD3 O7 130.4(1) . . 1_445 yes
O21 GD3 O23 70.5(1) 2_435 . 2_445 yes
O21 GD3 O13 120.2(1) 2_435 . 2_546 yes
O21 GD3 O7 67.4(1) 2_435 . 1_445 yes
O23 GD3 O13 147.7(2) 2_445 . 2_546 yes
O23 GD3 O7 68.6(1) 2_445 . 1_445 yes
O13 GD3 O7 87.0(2) 2_546 . 1_445 yes
O6 MO1 O1 111.5(2) . . . yes
O6 MO1 O7 109.3(2) . . . yes
O6 MO1 O8 108.6(2) . . . yes
O1 MO1 O7 111.3(2) . . . yes
O1 MO1 O8 109.3(2) . . . yes
O7 MO1 O8 106.7(2) . . . yes
O12 MO2 O10 110.5(2) . . . yes
O12 MO2 O5 111.3(2) . . . yes
O12 MO2 O11 109.8(2) . . . yes
O10 MO2 O5 108.2(2) . . . yes
O10 MO2 O11 107.4(2) . . . yes
O5 MO2 O11 109.6(2) . . . yes
O16 MO3 O14 109.0(2) . . . yes
O16 MO3 O13 110.7(2) . . . yes
O16 MO3 O4 109.8(2) . . . yes
O14 MO3 O13 112.7(2) . . . yes
O14 MO3 O4 106.1(2) . . . yes
O13 MO3 O4 108.5(2) . . . yes
O15 MO4 O17 102.9(2) 1_665 . 2_656 yes
O15 MO4 O9 97.9(1) 1_665 . . yes
O15 MO4 O8 90.1(2) 1_665 . . yes
O15 MO4 O11 161.2(2) 1_665 . 2_656 yes
O15 MO4 O22 86.3(2) 1_665 . 1_666 yes
O17 MO4 O9 98.6(2) 2_656 . . yes
O17 MO4 O8 95.2(2) 2_656 . . yes
O17 MO4 O11 93.7(2) 2_656 . 2_656 yes
O17 MO4 O22 170.7(2) 2_656 . 1_666 yes
O9 MO4 O8 162.0(1) . . . yes
O9 MO4 O11 88.2(1) . . 2_656 yes
O9 MO4 O22 81.3(1) . . 1_666 yes
O8 MO4 O11 79.6(2) . . 2_656 yes
O8 MO4 O22 83.1(2) . . 1_666 yes
O11 MO4 O22 77.0(2) 2_656 . 1_666 yes
O20 MO5 O3 109.4(2) . . 2_546 yes
O20 MO5 O19 108.9(2) . . . yes
O20 MO5 O21 106.7(2) . . . yes
O3 MO5 O19 110.6(2) 2_546 . . yes
O3 MO5 O21 109.2(2) 2_546 . . yes
O19 MO5 O21 112.0(2) . . . yes
O22 MO6 O2 103.1(2) . . 1_444 yes
O22 MO6 O23 98.1(2) . . . yes
O22 MO6 O18 99.3(2) . . . yes
O22 MO6 O18 161.8(2) . . 2_445 yes
O2 MO6 O23 109.4(2) 1_444 . . yes
O2 MO6 O18 111.1(2) 1_444 . . yes
O2 MO6 O18 95.1(2) 1_444 . 2_445 yes
O23 MO6 O18 130.4(2) . . . yes
O23 MO6 O18 75.6(2) . . 2_445 yes
O18 MO6 O18 73.5(2) . . 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
GD1 O3 2.289(4) . . yes
GD1 O1 2.349(4) . . yes
GD1 O2 2.352(4) . . yes
GD1 O4 2.377(4) . . yes
GD1 O6 2.385(4) . 2_656 yes
GD1 O4 2.459(4) . 2_556 yes
GD1 O5 2.501(4) . . yes
GD1 O5 2.673(5) . 2_556 yes
GD2 O14 2.311(4) . . yes
GD2 O23 2.336(4) . 1_556 yes
GD2 O10 2.362(4) . 2_556 yes
GD2 O21 2.363(4) . 1_566 yes
GD2 O20 2.375(4) . 2_546 yes
GD2 O15 2.382(4) . . yes
GD2 O12 2.419(4) . 1_556 yes
GD2 O7 2.531(4) . 2_556 yes
GD3 O16 2.319(4) . . yes
GD3 O17 2.359(4) . . yes
GD3 O19 2.368(4) . . yes
GD3 O18 2.400(4) . . yes
GD3 O21 2.402(4) . 2_435 yes
GD3 O23 2.443(4) . 2_445 yes
GD3 O13 2.451(4) . 2_546 yes
GD3 O7 2.456(4) . 1_445 yes
MO1 O6 1.740(4) . . yes
MO1 O1 1.746(5) . . yes
MO1 O7 1.768(4) . . yes
MO1 O8 1.786(4) . . yes
MO2 O12 1.746(4) . . yes
MO2 O10 1.749(4) . . yes
MO2 O5 1.766(4) . . yes
MO2 O11 1.785(4) . . yes
MO3 O16 1.738(4) . . yes
MO3 O14 1.751(5) . . yes
MO3 O13 1.754(4) . . yes
MO3 O4 1.793(4) . . yes
MO4 O15 1.707(4) . 1_665 yes
MO4 O17 1.710(4) . 2_656 yes
MO4 O9 1.8574(5) . . yes
MO4 O8 2.025(4) . . yes
MO4 O11 2.083(4) . 2_656 yes
MO4 O22 2.200(5) . 1_666 yes
MO5 O20 1.749(5) . . yes
MO5 O3 1.754(4) . 2_546 yes
MO5 O19 1.756(4) . . yes
MO5 O21 1.796(4) . . yes
MO6 O22 1.729(5) . . yes
MO6 O2 1.736(4) . 1_444 yes
MO6 O23 1.821(4) . . yes
MO6 O18 1.849(4) . . yes
MO6 O18 2.256(4) . 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
GD1 GD1 3.4502(6) . 2_556 yes
GD1 GD2 5.5124(4) . 2_556 yes
GD1 GD3 5.6644(4) . 2_546 yes
GD1 GD3 5.9807(4) . 2_556 yes
GD1 GD2 6.0964(4) . . yes
GD1 GD3 6.1256(4) . 1_666 yes
GD1 GD2 6.4165(4) . 2_557 yes
GD1 GD1 6.6627(6) . 2_656 yes
GD1 GD2 6.9255(4) . 1_655 yes
GD1 GD3 6.9610(4) . . yes
GD1 GD2 7.0067(4) . 1_665 yes
GD1 GD3 7.5690(4) . 1_665 yes
GD1 GD2 7.6012(4) . 1_554 yes
GD1 GD3 7.6142(4) . 1_565 yes
GD1 GD3 8.7307(4) . 2_445 yes
GD1 GD2 8.9182(4) . 2_657 yes
GD1 GD2 9.1584(4) . 2_446 yes
GD1 GD2 9.2410(4) . 2_546 yes
GD1 GD3 9.2824(5) . 2_446 yes
GD1 GD1 9.3409(3) . 1_655 yes
GD1 GD1 9.3409(3) . 1_455 yes
GD1 GD3 9.4400(5) . 2_656 yes
GD1 GD3 9.6294(4) . 2_545 yes
GD1 GD1 9.7367(5) . 2_657 yes
GD1 GD2 9.7953(5) . 2_456 yes
GD1 GD1 9.9205(5) . 2_667 yes
GD2 GD3 3.6484(4) . 2_446 yes
GD2 GD2 4.8760(5) . 2_557 yes
GD2 GD3 5.9740(4) . 2_546 yes
GD2 GD2 7.0723(5) . 2_446 yes
GD2 GD3 7.0910(4) . . yes
GD2 GD3 7.1152(4) . 1_566 yes
GD2 GD3 7.1992(4) . 1_556 yes
GD2 GD3 7.4709(4) . 1_666 yes
GD2 GD3 9.0519(5) . 1_455 yes
GD2 GD2 9.0617(5) . 2_447 yes
GD2 GD2 9.1357(6) . 2_457 yes
GD2 GD2 9.3409(3) . 1_655 yes
GD2 GD2 9.3409(3) . 1_455 yes
GD2 GD2 9.4609(5) . 2_547 yes
GD2 GD3 9.4652(4) . 2_556 yes
GD3 GD3 6.6295(5) . 2_546 yes
GD3 GD3 6.6642(5) . 2_435 yes
GD3 GD3 6.9401(5) . 2_445 yes
GD3 GD3 8.7846(6) . 2_446 yes
GD3 GD3 9.2480(6) . 2_545 yes
GD3 GD3 9.3409(3) . 1_655 yes
GD3 GD3 9.3409(3) . 1_455 yes
