#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/47/4114734.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_4114734
loop_
_publ_author_name
'Chuan-De Wu'
'Can-Zhong Lu'
'Hong-Hui Zhuang'
'Jin-Shun Huang'
_publ_contact_author_address
; 
  The State Key Laboratory of Structural Chemistry,
  Fujian Institute of Research on the Structure of Matter,
  the Chinese Academy of Sciences, 
  Fuzhou, Fujian 350002, 
  P. R. China
;
_publ_contact_author_email       czlu@ms.fjirsm.ac.cn
_publ_contact_author_fax         86-591-3714946
_publ_contact_author_name        'Can-Zhong Lu'
_publ_contact_author_phone       86-591-3792865
_publ_section_title
;
 Hydrothermal Assembly of a Novel Three-Dimensional Framework Formed by
 [GdMo12O42]9- Anions and Nine Coordinated GdIII Cations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3836
_journal_page_last               3837
_journal_paper_doi               10.1021/ja017782w
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'Gd4 H24 Mo12 O60'
_chemical_formula_weight         2764.47
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   17.2627(5)
_cell_length_b                   17.2627(5)
_cell_length_c                   25.6138(8)
_cell_measurement_reflns_used    3761
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.09
_cell_volume                     6610.3(3)
_computing_cell_refinement       'Siemens SMART & SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SMART & SAINT'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6613
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    9.364
_exptl_absorpt_correction_T_max  0.6639
_exptl_absorpt_correction_T_min  0.5106
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    4.167
_exptl_crystal_description       Prism
_exptl_crystal_F_000             7584
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.970
_refine_diff_density_min         -3.144
_refine_diff_density_rms         0.345
_refine_ls_extinction_coef       0.000036(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1311
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_gt           0.0467
_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)+(0.0500P)²+808.1702P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1209
_reflns_number_gt                1131
_reflns_number_total             1311
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja017782w_s3.cif
_cod_data_source_block           JA017782w
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'H24 Gd4 Mo12 O60'
_cod_database_code               4114734
#BEGIN Tags that were not found in dictionaries:
_refine_ls_r_factor_ref          0.0582
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Gd1 Gd 0.0000 0.66261(6) 0.2500 0.0241(3) Uani 1 2 d S
Gd2 Gd -0.3333 0.3333 0.3333 0.0148(4) Uani 1 6 d S
Mo1 Mo -0.11209(7) 0.47856(7) 0.36796(4) 0.0087(3) Uani 1 1 d .
Mo2 Mo -0.18686(7) 0.40450(7) 0.22697(4) 0.0105(3) Uani 1 1 d .
O1 O -0.0949(6) 0.5106(6) 0.2285(3) 0.017(2) Uani 1 1 d .
O2 O -0.2308(5) 0.4954(5) 0.3514(3) 0.0093(17) Uani 1 1 d .
O3 O -0.2326(5) 0.3730(6) 0.4122(3) 0.0109(18) Uani 1 1 d .
O4 O 0.0474(6) 0.6183(6) 0.1691(3) 0.0142(19) Uani 1 1 d .
O5 O 0.1516(6) 0.7777(6) 0.2246(3) 0.018(2) Uani 1 1 d .
O6 O 0.0788(8) 0.7481(7) 0.3295(5) 0.037(3) Uani 1 1 d .
O7 O -0.1337(6) 0.3291(6) 0.2370(3) 0.0155(19) Uani 1 1 d .
O8 O -0.2136(7) 0.3859(7) 0.1625(3) 0.020(2) Uani 1 1 d .
O9 O 0.0000 0.8012(10) 0.2500 0.058(6) Uani 1 2 d S
OW O 0.1295(16) 0.6667 0.4167 0.140(16) Uani 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 '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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Gd1 O1 80.3(4) . 6
O1 Gd1 O9 139.9(2) . .
O1 Gd1 O9 139.9(2) 6 .
O1 Gd1 O5 134.8(3) . .
O1 Gd1 O5 73.6(3) 6 .
O9 Gd1 O5 74.0(2) . .
O1 Gd1 O5 73.6(3) . 6
O1 Gd1 O5 134.8(3) 6 6
O9 Gd1 O5 74.0(2) . 6
O5 Gd1 O5 147.9(4) . 6
O1 Gd1 O4 70.3(3) . 6
O1 Gd1 O4 67.4(3) 6 6
O9 Gd1 O4 118.19(19) . 6
O5 Gd1 O4 127.9(3) . 6
O5 Gd1 O4 69.3(3) 6 6
O1 Gd1 O4 67.4(3) . .
O1 Gd1 O4 70.3(3) 6 .
O9 Gd1 O4 118.2(2) . .
O5 Gd1 O4 69.3(3) . .
O5 Gd1 O4 127.9(3) 6 .
O4 Gd1 O4 123.6(4) 6 .
O1 Gd1 O6 136.2(3) . .
O1 Gd1 O6 76.6(4) 6 .
O9 Gd1 O6 71.3(3) . .
O5 Gd1 O6 72.0(3) . .
O5 Gd1 O6 97.6(3) 6 .
O4 Gd1 O6 66.6(3) 6 .
O4 Gd1 O6 134.4(3) . .
O1 Gd1 O6 76.6(4) . 6
O1 Gd1 O6 136.2(3) 6 6
O9 Gd1 O6 71.3(3) . 6
O5 Gd1 O6 97.6(3) . 6
O5 Gd1 O6 72.0(3) 6 6
O4 Gd1 O6 134.4(3) 6 6
O4 Gd1 O6 66.6(3) . 6
O6 Gd1 O6 142.7(6) . 6
O2 Gd2 O2 63.35(11) 3_455 32_445
O2 Gd2 O2 63.35(11) 3_455 31_455
O2 Gd2 O2 116.64(11) 32_445 31_455
O2 Gd2 O2 180.00(16) 3_455 33
O2 Gd2 O2 116.64(11) 32_445 33
O2 Gd2 O2 116.65(11) 31_455 33
O2 Gd2 O2 116.64(11) 3_455 .
O2 Gd2 O2 63.36(11) 32_445 .
O2 Gd2 O2 179.998(1) 31_455 .
O2 Gd2 O2 63.36(11) 33 .
O2 Gd2 O2 116.64(11) 3_455 2_565
O2 Gd2 O2 180.0 32_445 2_565
O2 Gd2 O2 63.36(11) 31_455 2_565
O2 Gd2 O2 63.36(11) 33 2_565
O2 Gd2 O2 116.64(11) . 2_565
O2 Gd2 O3 63.8(3) 3_455 32_445
O2 Gd2 O3 62.7(3) 32_445 32_445
O2 Gd2 O3 64.6(3) 31_455 32_445
O2 Gd2 O3 116.2(3) 33 32_445
O2 Gd2 O3 115.4(3) . 32_445
O2 Gd2 O3 117.3(3) 2_565 32_445
O2 Gd2 O3 115.4(3) 3_455 31_455
O2 Gd2 O3 116.2(3) 32_445 31_455
O2 Gd2 O3 62.7(3) 31_455 31_455
O2 Gd2 O3 64.6(3) 33 31_455
O2 Gd2 O3 117.3(3) . 31_455
O2 Gd2 O3 63.8(3) 2_565 31_455
O3 Gd2 O3 62.7(3) 32_445 31_455
O2 Gd2 O3 117.3(3) 3_455 33
O2 Gd2 O3 64.6(3) 32_445 33
O2 Gd2 O3 116.2(3) 31_455 33
O2 Gd2 O3 62.7(3) 33 33
O2 Gd2 O3 63.8(3) . 33
O2 Gd2 O3 115.4(3) 2_565 33
O3 Gd2 O3 62.7(3) 32_445 33
O3 Gd2 O3 62.7(3) 31_455 33
O2 Gd2 O3 64.6(3) 3_455 .
O2 Gd2 O3 63.8(3) 32_445 .
O2 Gd2 O3 117.3(3) 31_455 .
O2 Gd2 O3 115.4(3) 33 .
O2 Gd2 O3 62.7(3) . .
O2 Gd2 O3 116.2(3) 2_565 .
O3 Gd2 O3 117.3(3) 32_445 .
O3 Gd2 O3 179.998(1) 31_455 .
O3 Gd2 O3 117.3(3) 33 .
O2 Gd2 O3 62.7(3) 3_455 3_455
O2 Gd2 O3 115.4(3) 32_445 3_455
O2 Gd2 O3 63.8(3) 31_455 3_455
O2 Gd2 O3 117.3(3) 33 3_455
O2 Gd2 O3 116.2(3) . 3_455
O2 Gd2 O3 64.6(3) 2_565 3_455
O3 Gd2 O3 117.3(3) 32_445 3_455
O3 Gd2 O3 117.3(3) 31_455 3_455
O3 Gd2 O3 179.998(1) 33 3_455
O3 Gd2 O3 62.7(3) . 3_455
O2 Gd2 O3 116.2(3) 3_455 2_565
O2 Gd2 O3 117.3(3) 32_445 2_565
O2 Gd2 O3 115.4(3) 31_455 2_565
O2 Gd2 O3 63.8(3) 33 2_565
O2 Gd2 O3 64.6(3) . 2_565
O2 Gd2 O3 62.7(3) 2_565 2_565
O3 Gd2 O3 180.0(4) 32_445 2_565
O3 Gd2 O3 117.3(3) 31_455 2_565
O3 Gd2 O3 117.3(3) 33 2_565
O3 Gd2 O3 62.7(3) . 2_565
O3 Gd2 O3 62.7(3) 3_455 2_565
O4 Mo1 O5 105.5(4) 6 35_445
O4 Mo1 O2 100.3(4) 6 32_445
O5 Mo1 O2 100.4(4) 35_445 32_445
O4 Mo1 O7 100.9(4) 6 33
O5 Mo1 O7 101.2(4) 35_445 33
O2 Mo1 O7 144.3(4) 32_445 33
O4 Mo1 O2 89.3(4) 6 .
O5 Mo1 O2 165.1(4) 35_445 .
O2 Mo1 O2 78.2(4) 32_445 .
O7 Mo1 O2 73.7(3) 33 .
O4 Mo1 O3 159.8(4) 6 .
O5 Mo1 O3 94.5(4) 35_445 .
O2 Mo1 O3 78.9(3) 32_445 .
O7 Mo1 O3 71.3(3) 33 .
O2 Mo1 O3 70.7(3) . .
O4 Mo1 Mo2 118.3(3) 6 33
O5 Mo1 Mo2 121.2(3) 35_445 33
O2 Mo1 Mo2 107.7(3) 32_445 33
O7 Mo1 Mo2 36.5(3) 33 33
O2 Mo1 Mo2 47.2(2) . 33
O3 Mo1 Mo2 45.1(2) . 33
O4 Mo1 Gd2 120.1(3) 6 .
O5 Mo1 Gd2 124.0(3) 35_445 .
O2 Mo1 Gd2 44.1(2) 32_445 .
O7 Mo1 Gd2 100.2(3) 33 .
O2 Mo1 Gd2 45.7(2) . .
O3 Mo1 Gd2 46.6(2) . .
Mo2 Mo1 Gd2 63.67(3) 33 .
O8 Mo2 O1 104.0(4) . .
O8 Mo2 O3 103.5(4) . 33
O1 Mo2 O3 97.5(4) . 33
O8 Mo2 O7 100.1(4) . .
O1 Mo2 O7 102.5(4) . .
O3 Mo2 O7 144.2(4) 33 .
O8 Mo2 O3 96.1(4) . 32_445
O1 Mo2 O3 159.9(4) . 32_445
O3 Mo2 O3 78.7(5) 33 32_445
O7 Mo2 O3 72.4(3) . 32_445
O8 Mo2 O2 166.2(4) . 32_445
O1 Mo2 O2 89.1(3) . 32_445
O3 Mo2 O2 78.5(3) 33 32_445
O7 Mo2 O2 72.4(3) . 32_445
O3 Mo2 O2 70.8(3) 32_445 32_445
O8 Mo2 Mo1 121.7(3) . 32_445
O1 Mo2 Mo1 118.6(3) . 32_445
O3 Mo2 Mo1 107.9(2) 33 32_445
O7 Mo2 Mo1 36.3(3) . 32_445
O3 Mo2 Mo1 46.5(2) 32_445 32_445
O2 Mo2 Mo1 45.9(2) 32_445 32_445
O8 Mo2 Gd2 127.6(3) . .
O1 Mo2 Gd2 118.4(3) . .
O3 Mo2 Gd2 44.8(2) 33 .
O7 Mo2 Gd2 99.3(3) . .
O3 Mo2 Gd2 46.1(2) 32_445 .
O2 Mo2 Gd2 45.4(2) 32_445 .
Mo1 Mo2 Gd2 63.04(3) 32_445 .
Mo2 O1 Gd1 161.0(5) . .
Mo1 O2 Mo1 133.6(4) 33 .
Mo1 O2 Mo2 132.7(4) 33 33
Mo1 O2 Mo2 86.9(3) . 33
Mo1 O2 Gd2 104.3(3) 33 .
Mo1 O2 Gd2 94.1(3) . .
Mo2 O2 Gd2 93.6(3) 33 .
Mo2 O3 Mo2 133.1(4) 32_445 33
Mo2 O3 Mo1 132.7(4) 32_445 .
Mo2 O3 Mo1 88.5(3) 33 .
Mo2 O3 Gd2 102.8(3) 32_445 .
Mo2 O3 Gd2 94.8(3) 33 .
Mo1 O3 Gd2 92.8(3) . .
Mo1 O4 Gd1 155.9(5) 6 .
Mo1 O5 Gd1 152.8(5) 29_455 .
Gd1 O6 OW 122.3(4) . .
Mo1 O7 Mo2 107.2(4) 32_445 .
O6 OW O8 135.7(3) . 8_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Gd1 O1 2.360(9) .
Gd1 O1 2.360(9) 6
Gd1 O9 2.393(16) .
Gd1 O5 2.454(9) .
Gd1 O5 2.454(9) 6
Gd1 O4 2.484(9) 6
Gd1 O4 2.484(9) .
Gd1 O6 2.484(12) .
Gd1 O6 2.484(12) 6
Gd2 O2 2.495(8) 3_455
Gd2 O2 2.495(8) 32_445
Gd2 O2 2.495(8) 31_455
Gd2 O2 2.495(8) 33
Gd2 O2 2.495(8) .
Gd2 O2 2.495(8) 2_565
Gd2 O3 2.527(8) 32_445
Gd2 O3 2.527(8) 31_455
Gd2 O3 2.527(8) 33
Gd2 O3 2.527(8) .
Gd2 O3 2.527(8) 3_455
Gd2 O3 2.527(8) 2_565
Mo1 O4 1.706(9) 6
Mo1 O5 1.719(9) 35_445
Mo1 O2 1.882(8) 32_445
Mo1 O7 1.938(9) 33
Mo1 O2 2.250(8) .
Mo1 O3 2.267(8) .
Mo1 Mo2 3.1268(14) 33
Mo2 O8 1.701(9) .
Mo2 O1 1.724(9) .
Mo2 O3 1.918(9) 33
Mo2 O7 1.948(9) .
Mo2 O3 2.214(9) 32_445
Mo2 O2 2.298(8) 32_445
Mo2 Mo1 3.1269(14) 32_445
O2 Mo1 1.882(8) 33
O2 Mo2 2.298(8) 33
O3 Mo2 1.918(9) 32_445
O3 Mo2 2.214(9) 33
O4 Mo1 1.706(9) 6
O5 Mo1 1.719(9) 29_455
O6 OW 2.99(2) .
O7 Mo1 1.938(9) 32_445
OW O8 3.04(2) 8_565
