#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:20:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179811 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/07/7010721.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_7010721
loop_
_publ_author_name
'Wu, Chuan-De'
'Lu, Can-Zhong'
'Liu, Jia-Cheng'
'Zhuang, Hong-Hui'
'Huang, Jin-Shun'
_publ_section_title
;
 A new heterometalate anion [GdMo6(CH3CHOCOO)6O15]3â€“
 with a nine-coordinate gadolinium encapsulated at the center
;
_journal_issue                   21
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3202
_journal_paper_doi               10.1039/b102926f
_journal_year                    2001
_chemical_formula_sum            'C18 H36 Gd Mo6 N3 O33'
_chemical_formula_weight         1555.39
_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                   16.344(4)
_cell_length_b                   16.344(4)
_cell_length_c                   26.728(7)
_cell_measurement_reflns_used    3860
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.48
_cell_measurement_theta_min      2.10
_cell_volume                     6183(3)
_computing_cell_refinement       'Siemens SMART & SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0660
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7392
_diffrn_reflns_theta_full        21.48
_diffrn_reflns_theta_max         21.48
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.461
_exptl_absorpt_correction_T_max  0.6357
_exptl_absorpt_correction_T_min  0.4893
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4470
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.00000(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.846
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.846
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          1.647
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                628
_reflns_number_total             798
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b102926f.txt
_cod_data_source_block           Mo6Gd
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               7010721
#BEGIN Tags that were not found in dictionaries:
_refine_ls_r_factor_ref          0.0486
#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
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd -0.6667 -0.3333 0.4167 0.0402(5) Uani 1 6 d S . .
Mo1 Mo -0.43276(6) -0.17759(6) 0.46938(3) 0.0526(5) Uani 1 1 d . . .
O1 O -0.3639(5) -0.2066(5) 0.4350(3) 0.074(2) Uani 1 1 d . . .
O2 O -0.3642(5) -0.0595(5) 0.4798(2) 0.0647(19) Uani 1 1 d . . .
O3 O -0.4197(4) -0.2208(5) 0.5341(2) 0.061(2) Uani 1 1 d . . .
O4 O -0.6090(5) -0.4527(5) 0.5203(2) 0.0555(17) Uani 1 1 d . . .
O5 O -0.5539(4) -0.3208(4) 0.4770(2) 0.0477(16) Uani 1 1 d . . .
O6 O -0.5177(5) -0.1844(5) 0.4167 0.050(2) Uani 1 2 d S . .
C1 C -0.4725(7) -0.3155(7) 0.5520(3) 0.057(3) Uani 1 1 d . . .
H1A H -0.4312 -0.3429 0.5518 0.069 Uiso 1 1 calc R . .
C2 C -0.5054(9) -0.3192(9) 0.6024(4) 0.076(3) Uani 1 1 d . . .
H2A H -0.4524 -0.2830 0.6240 0.114 Uiso 1 1 calc R . .
H2B H -0.5389 -0.3837 0.6135 0.114 Uiso 1 1 calc R . .
H2C H -0.5469 -0.2935 0.6032 0.114 Uiso 1 1 calc R . .
C3 C -0.5525(7) -0.3704(7) 0.5149(3) 0.048(2) Uani 1 1 d . . .
N1 N -0.2984(8) -0.3333 0.4167 0.083(4) 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
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'
N N 0.0061 0.0033 '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
_geom_angle_publ_flag
O5 Gd1 O5 79.1(2) 2_455 3_445 ?
O5 Gd1 O5 79.1(2) 2_455 . ?
O5 Gd1 O5 79.1(2) 3_445 . ?
O5 Gd1 O5 86.0(3) 2_455 10_455 ?
O5 Gd1 O5 145.0(3) 3_445 10_455 ?
O5 Gd1 O5 129.0(3) . 10_455 ?
O5 Gd1 O5 129.0(3) 2_455 12_345 ?
O5 Gd1 O5 86.0(3) 3_445 12_345 ?
O5 Gd1 O5 145.0(3) . 12_345 ?
O5 Gd1 O5 79.1(2) 10_455 12_345 ?
O5 Gd1 O5 145.0(3) 2_455 11_445 ?
O5 Gd1 O5 129.0(3) 3_445 11_445 ?
O5 Gd1 O5 86.0(3) . 11_445 ?
O5 Gd1 O5 79.1(2) 10_455 11_445 ?
O5 Gd1 O5 79.1(2) 12_345 11_445 ?
O5 Gd1 O6 64.50(14) 2_455 2_455 ?
O5 Gd1 O6 72.49(14) 3_445 2_455 ?
O5 Gd1 O6 137.00(15) . 2_455 ?
O5 Gd1 O6 72.49(14) 10_455 2_455 ?
O5 Gd1 O6 64.50(14) 12_345 2_455 ?
O5 Gd1 O6 137.00(15) 11_445 2_455 ?
O5 Gd1 O6 72.49(14) 2_455 . ?
O5 Gd1 O6 137.00(15) 3_445 . ?
O5 Gd1 O6 64.50(14) . . ?
O5 Gd1 O6 64.50(14) 10_455 . ?
O5 Gd1 O6 137.01(15) 12_345 . ?
O5 Gd1 O6 72.49(14) 11_445 . ?
O6 Gd1 O6 120.000(1) 2_455 . ?
O5 Gd1 O6 137.00(15) 2_455 3_445 ?
O5 Gd1 O6 64.50(14) 3_445 3_445 ?
O5 Gd1 O6 72.49(14) . 3_445 ?
O5 Gd1 O6 137.01(15) 10_455 3_445 ?
O5 Gd1 O6 72.49(14) 12_345 3_445 ?
O5 Gd1 O6 64.50(14) 11_445 3_445 ?
O6 Gd1 O6 120.000(2) 2_455 3_445 ?
O6 Gd1 O6 120.0 . 3_445 ?
O1 Mo1 O2 104.7(4) . . ?
O1 Mo1 O3 100.0(3) . . ?
O2 Mo1 O3 98.0(3) . . ?
O1 Mo1 O6 98.5(3) . . ?
O2 Mo1 O6 103.3(3) . . ?
O3 Mo1 O6 147.2(3) . . ?
O1 Mo1 O5 97.1(3) . . ?
O2 Mo1 O5 157.9(3) . . ?
O3 Mo1 O5 74.4(2) . . ?
O6 Mo1 O5 76.6(3) . . ?
O1 Mo1 O4 173.0(3) . 2_455 ?
O2 Mo1 O4 82.3(3) . 2_455 ?
O3 Mo1 O4 77.7(3) . 2_455 ?
O6 Mo1 O4 80.64(17) . 2_455 ?
O5 Mo1 O4 75.9(2) . 2_455 ?
Mo1 O1 N1 148.5(4) . . ?
C1 O3 Mo1 125.7(5) . . ?
C3 O4 Mo1 132.6(6) . 3_445 ?
C3 O5 Mo1 116.7(6) . . ?
C3 O5 Gd1 136.5(6) . . ?
Mo1 O5 Gd1 106.1(2) . . ?
Mo1 O6 Mo1 134.6(5) . 10_455 ?
Mo1 O6 Gd1 112.7(2) . . ?
Mo1 O6 Gd1 112.7(2) 10_455 . ?
O3 C1 C2 111.8(9) . . ?
O3 C1 C3 107.2(8) . . ?
C2 C1 C3 113.0(9) . . ?
O4 C3 O5 123.2(8) . . ?
O4 C3 C1 122.3(8) . . ?
O5 C3 C1 114.5(9) . . ?
O2 N1 O2 173.9(6) 21_556 28_445 ?
O2 N1 O1 88.1(3) 21_556 . ?
O2 N1 O1 96.5(3) 28_445 . ?
O2 N1 O1 96.5(3) 21_556 11_445 ?
O2 N1 O1 88.1(3) 28_445 11_445 ?
O1 N1 O1 82.9(5) . 11_445 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O5 2.379(6) 2_455 ?
Gd1 O5 2.379(6) 3_445 ?
Gd1 O5 2.379(6) . ?
Gd1 O5 2.379(6) 10_455 ?
Gd1 O5 2.379(6) 12_345 ?
Gd1 O5 2.379(6) 11_445 ?
Gd1 O6 2.434(9) 2_455 ?
Gd1 O6 2.434(9) . ?
Gd1 O6 2.434(9) 3_445 ?
Mo1 O1 1.693(7) . ?
Mo1 O2 1.701(7) . ?
Mo1 O3 1.919(6) . ?
Mo1 O6 1.942(3) . ?
Mo1 O5 2.192(6) . ?
Mo1 O4 2.476(7) 2_455 ?
O1 N1 2.810(12) . ?
O3 C1 1.426(12) . ?
O4 C3 1.200(11) . ?
O4 Mo1 2.476(7) 3_445 ?
O5 C3 1.305(11) . ?
O6 Mo1 1.942(3) 10_455 ?
C1 C2 1.440(13) . ?
C1 C3 1.525(13) . ?
N1 O2 2.805(6) 21_556 ?
N1 O2 2.805(6) 28_445 ?
N1 O1 2.810(12) 11_445 ?
