#------------------------------------------------------------------------------
#$Date: 2019-11-03 17:14:34 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221932 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/88/4128897.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_4128897
loop_
_publ_author_name
'Zheng, Qi'
'Kupper, Manuel'
'Xuan, Weimin'
'Oki, Hirofumi'
'Tsunashima, Ryo'
'Long, De-Liang'
'Cronin, Leroy'
_publ_section_title
;
 Anisotropic Polyoxometalate Cages Assembled via Layers of Heteroanion
 Templates.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13479
_journal_page_last               13486
_journal_paper_doi               10.1021/jacs.9b04533
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C14 H79 Mo2 N7 O70 Te W16'
_chemical_formula_weight         4726.92
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.1678(9)
_cell_length_b                   21.1678(9)
_cell_length_c                   15.6954(14)
_cell_measurement_reflns_used    8972
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      2.60
_cell_volume                     6090.5(7)
_computing_cell_refinement       Apex3
_computing_data_collection       Apex3
_computing_data_reduction        Apex3
_computing_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex II Quasar'
_diffrn_measurement_method       'ω & φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28942
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.723
_diffrn_reflns_theta_min         2.573
_diffrn_source                   '1uS Microfocus x-ray'
_exptl_absorpt_coefficient_mu    23.317
_exptl_absorpt_correction_T_max  0.547
_exptl_absorpt_correction_T_min  0.216
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.866
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             6276
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.81
_refine_diff_density_min         -2.39
_refine_diff_density_rms         0.25
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.237
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1408
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.237
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0458P)²+299.5382P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1234
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1142
_reflns_number_total             1408
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b04533_si_004.cif
_cod_data_source_block           qz61e
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'direct methods' was
changed to 'direct'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        6090.5(8)
_cod_database_code               4128897
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.204
_shelx_estimated_absorpt_t_max   0.389
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'-x, -x+y, -z'
'x-y, -y, -z'
'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+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'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+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'x, x-y, z'
'-x+y, y, z'
'-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+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'-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+2/3'
'x+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
W1 W 0.11642(5) 0.05821(2) 0.20852(8) 0.0620(4) Uani 0.8889 2 d S T P
W2 W 0.17007(3) 0.00657(3) 0.38428(5) 0.0547(3) Uani 0.8889 1 d . . P
Mo1 Mo 0.11642(5) 0.05821(2) 0.20852(8) 0.0620(4) Uani 0.1111 2 d S T P
Mo2 Mo 0.17007(3) 0.00657(3) 0.38428(5) 0.0547(3) Uani 0.1111 1 d . . P
Te1 Te 0.000000 0.000000 0.4187(3) 0.0421(10) Uani 0.5 6 d S T P
O1 O 0.0894(3) -0.0894(3) 0.3665(10) 0.057(4) Uani 1 2 d S T P
O2 O 0.2407(5) -0.0095(5) 0.3939(8) 0.068(3) Uani 1 1 d . . .
O3 O 0.1752(5) 0.0239(5) 0.2622(8) 0.064(3) Uani 1 1 d . . .
O4 O 0.0886(6) 0.0443(3) 0.3579(9) 0.046(3) Uani 1 2 d S T P
O5 O 0.2221(7) 0.1111(3) 0.3985(10) 0.055(4) Uani 1 2 d S T P
O6 O 0.1403(6) 0.000000 0.500000 0.059(4) Uani 1 2 d S T P
O7 O 0.0413(4) 0.0826(8) 0.1980(11) 0.063(4) Uani 1 2 d S T P
O8 O 0.1547(8) 0.0773(4) 0.1112(11) 0.075(5) Uani 1 2 d S T P
O9 O 0.329(4) 0.128(4) 0.213(4) 0.092(19) Uiso 0.2 1 d . . P
N1 N 0.2124(9) 0.7876(9) 0.502(2) 0.085(10) Uiso 0.6 2 d DS . P
C1 C 0.1785(8) 0.8215(8) 0.452(2) 0.055(8) Uiso 0.6 2 d DS . P
C2 C 0.173(4) 0.757(4) 0.584(3) 0.11(3) Uiso 0.3 1 d D . P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
W W -0.8490 6.8722 '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'
Te Te -0.5308 1.6751 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
O8 W1 O7 102.9(6) . .
O8 W1 O7 102.9(6) . 3
O7 W1 O7 86.8(8) . 3
O8 W1 O3 99.5(5) . .
O7 W1 O3 157.6(6) . .
O7 W1 O3 87.7(5) 3 .
O8 W1 O3 99.5(5) . 23
O7 W1 O3 87.7(5) . 23
O7 W1 O3 157.6(6) 3 23
O3 W1 O3 89.2(6) . 23
O8 W1 O4 167.6(6) . .
O7 W1 O4 86.0(5) . .
O7 W1 O4 86.0(5) 3 .
O3 W1 O4 71.9(4) . .
O3 W1 O4 71.9(4) 23 .
O2 W2 O6 101.1(6) . .
O2 W2 O1 102.1(5) . .
O6 W2 O1 88.5(5) . .
O2 W2 O5 99.4(5) . .
O6 W2 O5 87.2(4) . .
O1 W2 O5 158.5(5) . .
O2 W2 O3 98.9(5) . .
O6 W2 O3 159.9(5) . .
O1 W2 O3 89.6(6) . .
O5 W2 O3 87.2(5) . .
O2 W2 O4 170.4(5) . .
O6 W2 O4 85.3(5) . .
O1 W2 O4 85.1(4) . .
O5 W2 O4 73.5(4) . .
O3 W2 O4 74.6(4) . .
O4 Te1 O4 96.6(6) . 3
O4 Te1 O4 96.6(6) . 2
O4 Te1 O4 96.6(6) 3 2
O4 Te1 Te1 120.4(4) . 19_556
O4 Te1 Te1 120.4(4) 3 19_556
O4 Te1 Te1 120.4(4) 2 19_556
W2 O1 W2 156.2(8) . 22
W1 O3 W2 121.3(5) . .
Te1 O4 W2 118.3(5) . 23
Te1 O4 W2 118.3(5) . .
W2 O4 W2 94.0(4) 23 .
Te1 O4 W1 132.7(6) . .
W2 O4 W1 92.2(4) 23 .
W2 O4 W1 92.2(4) . .
W2 O5 W2 118.9(6) 23 .
W2 O6 W2 145.8(8) . 6_556
W1 O7 W1 151.1(8) . 2
O9 O9 O9 89.997(14) 11 23
C1 N1 C2 112(4) . .
C1 N1 C2 112(4) . 22_665
C2 N1 C2 59(6) . 22_665
C2 C2 N1 60(3) 22_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O8 1.681(17) .
W1 O7 1.909(4) .
W1 O7 1.909(4) 3
W1 O3 1.920(11) .
W1 O3 1.920(11) 23
W1 O4 2.399(14) .
W2 O2 1.699(9) .
W2 O6 1.904(4) .
W2 O1 1.911(3) .
W2 O5 1.929(6) .
W2 O3 1.944(12) .
W2 O4 2.272(8) .
Te1 O4 1.884(12) .
Te1 O4 1.884(12) 3
Te1 O4 1.884(12) 2
Te1 Te1 2.553(10) 19_556
O9 O9 1.45(12) 11
O9 O9 1.57(14) 23
N1 C1 1.471(19) .
N1 C2 1.49(2) .
N1 C2 1.49(2) 22_665
C2 C2 1.47(14) 22_665
