#------------------------------------------------------------------------------
#$Date: 2019-11-03 17:15:03 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221933 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/88/4128898.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_4128898
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 Se W16'
_chemical_formula_weight         4678.28
_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                120.000(15)
_cell_formula_units_Z            3
_cell_length_a                   21.1690(9)
_cell_length_b                   21.1690(13)
_cell_length_c                   15.8379(12)
_cell_measurement_reflns_used    1974
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.2
_cell_measurement_theta_min      2.80
_cell_volume                     6146.5(11)
_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 0.997
_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  0.0493
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7799
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.994
_diffrn_reflns_theta_min         2.802
_diffrn_source                   '1uS Microfocus x-ray'
_exptl_absorpt_coefficient_mu    23.200
_exptl_absorpt_correction_T_max  0.093
_exptl_absorpt_correction_T_min  0.057
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.792
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             6222
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.07
_refine_diff_density_min         -2.22
_refine_diff_density_rms         0.23
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1459
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0229P)²+267.9754P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.1010
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1121
_reflns_number_total             1459
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b04533_si_003.cif
_cod_data_source_block           qz62f_1
_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        6146.5(7)
_cod_database_code               4128898
_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   0.205
_shelx_estimated_absorpt_t_max   0.390
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'y, x, -z'
'-x+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'
'y+2/3, x+1/3, -z+1/3'
'-x+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'
'y+1/3, x+2/3, -z+2/3'
'-x+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'
'-y, -x, z'
'x-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'
'-y+2/3, -x+1/3, z+1/3'
'x-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'
'-y+1/3, -x+2/3, z+2/3'
'x-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
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.82965(3) 0.99385(3) 0.11546(4) 0.0493(2) Uani 0.8889 1 d . . P . .
W2 W 0.88356(4) 0.94178(2) 0.29055(7) 0.0598(3) Uani 0.8889 2 d S T P . .
Mo1 Mo 0.82965(3) 0.99385(3) 0.11546(4) 0.0493(2) Uani 0.1111 1 d . . P . .
Mo2 Mo 0.88356(4) 0.94178(2) 0.29055(7) 0.0598(3) Uani 0.1111 2 d S T P . .
Se1 Se 1.000000 1.000000 0.0949(4) 0.0358(13) Uani 0.5 6 d S T P . .
O1 O 0.9139(6) 0.9569(3) 0.1418(8) 0.042(3) Uani 1 2 d S T P . .
O2 O 0.9101(3) 1.0899(3) 0.1323(9) 0.054(3) Uani 1 2 d S T P . .
O3 O 0.8569(6) 1.000000 0.000000 0.055(3) Uani 1 2 d S T P . .
O4 O 0.7583(5) 1.0096(5) 0.1085(6) 0.061(3) Uani 1 1 d . . . . .
O5 O 0.7783(6) 0.8892(3) 0.1037(9) 0.054(3) Uani 1 2 d S T P . .
O6 O 0.8258(5) 0.9767(5) 0.2352(7) 0.059(3) Uani 1 1 d . . . . .
O9 O 0.9589(3) 1.0411(3) 0.3005(10) 0.064(4) Uani 1 2 d S T P . .
O10 O 0.8452(8) 0.9226(4) 0.3875(9) 0.068(4) Uani 1 2 d S T P . .
O11 O 0.665(5) 0.832(3) 0.255(6) 0.09(3) Uiso 0.2 2 d S . P A 1
O12 O 0.602(4) 0.935(4) 0.079(5) 0.043(18) Uiso 0.1 1 d . . P B 1
O13 O 1.000000 1.000000 1.046(8) 0.13(6) Uiso 0.3 6 d S . P C 1
O11' O 0.673(4) 0.793(4) 0.279(4) 0.034(16) Uiso 0.1 1 d . . P D 2
O12' O 0.604(4) 0.884(4) 0.027(4) 0.038(18) Uiso 0.1 1 d . . P E 2
N1 N 0.7888(7) 0.5776(13) -0.0018(16) 0.092(8) Uiso 0.8 2 d DS U P F 1
C1 C 0.8090(14) 0.6438(12) 0.0486(13) 0.036(6) Uiso 0.4 1 d D U P F 1
C2 C 0.751(4) 0.566(4) -0.086(3) 0.16(2) Uiso 0.4 1 d D U P F 1
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'
Se Se -0.0929 2.2259 '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
O4 W1 O3 101.1(5) . .
O4 W1 O2 101.9(4) . .
O3 W1 O2 89.0(4) . .
O4 W1 O6 98.1(4) . .
O3 W1 O6 160.5(4) . .
O2 W1 O6 89.7(5) . .
O4 W1 O5 100.0(4) . .
O3 W1 O5 87.9(4) . .
O2 W1 O5 158.1(4) . .
O6 W1 O5 86.1(5) . .
O4 W1 O1 170.0(4) . .
O3 W1 O1 86.4(5) . .
O2 W1 O1 84.6(4) . .
O6 W1 O1 74.1(4) . .
O5 W1 O1 73.5(4) . .
O10 W2 O9 103.1(6) . .
O10 W2 O9 103.1(6) . 2_765
O9 W2 O9 86.4(8) . 2_765
O10 W2 O6 100.7(4) . .
O9 W2 O6 87.5(5) . .
O9 W2 O6 156.3(5) 2_765 .
O10 W2 O6 100.7(4) . 23_565
O9 W2 O6 156.2(5) . 23_565
O9 W2 O6 87.5(5) 2_765 23_565
O6 W2 O6 89.0(5) . 23_565
O10 W2 O1 168.7(5) . .
O9 W2 O1 85.1(5) . .
O9 W2 O1 85.1(5) 2_765 .
O6 W2 O1 71.6(3) . .
O6 W2 O1 71.5(3) 23_565 .
O13 Se1 O1 115.2(5) 1_554 21_775
O13 Se1 O1 115.2(4) 1_554 2_765
O1 Se1 O1 103.2(5) 21_775 2_765
O13 Se1 O1 115.2(4) 1_554 .
O1 Se1 O1 103.2(5) 21_775 .
O1 Se1 O1 103.2(5) 2_765 .
O13 Se1 O13 0.000(18) 1_554 19_776
O1 Se1 O13 115.2(4) 21_775 19_776
O1 Se1 O13 115.2(4) 2_765 19_776
O1 Se1 O13 115.2(4) . 19_776
Se1 O1 W1 121.8(4) . .
Se1 O1 W1 121.8(4) . 23_565
W1 O1 W1 92.6(4) . 23_565
Se1 O1 W2 128.5(6) . .
W1 O1 W2 91.3(3) . .
W1 O1 W2 91.3(3) 23_565 .
W1 O2 W1 156.4(7) . 21_775
W1 O3 W1 148.7(7) 6_675 .
W1 O5 W1 120.3(6) . 23_565
W1 O6 W2 123.0(4) . .
W2 O9 W2 151.6(7) 21_775 .
Se1 O13 O13 180.00(17) 1_556 19_777
Se1 O13 Se1 180.0 1_556 19_776
O13 O13 Se1 0.00(6) 19_777 19_776
C1 N1 C1 21(2) . 24_655
C1 N1 C2 120(3) . .
C1 N1 C2 132(4) 24_655 .
C1 N1 C2 132(4) . 24_655
C1 N1 C2 120(3) 24_655 24_655
C2 N1 C2 53(5) . 24_655
C1 C1 N1 79.4(11) 24_655 .
C2 C2 N1 63(3) 24_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O4 1.705(8) .
W1 O3 1.902(3) .
W1 O2 1.909(3) .
W1 O6 1.924(10) .
W1 O5 1.929(6) .
W1 O1 2.315(7) .
W2 O10 1.688(14) .
W2 O9 1.907(3) .
W2 O9 1.907(3) 2_765
W2 O6 1.928(10) .
W2 O6 1.928(10) 23_565
W2 O1 2.420(12) .
Se1 O13 0.77(12) 1_554
Se1 O1 1.745(11) 21_775
Se1 O1 1.745(11) 2_765
Se1 O1 1.745(11) .
Se1 O13 2.24(13) 19_776
O13 O13 1.5(2) 19_777
O11' O11' 1.75(13) 17_655
N1 C1 1.477(18) .
N1 C1 1.477(18) 24_655
N1 C2 1.52(2) .
N1 C2 1.52(2) 24_655
C1 C1 0.54(5) 24_655
C2 C2 1.36(13) 24_655
