#------------------------------------------------------------------------------
#$Date: 2019-11-03 17:16:03 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221936 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/89/4128900.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_4128900
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 H90 Mo2 N7 O75 P W16'
_chemical_formula_weight         4721.37
_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_hydrogens   difmap
_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                   21.5987(10)
_cell_length_b                   21.5987(10)
_cell_length_c                   13.9195(15)
_cell_measurement_reflns_used    1655
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      3.12
_cell_volume                     5623.5(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    'SHELXT-2018 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_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  0.0807
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6807
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         1.824
_diffrn_source                   '1uS Microfocus x-ray'
_exptl_absorpt_coefficient_mu    24.903
_exptl_absorpt_correction_T_max  0.0942
_exptl_absorpt_correction_T_min  0.0376
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    4.182
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             6318
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         3.97
_refine_diff_density_min         -2.97
_refine_diff_density_rms         0.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1450
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0487
_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)+(0.0543P)²+212.8196P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1074
_reflns_number_total             1450
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b04533_si_002.cif
_cod_data_source_block           mak0235q
_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        5623.5(8)
_cod_database_code               4128900
_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   0.275
_shelx_estimated_absorpt_t_max   0.522
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
W1 W 0.60961(3) 0.39039(3) 0.00299(7) 0.0352(3) Uani 0.8889 2 d S T P
W2 W 0.50611(4) 0.33938(4) 0.20275(5) 0.0350(3) Uani 0.8889 1 d . . P
Mo1 Mo 0.60961(3) 0.39039(3) 0.00299(7) 0.0352(3) Uani 0.1111 2 d S T P
Mo2 Mo 0.50611(4) 0.33938(4) 0.20275(5) 0.0350(3) Uani 0.1111 1 d . . P
P1 P 0.666667 0.333333 0.2179(8) 0.010(3) Uani 0.5 6 d DS T P
O1 O 0.5899(5) 0.4101(5) -0.1065(12) 0.056(5) Uani 1 2 d S T P
O2 O 0.4211(6) 0.3253(6) 0.2124(8) 0.049(3) Uani 1 1 d . . .
O4 O 0.5186(6) 0.3553(6) 0.0655(7) 0.037(3) Uani 1 1 d . . .
O5 O 0.5575(4) 0.4425(4) 0.2156(10) 0.036(4) Uani 1 2 d S T P
O7 O 0.5861(9) 0.2931(5) -0.0085(10) 0.045(4) Uani 1 2 d S T P
O8 O 0.4903(8) 0.2452(4) 0.1850(10) 0.035(3) Uani 1 2 d S T P
O9 O 0.5277(7) 0.333333 0.333333 0.033(3) Uani 1 2 d S T P
O10 O 0.6245(4) 0.3755(4) 0.1750(11) 0.038(4) Uani 1 2 d S T P
O11 O 0.474(10) 0.474(10) 0.000000 0.14(9) Uiso 0.16 2 d S . P
O12 O 0.772(4) 0.666667 0.666667 0.08(2) Uiso 0.3 2 d S . P
N1 N 0.5385(11) 0.4615(11) 0.690(3) 0.080(11) Uiso 0.7 2 d DS U P
C1 C 0.584(3) 0.523(3) 0.755(4) 0.077(18) Uiso 0.35 1 d D U P
C2 C 0.5085(16) 0.4915(16) 0.619(4) 0.14(2) Uiso 0.7 2 d DS U P
H1 H 0.666667 0.333333 0.333333 0.010 Uiso 1 12 d DS U 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'
P P 0.1023 0.0942 '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
O1 W1 O7 103.8(6) . 21_665
O1 W1 O7 103.8(6) . .
O7 W1 O7 86.3(10) 21_665 .
O1 W1 O4 99.8(5) . .
O7 W1 O4 156.3(5) 21_665 .
O7 W1 O4 87.0(6) . .
O1 W1 O4 99.8(5) . 21_665
O7 W1 O4 87.0(6) 21_665 21_665
O7 W1 O4 156.3(5) . 21_665
O4 W1 O4 90.0(7) . 21_665
O1 W1 O10 167.3(7) . .
O7 W1 O10 85.3(5) 21_665 .
O7 W1 O10 85.3(5) . .
O4 W1 O10 71.5(4) . .
O4 W1 O10 71.5(4) 21_665 .
O2 W2 O9 101.0(6) . .
O2 W2 O8 102.6(6) . .
O9 W2 O8 88.3(4) . .
O2 W2 O4 98.7(5) . .
O9 W2 O4 160.2(6) . .
O8 W2 O4 89.8(5) . .
O2 W2 O5 98.3(5) . .
O9 W2 O5 88.4(4) . .
O8 W2 O5 159.1(6) . .
O4 W2 O5 86.4(5) . .
O2 W2 O10 170.1(5) . .
O9 W2 O10 85.1(6) . .
O8 W2 O10 85.2(5) . .
O4 W2 O10 75.0(5) . .
O5 W2 O10 74.0(5) . .
O10 P1 O10 108.2(6) . 2_655
O10 P1 O10 108.2(6) . 4_665
O10 P1 O10 108.2(6) 2_655 4_665
W1 O4 W2 122.7(5) . .
W2 O5 W2 119.0(8) 21_665 .
W1 O7 W1 151.6(10) 2_655 .
W2 O8 W2 156.7(8) 23 .
W2 O9 W2 147.5(9) 18 .
P1 O10 W2 124.4(5) . .
P1 O10 W2 124.4(5) . 21_665
W2 O10 W2 92.9(5) . 21_665
P1 O10 W1 123.8(8) . .
W2 O10 W1 90.7(5) . .
W2 O10 W1 90.7(5) 21_665 .
O12 O11 O11 179.99(4) 34_545 19_665
C1 N1 C1 101(6) . 21_665
C1 N1 C2 105(4) . .
C1 N1 C2 105(4) 21_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O1 1.693(15) .
W1 O7 1.907(4) 21_665
W1 O7 1.907(4) .
W1 O4 1.926(11) .
W1 O4 1.926(11) 21_665
W1 O10 2.457(15) .
W2 O2 1.711(12) .
W2 O9 1.897(5) .
W2 O8 1.904(3) .
W2 O4 1.935(10) .
W2 O5 1.937(8) .
W2 O10 2.302(10) .
P1 O10 1.688(16) .
P1 O10 1.688(16) 2_655
P1 O10 1.688(16) 4_665
O11 O12 0.8(2) 34_545
O11 O11 1.1(4) 19_665
N1 C1 1.49(2) .
N1 C1 1.49(2) 21_665
N1 C2 1.50(2) .
