#------------------------------------------------------------------------------
#$Date: 2021-01-03 21:48:43 +0200 (Sun, 03 Jan 2021) $
#$Revision: 260395 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/83/4518397.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_4518397
loop_
_publ_author_name
'Du, Ze-Yu'
'Yu, Yan-Zhao'
'Hong, Ya-Lin'
'Li, Ning-Fang'
'Han, Ye-Min'
'Cao, Jia-Peng'
'Sun, Qi'
'Mei, Hua'
'Xu, Yan'
_publ_section_title
;
 Polyoxometalate-Based Metal-Organic Frameworks with Unique
 High-Nuclearity Water Clusters.
;
_journal_issue                   51
_journal_name_full               'ACS applied materials & interfaces'
_journal_page_first              57174
_journal_page_last               57181
_journal_paper_doi               10.1021/acsami.0c18970
_journal_volume                  12
_journal_year                    2020
_chemical_formula_sum            'C72 H112 Cu12 Mo11 O130 P V'
_chemical_formula_weight         4957.34
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.454(15)
_cell_length_b                   26.454(15)
_cell_length_c                   26.454(15)
_cell_measurement_reflns_used    2049
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.09
_cell_measurement_theta_min      2.55
_cell_volume                     18513(18)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXL
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10812
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         1.333
_exptl_absorpt_coefficient_mu    2.223
_exptl_absorpt_correction_T_max  0.776
_exptl_absorpt_correction_T_min  0.717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             9728
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.160
_refine_diff_density_min         -1.770
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         911
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1130P)²+334.7371P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                688
_reflns_number_total             911
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            am0c18970_si_002.cif
_cod_data_source_block           a01_sq
_cod_original_cell_volume        18512(31)
_cod_database_code               4518397
_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   0.717
_shelx_estimated_absorpt_t_max   0.776
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'y, -x+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'x, z+1/2, -y+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'x, -z+1/2, y+1/2'
'z, y+1/2, -x+1/2'
'z, -y+1/2, x+1/2'
'-z, y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'z+1/2, x, y+1/2'
'z+1/2, -x, -y+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, z, -x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'y+1/2, -x, z+1/2'
'-y+1/2, x, z+1/2'
'x+1/2, z, -y+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'x+1/2, -z, y+1/2'
'z+1/2, y, -x+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'z+1/2, x+1/2, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, z+1/2, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'y+1/2, -x+1/2, z'
'-y+1/2, x+1/2, z'
'x+1/2, z+1/2, -y'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'x+1/2, -z+1/2, y'
'z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-z, -x+1/2, -y+1/2'
'-z, x+1/2, y+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, -z+1/2, -x+1/2'
'y, -z+1/2, x+1/2'
'-y, z+1/2, x+1/2'
'y, z+1/2, -x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'-y, x+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'-x, -z+1/2, y+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-x, z+1/2, -y+1/2'
'-z, -y+1/2, x+1/2'
'-z, y+1/2, -x+1/2'
'z, -y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x, y+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, -z, x+1/2'
'-y+1/2, z, x+1/2'
'y+1/2, z, -x+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'-y+1/2, x, -z+1/2'
'y+1/2, -x, -z+1/2'
'-x+1/2, -z, y+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-x+1/2, z, -y+1/2'
'-z+1/2, -y, x+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, -y, -x+1/2'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/2, y'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, -z+1/2, -x'
'y+1/2, -z+1/2, x'
'-y+1/2, z+1/2, x'
'y+1/2, z+1/2, -x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'-y+1/2, x+1/2, -z'
'y+1/2, -x+1/2, -z'
'-x+1/2, -z+1/2, y'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-x+1/2, z+1/2, -y'
'-z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, -x'
'z+1/2, y+1/2, x'
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
Cu1 Cu 0.000000 0.28512(3) 0.21488(3) 0.0225(5) Uani 1 4 d S T P . .
Mo1 Mo 0.000000 0.40493(3) 0.40493(3) 0.0493(5) Uani 0.9167 4 d S T P . .
V1 V 0.000000 0.40493(3) 0.40493(3) 0.0493(5) Uani 0.0833 4 d S T P . .
P1 P 0.000000 0.500000 0.500000 0.024(2) Uani 1 48 d S T P . .
O1 O 0.05247(17) 0.24342(16) 0.18322(17) 0.0358(11) Uani 1 1 d D . . . .
O2 O 0.000000 0.3609(3) 0.3609(3) 0.069(3) Uani 1 4 d S T P . .
O3 O -0.0341(5) 0.4659(5) 0.4659(5) 0.036(5) Uani 0.5 6 d S T P . 1
O4 O -0.0502(3) 0.3792(4) 0.4498(3) 0.091(4) Uani 1 2 d S T P . 2
C1 C 0.1344(2) 0.1987(3) 0.1344(2) 0.0300(18) Uani 1 2 d S T P . .
H1A H 0.119789 0.227132 0.119787 0.036 Uiso 1 2 calc R U P . .
C2 C 0.1125(3) 0.1777(2) 0.1777(2) 0.0305(19) Uani 1 2 d S T P . .
C3 C 0.0697(3) 0.2031(2) 0.2031(2) 0.0292(19) Uani 1 2 d S T P . .
O1W O 0.000000 0.3438(3) 0.1562(3) 0.087(4) Uani 1 4 d S TU P . .
O2W O 0.000000 0.2451(9) 0.0751(8) 0.214(8) Uani 1 2 d DS TU P . .
H2WA H 0.019(6) 0.232(4) 0.098(3) 0.322 Uiso 1 1 d D U . . .
O3W O 0.000000 0.1787(14) 0.000000 0.221(9) Uani 1 8 d DS TU P . .
H3WA H 0.000000 0.2109(16) 0.000000 0.332 Uiso 1 8 d DS U P . .
H3WB H 0.000000 0.160(3) 0.027(3) 0.332 Uiso 0.25 2 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
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'
O O 0.0106 0.0060 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
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
O1 Cu1 O1 169.0(3) 100 138 ?
O1 Cu1 O1 88.8(3) 100 43 ?
O1 Cu1 O1 90.1(3) 138 43 ?
O1 Cu1 O1 90.1(3) 100 . ?
O1 Cu1 O1 88.8(3) 138 . ?
O1 Cu1 O1 169.0(3) 43 . ?
O1 Cu1 O1W 95.50(13) 100 . ?
O1 Cu1 O1W 95.50(13) 138 . ?
O1 Cu1 O1W 95.50(13) 43 . ?
O1 Cu1 O1W 95.50(13) . . ?
O1 Cu1 Cu1 84.50(13) 100 121 ?
O1 Cu1 Cu1 84.50(13) 138 121 ?
O1 Cu1 Cu1 84.50(13) 43 121 ?
O1 Cu1 Cu1 84.50(13) . 121 ?
O1W Cu1 Cu1 180.0(3) . 121 ?
O2 Mo1 O4 100.8(4) . . ?
O2 Mo1 O4 100.8(4) . 100 ?
O4 Mo1 O4 88.3(6) . 100 ?
O2 Mo1 O4 100.8(4) . 174 ?
O4 Mo1 O4 158.3(7) . 174 ?
O4 Mo1 O4 87.7(5) 100 174 ?
O2 Mo1 O4 100.8(4) . 77_455 ?
O4 Mo1 O4 87.7(5) . 77_455 ?
O4 Mo1 O4 158.3(7) 100 77_455 ?
O4 Mo1 O4 88.2(6) 174 77_455 ?
O2 Mo1 O3 158.5(4) . 100 ?
O2 Mo1 O3 158.5(4) . . ?
O3 Mo1 O3 43.1(9) 100 . ?
O3 P1 O3 180.0(15) . 97_566 ?
O3 P1 O3 70.528(1) . 100 ?
O3 P1 O3 109.472(8) 97_566 100 ?
O3 P1 O3 109.471(4) . 2_565 ?
O3 P1 O3 70.529(1) 97_566 2_565 ?
O3 P1 O3 70.529(2) 100 2_565 ?
O3 P1 O3 70.529(7) . 98_556 ?
O3 P1 O3 109.471(1) 97_566 98_556 ?
O3 P1 O3 109.471(2) 100 98_556 ?
O3 P1 O3 180.0(8) 2_565 98_556 ?
O3 P1 O3 109.5 . 3_556 ?
O3 P1 O3 70.529(1) 97_566 3_556 ?
O3 P1 O3 70.529(2) 100 3_556 ?
O3 P1 O3 109.472(8) 2_565 3_556 ?
O3 P1 O3 70.528(1) 98_556 3_556 ?
O3 P1 O3 70.529(4) . 99_565 ?
O3 P1 O3 109.471(4) 97_566 99_565 ?
O3 P1 O3 109.471(1) 100 99_565 ?
O3 P1 O3 70.528(1) 2_565 99_565 ?
O3 P1 O3 109.472(1) 98_556 99_565 ?
O3 P1 O3 180.0(8) 3_556 99_565 ?
O3 P1 O3 109.472(1) . 4_566 ?
O3 P1 O3 70.528(2) 97_566 4_566 ?
O3 P1 O3 180.0(8) 100 4_566 ?
O3 P1 O3 109.471(4) 2_565 4_566 ?
O3 P1 O3 70.529(3) 98_556 4_566 ?
O3 P1 O3 109.471(1) 3_556 4_566 ?
O3 P1 O3 70.529(3) 99_565 4_566 ?
C3 O1 Cu1 123.2(4) . . ?
P1 O3 O3 54.739(2) . 99_565 ?
P1 O3 O3 54.739(3) . 98_556 ?
O3 O3 O3 90.005(3) 99_565 98_556 ?
P1 O3 O3 54.739(2) . 100 ?
O3 O3 O3 90.004(5) 99_565 100 ?
O3 O3 O3 90.004(4) 98_556 100 ?
P1 O3 Mo1 123.2(4) . . ?
O3 O3 Mo1 131.13(15) 99_565 . ?
O3 O3 Mo1 131.13(15) 98_556 . ?
O3 O3 Mo1 68.5(4) 100 . ?
P1 O3 Mo1 123.2(4) . 77_455 ?
O3 O3 Mo1 68.5(4) 99_565 77_455 ?
O3 O3 Mo1 131.13(15) 98_556 77_455 ?
O3 O3 Mo1 131.13(15) 100 77_455 ?
Mo1 O3 Mo1 92.9(6) . 77_455 ?
P1 O3 Mo1 123.2(4) . 57_455 ?
O3 O3 Mo1 131.13(15) 99_565 57_455 ?
O3 O3 Mo1 68.5(4) 98_556 57_455 ?
O3 O3 Mo1 131.13(15) 100 57_455 ?
Mo1 O3 Mo1 92.9(6) . 57_455 ?
Mo1 O3 Mo1 92.9(6) 77_455 57_455 ?
Mo1 O4 Mo1 137.7(6) . 57_455 ?
C2 C1 C2 121.3(8) 9 . ?
C2 C1 H1A 119.3 9 . ?
C2 C1 H1A 119.3 . . ?
C1 C2 C1 118.7(8) 5 . ?
C1 C2 C3 120.6(4) 5 . ?
C1 C2 C3 120.6(4) . . ?
O1 C3 O1 124.3(8) 115 . ?
O1 C3 C2 117.8(4) 115 . ?
O1 C3 C2 117.8(4) . . ?
H2WA O2W H2WA 73(10) . 100 ?
H3WA O3W H3WB 124(8) . . ?
H3WA O3W H3WB 124(8) . 98 ?
H3WB O3W H3WB 111(10) . 98 ?
H3WA O3W H3WB 124(8) . 21 ?
H3WB O3W H3WB 71(8) . 21 ?
H3WB O3W H3WB 71(8) 98 21 ?
H3WA O3W H3WB 124(8) . 118 ?
H3WB O3W H3WB 71(8) . 118 ?
H3WB O3W H3WB 71(8) 98 118 ?
H3WB O3W H3WB 111(10) 21 118 ?
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
Cu1 O1 1.961(4) 100 ?
Cu1 O1 1.961(4) 138 ?
Cu1 O1 1.961(4) 43 ?
Cu1 O1 1.961(4) . ?
Cu1 O1W 2.195(12) . ?
Cu1 Cu1 2.628(3) 121 ?
Mo1 O2 1.648(10) . ?
Mo1 O4 1.907(4) . ?
Mo1 O4 1.907(4) 100 ?
Mo1 O4 1.907(4) 174 ?
Mo1 O4 1.907(4) 77_455 ?
Mo1 O3 2.454(12) 100 ?
Mo1 O3 2.454(12) . ?
P1 O3 1.56(2) . ?
P1 O3 1.56(2) 97_566 ?
P1 O3 1.56(2) 100 ?
P1 O3 1.56(2) 2_565 ?
P1 O3 1.56(2) 98_556 ?
P1 O3 1.56(2) 3_556 ?
P1 O3 1.56(2) 99_565 ?
P1 O3 1.56(2) 4_566 ?
O1 C3 1.274(6) . ?
O3 O3 1.80(3) 99_565 ?
O3 O3 1.80(3) 98_556 ?
O3 O3 1.80(3) 100 ?
C1 C2 1.398(6) 9 ?
C1 C2 1.398(6) . ?
C1 H1A 0.9300 . ?
C2 C3 1.479(12) . ?
O2W H2WA 0.86(2) . ?
O2W H2WA 0.86(2) 100 ?
O3W H3WA 0.85(2) . ?
O3W H3WB 0.85(2) . ?
O3W H3WB 0.85(2) 98 ?
O3W H3WB 0.85(2) 21 ?
O3W H3WB 0.85(2) 118 ?
